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Preparation, Separation, Characterization and Application of Carbon Nanotubes

A special issue of Nanomaterials (ISSN 2079-4991). This special issue belongs to the section "2D and Carbon Nanomaterials".

Deadline for manuscript submissions: 20 May 2025 | Viewed by 6498

Special Issue Editor


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Guest Editor
Security and Disruptive Technologies Research Centre, National Research Council of Canada, 1200 Montreal Road, M-12, Ottawa, ON K1A 0R6, Canada
Interests: carbon nanotubes; conjugated polymers; transistors; sensors

Special Issue Information

Dear Colleagues,

Since the seminal discovery of carbon nanotubes by Sumio Iijima more than 30 years ago, research interest in this field has grown dramatically due to their unique optical and electronic properties. Synthesized raw tube material usually contains both semiconducting and metallic tubes with a wide diameter and chirality distribution, besides some other impurities, which means that it is usually not good enough for practical usage. Synthetic techniques have been improved substantially by finetuning the catalyst and preparation conditions used. Post-synthesis separation has also been sought out. The purity requirement is heavily dependent on the application. For example, for thin film transistors with channel lengths over 10 um, 99.9% semiconducting purity could be enough, but 99.9999% is desired for high-performance short-channel field-effect transistors. For optical applications, high-purity single-chirality samples are needed. Currently, high semiconducting purity and some single-chirality carbon nanotubes could be easily obtained from solution processes.

The present Special Issue of Nanomaterials is aimed at presenting the current state-of-the-art research related to carbon nanotubes, covering not only the preparation and enrichment process to address purity and chiral selectivity issues but also device applications, such as thin film transistors, photodetectors, single photo emission and sensors. For this Special Issue, we welcome contributions from leading groups in the field and hope to give a balanced view of the current state of the art in this discipline.

Dr. Zhao Li
Guest Editor

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Keywords

  • carbon nanotubes
  • purification
  • enrichment
  • transistors
  • sensors

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Published Papers (5 papers)

