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Materials, Volume 13, Issue 13 (July-1 2020) – 159 articles

Cover Story (view full-size image): The following article introduces technologies that build 3D objects by adding layer-upon-layer of material, called also additive manufacturing technologies. Furthermore, the most important features supporting the conscious choice of 3D printing methods for applications in micro- and nanomanufacturing were covered. The micromanufacturing method covers photopolymerization-based methods, such as those based on stereolithography (SLA), digital light processing (DLP), liquid crystal display–DLP coupled method, two-photon polymerisation (TPP), and inkjet. Functional photocurable materials with magnetic, conductive, or specific optical applications in the 3D printing processes were also reviewed. View this paper
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27 pages, 6193 KiB  
Review
Green and Durable Lightweight Aggregate Concrete: The Role of Waste and Recycled Materials
by Jiyu Wang, Kai Zheng, Na Cui, Xin Cheng, Kai Ren, Pengkun Hou, Lichao Feng, Zonghui Zhou and Ning Xie
Materials 2020, 13(13), 3041; https://doi.org/10.3390/ma13133041 - 7 Jul 2020
Cited by 23 | Viewed by 5461
Abstract
Lightweight aggregate concrete manufactured by solid waste or recycled by-products is a burgeoning topic in construction and building materials. It has significant merits in mitigating the negative impact on the environment during the manufacturing of Portland cement and reduces the consumption of natural [...] Read more.
Lightweight aggregate concrete manufactured by solid waste or recycled by-products is a burgeoning topic in construction and building materials. It has significant merits in mitigating the negative impact on the environment during the manufacturing of Portland cement and reduces the consumption of natural resources. In this review article, the agricultural and industrial wastes and by-products, which were used as cementitious materials and artificial lightweight aggregate concrete, are summarized. Besides, the mechanical properties, durability, and a few advanced microstructure characterization methods were reviewed as well. This review also provides a look to the future research trends that may help address the challenges or further enhance the environmental benefits of lightweight aggregate concrete manufactured with solid waste and recycled by-products. Full article
(This article belongs to the Special Issue Recycled Concrete with Waste and By-Products)
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<p>SEM images at 91 days for two different OPC-CSA mortar mixtures: (<b>a</b>) interfacial transition zones (ITZ) surrounding sand for OPC-CSA mixture made without light-weight sand (LWS) and (<b>b</b>) ITZ surrounding LWS for OPC-CSA mixture containing 20% LWS replacement [<a href="#B19-materials-13-03041" class="html-bibr">19</a>], with copyright permission from Elsevier.</p>
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<p>World palm oil production 1996–2000 [<a href="#B43-materials-13-03041" class="html-bibr">43</a>], with copyright permission from Elsevier.</p>
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<p>Oil palm shell (OPS) grains (darker) in lightweight concrete [<a href="#B49-materials-13-03041" class="html-bibr">49</a>], with copyright permission from Elsevier.</p>
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<p>Development of the compressive strength of concrete [<a href="#B50-materials-13-03041" class="html-bibr">50</a>], with copyright permission from Elsevier.</p>
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<p>Scanning electron microscopy image for the surface texture of oil-palm-boiler clinker (OPBC) and normal sand [<a href="#B50-materials-13-03041" class="html-bibr">50</a>], with copyright permission from Elsevier.</p>
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<p>Cross-section of concrete made of coconut shells as coarse aggregate [<a href="#B53-materials-13-03041" class="html-bibr">53</a>], with copyright permission from Elsevier.</p>
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<p>Crack width between cement paste and coconut shell aggregate (<b>a</b>) 3-day, (<b>b</b>) 7-day, and (<b>c</b>) 28-day [<a href="#B53-materials-13-03041" class="html-bibr">53</a>], with copyright permission from Elsevier.</p>
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<p>SEM images (100%) showing the morphologies of M<sub>0</sub>, M<sub>10</sub>, M<sub>20</sub>, and M<sub>30</sub> [<a href="#B62-materials-13-03041" class="html-bibr">62</a>], with copyright permission from Elsevier.</p>
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<p>Relationship between the strength of the mortar and of light weight aggregate concrete (LWAC) made with the same mortar [<a href="#B70-materials-13-03041" class="html-bibr">70</a>], with copyright permission from Elsevier.</p>
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<p>Typical failure modes of cubic specimens [<a href="#B77-materials-13-03041" class="html-bibr">77</a>], with copyright permission from Elsevier.</p>
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<p>Compression failure mechanisms: (<b>a</b>) plain LWAC specimens, (<b>b</b>) steel fiber LWAC specimens, (<b>c</b>) carbon fiber LWAC specimens [<a href="#B82-materials-13-03041" class="html-bibr">82</a>], with copyright permission from Elsevier.</p>
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<p>Natural crack crossing through the aggregate in NWC (<b>left</b>) and LWAC (<b>right</b>) [<a href="#B110-materials-13-03041" class="html-bibr">110</a>], with copyright permission from Elsevier.</p>
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<p>The cross-section of the concrete cube with (<b>a</b>) 30% and (<b>b</b>) 60% vol. aggregate replacement [<a href="#B114-materials-13-03041" class="html-bibr">114</a>], with copyright permission from Elsevier.</p>
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<p>Effect of aggregate saturation degree on mass loss [<a href="#B118-materials-13-03041" class="html-bibr">118</a>], with copyright from Elsevier.</p>
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<p>The SEM images of ITZ between the LWA and matrix: (<b>a</b>) Lytag LWA pre-wet for 0.25 h; (<b>b</b>) Lytag LWA pre-wet for 0.5 h; (<b>c</b>) Shale LWA pre-wet for 0.5 h; (<b>d</b>) Shale LWA pre-wet for 24 h [<a href="#B118-materials-13-03041" class="html-bibr">118</a>], with copyright permission from Elsevier.</p>
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<p>The SEM images of ITZ between the LWA and matrix: (<b>a</b>) Lytag LWA pre-wet for 0.25 h; (<b>b</b>) Lytag LWA pre-wet for 0.5 h; (<b>c</b>) Shale LWA pre-wet for 0.5 h; (<b>d</b>) Shale LWA pre-wet for 24 h [<a href="#B118-materials-13-03041" class="html-bibr">118</a>], with copyright permission from Elsevier.</p>
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12 pages, 5064 KiB  
Article
Quantification of the Morphological Signature of Roping Based on Multiscale Analysis and Autocorrelation Function Description
by Julie Marteau, Raphaël Deltombe and Maxence Bigerelle
Materials 2020, 13(13), 3040; https://doi.org/10.3390/ma13133040 - 7 Jul 2020
Cited by 4 | Viewed by 2383
Abstract
Roping or ridging is a visual defect affecting the surface of ferritic stainless steels, assessed using visual inspection of the surfaces. The aim of this study was to quantify the morphological signature of roping to link roughness results with five levels of roping [...] Read more.
Roping or ridging is a visual defect affecting the surface of ferritic stainless steels, assessed using visual inspection of the surfaces. The aim of this study was to quantify the morphological signature of roping to link roughness results with five levels of roping identified with visual inspection. First, the multiscale analysis of roughness showed that the texture aspect ratio Str computed with a low-pass filter of 32 µm gave a clear separation between the acceptable levels of roping and the non-acceptable levels (rejected sheets). To obtain a gradation description of roping instead of a binary description, a methodology based on the use of the autocorrelation function was created. It consisted of several steps: a low-pass filtering of the autocorrelation function at 150 µm, the segmentation of the autocorrelation into four stabilized portions, and finally, the computation of isotropy and the root-mean-square roughness Sq on the obtained quarters of function. The use of the isotropy combined with the root-mean-square roughness Sq led to a clear separation of the five levels of roping: the acceptable levels of roping corresponded to strong isotropy (values larger than 10%) coupled with low root-mean-square roughness Sq. Both methodologies can be used to quantitatively describe surface morphology of roping in order to improve our understanding of the roping phenomenon. Full article
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<p>Examples of topography measurements of 1188 µm × 891 µm for roping classified as Level 1 and Level 5, before and after tensile testing.</p>
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<p>(<b>a</b>) Full scale arithmetical mean height S<sub>a</sub> values as a function of the visual roping levels, after tensile testing, (<b>b</b>) Arithmetical mean height S<sub>a</sub> values obtained with a low-pass filter and a cut-off of 200 µm as a function of the visual roping levels, after tensile testing.</p>
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<p>Bearing index S<sub>bi</sub> values obtained with a band-pass filter with a cut-off of 20 µm and a bandwidth of 5 µm as a function of the visual roping levels, after tensile testing.</p>
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<p>Texture aspect ratio S<sub>tr</sub> values obtained with a low-pass filter of 32 µm as a function of the visual roping levels after tensile testing.</p>
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<p>Texture aspect ratio S<sub>tr</sub> results as a function of the threshold value.</p>
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<p>Representation of the regularity parameter S<sub>reg</sub> results for all the measured sheets in polar coordinates.</p>
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<p>Autocorrelation length S<sub>al</sub> as a function of the threshold.</p>
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<p>Methodology of extraction of quarters of autocorrelation functions.</p>
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<p>Topography of the autocorrelation function quarters for the five levels of roping (the X and Y axis units are micrometers).</p>
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<p>Isotropy as a function of the root-mean-square roughness S<sub>q</sub> computed for all the quarters of autocorrelation function.</p>
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14 pages, 4322 KiB  
Article
Mg-Zn-Ca Alloys for Hemostasis Clips for Vessel Ligation: In Vitro and In Vivo Studies of Their Degradation and Response
by Yen-Hao Chang, Chun Chieh Tseng, Chih-Yeh Chao, Chung-Hwan Chen, Sung-Yen Lin and Je-Kang Du
Materials 2020, 13(13), 3039; https://doi.org/10.3390/ma13133039 - 7 Jul 2020
Cited by 11 | Viewed by 3077
Abstract
To control the degradation rate of magnesium (Mg) alloys, chitosan (CHI) and L-glutamic acid (LGA) were used as coatings on Mg-Zn-Ca alloys via dip coating. In this study, either two or seven CHI/LGA layers were applied as a coating on Mg-2.8Zn-0.8Ca alloy (ZX31) [...] Read more.
To control the degradation rate of magnesium (Mg) alloys, chitosan (CHI) and L-glutamic acid (LGA) were used as coatings on Mg-Zn-Ca alloys via dip coating. In this study, either two or seven CHI/LGA layers were applied as a coating on Mg-2.8Zn-0.8Ca alloy (ZX31) and Mg-2.8Zn-0.8Ca hemostasis clips (ZX31 clips). The morphologies, compositions, and surface roughness of the specimens were characterized via scanning electron microscopy, Fourier transform infrared spectroscopy, and surface measurement devices. The degradation rates and behavior of the specimens were evaluated by immersing them in simulated body fluids and by applying these ZX31 clips on rabbits’ uterine tubes for five weeks. The specimen with seven layers (ZX31(CHI/LGA)7) exhibited improved corrosion behavior when compared with ZX31 or ZX31(CHI/LGA)2, with a reduced degradation rate of the Mg alloy in a simulated body environment. In vivo experiments showed that ZX31 clips exhibited good biocompatibilities in each group but could not maintain the clamping function for five weeks. The weight loss of ZX31(CHI/LGA)7 was significantly lower than that of the other groups. Consequently, it was verified that CHI can be used as a protective layer on a magnesium alloy surface via in vitro and in vivo experiments. Full article
(This article belongs to the Special Issue Corrosion and Degradation for Biomedical Materials)
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<p>Hemostatic Mg clips.</p>
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<p>Schematic illustration of the chitosan (CHI) and L-glutamic acid (LGA) coating process.</p>
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<p>SEM and 2-D texture height maps of (<b>a</b>) a specimen ground with #2000 SiC paper; (<b>b</b>) ZX31(CHI/LGA)<sub>2</sub> specimen; (<b>c</b>) ZX31(CHI/LGA)<sub>7</sub> specimen.</p>
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<p>FTIR spectra of pure CHI, ZX31(CHI/LGA)<sub>2</sub> and ZX31(CHI/LGA)<sub>7</sub> specimens.</p>
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<p>Volume of hydrogen for each of the specimens during a 30-day immersion test in SBF: (<b>a</b>) hydrogen evolution process of uncoated ZX31, ZX31(CHI/LGA)<sub>2</sub>, and ZX31(CHI/LGA)<sub>7</sub> specimens immersed in an SBF solution at 37 ± 0.2 °C for 30 days; (<b>b</b>) H<sub>2</sub> released per day.</p>
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<p>SEM observations and EDS point spectrum analysis of the corroded surfaces after 30 days of immersion for (<b>a</b>) ZX31; (<b>b</b>) ZX31(CHI/LGA)<sub>2</sub> and (<b>c</b>) ZX31(CHI/LGA)<sub>7</sub>.</p>
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<p>Placement of Mg clips on the uterine tubes of rabbits: (<b>a</b>,<b>b</b>) rabbit-1, for which three ZX31 and three ZX31(CHI/LGA)<sub>2</sub> Mg clips were used; (<b>c</b>,<b>d</b>) rabbit-2, for which three ZX31 and three ZX31(CHI/LGA)<sub>7</sub> Mg clips were used; (<b>e</b>,<b>f</b>) rabbit-3, for which three ZX31(CHI/LGA)<sub>7</sub> and three ZX31(CHI/LGA)<sub>2</sub> Mg clips were used.</p>
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<p>X-ray images of rabbits with Mg clips taken two and three weeks after surgery: (<b>a</b>) ZX31 and ZX31(CHI/LGA)<sub>2</sub> Mg clips on the left and right uterine tubes of rabbit-1, respectively (second week); (<b>b</b>) ZX31 and ZX31(CHI/LGA)<sub>7</sub> Mg clips on the left and right uterine tubes of rabbit-2, respectively (second week); (<b>c</b>) ZX31(CHI/LGA)<sub>7</sub> and ZX31(CHI/LGA)<sub>2</sub> Mg clips on the left and right uterine tubes of rabbit-3, respectively (second week); (<b>d</b>–<b>f</b>) the clips in the third week.</p>
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<p>Mg clips taken from the rabbits five weeks after surgery: (<b>a</b>) ZX31 clips; (<b>b</b>) ZX31(CHI/LGA)<sub>2</sub> clips; (<b>c</b>) ZX31(CHI/LGA)<sub>7</sub> clips.</p>
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<p>Weight loss of the Mg clips from each group five weeks after surgery (<span class="html-italic">p</span> values obtained via Scheffe’s method).</p>
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<p>Histological photographs of hematoxylin-and-eosin-stained sections of tissues.</p>
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14 pages, 3090 KiB  
Article
Graphitic Carbon Nitride for Photocatalytic Air Treatment
by Michal Baudys, Šárka Paušová, Petr Praus, Vlasta Brezová, Dana Dvoranová, Zuzana Barbieriková and Josef Krýsa
Materials 2020, 13(13), 3038; https://doi.org/10.3390/ma13133038 - 7 Jul 2020
Cited by 16 | Viewed by 3098
Abstract
Graphitic carbon nitride (g-C3N4) is a conjugated polymer, which recently drew a lot of attention as a metal-free and UV and visible light responsive photocatalyst in the field of solar energy conversion and environmental remediation. This is due to [...] Read more.
