CN116199208A - Preparation of conductive nano carbon sphere and calibration application of conductive nano carbon sphere in scanning electron microscope - Google Patents
Preparation of conductive nano carbon sphere and calibration application of conductive nano carbon sphere in scanning electron microscope Download PDFInfo
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- CN116199208A CN116199208A CN202310192306.0A CN202310192306A CN116199208A CN 116199208 A CN116199208 A CN 116199208A CN 202310192306 A CN202310192306 A CN 202310192306A CN 116199208 A CN116199208 A CN 116199208A
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- 229910021392 nanocarbon Inorganic materials 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 92
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 31
- 229920001690 polydopamine Polymers 0.000 claims abstract description 26
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 6
- 239000005543 nano-size silicon particle Substances 0.000 claims description 25
- 239000002077 nanosphere Substances 0.000 claims description 21
- 229910052799 carbon Inorganic materials 0.000 claims description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 8
- 239000011261 inert gas Substances 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 239000012298 atmosphere Substances 0.000 claims description 5
- 238000010000 carbonizing Methods 0.000 claims description 5
- 229960001149 dopamine hydrochloride Drugs 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 3
- 238000000197 pyrolysis Methods 0.000 claims 1
- 238000003384 imaging method Methods 0.000 abstract description 12
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 abstract description 10
- 230000001133 acceleration Effects 0.000 abstract description 8
- 229960003638 dopamine Drugs 0.000 abstract description 5
- 238000009826 distribution Methods 0.000 abstract description 3
- 238000010894 electron beam technology Methods 0.000 abstract description 3
- 239000012798 spherical particle Substances 0.000 abstract description 2
- 239000002245 particle Substances 0.000 description 8
- 238000005507 spraying Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000004321 preservation Methods 0.000 description 5
- 238000005336 cracking Methods 0.000 description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 4
- 239000010931 gold Substances 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 201000009310 astigmatism Diseases 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 241000238586 Cirripedia Species 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 241000237536 Mytilus edulis Species 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 235000020638 mussel Nutrition 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/26—Electron or ion microscopes; Electron or ion diffraction tubes
- H01J37/28—Electron or ion microscopes; Electron or ion diffraction tubes with scanning beams
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
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- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
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Abstract
The invention discloses a preparation method of a conductive nano carbon sphere and a calibration application of the conductive nano carbon sphere in a scanning electron microscope. The patent of the invention comprises the following steps: firstly, a preparation method of the conductive nano carbon sphere is provided, and secondly, the application of the conductive nano carbon sphere in the aspect of scanning electron microscope calibration is provided. The invention discloses a method for preparing conductive nano carbon spheres by using oxidation-self polymerization of dopamine to form a compact polydopamine layer on the surface of prepared spherical silicon dioxide and adopting a subsequent heat treatment mode. The preparation steps are simple, the cost is low, the repeated stability is good, and the large-scale batch preparation on the laboratory level can be realized. In addition, the prepared nano carbon spheres have good conductivity and uniform spherical particle size distribution, and can maintain high-resolution imaging under the bombardment of high vacuum and strong electron beams. Can be used for laboratory calibration of scanning electron microscope under low, medium and high magnification and acceleration voltage.
Description
Technical Field
The invention relates to the technical field of nanocomposite preparation, in particular to a coated conductive nanosphere, and relates to preparation of a conductive carbon nanosphere and calibration application of the conductive carbon nanosphere in a scanning electron microscope.
Background
The scanning electron microscope has the advantages of continuously adjustable magnification, high shooting resolution, ultra-large depth of field and the like, and has wide application in the fields of life science, material science, microelectronics science and the like. Since a scanning electron microscope performs progressive scanning by using an electron beam at the time of photographing, problems such as image magnification and image distortion occur over time. Only if the stable resolution and good imaging effect are maintained, the most accurate scientific image and measurement data can be provided, and the standard sample is required to be used for calibrating performance indexes such as resolution, imaging quality and the like regularly. The currently marketed calibration standards mainly comprise gold nano-standards, carbon-based gold standard, copper grid standard and carbon-based tin ball (SnO 2) standard, most of which are expensive, have harsh storage conditions and are not easy to prepare in a large scale in a laboratory. Therefore, it is important to design and synthesize a nano standard sample with the same calibration effect, low cost, easy obtaining and easy preservation on the laboratory level.