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Research

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19 pages, 13821 KiB  
Article
Structure and Electrocatalytic Properties of Sulfur-Containing Multi-Walled Carbon Nanotubes on a Titanium Substrate Modified by a Helium Ion Beam
by Petr M. Korusenko, Egor V. Knyazev, Alexander S. Vinogradov, Ksenia A. Kharisova, Sofya S. Filippova, Ulyana M. Rodionova, Oleg V. Levin and Elena V. Alekseeva
Nanomaterials 2024, 14(23), 1948; https://doi.org/10.3390/nano14231948 - 4 Dec 2024
Viewed by 456
Abstract
In this work, a set of analytical techniques, including scanning electron microscopy (SEM), Raman scattering spectroscopy, X-ray photoelectron spectroscopy (XPS), energy-dispersive X-ray microanalysis (EDX) and cyclic voltammetry (CV), were used to study the impact of high-energy He+ ion irradiation on the structural [...] Read more.
In this work, a set of analytical techniques, including scanning electron microscopy (SEM), Raman scattering spectroscopy, X-ray photoelectron spectroscopy (XPS), energy-dispersive X-ray microanalysis (EDX) and cyclic voltammetry (CV), were used to study the impact of high-energy He+ ion irradiation on the structural and electrochemical characteristics of sulfur-containing multi-walled carbon nanotubes (S-MWCNTs) placed on a titanium substrate. The results indicate that the ion beam treatment of the S-MWCNT system led to an increase in the level of imperfections on the surface structures of the nanotubes due to the formation of point defects on their outer walls and the appearance of oxygen-containing functional groups, including SOx groups, near these defects. At the same time, a significant increase in the sulfur concentration (by 6.4 times) was observed on the surface of the S-MWCNTs compared to the surface of unirradiated nanotubes. This was due to the redeposition of sulfur atoms near the point defects under the action of the ion beam, followed by the subsequent formation of direct S–C chemical bonds. Electrochemical studies demonstrated that the irradiated S-MWCNTs/Ti system exhibit enhanced catalytic activity, with improved oxygen reduction reaction (ORR) performance and a substantial increase in anodic current during the oxidation reaction of hydrogen peroxide under alkaline conditions, highlighting their potential for advanced electrocatalytic applications. Full article
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Graphical abstract
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<p>SEM images of MWCNTs/Ti (<b>a</b>,<b>d</b>) as well as S-MWCNTs/Ti before (<b>b</b>,<b>e</b>) and after irradiation with He<sup>+</sup> ions (<b>c</b>,<b>f</b>) at different magnifications.</p>
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<p>Raman spectra of MWCNTs/Ti as well as S-MWCNTs/Ti before and after irradiation by He<sup>+</sup> ions.</p>
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<p>Survey PE spectra of MWCNTs/Ti as well as S-MWCNTs/Ti before and after irradiation by He<sup>+</sup> ions.</p>
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<p>C 1<span class="html-italic">s</span> PE spectra of MWCNTs/Ti as well as S-MWCNTs/Ti before and after irradiation by He<sup>+</sup> ions.</p>
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<p>S 2<span class="html-italic">p</span> PE spectra of S-MWCNTs/Ti before and after irradiation by He<sup>+</sup> ions.</p>
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<p>O 1<span class="html-italic">s</span> PE spectra of MWCNTs/Ti as well as S-MWCNTs/Ti before and after irradiation by He<sup>+</sup> ions.</p>
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<p>Cyclic voltammograms for the MWCNTs/Ti. The initial and irradiated S-MWCNTs/Ti systems recorded in a 0.1 M KOH electrolyte at a scan rate of 10 mV/s (the horizontal dotted line indicates the onset current). The atmospheres in which the measurements were performed are given in brackets: argon (Ar) and oxygen (O<sub>2</sub>).</p>
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<p>Cyclic voltammograms of MWCNTs/Ti (<b>a</b>) and S-MWCNTs/Ti (<b>b</b>) at a scan rate of 50 mV/s in buffer solutions with a p<span class="html-italic">H</span> of 4 with different (10<sup>−2</sup> and 10<sup>−3</sup> M) H<sub>2</sub>O<sub>2</sub> concentrations.</p>