Graphitic carbon nitride (g-C3N4) is a conjugated polymer, which recently drew a lot of attention as a metal-free and UV and visible light responsive photocatalyst in the field of solar energy conversion and environmental remediation. This is due to its appealing electronic band structure, high physicochemical stability and earth-abundant nature. In the present work, bulk g-C3N4 was synthesized by thermal decomposition of melamine. This material was further exfoliated by thermal treatment. S-doped samples were prepared from thiourea or further treatment of exfoliated g-C3N4 by mesylchloride. Synthesized materials were applied for photocatalytic removal of air pollutants (acetaldehyde and NOx) according to the ISO 22197 and ISO 22197-1 methodology. The efficiency of acetaldehyde removal under UV irradiation was negligible for all g-C3N4 samples. This can be explained by the fact that g-C3N4 under irradiation does not directly form hydroxyl radicals, which are the primary oxidation species in acetaldehyde oxidation. It was proved by electron paramagnetic resonance (EPR) spectroscopy that the dominant species formed on the irradiated surface of g-C3N4 was the superoxide radical. Its production was responsible for a very high NOx removal efficiency not only under UV irradiation (which was comparable with that of TiO2), but also under visible irradiation. Full article
(This article belongs to the Special Issue Photocatalytic Properties and Kinetics of Materials)
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<p>Apparatus for the evaluation of photocatalytic activity in the gas phase. 1: black light tube, 2: reactor, 3: catalyst, 4: pollutant gas, 5: compressed (synthetic) air, MFC: mass flow controller, 6: bubbler for humidification, 7: valves, 8: analyzer. Reprinted with permission from [<a href="#B10-materials-13-03038" class="html-bibr">10</a>].</p>
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<p>Emission spectra (left axis) of used light sources, UV (fluorescent), VIS (LED), VIS (fluorescent tube) and Kubelka–Munk spectrum of Ex-CN material (right axis).</p>
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<p>Removal of acetaldehyde on a film of Ex-CN (0.5 mg/cm<sup>2</sup>).</p>
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<p>Removal of acetaldehyde on a film of TiO<sub>2</sub> P25 (0.5 mg/cm<sup>2</sup>).</p>
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<p>Removal of NO<sub>x</sub> on a film of Ex-CN (0.5 mg/cm<sup>2</sup>).</p>
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<p>Removal of NO<sub>x</sub> on a film of TiO<sub>2</sub> P25 (0.5 mg/cm<sup>2</sup>).</p>
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<p>Amount of removed NO, formed NO<sub>2</sub> and totally removed NO<sub>x</sub>, respectively, under UV irradiation for 1 h.</p>
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<p>Amount of removed NO, NO<sub>x</sub> and formed NO<sub>2</sub>, respectively, under VIS fluorescent irradiation during a 1 h NO<sub>x</sub> experiment.</p>
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<p>Amount of removed NO, NO<sub>x</sub> and formed NO<sub>2</sub> under VIS LED irradiation during 1 h of experiment.</p>
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<p>(<b>a</b>) EPR spectra obtained before and upon continuous ultraviolet A (UVA) (<span class="html-italic">λ</span><sub>max</sub> = 365 nm) and VIS (<span class="html-italic">λ</span> &gt; 420 nm) exposure of the CN powder sample at room temperature. (<b>b</b>) Relative EPR integral intensity increase monitored upon UVA and VIS exposure of the studied powder samples at room temperature.</p>
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<p>Position of valence-band and conduction-band edge for g-C<sub>3</sub>N<sub>4</sub> and TiO<sub>2</sub> at pH 7 [<a href="#B17-materials-13-03038" class="html-bibr">17</a>].</p>
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<p>Concentration of <sup>∙</sup>DMPO-O<sub>2</sub>/O<sub>2</sub>H and <sup>∙</sup>DMPO-OH spin-adducts evaluated from the EPR spectra measured upon UV exposure of aerated aqueous suspensions of photocatalysts in the presence of 5,5-dimethyl-1-pyrroline <span class="html-italic">N</span>-oxide (DMPO) spin trap. (<span class="html-italic">λ</span><sub>max</sub> = 365 nm, UVA dose 4.5 J/cm<sup>2</sup>, photocatalyst loading, 0.5 mg/mL; <span class="html-italic">c</span><sub>0</sub>(DMPO) = 0.04 mol/dm<sup>3</sup>). Inset: experimental spectrum (black line) obtained upon continuous irradiation of a Mes-Ex-CN suspension under the given experimental conditions along with its simulation (red line).</p>
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<p>Illustration of DMPO spin-adducts generation upon UV exposure of aerated aqueous suspensions of C<sub>3</sub>N<sub>4</sub>-based photocatalysts along with simulated EPR spectra (magnetic field sweep of 7 mT).</p>
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15 pages, 2258 KiB  
Article
Antimicrobial Activity of Hybrid Nanomaterials Based on Star and Linear Polymers of N,N′-Dimethylaminoethyl Methacrylate with In Situ Produced Silver Nanoparticles
by Paulina Teper, Anna Sotirova, Violeta Mitova, Natalia Oleszko-Torbus, Alicja Utrata-Wesołek, Neli Koseva, Agnieszka Kowalczuk and Barbara Mendrek
Materials 2020, 13(13), 3037; https://doi.org/10.3390/ma13133037 - 7 Jul 2020
Cited by 21 | Viewed by 2969
Abstract
Well-defined linear and multi-arm star polymer structures were used as the templates for in situ synthesis and stabilization of silver nanoparticles (AgNPs). This approach led to hybrid nanomaterials with high stability and antibacterial activity to both Gram-positive and Gram-negative bacterial strains. The ecologically [...] Read more.
Well-defined linear and multi-arm star polymer structures were used as the templates for in situ synthesis and stabilization of silver nanoparticles (AgNPs). This approach led to hybrid nanomaterials with high stability and antibacterial activity to both Gram-positive and Gram-negative bacterial strains. The ecologically friendly so called “green” synthesis of nanomaterials was performed through AgNPs preparation in the aqueous solutions of star and linear poly(N,N′-dimethylaminoethyl methacrylate)s (PDMAEMAs); the process was followed with time. The size, shape, and zeta potential of the obtained hybrids were determined. To our knowledge, this is the first time that the antibacterial activity of PDMAEMA hybrid nanomaterial against Bacillus subtilis, Escherichia coli and Pseudomonas aeruginosa was investigated and assessed by minimum inhibitory concentration (MIC) and minimum biocidal concentration (MBC). Completely quaternized with ethyl bromide, star and linear PDMAEMAs were used in comparative biological tests. The modification of the polymers with in situ-formed AgNPs increased the antibacterial properties against all studied strains of bacteria by several times in comparison to non-modified polymers and quaternized polymers. These results yield novel nanohybrid materials that can be useful for applications in medicine and biology. Full article
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Graphical abstract
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<p>Chromatograms of star and linear PDMAEMA (DMF, 1 mL/min).</p>
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<p>Selected time course images of AgNPs formed in aqueous solutions of (<b>a</b>) star PDMAEMA and (<b>b</b>) linear PDMAEMA.</p>
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<p>UV-Vis spectra of AgNPs formed in the aqueous solution of (<b>a</b>) star PDMAEMA (S-PDMAEMA, <a href="#materials-13-03037-t001" class="html-table">Table 1</a>) and (<b>b</b>) linear PDMAEMA (L-PDMAEMA, <a href="#materials-13-03037-t001" class="html-table">Table 1</a>); the polymer concentration was c = 1 mg/mL.</p>
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<p>Size distributions of AgNPs formed in solutions of (<b>a</b>) star PDMAEMA and (<b>b</b>) linear PDMAEMA (DLS, θ = 90°).</p>
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<p>TEM images of AgNPs formed in solutions of (<b>a</b>) star PDMAEMA and (<b>b</b>) linear PDMAEMA.</p>
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<p><sup>1</sup>H NMR (600 MHz, D<sub>2</sub>O) of quaternized (<b>a</b>) star PDMAEMA (<b>b</b>) linear PDMAEMA.</p>
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<p>The synthesis of (<b>a</b>) star and (<b>b</b>) linear poly(<span class="html-italic">N</span>,<span class="html-italic">N</span>′-dimethylaminoethyl methacrylate)s via ATRP.</p>
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<p>Preparation of the hybrid polymeric materials by (<b>a</b>) star polymer and (<b>b</b>) linear polymer with in situ-incorporated AgNPs.</p>
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16 pages, 4347 KiB  
Article
Synthesis of Ordered Mesoporous Zr-Al Composite Oxides with Excellent Structural and Textural Properties and Extremely High Stability
by Feng Yu, Shinan Bi, Tonghui Liu, Dahai Pan, Shuwei Chen, Xiaoliang Yan, Binbin Fan and Ruifeng Li
Materials 2020, 13(13), 3036; https://doi.org/10.3390/ma13133036 - 7 Jul 2020
Cited by 2 | Viewed by 2615
Abstract
Ordered mesoporous Zr-Al composite oxide materials (denoted as OMZA-x) with different Zr contents have been synthesized by a solvent evaporation-inducing self-assembly procedure associated with a thermal treatment at 100 °C. A cooperative co-assembly process of amphiphilic triblock copolymer F127 molecules and inorganic hydroxyl [...] Read more.
Ordered mesoporous Zr-Al composite oxide materials (denoted as OMZA-x) with different Zr contents have been synthesized by a solvent evaporation-inducing self-assembly procedure associated with a thermal treatment at 100 °C. A cooperative co-assembly process of amphiphilic triblock copolymer F127 molecules and inorganic hydroxyl species originated from the hydrolysis of Zr and Al precursors was proposed to explain the synthesis of OMZA-x. Compared to ordered mesoporous alumina prepared without introducing Zr species, the resultant OMZA-x exhibited a much more ordered mesostructure combined with a distinct increase in the pore volume and specific surface area. The highly homogenous doping of Zr into the mesopore walls together with the formation of Zr-O-Al bonds can effectively enhance the thermal and hydrothermal stability of OMZA-x. For instance, the ordered mesostructure and excellent textural properties of OMZA-6 prepared with the optimum atomic ratio of Al to Zr of 6 could be well maintained even after a high-temperature treatment at 1000 °C for 1 h or a hydrothermal treatment at 100 °C for 6 h. Full article
(This article belongs to the Special Issue New Insight into Microporous and Mesoporous Materials)
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Graphical abstract
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<p>Schematic illustration for the synthesis of ordered mesoporous Zr-Al composite oxide materials (OMZA-x).</p>
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<p>Small-angle X-ray diffraction (XRD) patterns of samples OMZA-x and OMA.</p>
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<p>Transmission electron microscopy (TEM) images of sample OMZA-6 viewed along the (110) (<b>a</b>) and (100) (<b>b</b>) directions, TEM image (<b>c</b>) of OMZA-6 thermally treated at 1000 °C for 1 h, and TEM image (<b>d</b>) of OMZA-6 hydrothermally treated at 100 °C for 6 h, respectively.</p>
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<p>Elemental analysis mapping showing the distribution of Al (<b>a</b>,<b>d</b>), O (<b>b</b>,<b>e</b>), and Zr (<b>c</b>,<b>f</b>) for two different regions of the sample OMZA-6.</p>
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<p>N<sub>2</sub> sorption isotherms (<b>a</b>) and pore size distribution curves (<b>b</b>) of samples OMZA-x and OMA. For clarity, in (<b>a</b>), the isotherms of OMZA-4, OMZA-6, OMZA-8, OMZA-10 and OMA are offset along the Y axis by 150, 300, 560, 750, and 950 cm<sup>3</sup>/g, respectively. In (<b>b</b>), the Y axis values are increased by 3.0, 6.0, 10.2, 13.8, and 17.8 cm<sup>3</sup>/g, respectively.</p>
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<p>FT-IR spectra of samples OMZA-6 and OMA.</p>
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<p><sup>27</sup>Al MAS NMR spectra of samples OMZA-6 and OMA.</p>
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<p>Small- (<b>a</b>) and wide- (<b>b</b>) angle XRD patterns of samples OMZA-x and OMA after thermal treatment at 1000 °C for 1 h.</p>
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<p>N<sub>2</sub> sorption isotherms (<b>a</b>) and pore size distribution curves (<b>b</b>) of samples OMZA-x and OMA after thermal treatment at 1000 °C for 1 h. For clarity, in (<b>a</b>), the isotherms of OMZA-4, OMZA-6, OMZA-8, OMZA-10 and OMA are offset along the Y axis by 160, 370, 560, 710 and 950 cm<sup>3</sup>/g, respectively. In (<b>b</b>), the Y axis values are increased by 2, 4.2, 7.5, 10.8 and 13.8 cm<sup>3</sup>/g, respectively.</p>
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<p>Small-angle XRD patterns of OMZA-6 (<b>a</b>) and OMA (<b>b</b>) before and after hydrothermal treatment at 100 °C for different time.</p>
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<p>N<sub>2</sub> sorption isotherms (<b>a</b>) and pore size distribution curves (<b>b</b>) of sample OMZA-6 before and after hydrothermal treatment at 100 °C for different time. For clarity, in (<b>a</b>), the isotherms of untreated OMZA-6 and OMZA-6 hydrothermally treated for 2 h are offset along the Y axis by 200 and 100 cm<sup>3</sup>/g, respectively. In (<b>b</b>), the Y axis values are increased by 3.1 and 1.5 cm<sup>3</sup>/g, respectively.</p>
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10 pages, 3710 KiB  
Article
A Facile Synthesis and Characterization of Highly Crystalline Submicro-Sized BiFeO3
by Dovydas Karoblis, Diana Griesiute, Kestutis Mazeika, Dalis Baltrunas, Dmitry V. Karpinsky, Anna Lukowiak, Pawel Gluchowski, Rimantas Raudonis, Arturas Katelnikovas, Aleksej Zarkov and Aivaras Kareiva
Materials 2020, 13(13), 3035; https://doi.org/10.3390/ma13133035 - 7 Jul 2020
Cited by 18 | Viewed by 3013
Abstract
In this study, a highly crystalline bismuth ferrite (BFO) powder was synthesized using a novel, very simple, and cost-effective synthetic approach. It was demonstrated that the optimal annealing temperature for the preparation of highly-pure BFO is 650 °C. At lower or higher temperatures, [...] Read more.
In this study, a highly crystalline bismuth ferrite (BFO) powder was synthesized using a novel, very simple, and cost-effective synthetic approach. It was demonstrated that the optimal annealing temperature for the preparation of highly-pure BFO is 650 °C. At lower or higher temperatures, the formation of neighboring crystal phases was observed. The thermal behavior of BFO precursor gel was investigated by thermogravimetric and differential scanning calorimetry (TG-DSC) measurements. X-ray diffraction (XRD) analysis and Mössbauer spectroscopy were employed for the investigation of structural properties. Scanning electron microscopy (SEM) was used to evaluate morphological features of the synthesized materials. The obtained powders were also characterized by magnetization measurements, which showed antiferromagnetic behavior of BFO powders. Full article
(This article belongs to the Special Issue Advances in Nanostructured Materials)
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<p>TG-DTG-DSC curves of BFO precursor gel.</p>
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<p>XRD patterns of BFO powders annealed at different temperatures.</p>
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<p>SEM micrographs of BFO powders annealed at 650 °C under different magnification (<b>a</b>) and (<b>b</b>).</p>
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<p>Magnetic hysteresis of BFO powders annealed at 650 °C.</p>
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<p>Mössbauer spectrum of BFO powders recorded at room temperature.</p>
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<p>Plot of (ahν)<sup>2</sup> versus photon energy for BFO powder annealed at 650 °C.</p>
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14 pages, 6665 KiB  
Article
Selective Laser Sintering (SLS) and Post-Processing of Prosopis Chilensis/Polyethersulfone Composite (PCPC)
by Aboubaker I. B. Idriss, Jian Li, Yangwei Wang, Yanling Guo, Elkhawad A. Elfaki and Shareef A. Adam
Materials 2020, 13(13), 3034; https://doi.org/10.3390/ma13133034 - 7 Jul 2020
Cited by 15 | Viewed by 2708
Abstract
The range of selective laser sintering (SLS) materials is currently limited, and the available materials are often of high cost. Moreover, the mechanical strength of wood–plastic SLS parts is low, which restricts the application of a SLS technology. A new composite material has [...] Read more.
The range of selective laser sintering (SLS) materials is currently limited, and the available materials are often of high cost. Moreover, the mechanical strength of wood–plastic SLS parts is low, which restricts the application of a SLS technology. A new composite material has been proposed to address these issues, while simultaneously valorizing agricultural and forestry waste. This composite presents several advantages, including reduced pollution associated with waste disposal and reduced CO2 emission with the SLS process in addition to good mechanical strength. In this article, a novel and low-cost Prosopis chilensis/polyethersulfone composite (PCPC) was used as a primary material for SLS. The formability of PCPC with various raw material ratios was investigated via single-layer experiments, while the mechanical properties and dimensional accuracy of the parts produced using the various PCPC ratios were evaluated. Further, the microstructure and particle distribution in the PCPC pieces were examined using scanning electron microscopy. The result showed that the SLS part produced via 10/90 (wt/wt) PCPC exhibited the best mechanical strength and forming quality compared to other ratios and pure polyethersulfone (PES), where bending and tensile strengths of 10.78 and 4.94 MPa were measured. To improve the mechanical strength, post-processing infiltration was used and the PCPC-waxed parts were enhanced to 12.38 MPa and 5.73 MPa for bending and tensile strength. Full article
(This article belongs to the Special Issue Additive Manufacturing of Polymer-Based Composites)
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<p>Preparation of the Prosopis chilensis/polyethersulfone composite (PCPC), with SEM micrographs of the (<b>a</b>) polyethersulfone (PES) powder particle morphology, (<b>b</b>) Prosopis chilensis powder (PCP) particle morphology, and a digital photograph of the (<b>c</b>) PCPC powder after mechanical mixing.</p>
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<p>Flow chart of the preparation process of Prosopis chilensis/PES composites (PCPC).</p>
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<p>Characteristic building process using a AFS-360 rapid prototyping machine.</p>
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<p>The post-processing flow chart of the PCPC parts.</p>
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<p>Surface morphology of (<b>A</b>) the PES powder and (<b>B</b>) the PCP.</p>
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<p>DSC curve of the PES and PCP powders between 20 °C and 240 °C at a heating rate of 10 °C/min.</p>
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<p>Single-layer sintered PCPC and PES samples prepared using different PCP and PES powder ratios, namely, (<b>a</b>) 10% PCP (10/90), (<b>b</b>) 15% PCP (15/85), (<b>c</b>) 20% PCP (20/80), and (<b>d</b>) pure PES.</p>
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<p>Surface morphology of (<b>a</b>) PCPC parts (20% PCP) and (<b>b</b>) PCPC parts (10% PCP).</p>
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<p>Selective laser sintering (SLS) samples for (<b>a</b>) the tensile and bending tests, and (<b>b</b>) the waxing test.</p>
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<p>Mechanical properties of the PCPC parts with varying mixture ratios, namely, (<b>a</b>) bending strength, (<b>b</b>) tensile strength, and (<b>c</b>) density. (Note: zero mass ratio represents a pure PES sintered part).</p>
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<p>Mechanical properties of the PCPC parts with varying PCP/PES ratios including the standard deviation of the mean. The lower and upper limits of the bending tests were (7.22, 9.22), (10.13, 11.43), (6.55, 7.85), and (4.45, 5.75), respectively, from pure PES to PCPC (20/80); and the lower and upper limits of the tensile tests parts were (4.27, 5.43), (4.30, 5.59), (2.47, 3.78), and (1.85, 3.15), respectively, from pure PES to PCPC (20/80). Note: the lower and upper limits of the bending and tensile strength are the 95% confidence intervals for the means. *: means any mean value in chart became between the upper and lower values.</p>
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<p>Surface roughness of the PCPC parts before and after post-processing (wax infiltration and polishing).</p>
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16 pages, 805 KiB  
Article
Effective 1D Time-Dependent Schrödinger Equations for 3D Geometrically Correlated Systems
by Devashish Pandey, Xavier Oriols and Guillermo Albareda
Materials 2020, 13(13), 3033; https://doi.org/10.3390/ma13133033 - 7 Jul 2020
Viewed by 2645
Abstract
The so-called Born–Huang ansatz is a fundamental tool in the context of ab-initio molecular dynamics, viz., it allows effectively separating fast and slow degrees of freedom and thus treating electrons and nuclei with different mathematical footings. Here, we consider the use of a [...] Read more.