Disclosure of Invention
The invention provides a preparation method of a conductive nano carbon sphere which can be realized on the laboratory level and a calibration application in a scanning electron microscope, aiming at solving the problems of high price and difficult preservation of the existing calibration standard sample sold in the market of the scanning electron microscope. The method has the advantages of low preparation cost and good repeated stability, and the prepared nano carbon spheres have good conductivity and uniform particle size distribution and are suitable for calibrating the scanning electron microscope under different shooting conditions.
The invention provides a technical scheme that: a method of preparing a conductive nanocarbon sphere, the method comprising:
s1, providing spherical nano silicon dioxide;
s2, forming a polydopamine compact layer on the surface of the spherical silicon dioxide;
and S3, performing heat treatment on the polydopamine compact layer to obtain the conductive nano carbon spheres.
Preferably, in step S1, the specific preparation method is as follows: weighing 1-4ml of 25% ammonia water, 12-48ml of 99.5% absolute ethyl alcohol and 80-100ml of deionized water, vigorously stirring for 20-40min, dropwise adding 1-3ml tetraethoxysilane, and continuously vigorously stirring for 15-45min.
Preferably, in step S2, the specific preparation method is as follows: adding 50mg/ml dopamine hydrochloride 6-12ml into the spherical nano silicon dioxide solution prepared in the step S1 for self-polymerization for 12-36 hours to obtain brown mixed solution, washing with deionized water to be neutral, and carrying out suction filtration to obtain a brown black solid, namely the spherical nano silicon dioxide coated with polydopamine.
Preferably, in step S3, the conductive nanocarbon balls are obtained by high temperature-cracking under an inert gas atmosphere, wherein the inert gas may be selected from nitrogen, argon, and helium; the preparation method comprises the following steps: drying the spherical nano silicon dioxide coated with polydopamine obtained in the step S2 in an oven at 80 ℃ for 12 hours, carbonizing the spherical nano silicon dioxide by using a tube furnace with temperature programming under the protection of nitrogen atmosphere, heating at a speed of 5-10 ℃/min, heating at a temperature of 700-900 ℃ for 120-240min, and finally grinding to obtain the conductive nano carbon spheres.
The invention provides another technical scheme that: any of the conductive nanocarbon balls described above is applied to scanning electron microscope calibration.
The beneficial effects of the invention are as follows:
(1) The synthesis thought of the conductive carbon coated silica nanospheres is novel, polydopamine (PDA) has the property similar to mussels and barnacle adhesion proteins, can be adhered to the surfaces of almost all materials, forms a PDA layer on the silica surfaces by oxidation-self polymerization of dopamine, and then prepares the nanospheres through subsequent treatment. The method has the advantages of simple steps, low preparation cost and good repeated stability, and can realize large-scale preparation at the laboratory level.
(2) The prepared carbon-coated silica nanospheres have good conductivity and uniform spherical particle size distribution, can perform conventional calibration on a (environment) scanning electron microscope under the condition of no metal spraying, and can be recycled.
(3) Under high vacuum and strong electron beam bombardment, the carbon-coated silica nanosphere calibration standard sample can still keep higher resolution and good secondary electron yield, and can be used for calibration under different amplification factors (low, medium and high) and different acceleration voltages (low, medium and high).