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<p>Cyclic voltammograms of helium-irradiated S-MWCNTs/Ti electrodes at different scan rates (10, 50 and 100 mV/s) in buffer solutions with p<span class="html-italic">H</span>s of 4, 7 and 9 without H<sub>2</sub>O<sub>2</sub> (<b>a</b>,<b>c</b>,<b>e</b>) and at a scan rate of 50 mV/s in buffer solutions with different (10<sup>−2</sup> and 10<sup>−3</sup> M) H<sub>2</sub>O<sub>2</sub> concentrations (<b>b</b>,<b>d</b>,<b>f</b>), as well as a comparison of CV curves in buffer solutions with p<span class="html-italic">H</span>s 4, 7 and 9 with a concentration of 10<sup>−2</sup> M H<sub>2</sub>O<sub>2</sub> (<b>g</b>).</p>
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<p>Cyclic voltammograms of helium-irradiated S-MWCNTs/Ti electrodes at different scan rates (10, 50 and 100 mV/s) in buffer solutions with p<span class="html-italic">H</span>s of 4, 7 and 9 without H<sub>2</sub>O<sub>2</sub> (<b>a</b>,<b>c</b>,<b>e</b>) and at a scan rate of 50 mV/s in buffer solutions with different (10<sup>−2</sup> and 10<sup>−3</sup> M) H<sub>2</sub>O<sub>2</sub> concentrations (<b>b</b>,<b>d</b>,<b>f</b>), as well as a comparison of CV curves in buffer solutions with p<span class="html-italic">H</span>s 4, 7 and 9 with a concentration of 10<sup>−2</sup> M H<sub>2</sub>O<sub>2</sub> (<b>g</b>).</p>
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10 pages, 2127 KiB  
Article
Polymer Coating Enabled Carrier Modulation for Single-Walled Carbon Nanotube Network Inverters and Antiambipolar Transistors
by Zhao Li, Jenner H. L. Ngai and Jianfu Ding
Nanomaterials 2024, 14(18), 1477; https://doi.org/10.3390/nano14181477 - 11 Sep 2024
Viewed by 673
Abstract
The control of the performance of single-walled carbon nanotube (SWCNT) random network-based transistors is of critical importance for their applications in electronic devices, such as complementary metal oxide semiconducting (CMOS)-based logics. In ambient conditions, SWCNTs are heavily p-doped by the H2O/O [...] Read more.
The control of the performance of single-walled carbon nanotube (SWCNT) random network-based transistors is of critical importance for their applications in electronic devices, such as complementary metal oxide semiconducting (CMOS)-based logics. In ambient conditions, SWCNTs are heavily p-doped by the H2O/O2 redox couple, and most doping processes have to counteract this effect, which usually leads to broadened hysteresis and poor stability. In this work, we coated an SWCNT network with various common polymers and compared their thin-film transistors’ (TFTs’) performance in a nitrogen-filled glove box. It was found that all polymer coatings will decrease the hysteresis of these transistors due to the partial removal of charge trapping sites and also provide the stable control of the doping level of the SWCNT network. Counter-intuitively, polymers with electron-withdrawing functional groups lead to a dramatically enhanced n-branch in their transfer curve. Specifically, SWCNT TFTs with poly (vinylidene fluoride) coating show an n-type mobility up to 61 cm2/Vs, with a decent on/off ratio and small hysteresis. The inverters constructed by connecting two ambipolar TFTs demonstrate high gain but with certain voltage loss. P-type or n-type doping from polymer coating layers could suppress unnecessary n- or p-branches, shift the threshold voltage and optimize the performance of these inverters to realize rail-to-rail switching. Similar devices also demonstrate interesting antiambipolar performance with tunable on and off voltage when tested in a different configuration. Full article
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<p>SEM images of SWCNT random network on SiO<sub>2</sub> substrate at (<b>a</b>) low and (<b>b</b>) high magnification; (<b>c</b>) schematic illustration of TFT device structure.</p>
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<p>Representative transfer curves of SWCNT random network TFTs: (<b>a</b>) Ctrl, (<b>b</b>) coated with PS and PVC, (<b>c</b>) coated with PMMA or Formvar, (<b>d</b>) coated with PVdF or PAN; (<b>e</b>) extracted threshold voltage for n-branch (V<sub>Tn</sub>) and corresponding electron mobility (µ<sub>e</sub>) vs. Hommett substituent constant of structure similar functional groups within polymer; (<b>f</b>) comparison of mobility and hysteresis (normalized by V<sub>G</sub> sweeping range) from PVdF-coated n-type CNT TFTs in this work with other reported random network CNT TFTs [<a href="#B6-nanomaterials-14-01477" class="html-bibr">6</a>,<a href="#B10-nanomaterials-14-01477" class="html-bibr">10</a>,<a href="#B20-nanomaterials-14-01477" class="html-bibr">20</a>,<a href="#B21-nanomaterials-14-01477" class="html-bibr">21</a>,<a href="#B22-nanomaterials-14-01477" class="html-bibr">22</a>,<a href="#B23-nanomaterials-14-01477" class="html-bibr">23</a>,<a href="#B24-nanomaterials-14-01477" class="html-bibr">24</a>,<a href="#B25-nanomaterials-14-01477" class="html-bibr">25</a>,<a href="#B26-nanomaterials-14-01477" class="html-bibr">26</a>].</p>