The so-called Born–Huang ansatz is a fundamental tool in the context of ab-initio molecular dynamics, viz., it allows effectively separating fast and slow degrees of freedom and thus treating electrons and nuclei with different mathematical footings. Here, we consider the use of a Born–Huang-like expansion of the three-dimensional time-dependent Schrödinger equation to separate transport and confinement degrees of freedom in electron transport problems that involve geometrical constrictions. The resulting scheme consists of an eigenstate problem for the confinement degrees of freedom (in the transverse direction) whose solution constitutes the input for the propagation of a set of coupled one-dimensional equations of motion for the transport degree of freedom (in the longitudinal direction). This technique achieves quantitative accuracy using an order less computational resources than the full dimensional simulation for a typical two-dimensional geometrical constriction and upto three orders for three-dimensional constriction. Full article
(This article belongs to the Special Issue Nanowire Field-Effect Transistor (FET))
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<p>Two different nanojunctions, viz., (<b>a</b>,<b>c</b>), defined by Equation (A18a,b) in <a href="#app4-materials-13-03033" class="html-app">Appendix D</a> and using <math display="inline"><semantics> <mrow> <mi mathvariant="script">A</mi> <mo>=</mo> <mn>180</mn> </mrow> </semantics></math>, <math display="inline"><semantics> <mrow> <mi mathvariant="script">B</mi> <mo>=</mo> <mn>220</mn> </mrow> </semantics></math>, <math display="inline"><semantics> <mrow> <msub> <mi>a</mi> <mn>1</mn> </msub> <mo>=</mo> <mn>630</mn> </mrow> </semantics></math>, <math display="inline"><semantics> <mrow> <msub> <mi>a</mi> <mn>2</mn> </msub> <mo>=</mo> <mn>870</mn> </mrow> </semantics></math>, with <math display="inline"><semantics> <mrow> <mi>γ</mi> <mo>=</mo> <mn>10</mn> </mrow> </semantics></math> in (<b>a</b>) and <math display="inline"><semantics> <mrow> <mi>γ</mi> <mo>=</mo> <mn>20</mn> </mrow> </semantics></math> in (<b>c</b>). Panels (<b>b</b>,<b>d</b>) show the associated second order (non-adiabatic) couplings <math display="inline"><semantics> <msup> <mi>S</mi> <mrow> <mi>k</mi> <mi>l</mi> </mrow> </msup> </semantics></math> (solid blue lines) and the associated potential-energies <math display="inline"><semantics> <msubsup> <mi mathvariant="script">E</mi> <mi>x</mi> <mi>k</mi> </msubsup> </semantics></math> (solid black lines) for the geometries in (<b>a</b>,<b>c</b>), respectively. Note that, due to the symmetry of the states defined in Equation (16), the coupling between odd and even states is zero, i.e., <math display="inline"><semantics> <mrow> <msup> <mi>F</mi> <mrow> <mi>k</mi> <mi>l</mi> </mrow> </msup> <mrow> <mo>(</mo> <mi>x</mi> <mo>)</mo> </mrow> <mo>=</mo> <msup> <mi>S</mi> <mrow> <mi>k</mi> <mi>l</mi> </mrow> </msup> <mrow> <mo>(</mo> <mi>x</mi> <mo>)</mo> </mrow> <mo>=</mo> <mn>0</mn> <mo>,</mo> <mspace width="0.277778em"/> <mo>∀</mo> <mi>k</mi> <mo>+</mo> <mi>l</mi> <mo>=</mo> <mi>odd</mi> </mrow> </semantics></math>.</p>
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<p>Panels (<b>a</b>,<b>b</b>) represent the probability density <math display="inline"><semantics> <msup> <mrow> <mo>|</mo> <mo>Ψ</mo> <mrow> <mo>(</mo> <mi>x</mi> <mo>,</mo> <mi>y</mi> <mo>,</mo> <mn>0</mn> <mo>)</mo> </mrow> <mo>|</mo> </mrow> <mn>2</mn> </msup> </semantics></math> associated with the wavefunctions in Equations (19) and (20) respectively. Red regions in the plots correspond to higher probability densities, while blue regions correspond to lower probabilities.</p>
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<p>Time-evolution of the initial wavefunction in Equation (19). The reduced density in Equation (13) (dashed green line), as well as the reduced density in Equation (22) for <math display="inline"><semantics> <mrow> <msub> <mi>N</mi> <mi>e</mi> </msub> <mo>=</mo> <mn>11</mn> </mrow> </semantics></math> (solid dark blue) are shown at times <math display="inline"><semantics> <mrow> <mi>t</mi> <mo>=</mo> <mn>300</mn> </mrow> </semantics></math> a.u., <math display="inline"><semantics> <mrow> <mi>t</mi> <mo>=</mo> <mn>5010</mn> </mrow> </semantics></math> a.u., and <math display="inline"><semantics> <mrow> <mi>t</mi> <mo>=</mo> <mn>9000</mn> </mrow> </semantics></math> a.u. in panels (<b>a</b>), (<b>b</b>), and (<b>c</b>), respectively. The rest of the lines correspond to the absolute squared value of the longitudinal coefficients <math display="inline"><semantics> <mrow> <msup> <mi>χ</mi> <mi>k</mi> </msup> <mrow> <mo>(</mo> <mi>x</mi> <mo>,</mo> <mi>t</mi> <mo>)</mo> </mrow> </mrow> </semantics></math>. The evolution of the adiabatic populations in Equation (23) can be found in panel (<b>d</b>), using the same color code as in panels (<b>a</b>–<b>c</b>).</p>
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<p>Time-evolution of the initial wavefunction in Equation (20). The reduced density in Equation (13) (dashed green line), as well as the reduced density in Equation (22) for <math display="inline"><semantics> <mrow> <msub> <mi>N</mi> <mi>e</mi> </msub> <mo>=</mo> <mn>15</mn> </mrow> </semantics></math> (solid dark blue line) are shown at times <math display="inline"><semantics> <mrow> <mi>t</mi> <mo>=</mo> <mn>0</mn> </mrow> </semantics></math> a.u., <math display="inline"><semantics> <mrow> <mi>t</mi> <mo>=</mo> <mn>4620</mn> </mrow> </semantics></math> a.u., and <math display="inline"><semantics> <mrow> <mi>t</mi> <mo>=</mo> <mn>7320</mn> </mrow> </semantics></math> a.u. in panels (<b>a</b>), (<b>b</b>), and (<b>c</b>), respectively. The rest of the lines correspond to the absolute squared value of the longitudinal coefficients <math display="inline"><semantics> <mrow> <msup> <mi>χ</mi> <mi>k</mi> </msup> <mrow> <mo>(</mo> <mi>x</mi> <mo>,</mo> <mi>t</mi> <mo>)</mo> </mrow> </mrow> </semantics></math>. The evolution of the adiabatic populations in Equation (23) can be found in panel (<b>d</b>), using the same color code as in panels (<b>a</b>–<b>c</b>).</p>
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<p>Figure depicting the transmission coefficient, <span class="html-italic">T</span>, under different bias voltages applied along the longitudinal direction. This plot provides a comparison for <span class="html-italic">T</span> between the exact 2D simulation (shown in dashed green line) and the 1D simulation (shown in solid red line for <math display="inline"><semantics> <mrow> <msub> <mi>N</mi> <mi>e</mi> </msub> <mo>=</mo> <mn>15</mn> </mrow> </semantics></math> states and in the solid blue line for <math display="inline"><semantics> <mrow> <msub> <mi>N</mi> <mi>e</mi> </msub> <mo>=</mo> <mn>25</mn> </mrow> </semantics></math> states). For a voltage range of <math display="inline"><semantics> <mrow> <mn>0.0075</mn> <mspace width="0.277778em"/> <mrow> <mi mathvariant="normal">a</mi> <mo>.</mo> <mi mathvariant="normal">u</mi> <mo>.</mo> </mrow> <mo>≤</mo> <msub> <mi>V</mi> <mrow> <mi>e</mi> <mi>x</mi> <mi>t</mi> </mrow> </msub> <mo>≤</mo> <mn>0.045</mn> <mspace width="0.277778em"/> <mrow> <mi mathvariant="normal">a</mi> <mo>.</mo> <mi mathvariant="normal">u</mi> <mo>.</mo> </mrow> </mrow> </semantics></math>, <math display="inline"><semantics> <mrow> <msub> <mi>N</mi> <mi>e</mi> </msub> <mo>=</mo> <mn>25</mn> </mrow> </semantics></math> states are enough to capture the exact 2D case. For <math display="inline"><semantics> <mrow> <mi>max</mi> <mo>[</mo> <msub> <mi>V</mi> <mrow> <mi>e</mi> <mi>x</mi> <mi>t</mi> </mrow> </msub> <mo>]</mo> <mo>=</mo> <mn>0.027</mn> </mrow> </semantics></math> a.u., <math display="inline"><semantics> <mrow> <msub> <mi>N</mi> <mi>e</mi> </msub> <mo>=</mo> <mn>15</mn> </mrow> </semantics></math> states sufficiently capture the exact 2D case.</p>
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19 pages, 4552 KiB  
Article
Double-Recycled Reclaimed Asphalt Pavement: A Laboratory Investigation at Low Temperatures Based on Different Mathematical Approaches
by Ki Hoon Moon and Augusto Cannone Falchetto
Materials 2020, 13(13), 3032; https://doi.org/10.3390/ma13133032 - 7 Jul 2020
Cited by 7 | Viewed by 2460
Abstract
Using recyclable materials in asphalt pavement is a fundamental design approach not only for limiting the environmental impact of the construction industry, but also for reducing the overall costs of the road infrastructures. Over the past years, road agencies have developed different policies [...] Read more.
Using recyclable materials in asphalt pavement is a fundamental design approach not only for limiting the environmental impact of the construction industry, but also for reducing the overall costs of the road infrastructures. Over the past years, road agencies have developed different policies to incorporate various types of recyclable material into conventional asphalt mixtures. reclaimed asphalt pavement (RAP) is one of the most highly recycled construction materials. However, the aged RAP binder and its stiffer and brittle characteristics compared to the fresh binder may negatively affect the performance of the recycled mixture, especially when operating in cold climates. In this study, the low-temperature response of asphalt mixture prepared with single-recycled RAP (SRRAP) and double-recycled RAP (DRRAP), prepared in the laboratory, is experimentally investigated based on creep testing performed with the bending beam rheometer (BBR). Then, the data were analyzed based on three simple mathematical models to extract information on material behavior. Finally, a new indicator named thermal stress factor (TFS) on low-temperature response is proposed. Relatively poorer performance was observed from SRRAP mixture compared to the asphalt mixture prepared with virgin material. However, the low-temperature response between SRRAP and DRRAP did not present significant differences. The values of TFS support the experimental results and suggest the possibility of considering re-recycling technology for further research with the objective of a possible application in the asphalt pavement industry. Full article
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<p>Schematic flow chart of the research approach.</p>
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<p>Asphalt mixture samples (two asphalt mixture samples were prepared for each mixture type).</p>
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<p>Testing setup of bending beam rheometer (BBR) mixture creep test: (<b>a</b>) BBR testing device, (<b>b</b>) mixture beam sample.</p>
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<p>SAP (Single Asymptote Procedure) approach.</p>
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<p>Creep stiffness, <span class="html-italic">S</span>(<span class="html-italic">t</span>), at different testing time. (<b>a</b>) T = −12 °C; (<b>b</b>) T = −24 °C.</p>
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<p><span class="html-italic">m</span>-value, <span class="html-italic">m</span>(<span class="html-italic">t</span>), at different testing time. (<b>a</b>) T = −12 °C; (<b>b</b>) T = −24 °C.</p>
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<p><span class="html-italic">σ</span>(<span class="html-italic">T</span>) computation results (Simple Power law): (<b>a</b>) 2 °C/h; (<b>b</b>) 20 °C/h.</p>
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<p><span class="html-italic">σ</span>(<span class="html-italic">T</span>) computation results (Hopkins and Hamming, 1957): (<b>a</b>) 2 °C/h; (<b>b</b>) 20 °C/h.</p>
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<p><span class="html-italic">σ</span>(<span class="html-italic">T</span>) computation results (Laplace transformation): (<b>a</b>) 2 °C/h; (<b>b</b>) 20 °C/h.</p>
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<p><span class="html-italic">σ</span>(<span class="html-italic">T</span>) computation results (Control mixture).</p>
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<p><span class="html-italic">σ</span>(<span class="html-italic">T</span>) computation results: (<b>a</b>) SRRAP 25% mixture; (<b>b</b>) DRRAP 25% mixture.</p>
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<p><span class="html-italic">σ</span>(<span class="html-italic">T</span>) computation results: (<b>a</b>) SRRAP 40% mixture; (<b>b</b>) DRRAP 40% mixture.</p>
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<p>Schematic of the thermal stress factor (<span class="html-italic">TSF</span>) computation.</p>
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17 pages, 6792 KiB  
Article
Dynamic Mechanical Response and Damage Mechanism of HTPB Propellant under Impact Loading
by Hengning Zhang, Meng Liu, Yinggang Miao, Han Wang, Tao Chen, Xuezhong Fan and Hai Chang
Materials 2020, 13(13), 3031; https://doi.org/10.3390/ma13133031 - 7 Jul 2020
Cited by 31 | Viewed by 3186
Abstract
The dynamic mechanical behaviors of Hydroxyl-terminated polybutadiene (HTPB) propellant was studied by a split Hopkinson pressure bar apparatus (SHPB) at strain rates ranging from 103 to 104 s−1. The obtained stress–strain curves indicated that the mechanical features, such as [...] Read more.