Drawings
FIG. 1 is a graph showing the scanning electron microscope and the particle size statistics of the conductive nanocarbon ball in example 1;
FIG. 2 is a transmission electron microscope image of the conductive nanocarbon ball in example 1;
FIG. 3 is an EDS spectrum of the conductive nanocarbon ball of application example 1;
fig. 4 is a calibration image of the conductive nanocarbon ball of application example 1 on a scanning electron microscope under different conditions (acceleration voltage 25kV, magnification 20000 times);
FIG. 5 is a graph of the conductive nanocarbon ball of application example 2 (acceleration voltage 25kV, magnification factor 8000) for calibrating a scanning electron microscope under different conditions;
fig. 6 is a calibration image of the conductive nanocarbon ball of application example 3 on a scanning electron microscope under different conditions (acceleration voltage 25kV, magnification 15000 times).
Detailed Description
The present invention is described in detail below with reference to specific embodiments, and it should be noted that the following embodiments are only for further description of the present invention and should not be construed as limiting the scope of the present invention, and some insubstantial modifications and adjustments of the present invention by those skilled in the art from the present disclosure are still within the scope of the present invention.
Example 1:
the embodiment provides a preparation method of a conductive nano carbon sphere, which comprises the following steps:
s1, providing spherical nano silicon dioxide;
s2, forming a polydopamine compact layer on the surface of the spherical silicon dioxide;
s3, conducting heat treatment on the polydopamine compact layer to obtain conductive nano carbon spheres;
in step S1, the silica is prepared by hydrolysis-condensation of tetraethoxysilane under alkaline conditions. The preparation method comprises the following steps: 1ml of 25% ammonia water, 12ml of 99.5% absolute ethanol and 80ml of deionized water are weighed, vigorously stirred for 20min, 1ml of tetraethoxysilane is added dropwise, and vigorously stirred for 15min.
In step S2, the dense polydopamine layer needs to be formed in an alkaline environment in step S1 by oxidation-polymerization of dopamine itself. The preparation method comprises the following steps: adding 50mg/ml dopamine hydrochloride 6ml into the spherical nano silicon dioxide solution prepared in the step S1 for self-polymerization for 12 hours to obtain brown mixed solution, and then washing with deionized water to neutrality and suction filtering to obtain brown black solid, namely polydopamine coated spherical nano silicon dioxide.
In the step S3, the conductive nanocarbon ball is obtained by high temperature-cracking under an inert gas atmosphere. The preparation method comprises the following steps: and (3) drying the spherical nano silicon dioxide coated with polydopamine obtained in the step (S2) in an oven at 80 ℃ for 12 hours, carbonizing the spherical nano silicon dioxide by using a tube furnace with temperature programming under the protection of nitrogen atmosphere, wherein the temperature increasing rate is 5 ℃/min, the temperature increasing is 700 ℃, the heat preservation time is 120min, and finally grinding to obtain the conductive nano carbon spheres. As shown in a scanning electron microscope in FIG. 1, the prepared conductive nano carbon spheres have good sphericity, smooth surface and relatively uniform dispersion; as shown in fig. 2, the outer surface of the silica was uniformly coated with a dense carbon layer.
Example 2:
the embodiment provides a preparation method of a conductive nano carbon sphere, which comprises the following steps:
s1, providing spherical nano silicon dioxide;
s2, forming a polydopamine compact layer on the surface of the spherical silicon dioxide;
s3, conducting heat treatment on the polydopamine compact layer to obtain conductive nano carbon spheres;
in step S1, the silica is prepared by hydrolysis-condensation of tetraethoxysilane under alkaline conditions. The preparation method comprises the following steps: 2ml of 25% ammonia water, 36ml of 99.5% absolute ethanol and 90ml of deionized water are measured, the mixture is vigorously stirred for 30min, 2ml of tetraethoxysilane is added dropwise, and the vigorous stirring is continued for 30min.
In step S2, the dense polydopamine layer needs to be formed in an alkaline environment in step S1 by oxidation-polymerization of dopamine itself. The preparation method comprises the following steps: adding 50mg/ml dopamine hydrochloride 10ml into the spherical nano silicon dioxide solution prepared in the step S1 for self-polymerization for 24 hours to obtain brown mixed solution, and then washing with deionized water to neutrality and suction filtering to obtain brown black solid, namely polydopamine coated spherical nano silicon dioxide.