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<p>(<b>a</b>) Representative transfer curves from blends of Formvar and PAN-covered SWCNT network TFTs. (<b>b</b>) Threshold voltage and electron mobility vs. weight percentage of PAN within Formvar. (<b>c</b>) P-type transfer curves from PAA or photoresistor S1813-covered SWCNT network TFTs.</p>
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<p>(<b>a</b>) Voltage transfer characteristics of inverter by connecting two ambipolar Ctrl TFTs; inset is circuit diagram; (<b>b</b>) gain at V<sub>DD</sub> of 14V; (<b>c</b>) hysteresis and gain vs. V<sub>DD</sub>; (<b>d</b>) output characteristics of representative Ctrl TFT.</p>
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<p>(<b>a</b>) Output characteristics of p-type and n-type polymer-coated CNT TFTs; (<b>b</b>) voltage transfer characteristics of inverter by connecting p/n-type TFTs, with inserted circuit diagram; (<b>c</b>) gain at various V<sub>DD</sub>; (<b>d</b>) input and output waveforms of inverter operated at 5 V.</p>
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<p>(<b>a</b>) Drain current—V<sub>G</sub> curves of the antiambipolar transistor by connecting two SWCNT TFTs with different polymer coating layers; the circuit diagram is shown in the inset; (<b>b</b>) a 3D plot of the drain current depending on both drain and gate bias voltage; (<b>c</b>) normalized drain current—V<sub>G</sub> curves of three antiambipolar transistors with finetuned doping levels for each TFT, with the coating polymers for each AAT shown on the left; (<b>d</b>) drain current—V<sub>G</sub> curves of a double antiambipolar transistor by connecting three SWCNT TFTs with different doping levels.</p>
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13 pages, 2347 KiB  
Article
Ultra-Mild Fabrication of Highly Concentrated SWCNT Dispersion Using Spontaneous Charging in Solvated Electron System
by Junho Shin, Jung Hoon Kim, Jungeun Lee, Sangyong Lee, Jong Hwan Park, Seung Yol Jeong, Hee Jin Jeong, Joong Tark Han, Seon Hee Seo, Seoung-Ki Lee and Jungmo Kim
Nanomaterials 2024, 14(13), 1094; https://doi.org/10.3390/nano14131094 - 26 Jun 2024
Viewed by 1524
Abstract
The efficient dispersion of single-walled carbon nanotubes (SWCNTs) has been the subject of extensive research over the past decade. Despite these efforts, achieving individually dispersed SWCNTs at high concentrations remains challenging. In this study, we address the limitations associated with conventional methods, such [...] Read more.
The efficient dispersion of single-walled carbon nanotubes (SWCNTs) has been the subject of extensive research over the past decade. Despite these efforts, achieving individually dispersed SWCNTs at high concentrations remains challenging. In this study, we address the limitations associated with conventional methods, such as defect formation, excessive surfactant use, and the use of corrosive solvents. Our novel dispersion method utilizes the spontaneous charging of SWCNTs in a solvated electron system created by dissolving potassium in hexamethyl phosphoramide (HMPA). The resulting charged SWCNTs (c-SWCNTs) can be directly dispersed in the charging medium using only magnetic stirring, leading to defect-free c-SWCNT dispersions with high concentrations of up to 20 mg/mL. The successful dispersion of individual c-SWCNT strands is confirmed by their liquid-crystalline behavior. Importantly, the dispersion medium for c-SWCNTs exhibits no reactivity with metals, polymers, or other organic solvents. This versatility enables a wide range of applications, including electrically conductive free-standing films produced via conventional blade coating, wet-spun fibers, membrane electrodes, thermal composites, and core-shell hybrid microparticles. Full article
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Graphical abstract