The dynamic mechanical behaviors of Hydroxyl-terminated polybutadiene (HTPB) propellant was studied by a split Hopkinson pressure bar apparatus (SHPB) at strain rates ranging from 103 to 104 s−1. The obtained stress–strain curves indicated that the mechanical features, such as ultimate stress and strain energy, were strongly dependent on the strain rate. The real time deformation and fracture evolution of HTPB propellant were captured by a high-speed digital camera accompanied with an SHPB setup. Furthermore, microscopic observation for the post-test specimen was conducted to explore the different damage mechanisms under various conditions of impact loading. The dominated damage characteristics of HTPB propellant were changed from debonding and matrix tearing to multiple cracking modes of ammonium perchlorate (AP) particles, along with the increase of the strain rate. For the first time, the influence of AP particle density on the dynamic response of HTPB propellant was studied by analyzing the strain-rate sensitivity (SRS) index of HTPB propellant with two different filler content (80 wt.% and 85 wt.%), which deduced from a power function of ultimate stress and strain energy density. The result of this study is of significance for evaluating the structural integrity and security of HTPB propellant. Full article
(This article belongs to the Collection Materials Investigations in Mechanical Systems)
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<p>Photographs of two sizes of machined specimens for the (<b>a</b>) low-strain-rate loading test and (<b>b</b>) high-strain-rate loading test.</p>
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<p>(<b>a</b>) A photograph of the split Hopkinson pressure bar device fitted with a high-speed digital camera. (<b>b</b>) Scheme of the split Hopkinson pressure bar device.</p>
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<p>Original signals of incident, reflected, and transmitted waves recorded by the strain gauges.</p>
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<p>True stress–strain curve of H-80W under the strain rate of 2460 s<sup>−1</sup> without causing an ultimate fracture. The green numbers in the curve correspond to the numbers marked in the images recorded by a high-speed digital camera in <a href="#materials-13-03031-f005" class="html-fig">Figure 5</a>.</p>
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<p>Deformation processes of H-80W recorded by a high-speed digital camera under a strain rate of 2460 s<sup>−1</sup>. The green numbers in the images correspond to the numbers marked in <a href="#materials-13-03031-f004" class="html-fig">Figure 4</a>.</p>
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<p>SEM micrographs of the non-fractured H-80W after split Hopkinson pressure bar apparatus (SHPB) testing at room temperature under a strain rate of 2460 s<sup>−1</sup>: (<b>a</b>) ammonium perchlorate (AP) particles embedding within the HTPB matrices as well as the distinct interfaces of the particle-binder in an untested specimen; (<b>b</b>) debonding of the particle–binder interface induced by impact loading; (<b>c</b>) the unbroken AP particle with covering residual binder polymer; (<b>d</b>) the strip-shape polymer caused by severe binder matrix tearing.</p>
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<p>SEM micrographs of the non-fractured H-80W after split Hopkinson pressure bar apparatus (SHPB) testing at room temperature under a strain rate of 2460 s<sup>−1</sup>: (<b>a</b>) ammonium perchlorate (AP) particles embedding within the HTPB matrices as well as the distinct interfaces of the particle-binder in an untested specimen; (<b>b</b>) debonding of the particle–binder interface induced by impact loading; (<b>c</b>) the unbroken AP particle with covering residual binder polymer; (<b>d</b>) the strip-shape polymer caused by severe binder matrix tearing.</p>
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<p>True stress-strain curve of H-80W under a strain rate of 6100 s<sup>−1</sup>, causing a final fracture, the green numbers in the curve correspond to the numbers marked in the images recorded by a high-speed digital camera in <a href="#materials-13-03031-f008" class="html-fig">Figure 8</a>.</p>
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<p>Deformation and fracture processes of H-80W recorded by a high-speed digital camera under the strain rate of 6100 s<sup>−1</sup>, the green numbers in the images correspond to the numbers marked in <a href="#materials-13-03031-f007" class="html-fig">Figure 7</a>.</p>
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<p>SEM micrographs of the fractured H-80W after SHPB testing at room temperature under a strain rate of 6100 s<sup>−1</sup>: (<b>a</b>) cracking of AP particle and pieces of broken AP spreading on the fracture surface; (<b>b</b>) individual cracking AP particle without direct contact with other particles; (<b>c</b>) the multiple porosity and binder matrix tearing induced by high-speed impact loading; (<b>d</b>) cracking propagating through binder matrix into AP particles; (<b>e</b>) cracking propagating through the AP particle-binder interface into the AP particles; (<b>f</b>) cracking propagating through the adjacent AP particles.</p>
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<p>SEM micrographs of the fractured H-80W after SHPB testing at room temperature under a strain rate of 6100 s<sup>−1</sup>: (<b>a</b>) cracking of AP particle and pieces of broken AP spreading on the fracture surface; (<b>b</b>) individual cracking AP particle without direct contact with other particles; (<b>c</b>) the multiple porosity and binder matrix tearing induced by high-speed impact loading; (<b>d</b>) cracking propagating through binder matrix into AP particles; (<b>e</b>) cracking propagating through the AP particle-binder interface into the AP particles; (<b>f</b>) cracking propagating through the adjacent AP particles.</p>
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<p>True stress–strain plots of H-80W under various strain rates.</p>
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<p>True stress–strain plots of H-85W under various strain rates.</p>
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<p>The strain rate dependence on ultimate stress and strain energy density of (<b>a</b>) H-80W and (<b>b</b>) H-85W.</p>
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<p>The rate-dependent relations of ultimate stress fitted by Equation (3) for H-80W, H-85W and other reported HTPB based materials.</p>
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18 pages, 11677 KiB  
Article
Stiffness Prediction of Connections between CHS Tubes and Externally Welded I-Beams: FE Analyses and Analytical Study
by Sabatino Di Benedetto, Massimo Latour and Gianvittorio Rizzano
Materials 2020, 13(13), 3030; https://doi.org/10.3390/ma13133030 - 7 Jul 2020
Cited by 8 | Viewed by 5500
Abstract
Double-tee profiles are the most popular members in Europe and the USA for steel structures. However, more efficient cross-sections, such as circular hollow sections (CHSs), could be adopted, since they can provide higher aesthetic, economic and mechanical benefits, with the only drawback of [...] Read more.
Double-tee profiles are the most popular members in Europe and the USA for steel structures. However, more efficient cross-sections, such as circular hollow sections (CHSs), could be adopted, since they can provide higher aesthetic, economic and mechanical benefits, with the only drawback of more complex connections such as in the case of I-beams welded to the external surface of circular hollow profiles. Based on the ring model theory, developed by Togo, a rule to design the flexural resistance of such a connection has been included in the Eurocode 3 part 1.8, while no formulations are provided to predict the corresponding initial stiffness. The present work aims at filling this knowledge gap, adopting an approach based on experimental, numerical and analytical work. A monotonic and a cyclic test have been performed on two beam-to-column sub-assemblies; the experimental outcomes have been exploited to validate a finite element (FE) model developed in Abaqus and used to numerically perform the monotonic loading simulations of 30 joints. Afterwards, starting from the extracted information about stiffness, a regression analysis was carried out to define the coefficient of a design equation analytically derived applying the component method approach. The regression analysis is characterized by a coefficient of variation equal to 0.19. Full article
(This article belongs to the Special Issue Conventional vs. Innovative Materials, Tradition and Innovation)
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<p>Analysed connection: plan-views (<b>a</b>) and 3D view (<b>b</b>).</p>
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<p>Welding detail.</p>
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<p>Results of the coupon tests: stress-strain laws referred to the column, f<sub>y</sub> = 348.2 MPa (<b>a</b>); stress-strain laws referred to the beam, f<sub>y</sub> = 391.9 MPa (<b>b</b>).</p>
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<p>Schematic drawing of the experimental set-up.</p>
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<p>Arrangement of strain-gauges and transducers.</p>
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<p>Tested specimens subjected to cyclic and monotonic loading histories.</p>
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<p>Structural scheme referring to which Equation (3) has been derived (adapted from [<a href="#B51-materials-13-03030" class="html-bibr">51</a>]).</p>
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<p>Mesh size selection (<b>a</b>) and finite element (FE) model (<b>b</b>).</p>
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<p>Sensitivity of the mesh size on the numerical results.</p>
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<p>Overlap of FE and experimental results.</p>
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<p>Experimental versus FE results: cyclic test (<b>a</b>) and monotonic test (<b>b</b>).</p>
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<p>Main sources of deformability: hss (hollow section in shear), hsc (hollow section in transverse compression), hst (hollow section in transverse tension).</p>
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<p>Proposal vs. FEM stiffness.</p>
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10 pages, 5964 KiB  
Article
Magnetic, Structural and Spectroscopic Properties of Iron(II)-Octacyanoniobate(IV) Crystalline Film Obtained by Ion-Exchange Synthesis
by Wojciech Sas, Dawid Pinkowicz, Marcin Perzanowski and Magdalena Fitta
Materials 2020, 13(13), 3029; https://doi.org/10.3390/ma13133029 - 7 Jul 2020
Cited by 3 | Viewed by 2153
Abstract
Over recent years, investigations of coordination polymer thin films have been initiated due to their unique properties, which are expected to be strongly enhanced in the thin film form. In this work, a crystalline [FeII(H2O)2]2[Nb [...] Read more.
Over recent years, investigations of coordination polymer thin films have been initiated due to their unique properties, which are expected to be strongly enhanced in the thin film form. In this work, a crystalline [FeII(H2O)2]2[NbIV(CN)8]∙4H2O (1) film on a transparent Nafion membrane was obtained, for the first time, via ion-exchange synthesis. The proper film formation and its composition was confirmed with the use of energy dispersive X-ray spectroscopy and infrared spectroscopy, as well as in situ Ultraviolet-Visible (UV-Vis) spectroscopy. The obtained film were also characterized by scanning electron microscopy, X-ray diffraction, and magnetic measurements. The [FeII(H2O)2]2[NbIV(CN)8]∙4H2O film shows a sharp phase transition to a long-range magnetically ordered state at Tc = 40 K. The 1 film is a soft ferromagnet with the coercive field Hc = 1.2 kOe. Compared to the bulk counterpart, a decrease in critical temperature and a significant increase in the coercive field were observed in the films indicating a distinct size effect. The decrease in Tc could also have been related to the possible partial oxidation of FeII ions to FeIII, which could be efficient, due to the large surface of the thin film sample. Full article
(This article belongs to the Special Issue Advances in Molecular Magnetic Materials)
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<p>Packing diagrams presenting the crystal structure of {[Fe<sup>II</sup>(H<sub>2</sub>O)<sub>2</sub>]<sub>2</sub>[Nb<sup>IV</sup>(CN)<sub>8</sub>]·4H<sub>2</sub>O}<sub>n</sub> as viewed along the <span class="html-italic">a</span> (<b>left</b>) and <span class="html-italic">c</span> (<b>right</b>) crystallographic direction (crystallization water molecules and hydrogen atoms omitted for the sake of clarity).</p>
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<p>The XRD pattern measured for the Nafion<sup>®</sup> 117 membrane, {[Fe<sup>II</sup>(H<sub>2</sub>O)<sub>2</sub>]<sub>2</sub>[Nb<sup>IV</sup>(CN)<sub>8</sub>]·4H<sub>2</sub>O}<sub>n</sub> film deposited on the Nafion<sup>®</sup> 117 and {[Fe<sup>II</sup>(H<sub>2</sub>O)<sub>2</sub>]<sub>2</sub>[Nb<sup>IV</sup>(CN)<sub>8</sub>]·4H<sub>2</sub>O}<sub>n</sub> bulk sample.</p>
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<p>FT-IR spectra of [Fe<sup>II</sup>(H<sub>2</sub>O)<sub>2</sub>]<sub>2</sub>[Nb<sup>IV</sup>(CN)<sub>8</sub>]·4H<sub>2</sub>O recorded in KBr pellets with a tentative band assignment.</p>
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<p>(<b>a</b>) UV-visible spectra obtained for [Fe<sup>II</sup>(H<sub>2</sub>O)<sub>2</sub>]<sub>2</sub>[Nb<sup>IV</sup>(CN)<sub>8</sub>]·4H<sub>2</sub>O film during the ion-exchange synthesis; (<b>b</b>) Time dependence of the absorbance of the film at the wavelength of 500 nm.</p>
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<p>The SEM images of [Fe<sup>II</sup>(H<sub>2</sub>O)<sub>2</sub>]<sub>2</sub>[Nb<sup>IV</sup>(CN)<sub>8</sub>]·4H<sub>2</sub>O film obtained after 10 s (<b>a</b>); 30 s (<b>b</b>); 60 s (<b>c</b>); and 180 s (<b>d</b>).</p>
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<p>Temperature dependence of real (<b>a</b>) and imaginary (<b>b</b>) component of AC susceptibility of [Fe<sup>II</sup>(H<sub>2</sub>O)<sub>2</sub>]<sub>2</sub>[Nb<sup>IV</sup>(CN)<sub>8</sub>]·4H<sub>2</sub>O film.</p>
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<p>(<b>a</b>) Thermal variation of the DC susceptibility measured for (1) film and (1) bulk under zero field cooled (ZFC) and field cooled (FC) conditions in the applied field of 100 Oe; (<b>b</b>) Temperature dependence of <span class="html-italic">χ</span>·<span class="html-italic">T</span> for (1) film. Inset, thermal variation of the reciprocal magnetic susceptibility.</p>
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<p>M(H) dependence (<b>a</b>) and hysteresis loop (<b>b</b>) measured for (1) film at <span class="html-italic">T</span> = 2 K. The hysteresis plot obtained for the bulk sample is included for comparison.</p>
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19 pages, 7827 KiB  
Article
Multiscale Characterizations of Surface Anisotropies
by Tomasz Bartkowiak, Johan Berglund and Christopher A. Brown
Materials 2020, 13(13), 3028; https://doi.org/10.3390/ma13133028 - 7 Jul 2020
Cited by 23 | Viewed by 3204
Abstract
Anisotropy can influence surface function and can be an indication of processing. These influences and indications include friction, wetting, and microwear. This article studies two methods for multiscale quantification and visualization of anisotropy. One uses multiscale curvature tensor analysis and shows anisotropy in [...] Read more.
Anisotropy can influence surface function and can be an indication of processing. These influences and indications include friction, wetting, and microwear. This article studies two methods for multiscale quantification and visualization of anisotropy. One uses multiscale curvature tensor analysis and shows anisotropy in horizontal coordinates i.e., topocentric. The other uses multiple bandpass filters (also known as sliding bandpass filters) applied prior to calculating anisotropy parameters, texture aspect ratios (Str) and texture directions (Std), showing anisotropy in horizontal directions only. Topographies were studied on two milled steel surfaces, one convex with an evident large scale, cylindrical form anisotropy, the other nominally flat with smaller scale anisotropies; a µEDMed surface, an example of an isotropic surface; and an additively manufactured surface with pillar-like features. Curvature tensors contain the two principal curvatures, i.e., maximum and minimum curvatures, which are orthogonal, and their directions, at each location. Principal directions are plotted for each calculated location on each surface, at each scale considered. Histograms in horizontal coordinates show altitude and azimuth angles of principal curvatures, elucidating dominant texture directions at each scale. Str and Std do not show vertical components, i.e., altitudes, of anisotropy. Changes of anisotropy with scale categorically failed to be detected by traditional characterization methods used conventionally. These multiscale methods show clearly in several representations that anisotropy changes with scale on actual surface measurements with markedly different anisotropies. Full article
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<p>Relations between curvature principal directions <b>k<sub>1</sub></b> and <b>k<sub>2</sub></b> and normal vector and visualization of geometrical direction angles for principal direction <b>k<sub>1</sub></b> in spherical coordinates.</p>
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<p>Renderings of measured topographies of (<b>a</b>) MilledC, (<b>b</b>) µEDMed, (<b>c</b>) L-PBFed, and (<b>d</b>) MilledF. Please note that black arrows indicate visual impression of apparent anisotropy.</p>
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<p>Polar plots showing dominant directions of anisotropy with texture direction (Std) in degrees, magnitude with the complement of the texture aspect ratios (1 − Str), and scales vertically with scale number corresponding to the band numbers from <a href="#materials-13-03028-t002" class="html-table">Table 2</a>, with 1 the smallest scale as the highest, calculated for: (<b>a</b>) MilledC, (<b>b</b>) µEDMed, (<b>c</b>) L-PBFed, and (<b>d</b>) MilledF.</p>
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<p>Directions of maximum principal curvatures calculated for MilledC, µEDMed, and MilledF at two scales: 5× and 30× the original sampling interval, plotted together with color-coded height maps. Please note that red arrows indicate a direction of maximum curvature at a given location.</p>
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<p>Directions of maximum principal curvature calculated for L-PBFed at the original sampling interval. Please note that red arrows indicate a direction of maximum curvature at a given location.</p>
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<p>2D histograms created from direction cosines of maximum curvature calculated for (<b>a</b>) MilledC, (<b>b</b>) µEDMed, (<b>c</b>) L-PBFed, and (<b>d</b>) MilledF at the indicated scales.</p>
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<p>Linear histograms of maximum principal curvature directions in horizontal coordinate system (HCS), i.e., topocentric coordinates at three different scales.</p>
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<p>Logarithmic histograms of maximum principal curvature directions in horizontal coordinate system (HCS), i.e., topocentric coordinates at two different scales for the L-PBFed surface.</p>
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<p>Rosette plots created with a conventional, non-multiscale method using Fourier spectra in polar coordinates, for (<b>a</b>) MilledC, (<b>b</b>) µEDMed, (<b>c</b>) SLMed, and (<b>d</b>) MilledF.</p>
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10 pages, 1421 KiB  
Article
Removal of Composite Restoration from the Root Surface in the Cervical Region Using Er: YAG Laser and Drill—In Vitro Study
by Wojciech Zakrzewski, Maciej Dobrzynski, Piotr Kuropka, Jacek Matys, Malgorzata Malecka, Jan Kiryk, Zbigniew Rybak, Marzena Dominiak, Kinga Grzech-Lesniak, Katarzyna Wiglusz and Rafal J. Wiglusz
Materials 2020, 13(13), 3027; https://doi.org/10.3390/ma13133027 - 7 Jul 2020
Cited by 14 | Viewed by 3269
Abstract
Background: Recently, the defects of the tooth surface in the cervical region are often restored using composite filling materials. It should meet the needs of the patients regarding esthetics and material stability. The aim of the study was to analyze the tooth root [...] Read more.
Background: Recently, the defects of the tooth surface in the cervical region are often restored using composite filling materials. It should meet the needs of the patients regarding esthetics and material stability. The aim of the study was to analyze the tooth root surface at the cervical region after the removal of the composite filling material by means of the Erbium-doped Yttrium Aluminium Garnet (Er: YAG) laser or drill using the scanning electron microscopy (SEM) and fluorescence microscopy. Materials and Methods: For the purposes of this study, 14 premolar teeth (n = 14) were removed due to orthodontic reasons. The rectangular shape cavities with 3 mm in width and 1.5 mm in height were prepared with a 0.8 mm bur on high-speed contra-angle in the tooth surface just below cemento-enamel junction (CEJ) and filled with the composite material. The composite material was removed with the Er: YAG laser at a power of 3.4 W, energy 170 mJ, frequency 20 Hz, pulse duration 300 μs, tip diameter 0.8 mm, air/fluid cooling 3 mL/s, and time of irradiation: 6 sec, at a distance from teeth of 2 mm (G1 group, n = 7) or a high-speed contra-angle bur (G2 group, n = 7). After the removal of composite material, the surfaces of teeth were examined using the scanning electron microscopy (SEM) and fluorescence microscopy. Results: The Er: YAG irradiation allowed to remove completely the composite material from the tooth cavity. The study confirmed, that the ends of collagen fibers were only partially denatured after the Er: YAG laser application. Conclusion: It has been proved that using the Er: YAG laser is an effective and safe method of composite removal for the dentin surface. Full article
(This article belongs to the Collection Laser Processing for Bioengineering)
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<p>The absorption curve of water in the middle infrared region. The position of Erbium-doped Yttrium Aluminium Garnet (Er: YAG) laser (2.94 µm) used for hard-tissue ablation has been shown in the plot (based on Handbook of optical materials) [<a href="#B36-materials-13-03027" class="html-bibr">36</a>].</p>
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<p>The image of a model preparation of the root surface in the cervical region.</p>
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<p>Surfaces of teeth after laser (<b>A</b>,<b>C</b>) and drill treatment (<b>B</b>,<b>D</b>) examined by fluorescence microscope, magnification 40×.</p>
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<p>Analysis of tooth surface after laser (<b>A</b>,<b>C</b>) and drill (<b>B</b>,<b>D</b>) preparation.</p>
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11 pages, 3047 KiB  
Article
Influence of Dentine Pre-Treatment by Sandblasting with Aluminum Oxide in Adhesive Restorations. An In Vitro Study
by Bruna Sinjari, Manlio Santilli, Gianmaria D’Addazio, Imena Rexhepi, Alessia Gigante, Sergio Caputi and Tonino Traini
Materials 2020, 13(13), 3026; https://doi.org/10.3390/ma13133026 - 7 Jul 2020
Cited by 15 | Viewed by 4066
Abstract
Dentine pretreatment through sandblasting procedures has been widely studied but no curve test results are currently available. Thus, the aim herein was to in vitro compare the adhesive strength in sandblasted or not samples using a universal testing machine. Thirty -two bovine teeth [...] Read more.
Dentine pretreatment through sandblasting procedures has been widely studied but no curve test results are currently available. Thus, the aim herein was to in vitro compare the adhesive strength in sandblasted or not samples using a universal testing machine. Thirty -two bovine teeth were divided into two groups, namely test (n = 16 bars), sandblasting with aluminum oxide particles (50 µm) was performed before the adhesion procedures), and control (n = 16 bars), where no sandblasting procedure was performed. A bi-material curve test was used to evaluate the characteristics of the dentine pretreatment in terms of tensile stress and fracture strength. A scanning electron microscope (SEM) was used to analyze the fracture topography in the composite, bonding, dentin, and at the relative interfaces. The results demonstrated a statistically significant difference between the two groups in terms of tensile stress at maximum load showing values of 84.300 ± 51.342 MPa and 35.071 ± 16.609 MPa, respectively for test and control groups (p = 0.033). Moreover, a fracture strength test showed values of 18.543 ± 8.145 MPa for test and 8.186 ± 2.833 MPa for control group (p = 0.008). In conclusion, the sandblasting treatment of the dentine significantly influenced the mechanical resistance of the adhesion in this in vitro study. Full article
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<p>Sample preparation: (<b>a</b>) Detail of the crown’s cross section Shift reagent stained. Please note that this staining bonds the organic component highlighting the areas made up of dentin; (<b>b</b>) Dentine bars, size 2 × 2 × 8mm. (<b>c</b>) Sample mounted on the traction machine.</p>
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<p>Notches creation: (<b>a</b>) The red arrows indicate the pre-crack areas; (<b>b</b>) Comparison between Conventional Test and bi-material Curved Test. In Curved Test, notches (created both on the dentine and composite sides) will be the pre-cracks from which the two fracture lines originate.</p>
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<p>The graph shows the values of the two groups at Breaking Stress and at Maximum Load Stress.</p>
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<p>Scanning electron microscope (SEM) of Group 1 (Test) and Group 2 (Control): (<b>a</b>) SEM image of Group 1 at 80 × magnification. The fracture involved dentin with several direction changes; (<b>b</b>) SEM image of Group 2 at 80 × magnification. The fracture involved both dentin and the composite with direction changes; (<b>c</b>) Detail of Group 1 (interface) at 500 × magnification; (<b>d</b>) Detail of Group 2 at 500 × magnification.</p>
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<p>Scanning electron microscope images: (<b>a</b>) of Group 1 at 1.00K × magnification. At the interface there are no detachments; (<b>b</b>) SEM image of adhesive part, in detail observe the Hackle lines; (<b>c</b>) SEM image of Group 2 at 1.00K × magnification; it is shown a clear failure at the interface between dentin and adhesive; (<b>d</b>) 1.00K × magnification of both composite and dentin. sides.</p>
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17 pages, 6903 KiB  
Article
Study on the Self-Organization of an Fe-Mn-C-B Coating during Friction with Surface-Active Lubricant
by Marcin Barszcz, Mykhaylo Pashechko, Krzysztof Dziedzic and Jerzy Jozwik
Materials 2020, 13(13), 3025; https://doi.org/10.3390/ma13133025 - 6 Jul 2020
Cited by 8 | Viewed by 2126
Abstract
This paper investigates the friction process between an Fe-based coating and C45 steel with surface-active lubrication, as well as examines the coating surface before and after tribological testing. As a result, it is possible to determine whether the surface undergoes self-organization during friction. [...] Read more.
This paper investigates the friction process between an Fe-based coating and C45 steel with surface-active lubrication, as well as examines the coating surface before and after tribological testing. As a result, it is possible to determine whether the surface undergoes self-organization during friction. Coatings were produced by hardfacing a subeutectic alloy Fe-Mn-C-B modified by silicon, nickel, chromium and copper. Tribological tests were performed using a pin-on-disc tribometer. The pin (coating) and the disc made of steel C45 were subjected to heat treatment (hardening and tempering). The tests were carried out under loads of 3 MPa, 7 MPa and 10 MPa at a constant sliding velocity of 0.4 m/s and a sliding distance of 5700 m using a surface-active lubricant (glycerine oil). Obtained results were compared with the published results of previous tests carried out under the same conditions but under a load of 20 MPa. Obtained microscopic and spectroscopic results demonstrate that that the friction pair materials (the coating made of subeutectic alloy Fe-Mn-C-B modified by Si, Ni, Cr, Cu and C45 steel) and the surface-active lubricant cause self-organization during friction. The friction surface of the coatings has a flay-laminar structure and is covered with triboreaction products. The surface shows the presence of wear-resistant compounds such as oxides, carbides, borides and nitrides. Full article
(This article belongs to the Section Manufacturing Processes and Systems)
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<p>View of (<b>a</b>) modernized Amsler tribometer; (<b>b</b>) friction pair; 1—sample with a coating (pin), 2—counterbody (disk).</p>
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<p>View (<b>a</b>) Nikon Eclipse MA 200 metallurgical microscope; (<b>b</b>) FEI Quanta 3D FEG scanning electron microscope; (<b>c</b>) multi-chamber ultra-high vacuum (UHV) analytical system (Prevac); (<b>d</b>) Empyrean high-resolution X-ray diffractometer (Panalytica).</p>
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<p>Microstructure of: (<b>a</b>) coating-substrate, (<b>b</b>) coating made of Fe-Mn-C-B alloy modified by silicon, nickel, chromium and copper.</p>
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<p>Average mass loss of friction pair materials in tribological tests conducted under 3 MPa, 7 MPa, 10 MPa and 20 MPa [<a href="#B8-materials-13-03025" class="html-bibr">8</a>] and with the use of lubricant (glycerine oil).</p>
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<p>Mass loss of (<b>a</b>) samples and (<b>b</b>) counterbodies versus friction time under 3 MPa, 7 MPa, 10 MPa and 20 MPa and with glycerine oil lubrication.</p>
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<p>Mass loss of (<b>a</b>) samples and (<b>b</b>) counterbodies versus friction time under 3 MPa, 7 MPa, 10 MPa and 20 MPa and with glycerine oil lubrication.</p>
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<p>Variations in the coefficient of friction under 3 MPa, 7 MPa, 10 MPa and 20 MPa.</p>
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<p>Changes in glycerine during copper coating formation during selective transfer: Stage I (<b>a</b>), Stage II (<b>b</b>).</p>
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<p>Changes in glycerine during copper coating formation during selective transfer: Stage I (<b>a</b>), Stage II (<b>b</b>).</p>
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<p>Surface roughness of samples and counterbodies before and after friction under 10 and 20 MPa and with glycerine oil lubrication.</p>
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<p>Microscopic images of the coating surface: (<b>a</b>) before and after friction under; (<b>b</b>) 10 MPa; (<b>c</b>) 20 MPa [<a href="#B8-materials-13-03025" class="html-bibr">8</a>] and with glycerine oil lubrication.</p>
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<p>Microscopic images of the coating surface after friction with glycerine oil lubrication and under unit pressure of (<b>a</b>,<b>b</b>) 10 MPa and (<b>c</b>,<b>d</b>) 20 MPa [<a href="#B8-materials-13-03025" class="html-bibr">8</a>].</p>
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<p>Chemical composition of coating and elemental content on the friction surface and at 10 nm depth under 10 MPa and 20 MPa and with glycerine oil lubrication.</p>
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<p>Examples of XPS spectra after friction with glycerine oil lubrication and under unit pressure of (<b>a</b>,<b>b</b>) 10 MPa and (<b>c</b>,<b>d</b>) 20 MPa, as analysed (<b>a</b>,<b>c</b>) on friction trace surface and (<b>b</b>,<b>d</b>) at 10 nm distance from the surface.</p>
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<p>Examples of XPS spectra after friction with glycerine oil lubrication and under unit pressure of (<b>a</b>,<b>b</b>) 10 MPa and (<b>c</b>,<b>d</b>) 20 MPa, as analysed (<b>a</b>,<b>c</b>) on friction trace surface and (<b>b</b>,<b>d</b>) at 10 nm distance from the surface.</p>
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14 pages, 3235 KiB  
Article
Enhancement of Gas Barrier Properties of Graphene Oxide/Poly (Lactic Acid) Films Using a Solvent-free Method
by Fenfen Li, Caili Zhang, Yunxuan Weng, Xiaoqian Diao, Yingxin Zhou and Xinyu Song
Materials 2020, 13(13), 3024; https://doi.org/10.3390/ma13133024 - 6 Jul 2020
Cited by 24 | Viewed by 3249
Abstract
Graphene oxide(GO)/polylactic acid (PLA) nanocomposite, prepared using a solvent-free melt mixing processing, is investigated as a potential oxygen barrier packaging film in this work. In order to disperse GO homogeneously in PLA matrix, hydrophobic silane coupling agent, i.e., γ-(2,3-epoxypropoxy)propyltrimethoxysilane (KH560), is used to [...] Read more.
Graphene oxide(GO)/polylactic acid (PLA) nanocomposite, prepared using a solvent-free melt mixing processing, is investigated as a potential oxygen barrier packaging film in this work. In order to disperse GO homogeneously in PLA matrix, hydrophobic silane coupling agent, i.e., γ-(2,3-epoxypropoxy)propyltrimethoxysilane (KH560), is used to modify the graphene oxide sheets. The modified GO is able to be well bonded to the PLA due to the formation of covalent bonds between the epoxy groups of KH560 and the carboxyl and hydroxyl terminal groups of PLA. Furthermore, the thermal stability of GO is enhanced due to the long alkyl side chain of KH560, which could also increase the crystallinity of PLA. As a result, the crystallinity of PLA is significantly improved because of the linear KH560 chains, which can act as nucleating agents to improve the crystallization. The KH560-GO helps to reduce the O2 permeability of KH560-GO/PLA composite films via a dual-action mechanism: (1) providing physical barrier due to their native barrier properties, and (2) by resulting in higher degree of crystallinity. The as-prepared KH560-GO0.75/PLA is able to exhibit ca. 33% and ca. 13% decrease in the PO2 than the neat PLA and GO0.75/PLA film, respectively. Finally, the mechanical properties and impact fractured surfaces indicate that the increase in the tensile strength and elongation at break value of KH560-GO/PLA are due to the strong interfacial adhesion and the strong bonding between the epoxy group of KH560-GO and hydroxyl and carboxyl acid terminal groups of PLA matrix. Full article
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<p>(<b>a</b>) Raman spectra and (<b>b</b>) TGA profiles of GO powder and GO-KH560 powder.</p>
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<p>AFM image and height profiles of GO (<b>a</b>,<b>b</b>) and KH560-GO (<b>c</b>,<b>d</b>).</p>
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<p>XRD curves of (<b>a</b>) GO/PLA and (<b>b</b>) KH560-GO/PLA nanocomposites.</p>
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<p>Second heating curves of (<b>a</b>) GO/PLA and (<b>b</b>) KH560-GO/PLA nanocomposites.</p>
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<p>O<sub>2</sub> permeability of (<b>a</b>) GO/PLA and (<b>b</b>) KH560-GO/PLA samples as a function of GO and KH560-GO content.</p>
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<p>Experimental data about <span class="html-italic">P</span><sub>O2</sub> and the Bharadwaj model for the relative permeability in terms of GO and KH560-GO loadings are compared (the yellow symbols refer to GO/PLA and the blue symbols refer to KH560-GO/PLA).</p>
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<p>(<b>a</b>) stress-strain curves of GO/PLA nanocomposites, (<b>b</b>) comparison of stress-strain curves of GO0.75/PLA and KH560-GO0.75/PLA, (<b>c</b>) tensile strength and (<b>d</b>) elongation at break of GO/PLA and KH560-GO/PLA nanocomposites.</p>
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<p>SEM images of (<b>a</b>) neat PLA, (<b>b</b>) GO0.25/PLA, (<b>c</b>) GO0.75/PLA, and (<b>d</b>) GO1.0/PLA.</p>
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<p>SEM images of (<b>a</b>) GO0.75/PLA and (<b>b</b>) KH560-GO0.75/PLA.</p>
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14 pages, 4955 KiB  
Article
Potential of Mineral Fraction in Compost-Like-Output, Methods of Its Obtaining and the Possibility of Using It in the Context of Circular Economy
by Jacek Połomka and Andrzej Jędrczak
Materials 2020, 13(13), 3023; https://doi.org/10.3390/ma13133023 - 6 Jul 2020
Cited by 7 | Viewed by 2368
Abstract
Most of the systems for the mechanical and biological treatment of waste used in Poland send the 0–80 mm fraction separated from the municipal waste stream, after biostabilization, entirely to a landfill. Such action is not in line with the adopted EU strategy [...] Read more.