Graphical abstract
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<p>Charging behavior of SWCNTs in solvated electron system. (<b>a</b>) Schematic of c-SWCNT dispersion process. (<b>b</b>) Digital images of (i) p-SWCNT powder, (ii) c-SWCNT cake formed by the addition of electron solution. (<b>c</b>) XRD result of p-SWCNTs and c-SWCNTs. (<b>d</b>) Raman spectra of p-SWCNTs and c-SWCNTs exposed to electron solutions with different potassium concentration.</p>
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<p>Characterization of c-SWCNT dispersion. (<b>a</b>) Digital image of c-SWCNT dispersion (20 mg/mL). (<b>b</b>) POM images of c-SWCNT dispersion (20 mg/mL): bright field image (<b>left</b>); dark field image (<b>right</b>). (<b>c</b>) AFM image of c-SWCNT sampled on SiO2 wafer (<b>top</b>); height profile corresponding to the dotted line in the AFM image (<b>bottom</b>). (<b>d</b>) Normalized Raman spectra of c-SWCNT and p-SWCNT films. (<b>e</b>) XPS survey of c-SWCNT and p-SWCNT films. (<b>f</b>) C1s scan of c-SWCNT and p-SWCNT films.</p>
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<p>Free-standing film and fiber fabricated with c-SWCNT dispersion. (<b>a</b>) Digital images of (<b>i</b>) c-SWCNT dispersion coated on Al foil using blade coating, (<b>ii</b>) dried c-SWCNT film. (<b>b</b>) SEM images of c-SWCNT film fabricated with c-SWCNT dispersion with K concentrations of (<b>i</b>) 0.25 M, (<b>ii</b>) 0.5 M, (<b>iii</b>) 0.75 M, and (<b>iv</b>) 1 M. (<b>c</b>) Stress–strain curve of the c-SWCNT film (0.25 M). (<b>d</b>) Digital image and SEM image of the wet-spun c-SWCNT fiber. (<b>e</b>) SEM images of wet-spun c-SWCNT fiber fabricated using (<b>i</b>) DI water coagulant, (<b>ii</b>) DI water–ethanol solution coagulant.</p>
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<p>Versatile applications of c-SWCNT. (<b>a</b>) Galvanostatic charge–discharge profile of c-SWCNT and p-SWCNT cathodes (current density = 0.1 A g<sup>−1</sup>). (<b>b</b>) Rate capability comparison of c-SWCNT and p-SWCNT cathodes. (<b>c</b>) (<b>i</b>) Digital image of SWCNT-PVDF composite (1 wt%); (<b>ii</b>) thermal enhancement in c-SWCNT-PVDF composite. (<b>d</b>) SEM images of hybridized c-SWCNT-PS microsphere fabricated with c-SWCNT dispersions with concentrations of (<b>i</b>,<b>ii</b>) 2 mg/mL, (<b>iii</b>) 5 mg/mL, and (<b>iv</b>) 1 mg/mL.</p>
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12 pages, 6429 KiB  
Article
Improving the Adhesion of Multi-Walled Carbon Nanotubes to Titanium by Irradiating the Interface with He+ Ions: Atomic Force Microscopy and X-ray Photoelectron Spectroscopy Study
by Petr M. Korusenko, Egor V. Knyazev, Olga V. Petrova, Denis V. Sokolov, Sergey N. Povoroznyuk, Konstantin E. Ivlev, Ksenia A. Bakina, Vyacheslav A. Gaas and Alexander S. Vinogradov
Nanomaterials 2024, 14(8), 699; https://doi.org/10.3390/nano14080699 - 17 Apr 2024
Cited by 2 | Viewed by 1303
Abstract
A complex study of the adhesion of multi-walled carbon nanotubes to a titanium surface, depending on the modes of irradiation with He+ ions of the “MWCNT/Ti” system, was conducted using atomic force microscopy and X-ray photoelectron spectroscopy. A quantitative assessment of the [...] Read more.
A complex study of the adhesion of multi-walled carbon nanotubes to a titanium surface, depending on the modes of irradiation with He+ ions of the “MWCNT/Ti” system, was conducted using atomic force microscopy and X-ray photoelectron spectroscopy. A quantitative assessment of the adhesion force at the interface, performed using atomic force microscopy, demonstrated its significant increase as a result of treatment of the “MWCNT/Ti” system with a beam of helium ions. The nature of the chemical bonding between multi-walled carbon nanotubes and the surface of the titanium substrate, which causes this increase in the adhesion of nanotubes to titanium as a result of ion irradiation, was investigated by X-ray photoelectron spectroscopy. It was established that this bonding is the result of the formation of chemical C–O–Ti bonds between titanium and carbon atoms with the participation of oxygen atoms of oxygen-containing functional groups, which are localized on defects in the nanotube walls formed during ion irradiation. It is significant that there are no signs of direct bonding between titanium and carbon atoms. Full article
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Figure 1
<p>SEM images of “MWCNT/Ti” surface layer: (<b>a</b>) initial and irradiated with He<sup>+</sup> for (<b>b</b>) 10 min, (<b>c</b>) 20 min, and (<b>d</b>) 30 min.</p>
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<p>AFM images of “MWCNT/Ti” surface layer: (<b>a</b>) initial and irradiated with He<sup>+</sup> for (<b>b</b>) 10 min, (<b>c</b>) 20 min and (<b>d</b>) 30 min.</p>
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<p>Survey PE spectra of “MWCNT/Ti” surface: (<span class="html-italic">a</span>) initial and irradiated with He<sup>+</sup> for (<span class="html-italic">b</span>) 10 min, (<span class="html-italic">c</span>) 20 min, and (<span class="html-italic">d</span>) 30 min.</p>
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<p>C 1s PE spectra of “MWCNT/Ti” surface: (<b>a</b>) initial and irradiated with He<sup>+</sup> for (<b>b</b>) 10 min, (<b>c</b>) 20 min, and (<b>d</b>) 30 min.</p>
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<p>Ti 2p<sub>1/2,3/2</sub> PE spectra of “MWCNT/Ti” surface: (<b>a</b>) initial and irradiated with He<sup>+</sup> for (<b>b</b>) 10 min, (<b>c</b>) 20 min, and (<b>d</b>) 30 min.</p>
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<p>O 1s PE spectra of “MWCNT/Ti” surface: (<b>a</b>) initial and irradiated with He<sup>+</sup> for (<b>b</b>) 10 min, (<b>c</b>) 20 min, and (<b>d</b>) 30 min.</p>
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Review