Most of the systems for the mechanical and biological treatment of waste used in Poland send the 0–80 mm fraction separated from the municipal waste stream, after biostabilization, entirely to a landfill. Such action is not in line with the adopted EU strategy focused on waste management in the circular cycle. The purpose of this work was to assess the technical feasibility of recovering the mineral fractions contained in compost-like-output (CLO) on the proprietary technological line designed for glass recovery. The research was launched in January 2019, and lasted for a subsequent 12 months. In the article, the amounts of mineral fractions possible to be separated from CLO are presented, as well as their morphological composition and selected properties being determined. The processing of CLO on the line allowed to recover on average 69.4 ± 7.0% of the glass. This product was accepted by glass recycling plants. Mineral fractions constituting waste from the glass separation process were tested for their use in winter road maintenance. Tests were also carried out confirming the possibility of using selected mineral fractions (0–10 mm) from CLO to obtain a waste cement mix useful for constructing road foundations using a standard amount of cement. Full article
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<p>Technological scheme of the compost-like-output (CLO) processing line.</p>
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<p>Machines used for the separation process: (<b>A</b>) ZIG ZAG Air Separator, (<b>B</b>) Autosort Laser Separator, (<b>C</b>) Combisense Chute Optical Separator, (<b>D</b>) NIHOT Air Separator.</p>
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<p>Mass and material composition of intermediate products obtained in subsequent stages of the stabilization process from Marszów and entrusted from other mechanical and biological waste treatment (MBT) systems on CLO.</p>
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<p>Mass and material composition of intermediate products obtained in subsequent stages of the stabilization process from Marszów and entrusted from other mechanical and biological waste treatment (MBT) systems on CLO.</p>
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<p>Average levels of debris and stone recovery (inert) from CLOs in subsequent stages of their treatment process ((<b>A</b>)—waste from Marszów, (<b>B</b>)—entrusted waste).</p>
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<p>Rubble and stone fractions (inert) from CLOs after the M-2 laser and after the Nihot M-4 separator.</p>
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<p>Average levels of glass recovery from CLOs in subsequent stages of their treatment process ((<b>A</b>)—waste from Marszów, (<b>B</b>)—entrusted waste).</p>
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<p>Fractions after subsequent stages of the glass recovery process from CLOs.</p>
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<p>Currently, the blocks are used successfully in ZZO Marszów.</p>
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<p>Road surface during repair and currently.</p>
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13 pages, 480 KiB  
Article
New Zirconium Diboride Polymorphs—First-Principles Calculations
by Marcin Maździarz and Tomasz Mościcki
Materials 2020, 13(13), 3022; https://doi.org/10.3390/ma13133022 - 6 Jul 2020
Cited by 8 | Viewed by 2400
Abstract
Two new hypothetical zirconium diboride (ZrB 2 ) polymorphs: (hP6-P6 3 /mmc-space group, no. 194) and (oP6-Pmmn-space group, no. 59), were thoroughly studied under the first-principles density functional theory calculations from the structural, mechanical and thermodynamic properties point of [...] Read more.
Two new hypothetical zirconium diboride (ZrB 2 ) polymorphs: (hP6-P6 3 /mmc-space group, no. 194) and (oP6-Pmmn-space group, no. 59), were thoroughly studied under the first-principles density functional theory calculations from the structural, mechanical and thermodynamic properties point of view. The proposed phases are thermodynamically stable (negative formation enthalpy). Studies of mechanical properties indicate that new polymorphs are less hard than the known phase (hP3-P6/mmm-space group, no. 191) and are not brittle. Analysis of phonon band structure and density of states (DOS) also show that the phonon modes have positive frequencies everywhere and the new ZrB 2 phases are not only mechanically but also dynamically stable. The estimated acoustic Debye temperature, Θ D , for the two new proposed ZrB 2 phases is about 760 K. The thermodynamic properties such as internal energy, free energy, entropy and constant-volume specific heat are also presented. Full article
(This article belongs to the Section Materials Simulation and Design)
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<p>ZB<math display="inline"> <semantics> <msub> <mrow/> <mn>2</mn> </msub> </semantics> </math>-Basic cells: (<b>a</b>) <span class="html-italic">hP3</span>-P6/mmm, (<b>b</b>) <span class="html-italic">hP6</span>-P6<math display="inline"> <semantics> <msub> <mrow/> <mn>3</mn> </msub> </semantics> </math>/mmc and (<b>c</b>) <span class="html-italic">oP6</span>-Pmmn.</p>
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<p>ZrB<math display="inline"> <semantics> <msub> <mrow/> <mn>2</mn> </msub> </semantics> </math>(<span class="html-italic">hP3</span>-P6/mmm-space group, no. 191)-phonon band structure and densities of states (DOS).</p>
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<p>ZrB<math display="inline"> <semantics> <msub> <mrow/> <mn>2</mn> </msub> </semantics> </math>(<span class="html-italic">hP6</span>-P6<math display="inline"> <semantics> <msub> <mrow/> <mn>3</mn> </msub> </semantics> </math>/mmc-space group, no. 194)-phonon band structure and DOS.</p>
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<p>ZrB<math display="inline"> <semantics> <msub> <mrow/> <mn>2</mn> </msub> </semantics> </math>(<span class="html-italic">oP6</span>-P6/mmm-space group, no.59)-phonon band structure and DOS.</p>
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<p>ZrB<math display="inline"> <semantics> <msub> <mrow/> <mn>2</mn> </msub> </semantics> </math>(<span class="html-italic">hP3</span>-P6/mmm-space group, no. 191)-thermodynamic properties: internal energy, free energy, entropy and constant-volume specific heat.</p>
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<p>ZrB<math display="inline"> <semantics> <msub> <mrow/> <mn>2</mn> </msub> </semantics> </math>(<span class="html-italic">hP6</span>-P6<math display="inline"> <semantics> <msub> <mrow/> <mn>3</mn> </msub> </semantics> </math>/mmc-space group, no.194)-thermodynamic properties: internal energy, free energy, entropy and constant-volume specific heat.</p>
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<p>ZrB<math display="inline"> <semantics> <msub> <mrow/> <mn>2</mn> </msub> </semantics> </math>(<span class="html-italic">oP6</span>-P6/mmm-space group, no.59)-thermodynamic properties: internal energy, free energy, entropy and constant-volume specific heat.</p>
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25 pages, 4171 KiB  
Article
Cross-Linked Polythiomethacrylate Esters Based on Naphthalene—Synthesis, Properties and Reprocessing
by Karolina Fila, Beata Podkościelna and Maciej Podgórski
Materials 2020, 13(13), 3021; https://doi.org/10.3390/ma13133021 - 6 Jul 2020
Cited by 6 | Viewed by 3185
Abstract
Two structurally different aromatic dithioesters were synthesized from two dithiols and methacryloyl chloride. The polymer networks based on methyl methacrylate and/or styrene and the new dimethacrylates were subsequently prepared. The polymerization yields of copolymers were in the range of 95–99%. The thermal and [...] Read more.
Two structurally different aromatic dithioesters were synthesized from two dithiols and methacryloyl chloride. The polymer networks based on methyl methacrylate and/or styrene and the new dimethacrylates were subsequently prepared. The polymerization yields of copolymers were in the range of 95–99%. The thermal and mechanical properties of the copolymers were determined by means of differential scanning calorimetry (DSC), thermogravimetric analysis (TG/DTG), and Shore D hardness. The addition of dithioesters—1,5-NAF-S-Met (or 1,4(1,5)-NAF-CH2S-Met) (from 0.5% to 5%) to MMA- or ST-based polymers results in lowering the glass transition temperature (Tg) by about 8 °C. The thioester-containing polymers based on MMA exhibit lower thermal stability than those with ST. The polythioesters are stable up to 250 °C. The UV/vis spectra and refractive indexes of prepared liquid compositions were also measured. The 1,5-NAF-S-Met (and 1,4(1,5)-NAF-CH2S-Met) improved the refractive index values of ST and MMA compositions. The double bond conversion was also determined for all synthesized materials. The swelling studies of polymers with 20% addition of thioester crosslinkers were investigated. For all polymeric materials with 20% addition of thioesters, depolymerization of the network was carried out by thiol-thioester exchange. The depolymerization products were re-reacted in a thiol-ene reaction with 2-hydroxyethyl methacrylate by thermal initiation. The thiol-ene procedure enabled reprocessing of starting polymers and obtaining new materials characterized by distinctly different thermal, mechanical, and swelling properties. The thiol-ene materials exhibit a lower Shore hardness in the range of 20–50 °Sh, as well as decreased Tg values when compared to starting copolymers. Due to these possible exchange reactions, one can facilely manipulate the properties of the polymers which could lead to the manufacturing of the new products with the desired features. Degradation of the cross-linked structure and recycling of copolymers were also discussed. Full article
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<p>The structures of synthesized thioesters.</p>
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<p>Scheme of thiol-thioester exchange and possible reaction pathways for the thiol-methacrylate system in our studies.</p>
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<p>The attenuated total reflectance (ATR)/FTIR spectra of poly-methyl methacrylate (MMA) and its copolymers with 5% and 20% addition of 1,5-NAF-S-Met and 1,4(1,5)-NAF-CH2S-Met.</p>
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<p>The ATR/FTIR spectra of poly-styrene (ST) and its copolymers with 5% and 20% addition of 1,5-NAF-S-Met and 1,4(1,5)-NAF-CH2S-Met.</p>
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<p>FTIR spectra of 1,5-NAF-S-Met polymers: (<b>A</b>) copolymers with MMA; (<b>B</b>) copolymers with ST.</p>
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<p>FTIR spectra of 1,4(1,5)-NAF-CH<sub>2</sub>S-Met polymers: (<b>A</b>) copolymers with MMA; (<b>B</b>) copolymers with ST.</p>
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<p>Influence of various addition of 1,5-NAF-S-Met on the glass transition temperature (T<sub>g</sub>) values of MMA- (<b>A</b>) or ST- based (<b>B</b>) polymers.</p>
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<p>Influence of various addition of 1,4(1,5)-NAF-CH<sub>2</sub>S-Met on the T<sub>g</sub> values of MMA- (<b>A</b>) or ST- based (<b>B</b>) polymers.</p>
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<p>The TG (<b>A</b>) and DTG (<b>B</b>) curves of poly-MMA and its copolymers with 5% and 20% content of 1,5-NAF-S-Met and 1,4(1,5)-NAF-CH<sub>2</sub>S-Met.</p>
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<p>The TG (<b>A</b>) and DTG (<b>B</b>) curves of poly-ST and its copolymers with 5% and 20% content of 1,5-NAF-S-Met and 1,4(1,5)-NAF-CH<sub>2</sub>S-Met.</p>
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<p>The UV/vis transmittance spectra of the prepared liquid compositions with the different addition of dithioesters: MMA+1,5-NAF-S-Met (<b>A</b>), MMA+1,4(1,5)-NAF-CH<sub>2</sub>S-Met (<b>B</b>), ST+1,5-NAF-S-Met (<b>C</b>), and ST+1,4(1,5)-NAF-CH<sub>2</sub>S-Met (<b>D</b>).</p>
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<p>The values of Shore hardness tests of obtained cross-linked polymers with addition of 1,5-NAF-S-Met (<b>A</b>) and 1,4(1,5)-NAF-CH<sub>2</sub>S-Met (<b>B</b>).</p>
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<p>The swelling coefficients of obtained MMA and ST polymers with 20% addition of1,5-NAF-S-Met and 1,4(1,5)-NAF-CH<sub>2</sub>S-Met.</p>
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<p>ATR/FT-IR spectra of ST (1a–c) and MMA (2a–c) copolymers.</p>
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<p>ATR/FT-IR spectra of ST (3a–c) and MMA (4a–c) copolymers.</p>
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<p>ATR/FT-IR spectra of 4,4′-thiobisbenzenethiol (TBT) and 2-hydroxyethyl methacrylate (HEMA).</p>
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<p>Images of materials obtained with ST (3a–c) and MMA (4a–c) copolymers with 1,4(1,5)-NAF-CH<sub>2</sub>S-Met.</p>
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<p>Differential scanning calorimetry (DSC) curves of starting (1a, 2a, 3a, 4a) and new (1c, 2c, 3c, 4c) materials obtained after thiol-ene reactions with HEMA.</p>
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15 pages, 2864 KiB  
Article
Carbonyl-Terminated Quinoidal Oligothiophenes as p-Type Organic Semiconductors
by Takato Asoh, Kohsuke Kawabata and Kazuo Takimiya
Materials 2020, 13(13), 3020; https://doi.org/10.3390/ma13133020 - 6 Jul 2020
Cited by 7 | Viewed by 3394
Abstract
A series of quinoidal oligothiophenes terminated with carbonyl groups (nTDs, n = 2–4) are studied as p-type organic semiconductors for the active materials in organic field-effect transistors (OFETs) both by the theoretical and experimental approaches. The theoretical calculations clearly show their [...] Read more.
A series of quinoidal oligothiophenes terminated with carbonyl groups (nTDs, n = 2–4) are studied as p-type organic semiconductors for the active materials in organic field-effect transistors (OFETs) both by the theoretical and experimental approaches. The theoretical calculations clearly show their high-lying highest occupied molecular orbital (HOMO) energy levels (EHOMOs), small reorganization energies for hole transport (λholes), and large contribution of sulfur atoms to HOMOs, all of which are desirable for p-type organic semiconductors. Thus, we synthesized nTDs from the corresponding aromatic oligothiophene precursors and then evaluated their physicochemical properties and structural properties. These experimental evaluations of nTDs nicely proved the theoretical predictions, and the largest 4TDs in the series (4,4′′′-dihexyl- and 3′,4,4″,4′′′-tetrahexyl-5H,5′′′H-[2,2′:5′,2″:5″,2′′′-quaterthiophene]-5,5′′′-dione) can afford solution-processed OFETs showing unipolar p-type behaviors and hole mobility as high as 0.026 cm2 V−1 s−1. Full article
(This article belongs to the Special Issue Organic Transistors: Current Status and Opportunities)
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<p>Molecular structures of carbonyl-terminated quinoidal oligothiophenes in this study.</p>
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<p>HOMOs and LUMOs of (E)-2TD, (EE)-3TD, (EEE)-4TDa, (EEE)-4TDb, 2T, 3T, and 4T.</p>
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<p>Molecular structures and the bond lengths (Å) of (<span class="html-italic">E</span>)-2TD (<b>a</b>,<b>c</b>) and (<span class="html-italic">ZEZ</span>)-4TDa (<b>b,d</b>) elucidated by single-crystal X-ray analyses. The alkyl groups are omitted for clarity.</p>
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<p>Cyclic voltammograms of <span class="html-italic">n</span>TDs. Dotted voltammograms were recorded by reversing the scanning direction after the first oxidation.</p>
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<p>UV-vis absorption of <span class="html-italic">n</span>TDs in chloroform solution (<b>a</b>) and in thin film (<b>b</b>).</p>
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<p>Packing structure and transfer integrals for hole transport of (<span class="html-italic">E</span>)-2TD (<b>a</b>,<b>b</b>) and (<span class="html-italic">ZEZ</span>)-4TDa (<b>c</b>,<b>d</b>). Alkyl groups were omitted for clarity in (<b>b</b>,<b>d</b>).</p>
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<p>Output and transfer curves, gate-voltage-dependent mobilities of 4TDa (<b>a</b>–<b>c</b>) and 4TDb (<b>d</b>–<b>f</b>), respectively.</p>
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<p>Out-of-plane X-ray diffraction patterns of spin-coated films of 4TDa and 4TDb.</p>
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<p>Synthesis of <span class="html-italic">n</span>TDs.</p>
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14 pages, 7690 KiB  
Article
The Stress Concentration Mechanism of Pores Affecting the Tensile Properties in Vacuum Die Casting Metals
by Hanxue Cao, Ziwei Luo, Chengcheng Wang, Jing Wang, Tao Hu, Lang Xiao and Junqi Che
Materials 2020, 13(13), 3019; https://doi.org/10.3390/ma13133019 - 6 Jul 2020
Cited by 23 | Viewed by 3106
Abstract
The absolute pressure strongly affects the porosity and mechanical properties of castings produced by vacuum high-pressure die casting (V-HPDC) technology. The pore size, quantity and distribution of AlSi9Cu3 samples under three absolute pressures were evaluated by X-ray tomography and optical [...] Read more.
The absolute pressure strongly affects the porosity and mechanical properties of castings produced by vacuum high-pressure die casting (V-HPDC) technology. The pore size, quantity and distribution of AlSi9Cu3 samples under three absolute pressures were evaluated by X-ray tomography and optical and electron microscopy. The paper presents an elaboration the stress concentration mechanism of pores affecting the tensile properties. According to a mathematical analysis of a sample under uniaxial stress, the greater the radius of the pore, the higher the stress value is at the pore perimeter. When the absolute pressure drops from 1013 mbar to 100 mbar, the porosity decreases from 6.8% to 2.8%, and the pore number and mean size decreases. In tensile tests, the pore sizes of the fracture surface decrease with decreasing absolute pressure, and the pore distribution becomes uniform. The tensile properties and extensibility of the sample are improved, and the microscopic fracture surface of the sample changes from cleavage fracture to quasi-cleavage fracture. The number, size and distribution of pores in die casting collectively affect the properties of the sample. Large-size or complex pores or pores with concentrated distributions produce large stress concentrations, decreasing the strength of the metal. Full article
(This article belongs to the Section Materials Physics)
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<p>The three-dimensional diagram of engine cylinder blocks.</p>
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<p>The dimensions of the tensile sample.</p>
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<p>Full microscope images of samples under different degrees of vacuum: (<b>a</b>) 1013 mbar, (<b>b</b>) 200 mbar and (<b>c</b>) 100 mbar.</p>
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<p>The calculation results of the pore numbers and dimensions.</p>
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<p>Comparison of porosity microstructure in samples: (<b>a</b>) OM image at 1013 mbar; (<b>b</b>) X-ray image at 1013 mbar; (<b>c</b>) OM image at 200 mbar; (<b>d</b>) X-ray image at 200 mbar; (<b>e</b>) OM image at 100 mbar; (<b>f</b>) X-ray imaging at 100 mbar.</p>
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<p>Tensile strength and elongation at different absolute pressures: (<b>a</b>) tensile strength and (<b>b</b>) elongation.</p>
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<p>SEM images of tensile fracture morphologies of samples cast under different absolute pressures: (<b>a</b>), (<b>b</b>) 1013 mbar; (<b>c</b>), (<b>d</b>) 200 mbar and (<b>e</b>), (<b>f</b>) 100 mbar.</p>
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<p>Isostress diagram of circular pores under tension: (<b>a</b>): <math display="inline"><semantics> <mrow> <msub> <mi>τ</mi> <mrow> <mi>m</mi> <mi>a</mi> <mi>x</mi> </mrow> </msub> </mrow> </semantics></math> and (<b>b</b>): <math display="inline"><semantics> <mrow> <msub> <mi>σ</mi> <mrow> <mi>m</mi> <mi>a</mi> <mi>x</mi> </mrow> </msub> </mrow> </semantics></math> and (<b>c</b>): <math display="inline"><semantics> <mrow> <msub> <mi>σ</mi> <mrow> <mi>m</mi> <mi>i</mi> <mi>n</mi> </mrow> </msub> </mrow> </semantics></math>.</p>
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<p>Principal stress trajectory of a circular pore under tension.</p>
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11 pages, 2584 KiB  
Article
Effects of a New Type of Shrinkage-Reducing Agent on Concrete Properties
by Mari Masanaga, Tsuyoshi Hirata, Hirokatsu Kawakami, Yuka Morinaga, Toyoharu Nawa and Yogarajah Elakneswaran
Materials 2020, 13(13), 3018; https://doi.org/10.3390/ma13133018 - 6 Jul 2020
Cited by 9 | Viewed by 2737
Abstract
Shrinkage-reducing agents have been developed to mitigate shrinkage and to control cracks in concrete. This study aims to evaluate the impact of a newly developed shrinkage-reducing agent (N-SRA) on concrete properties and to compare its properties with a conventional shrinkage-reducing agent (C-SRA). The [...] Read more.
Shrinkage-reducing agents have been developed to mitigate shrinkage and to control cracks in concrete. This study aims to evaluate the impact of a newly developed shrinkage-reducing agent (N-SRA) on concrete properties and to compare its properties with a conventional shrinkage-reducing agent (C-SRA). The hydration rate, compressive strength, splitting tensile strength, shrinkage, occurrence of cracking, and freezing and thawing were investigated. N-SRA showed higher surface tension than C-SRA and reduced shrinkage to the same degree as C-SRA with half the dosage of C-SRA. The addition of N-SRA or C-SRA did not influence the early compressive strength but slightly reduced splitting tensile strength at seven days. Concrete with N-SRA showed higher compressive strength at 28 days than those of concrete with C-SRA or without SRA. Furthermore, concrete with N-SRA extended the period for the occurrence of shrinkage cracking under restrained conditions. It was found that N-SRA provided excellent freezing and thawing resistance because of the formation of good air voids, while C-SRA demonstrated inefficient behaviour in such an environment. Full article
(This article belongs to the Special Issue Innovative Materials for Construction)
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<p>Grading curves for fine and coarse aggregates.</p>
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<p>Schematic diagram of specimen for restrained shrinkage cracking test.</p>
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<p>Surface tension of newly developed (N-SRA) and conventional (C-SRA) shrinkage-reducing agent in deionic water.</p>
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<p>Calorimetric curve during the initial cement hydration.</p>
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<p>(<b>A</b>) Compressive strength and (<b>B</b>) splitting tensile strength of concrete with N-SRA and C-SRA compared with reference.</p>
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<p>Total hydration degree of cement paste hydrated for three and nine weeks with and without N-SRA.</p>
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<p>Free shrinkage strain of N-SRA and C-SRA.</p>
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<p>Relationships of restrained stress of reinforced steel and drying age. (<b>A</b>) Specimen 1 (<b>B</b>) Specimen 2.</p>
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<p>Resistance to restrained shrinkage cracking for concrete with N-SRA or C-SRA.</p>
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<p>Freezing and thawing test results.</p>
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17 pages, 10496 KiB  
Article
The Effects of Micro-Segregation on Isothermal Transformed Nano Bainitic Microstructure and Mechanical Properties in Laser Cladded Coatings
by Yanbing Guo, Zhuguo Li, Liqun Li and Kai Feng
Materials 2020, 13(13), 3017; https://doi.org/10.3390/ma13133017 - 6 Jul 2020
Cited by 3 | Viewed by 2427
Abstract
The design of metastable retained austenite is the key issue to obtain nano bainitic steel with high strength and toughness. In this study, nanostructured Fe-based bainitic coatings were fabricated using laser cladding and following isothermal heat treatment. The microstructures and mechanical properties of [...] Read more.
The design of metastable retained austenite is the key issue to obtain nano bainitic steel with high strength and toughness. In this study, nanostructured Fe-based bainitic coatings were fabricated using laser cladding and following isothermal heat treatment. The microstructures and mechanical properties of the laser cladded coating were investigated. The results show that the Mn, Cr, Co, and Al segregated at the solidified prior grain boundaries. The micro-segregation of the solutes strongly influenced the stability of the austenite. As the isothermal temperature decreases, the interface of the bainite and blocky retained austenite approach to the prior interdendritic regions with the decreasing isothermal temperature, and the final volume fraction also decreases. The volume fractions of each phase and microstructure morphology of the coatings were determined by the interdendritic micro-segregation and isothermal temperatures. The stability of the blocky retained austenite distributed at the interdendritic area was lower than that of film and island-like morphology. This phenomenon contributed to the ductile and tough nano bainitic coatings with tunable mechanical properties. Full article
(This article belongs to the Special Issue Advanced Surface Treatment Technologies for Metallic Alloys)
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<p>The appearance of the coating and the tensile test specimen.</p>
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<p>The profile of the laser cladded coating (<b>a</b>), and detailed images of the isothermal microstructures in the center region observed by OM (<b>b</b>) and SEM (<b>c</b>).</p>
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<p>(<b>a</b>) A composite map of elements segregation across the interdendritic region. The white line represents the area incorporated into the vertically integrated line scanning shown in (<b>b</b>).</p>
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<p>SEM morphologies of microstructure: (<b>a</b>) 200 °C transformed for 24 h, (<b>b</b>) 250 °C transformed for 16 h, (<b>c</b>) 300 °C transformed for 8 h.</p>
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<p>Schematic diagram of the interdendritic segregation effect on bainite and retained austenite distribution under different isothermal temperature (PRAG means the prior austenite grain).</p>
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<p>Magnified scanning electron micrographs of the inner dendrite regions in the coatings (<b>a</b>) obtained at 200 °C for 24 h, (<b>b</b>) obtained at 250 °C for 16 h, (<b>c</b>) obtained at 300 °C for 8 h.</p>
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<p>Typical TEM micrograph of the bainite transformed at (<b>a</b>) 200 °C, (<b>b</b>) 250 °C, and (<b>c</b>) 300 °C.</p>
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<p>TEM images of the stacking fault bundles in the blocky RA of the 200 °C: (<b>a</b>) bright-field image, (<b>b</b>) dark-field images, and (<b>c</b>) SAED pattern.</p>
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<p>TEM morphology of ε-martensite in 200 °C transformed coating: (<b>a</b>) bright. field image, (<b>b</b>) SAED pattern.</p>
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<p>The XRD patterns of the isothermal transformed coatings (<b>a</b>), detailed of XRD patterns from 40° to 55° (<b>b</b>).</p>
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<p>Nano-hardness load-displacement curves, the corresponding distributions of the nano-indentation hardness and elastic modulus in the nano bainitic coatings obtained at 200 °C (<b>a</b>–<b>c</b>); 250 °C (<b>d</b>–<b>f</b>); 300 °C (<b>h</b>–<b>j</b>).</p>
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<p>Mechanical properties of the laser cladded bainitic coatings.</p>
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<p>Typical tensile fractography of (<b>a</b>) the coatings obtained at 200 °C, and (<b>b</b>) the coatings obtained at 250 °C, and (<b>c</b>) the coatings obtained at 300 °C.</p>
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<p>The micro-crack in the microstructure under the water cooling and the ε-martensite in the blocky austenite (<b>a</b>), the magnified view of the cracks (<b>b</b>).</p>
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16 pages, 1867 KiB  
Article
Energy Localization through Locally Resonant Materials
by Marco Moscatelli, Claudia Comi and Jean-Jacques Marigo
Materials 2020, 13(13), 3016; https://doi.org/10.3390/ma13133016 - 6 Jul 2020
Cited by 5 | Viewed by 2079
Abstract
Among the attractive properties of metamaterials, the capability of focusing and localizing waves has recently attracted research interest to establish novel energy harvester configurations. In the same frame, in this work, we develop and optimize a system for concentrating mechanical energy carried by [...] Read more.
Among the attractive properties of metamaterials, the capability of focusing and localizing waves has recently attracted research interest to establish novel energy harvester configurations. In the same frame, in this work, we develop and optimize a system for concentrating mechanical energy carried by elastic anti-plane waves. The system, resembling a Fabry-Pérot interferometer, has two barriers composed of Locally Resonant Materials (LRMs) and separated by a homogeneous internal cavity. The attenuation properties of the LRMs allow for the localization of waves propagating at particular frequencies. With proper assumptions on the specific ternary LRMs, the separation of scales (between the considered wave lengths and the characteristic dimension of the employed unit cells) enables the use of a two-scale asymptotic technique for computing the effective behavior of the employed LRMs. This leads to a complete analytic description of the motion of the system. Here we report the results achieved by optimizing the geometry of the system for obtaining a maximum focusing of the incoming mechanical energy. The analytic results are then validated through numerical simulations. Full article
(This article belongs to the Special Issue Advanced Locally Resonant Materials)
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Figure 1
<p>Top-view of the studied system. The wave shown in the figure represents an out-of-plane wave propagating throughout all the five domains. The dots denote the fact that the system must be extended along the <math display="inline"><semantics> <msub> <mi>x</mi> <mn>2</mn> </msub> </semantics></math> direction.</p>
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<p>Lattice of the LRM and zoom over a unit cell composing it. <math display="inline"><semantics> <msub> <mi>R</mi> <mi>f</mi> </msub> </semantics></math> and <math display="inline"><semantics> <msub> <mi>R</mi> <mi>c</mi> </msub> </semantics></math> are respectively the fiber and coating external radii.</p>
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<p>One-dimensional counterpart of the two-dimensional homogenized problem. The system is simplified by fixing a position along the <math display="inline"><semantics> <msub> <mi>x</mi> <mn>2</mn> </msub> </semantics></math> axis and by considering <math display="inline"><semantics> <mrow> <msub> <mi>x</mi> <mn>1</mn> </msub> <mo>=</mo> <mi>x</mi> </mrow> </semantics></math>. The dashed ends are used to indicate that the domain is infinitely extended toward <math display="inline"><semantics> <mrow> <mo>−</mo> <mo>∞</mo> </mrow> </semantics></math> and <math display="inline"><semantics> <mrow> <mo>+</mo> <mo>∞</mo> </mrow> </semantics></math>.</p>
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<p>Sketch of the studied limit case. The barriers are infinitely extended toward <math display="inline"><semantics> <mrow> <mo>−</mo> <mo>∞</mo> </mrow> </semantics></math> and <math display="inline"><semantics> <mrow> <mo>+</mo> <mo>∞</mo> </mrow> </semantics></math>.</p>
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<p>(<b>a</b>) Effective mass density vs. frequency, shaded areas correspond to negative effective mass, (<b>b</b>) dispersion plot with shaded band gaps obtained from the numerical Bloch-Floquet’s analysis; Irreducible Brillouin Zone and path followed for the numerical analysis is reported in the inset.</p>
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<p>Ratio of the averaged mechanical energy density along the whole system, with respect to the incoming one. Orange: analytic results and blue: numerical results. Each part composing the REH is separated by the vertical dashed lines.</p>
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<p>Transmission coefficient modulus <math display="inline"><semantics> <mrow> <mo>|</mo> <mi mathvariant="sans-serif">T</mi> <mo>|</mo> </mrow> </semantics></math> as a function of the frequency <math display="inline"><semantics> <mrow> <mi>ω</mi> </mrow> </semantics></math> in presence of the cavity (<b>a</b>) and without any cavity (<b>b</b>). The vertical red lines define the band gap. Orange: analytic results and blue: numerical results of analyses in the frequency domain, considering a sweep of frequencies from 0 to 20 KHz.</p>
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<p>First (<b>a</b>) and second (<b>b</b>) optimal <math display="inline"><semantics> <mrow> <msub> <mover accent="true"> <mi>d</mi> <mo>˜</mo> </mover> <mi>n</mi> </msub> </mrow> </semantics></math> plotted with respect to the the frequency <math display="inline"><semantics> <mrow> <mi>ω</mi> </mrow> </semantics></math> inside the first band gap and the width <span class="html-italic">l</span> of the barriers.</p>
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<p>The contours (<b>a</b>,<b>b</b>) show respectively the indexes IC and the AIC for the first optimal cavity widths <math display="inline"><semantics> <mrow> <mn>2</mn> <msub> <mover accent="true"> <mi>d</mi> <mo>˜</mo> </mover> <mn>1</mn> </msub> </mrow> </semantics></math> while (<b>c</b>,<b>d</b>) for the second optimal cavity widths <math display="inline"><semantics> <mrow> <mn>2</mn> <msub> <mover accent="true"> <mi>d</mi> <mo>˜</mo> </mover> <mn>2</mn> </msub> </mrow> </semantics></math>. The plots are obtained using analytic expressions.</p>
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<p>Each panel (<b>a</b>–<b>d</b>) shows the index IC on the first row and AIC on the second row, for the first optimal cavitywidths <math display="inline"><semantics> <mrow> <mn>2</mn> <msub> <mover accent="true"> <mi>d</mi> <mo>˜</mo> </mover> <mn>1</mn> </msub> </mrow> </semantics></math>. The following geometrical dimensions are used: (<b>a</b>) <math display="inline"><semantics> <mrow> <msub> <mi>R</mi> <mi>c</mi> </msub> <mo>=</mo> <mn>0.475</mn> <mi>L</mi> <mo>,</mo> <msub> <mi>R</mi> <mi>f</mi> </msub> <mo>=</mo> <mn>0.9</mn> <msub> <mi>R</mi> <mi>c</mi> </msub> <mo>,</mo> </mrow> </semantics></math> (<b>b</b>) <math display="inline"><semantics> <mrow> <msub> <mi>R</mi> <mi>c</mi> </msub> <mo>=</mo> <mn>0.475</mn> <mi>L</mi> <mo>,</mo> <msub> <mi>R</mi> <mi>f</mi> </msub> <mo>=</mo> <mn>0.4</mn> <msub> <mi>R</mi> <mi>c</mi> </msub> <mo>,</mo> </mrow> </semantics></math> (<b>c</b>) <math display="inline"><semantics> <mrow> <msub> <mi>R</mi> <mi>c</mi> </msub> <mo>=</mo> <mn>0.355</mn> <mi>L</mi> <mo>,</mo> <msub> <mi>R</mi> <mi>f</mi> </msub> <mo>=</mo> <mn>0.9</mn> <msub> <mi>R</mi> <mi>c</mi> </msub> <mo>,</mo> </mrow> </semantics></math> and (<b>d</b>) <math display="inline"><semantics> <mrow> <msub> <mi>R</mi> <mi>c</mi> </msub> <mo>=</mo> <mn>0.355</mn> <mi>L</mi> <mo>,</mo> <msub> <mi>R</mi> <mi>f</mi> </msub> <mo>=</mo> <mn>0.4</mn> <msub> <mi>R</mi> <mi>c</mi> </msub> </mrow> </semantics></math>.</p>
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19 pages, 6006 KiB  
Article
Experimental Study on Mechanical and Functional Properties of Reduced Graphene Oxide/Cement Composites
by Ning Zhang, Wei She, Fengyin Du and Kaili Xu
Materials 2020, 13(13), 3015; https://doi.org/10.3390/ma13133015 - 6 Jul 2020
Cited by 42 | Viewed by 3291
Abstract
This study develops a novel self-sensing cement composite by simply mixing reduced graphene oxide (rGO) in cementitious material. The experimental results indicate that, owing to the excellent dispersion method, the nucleation and two-dimensional morphological effect of rGO optimizes the microstructure inside cement-based material. [...] Read more.