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20 pages, 3745 KiB  
Review
The Effectiveness Mechanisms of Carbon Nanotubes (CNTs) as Reinforcements for Magnesium-Based Composites for Biomedical Applications: A Review
by Abbas Saberi, Madalina Simona Baltatu and Petrica Vizureanu
Nanomaterials 2024, 14(9), 756; https://doi.org/10.3390/nano14090756 - 25 Apr 2024
Cited by 7 | Viewed by 1841
Abstract
As a smart implant, magnesium (Mg) is highly biocompatible and non-toxic. In addition, the elastic modulus of Mg relative to other biodegradable metals (iron and zinc) is close to the elastic modulus of natural bone, making Mg an attractive alternative to hard tissues. [...] Read more.
As a smart implant, magnesium (Mg) is highly biocompatible and non-toxic. In addition, the elastic modulus of Mg relative to other biodegradable metals (iron and zinc) is close to the elastic modulus of natural bone, making Mg an attractive alternative to hard tissues. However, high corrosion rates and low strength under load relative to bone are some challenges for the widespread use of Mg in orthopedics. Composite fabrication has proven to be an excellent way to improve the mechanical performance and corrosion control of Mg. As a result, their composites emerge as an innovative biodegradable material. Carbon nanotubes (CNTs) have superb properties like low density, high tensile strength, high strength-to-volume ratio, high thermal conductivity, and relatively good antibacterial properties. Therefore, using CNTs as reinforcements for the Mg matrix has been proposed as an essential option. However, the lack of understanding of the mechanisms of effectiveness in mechanical, corrosion, antibacterial, and cellular fields through the presence of CNTs as Mg matrix reinforcements is a challenge for their application. This review focuses on recent findings on Mg/CNT composites fabricated for biological applications. The literature mentions effective mechanisms for mechanical, corrosion, antimicrobial, and cellular domains with the presence of CNTs as reinforcements for Mg-based nanobiocomposites. Full article
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Figure 1
<p>Schematic of effective mechanisms of CNTs on Mg/CNT composite.</p>
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<p>Schematic of carbon nanotubes applications in biomedicine.</p>
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<p>(<b>a</b>) Schematic diagram showing the dislocations pinned by CNTs, FE-SEM images of Mg-3Zn/fCNTs (<b>b</b>) crack bridging, (<b>c</b>) crack branching, (<b>d</b>) crack deflection and (<b>e</b>) fCNTs pull out [<a href="#B95-nanomaterials-14-00756" class="html-bibr">95</a>]. (<b>f</b>) Crack deflection; (<b>g</b>) Crack bridging and (<b>h</b>,<b>i</b>) Crack branching mechanisms of Mg/CNT-GNPs composites; (<b>j</b>) EDS mapping of Crack branching mechanism [<a href="#B55-nanomaterials-14-00756" class="html-bibr">55</a>].</p>
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<p>SEM images of (<b>a</b>) Mg-3Zn-1Mn alloy, (<b>b</b>) Mg-3Zn-1Mn/CNT, (<b>c</b>,<b>d</b>) Mg-3Zn-1Mn/MgO-CNT nanocomposites after 7 days of immersion in SBF under physiological condition of 5% CO<sub>2</sub> at 37 °C, and (<b>e</b>) XRD pattern of Mg-3Zn-1Mn/MgO-CNTs immersed in SBF for 7 days [<a href="#B99-nanomaterials-14-00756" class="html-bibr">99</a>].</p>
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<p>Schematic of the antimicrobial mechanism of CNT reinforcement.</p>
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<p>(<b>a</b>) Images of water contact angle, (<b>b</b>) Fluorescent DAPI staining ofMG-63 cells grown after 24 h, and (<b>c</b>) SEM images of the morphology and adhesion of these cells for 3 days on Mg–3Zn alloy matrix, Mg-3Zn/0.2fCNTs, Mg-3Zn/0.4fCNTs and Mg-3Zn/0.8fCNTs nanocomposites [<a href="#B95-nanomaterials-14-00756" class="html-bibr">95</a>].</p>
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