This study develops a novel self-sensing cement composite by simply mixing reduced graphene oxide (rGO) in cementitious material. The experimental results indicate that, owing to the excellent dispersion method, the nucleation and two-dimensional morphological effect of rGO optimizes the microstructure inside cement-based material. This would increase the electric conductivity, thermal property and self-induction system of cement material, making it much easier for cementitious material to better warn about impending damage. The use of rGO can improve the electric conductivity and electric shielding property of rGO-paste by 23% and 45%. The remarkable enhancement was that the voltage change rate of 1.00 wt.%-rGO paste under six-cycle loads increased from 4% to 12.6%, with strain sensitivity up to 363.10, without compromising the mechanical properties. The maximum compressive strength of the rGO-mortar can be increased from 55 MPa to 71 MPa. In conclusion, the research findings provide an effective strategy to functionalize cement materials by mixing rGO and to achieve the stronger electric shielding property and higher-pressure sensitivity of rGO–cement composites, leading to the development of a novel high strength self-sensing cement material with a flexural strength up to 49%. Full article
(This article belongs to the Special Issue Concrete and Construction Materials)
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<p>The size distribution of reduced graphene oxide (rGO).</p>
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<p>The preparation process of samples.</p>
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<p>Preparation of specimen.</p>
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<p>The test device of pressure sensitivity.</p>
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<p>The mechanical properties of cement mortar with different ages and rGO content, (<b>a</b>) Compressive strength, (<b>b</b>) Flexural strength.</p>
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<p>The porosity of cement mortar with different rGO content.</p>
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<p>The pore size distribution pf slurry with different rGO content.</p>
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<p>The relationship between electrical resistivity and rGO content.</p>
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<p>The thermal conductivity coefficient of different cement mortar.</p>
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<p>The schematic analysis of electromagnetic shielding mechanism.</p>
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<p>The shielding effectiveness of cement paste with rGO.</p>
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<p>The electromagnetic parameters of cement paste with different rGO. (<b>a</b>) real part of dielectric conductivity (<b>b</b>) imaginary part of dielectric conductivity; (<b>c</b>) real part of magnetic conductivity (<b>d</b>) imaginary part of maginary conductivity.</p>
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<p>Voltage change ratio and pressure stress of different rGO–pastes under six-cycle loading (<b>a</b>) 0 wt.% rGO (<b>b</b>) 0.05 wt.% rGO (<b>c</b>) 0.5 wt.% rGO (<b>d</b>) 1 wt.% rGO (<b>e</b>) 2 wt.% rGO (<b>f</b>) 4 wt.% rGO.</p>
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<p>Voltage change ratio and pressure stress of different rGO–pastes under six-cycle loading (<b>a</b>) 0 wt.% rGO (<b>b</b>) 0.05 wt.% rGO (<b>c</b>) 0.5 wt.% rGO (<b>d</b>) 1 wt.% rGO (<b>e</b>) 2 wt.% rGO (<b>f</b>) 4 wt.% rGO.</p>
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<p>The relationship between maximum voltage change ratio and rGO content.</p>
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<p>Stress and strain sensitivity coefficients of pastes with different rGO content (<b>a</b>) stress (<b>b</b>) strain.</p>
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<p>The voltage change ratio and pressure stress of different rGO–mortars under six-cycle loading (<b>a</b>) 0 wt.% rGO, (<b>b</b>) 0.05 wt.% rGO, (<b>c</b>) 0.5 wt.% rGO, (<b>d</b>) 1.0 wt.% rGO, (<b>e</b>) 2.0 wt.% rGO, (<b>f</b>) 4.0 wt.% rGO.</p>
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<p>The voltage change ratio and pressure stress of different rGO–mortars under six-cycle loading (<b>a</b>) 0 wt.% rGO, (<b>b</b>) 0.05 wt.% rGO, (<b>c</b>) 0.5 wt.% rGO, (<b>d</b>) 1.0 wt.% rGO, (<b>e</b>) 2.0 wt.% rGO, (<b>f</b>) 4.0 wt.% rGO.</p>
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<p>The relationship between the voltage change ratio and rGO content.</p>
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<p>The stress and strain sensitivity coefficients of different rGO–mortars (<b>a</b>) stress (<b>b</b>) strain.</p>
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<p>The schematic diagram of pressure sensitive performance of rGO composites.</p>
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<p>SEM photographs of cement paste with 1.00 wt.% rGO (<b>a</b>) rGO (<b>b</b>) paste (<b>c</b>) area ① (<b>d</b>) magnifying view of area ① (<b>e</b>) area ② (<b>f</b>) magnifying view of area ②.</p>
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<p>SEM photographs of cement paste with 4.00 wt.% rGO, (<b>a</b>) rGO (<b>b</b>) paste (<b>c</b>) area ② (<b>d</b>) magnified view of area ②.</p>
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12 pages, 1975 KiB  
Article
The Luminescence of 1,8-Diazafluoren-9-One/Titanium Dioxide Composite Thin Films for Optical Application
by Aneta Lewkowicz, Robert Bogdanowicz, Piotr Bojarski, Mattia Pierpaoli, Ignacy Gryczyński, Anna Synak, Michał Mońka, Jakub Karczewski, Wiktoria Struck-Lewicka, Renata Wawrzyniak and Michał J. Markuszewski
Materials 2020, 13(13), 3014; https://doi.org/10.3390/ma13133014 - 6 Jul 2020
Cited by 6 | Viewed by 2904
Abstract
The investigation of innovative label-free α-amino acids detection methods represents a crucial step for the early diagnosis of several diseases. While 1,8-diazafluoren-9-one (DFO) is known in forensic application because of the fluorescent products by reacting with the amino acids present in the papillary [...] Read more.
The investigation of innovative label-free α-amino acids detection methods represents a crucial step for the early diagnosis of several diseases. While 1,8-diazafluoren-9-one (DFO) is known in forensic application because of the fluorescent products by reacting with the amino acids present in the papillary exudate, its application for diagnostic purposes has not been fully investigated. The stabilization of DFO over a transparent substrate allows its complexation with biomolecules for the detection of α-amino acids. In this study, DFO was immobilized into a titanium dioxide (TiO2) matrix for the fluorescence detection of glycine, as a target α-amino acid (a potential marker of the urogenital tract cancers). The DFO/TiO2 composite was characterized by atomic force microscopy, spectroscopic ellipsometry, fluorescence spectroscopy and fluorescence microscopy. The performed fluorescent studies indicate spectacular formation of aggregates at higher concentration. The measurements performed using various fluorescence and microscopic techniques together with the suitable analysis show that the aggregates are able to emit short-lived fluorescence. Full article
(This article belongs to the Special Issue Hybrid and Composite Coatings and Thin Films)
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<p>AFM image of thin films of: (<b>a</b>) TiO<sub>2</sub>; (<b>b</b>) 10<sup>−5</sup>M DFO/TiO<sub>2</sub>; and (<b>c</b>) 2·10<sup>−2</sup> M DFO/TiO<sub>2</sub>.</p>
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<p>The variation of optical constants of DFO/TiO<sub>2</sub> thin nanocomposite films as a function of DFO dye concentration.</p>
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<p>Time-resolved emission spectra of DFO/TiO<sub>2</sub> thin films at several DFO concentrations ((<b>a</b>,<b>d</b>) 2 × 10<sup>−2</sup> [M] DFO/TiO<sub>2</sub>; (<b>b</b>,<b>e</b>) 1 × 10<sup>−5</sup> [M] DFO/TiO<sub>2</sub>; and (<b>c</b>,<b>f</b>) 0 [M]DFO/TiO<sub>2</sub>) at room temperature (T = 293 K). The excitation wavelength was 380 nm.</p>
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<p>(<b>a</b>) Reaction of DFO with α-amino acids: The hemiketal attack from the nitrogen of amino acid at the electron-deficient carbon; after the loss of water, the imine is formed, which maintains the alkyl fragment from the amino acid and decarboxylation to form (IV). Hydrolysis shows at the nitrogen-carbon double bond formatting of an aromatic amine (V) and acetaldehyde and reacts with another DFO molecule to create 9-(1,8-diazafluoren-9-ylidene)amino-1,8-diazafluorenone (VI) [<a href="#B40-materials-13-03014" class="html-bibr">40</a>]. (<b>b</b>) Fluorescence micrograph of DFO in TiO<sub>2</sub> thin films at different DFO concentrations after reacting with glycine, with λ<sub>exc</sub> = 450 nm.</p>
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19 pages, 10952 KiB  
Article
Microstructure and Charpy Impact Toughness of a 2.25Cr-1Mo-0.25V Steel Weld Metal
by Kefan Wu, Yingjie Yan, Rui Cao, Xinyu Li, Yong Jiang, Fei Yang, Xingwang Jia and Jianhong Chen
Materials 2020, 13(13), 3013; https://doi.org/10.3390/ma13133013 - 6 Jul 2020
Cited by 13 | Viewed by 3274
Abstract
The demand for heat-resistant steel has increased owing to its utility in numerous devices that must withstand high steam pressures and high temperatures, such as turbine rotors and blades in ultra-supercritical power plants. It is inevitable to join heat-resistance steel part by welding [...] Read more.
The demand for heat-resistant steel has increased owing to its utility in numerous devices that must withstand high steam pressures and high temperatures, such as turbine rotors and blades in ultra-supercritical power plants. It is inevitable to join heat-resistance steel part by welding method, so it is important to maintain the toughness of the weld metals. In this study, the microstructure, low-temperature impact toughness, and fracture surface of as-welded and post-weld heat treatment (PWHT) of 2.25Cr-1Mo-0.25V weld metal were investigated. The microstructures of the as-welded and PWHT specimens are granular bainite and ferrite, respectively. This work revealed the relationship between effective microstructure nearby crack initiation origin and low temperature impact toughness for both the as-welded and PWHT specimens. The evolution of the microstructure and prior austenite was then investigated using confocal laser scanning microscopy (CLSM) to observe the formation of coarse ferrite grain structures. A suggestion for enhancing the low-temperature toughness was provided based on the effect of adjusting Mn content and forming acicular ferrite. Full article
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Figure 1
<p>Schematic diagrams of (<b>a</b>) multi-layer multi-pass welding welded joint and (<b>b</b>) welded joint sampling impact specimen.</p>
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<p>Thermal expansion curve of as-welded specimen.</p>
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<p>Schematic of metallographic sections from the fractured impact specimens, (<b>a</b>) the cutting cross-section parallel to the notch for observation of microstructure nearby fracture initiation, (<b>b</b>) the cutting vertical-section perpendicular to the notch for the observation of the retained cracks</p>
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<p>Microstructure of the weld metal for (<b>a</b>) as-welded and (<b>b</b>) post-weld heat treatment (PWHT) specimens; high magnification images of the weld metal for (<b>c</b>) as-welded and (<b>d</b>) PWHT specimens.</p>
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<p>Microstructure of the weld metal for (<b>a</b>) as-welded and (<b>b</b>) post-weld heat treatment (PWHT) specimens; high magnification images of the weld metal for (<b>c</b>) as-welded and (<b>d</b>) PWHT specimens.</p>
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<p>Hardness of the weld metal for as-welded and PWHT specimens.</p>
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<p>Macro-fracture surface showing the integrating measurements of stretch zone width (SZW), fibrous crack length (SCL), and the x<sub>f</sub> from PWHT specimen.</p>
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<p>Fracture surface of as-welded specimen (<b>a,b</b>) and PWHT specimen (<b>c,d</b>).</p>
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<p>Microstructure of cross-section in <a href="#materials-13-03013-f003" class="html-fig">Figure 3</a>a for as-welded specimen (<b>a</b>), and for PWHT specimen (<b>b–d</b>).</p>
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<p>Retained cracks of vertical-section in <a href="#materials-13-03013-f003" class="html-fig">Figure 3</a>b for as-welded specimen (<b>a</b>), and for PWHT specimen (<b>b</b>).</p>
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<p>Optical microscopy (OM) images of columnar grain zone of (<b>a</b>) as-welded specimen and (<b>b</b>) PWHT specimen.</p>
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<p>CLSM images of the weld metal for (<b>a</b>) heating stage, (<b>b</b>) initial stage of temperature holding stage, (<b>c</b>) temperature holding stage, (<b>d</b>) end stage of temperature holding stage.</p>
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<p>CLSM images of the weld metal for (<b>a</b>) heating stage, (<b>b</b>) initial stage of temperature holding stage, (<b>c</b>) temperature holding stage, (<b>d</b>) end stage of temperature holding stage.</p>
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<p>Confocal laser scanning microscopy (CLSM) images of the weld metal for (<b>a</b>) initial stage of cooling stage, (<b>b</b>) cooling stage at 754 °C, (<b>c</b>) cooling stage at 433 °C, (<b>d</b>) end stage of cooling stage.</p>
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<p>Microstructure of the specimen after CLSM.</p>
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<p>Fracture surface of HM specimen for (<b>a</b>) marco, (<b>b</b>) crack initiation origin.</p>
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<p>Microstructure of HM specimen.</p>
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<p>Schematic diagrams showing fracture processes for (<b>a</b>) as-welded impact specimen and (<b>b</b>) for PWHT impact specimen.</p>
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18 pages, 2722 KiB  
Article
Assessment and Characterization of Some New Photosensitizers for Antimicrobial Photodynamic Therapy (aPDT)
by Laura Monica Dascalu (Rusu), Marioara Moldovan, Doina Prodan, Irina Ciotlaus, Violeta Popescu, Ioana Baldea, Rahela Carpa, Sorina Sava, Radu Chifor and Mindra Eugenia Badea
Materials 2020, 13(13), 3012; https://doi.org/10.3390/ma13133012 - 6 Jul 2020
Cited by 18 | Viewed by 3642
Abstract
The novelty of this study consists on the formulation and evaluation of five complex experimental natural photosensitizers (PS): gel with oregano essential oil (O), gel with methylene blue (AM), gel with a mixture of essential oils (Thieves-H), gel with arnica oil and curcuma [...] Read more.
The novelty of this study consists on the formulation and evaluation of five complex experimental natural photosensitizers (PS): gel with oregano essential oil (O), gel with methylene blue (AM), gel with a mixture of essential oils (Thieves-H), gel with arnica oil and curcuma extract (CU) and gel with frankincense essential oil (T), used as photosensitizing agents (PS) in antimicrobial photodynamic therapy (aPDT) in the control of microbial biofilm in oral cavity. The experimental PS were characterized by gas chromatography-mass spectrometry (GC-MS), Fourier-transform infrared spectroscopy (FTIR), UV-Vis spectroscopy, cytotoxicity assay, antimicrobial effect and scanning electron microscopy (SEM). The IR spectra of the experimental PS with essential oils exhibit absorption bands due to the presence of water and glycerol in high quantities. The studied compounds had a reduced cytotoxic effect on cell cultures. The lowest cytotoxic effect was observed in experimental PS with oregano essential oil and methylene blue PS. Essential oils with proven antibacterial capabilities used in experimental PS confer antibacterial activity to the gels in which they are incorporated, an activity that may be more efficient use of a PDT therapy. Single bacteria were detected mainly by SEM after 12 h, while aggregate bacteria and micro colonies dominated the samples at 48 h. Full article
(This article belongs to the Special Issue Novel Dental Restorative Materials)
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<p>Application of various types of gels on sterile disks (left = <span class="html-italic">E. coli</span>; right = <span class="html-italic">S. aureus</span>).</p>
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<p>UV-VIS spectra of the experimental PS with AM, H, T, O and CU.</p>
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<p>IR spectra for the experimental PS gels with essential oils and for dried gels.</p>
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<p>Cytotoxicity assay of the tested photosensitizers in different gel extract concentrations—0.001, 0.002, 0.005, 0.01; control PS (M), O with oregano essential oil, AM with Methylene Blue, CU with curcuma extract, H with Thieves mix essential oil, T with frankincense essential oil; Each bar represents mean ± standard deviation (<span class="html-italic">n</span> = 3), * represents <span class="html-italic">p</span> &lt; 0.05, compared to untreated control.</p>
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<p>Antimicrobial activity of experimental PS after incubation (left = <span class="html-italic">E. coli</span>; right = <span class="html-italic">S. aureus</span>).</p>
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<p>Antimicrobial activity of experimental PS—the diameters (mm) of the inhibition zone.</p>
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<p>SEM images of teeth before and after treatment with photosensitizers: (<b>a</b>) after bacterial colonization, 15,000× magnification; (<b>b</b>) after treatment with commercial gel HELBO, 10000× magnification; (<b>c</b>) 5000× magnification; (<b>d</b>) after bacterial colonization, 10,000× magnification; (<b>e</b>) after treatment with experimental gel AM, 10000× magnification; (<b>f</b>) 5000× magnification; (<b>g</b>) after bacterial colonization, 10,000× magnification; (<b>h</b>) after treatment with experimental gel O, 5000× magnification; (<b>i</b>) 10,000× magnification; (<b>j</b>) after bacterial colonization, with 5000× magnification; (<b>k</b>) after treatment with experimental gel CU, 5000× magnification; (<b>l</b>) after treatment with gel CU, 10,000× magnification.</p>
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