In the step S3, the conductive nanocarbon ball is obtained by high temperature-cracking under an inert gas atmosphere. The preparation method comprises the following steps: and (3) drying the spherical nano silicon dioxide coated with polydopamine obtained in the step (S2) in an oven at 80 ℃ for 12 hours, carbonizing the spherical nano silicon dioxide by using a tube furnace with temperature programming under the protection of nitrogen atmosphere, wherein the temperature increasing rate is 8 ℃/min, the temperature increasing is 800 ℃, the heat preservation time is 180min, and finally grinding to obtain the conductive nano carbon spheres.
Example 3:
the embodiment provides a preparation method of a conductive nano carbon sphere, which comprises the following steps:
s1, providing spherical nano silicon dioxide;
s2, forming a polydopamine compact layer on the surface of the spherical silicon dioxide;
s3, conducting heat treatment on the polydopamine compact layer to obtain conductive nano carbon spheres;
in step S1, the silica is prepared by hydrolysis-condensation of tetraethoxysilane under alkaline conditions. The preparation method comprises the following steps: weighing 4ml of 25% ammonia water, 48ml of 99.5% absolute ethyl alcohol and 100ml of deionized water, vigorously stirring for 40min, dropwise adding 3ml of tetraethoxysilane, and continuously vigorously stirring for 45min.
In step S2, the dense polydopamine layer needs to be formed in an alkaline environment in step S1 by oxidation-polymerization of dopamine itself. The preparation method comprises the following steps: adding 12ml of dopamine hydrochloride with the concentration of 50mg/ml into the spherical nano silicon dioxide solution prepared in the step S1 for self-polymerization for 36 hours to obtain brown mixed solution, and then washing with deionized water to neutrality and suction filtering to obtain brown black solid, namely the spherical nano silicon dioxide coated with polydopamine.
In the step S3, the conductive nanocarbon ball is obtained by high temperature-cracking under an inert gas atmosphere. The preparation method comprises the following steps: and (3) drying the spherical nano silicon dioxide coated with polydopamine obtained in the step (S2) in an oven at 80 ℃ for 12 hours, carbonizing the spherical nano silicon dioxide by using a tube furnace with temperature programming under the protection of nitrogen atmosphere, wherein the temperature increasing rate is 10 ℃/min, the temperature increasing is 900 ℃, the heat preservation time is 240min, and finally grinding to obtain the conductive nano carbon spheres.
Application example 1:
the conductive carbon coated silica nanospheres prepared in example 1 were fixed on a sample-carrying stage of a (environmental) scanning electron microscope, and scanning photographic imaging calibration was directly performed without any metal spraying treatment. Shooting is carried out under the condition of accelerating voltage of 25kV and magnification of 20000 times (the size of a scale is 1 mu m), and the same area is selected for shooting in different time periods through the steps of focusing, adjusting contrast, brightness, eliminating astigmatism and the like, and 4 images are shot in each area. The imaging effect of the calibration standard sample is described as follows: (1) whether the image is clearly visible, (2) whether the sphere is deviated or distorted, and (3) whether the brightness and contrast of the image are moderate, and carrying out particle size statistics on the same nanospheres.
The EDS spectrum of fig. 3 shows that the photographed conductive carbon coated silica nanosphere calibration standard is composed of C, O, si elements, and that no characteristic peak of Au element remained after gold spraying appears, which is sufficient to prove that the prepared calibration standard is not subjected to gold spraying treatment. The scanned image of fig. 4 shows that at the high acceleration voltage and magnification described above, the obtained image is excellent in sharpness, moderate in contrast, moderate in brightness, free from distortion and lateral stripes due to poor conductivity. Meanwhile, the same nanospheres photographed in different time periods have smaller particle size statistical error ranges, and the prepared conductive carbon coated silica nanospheres are proved to have good calibration imaging level.
Application example 2:
the conductive carbon coated silica nanospheres prepared in example 1 were fixed on a sample-carrying stage of a (environmental) scanning electron microscope, and scanning photographic imaging calibration was directly performed without any metal spraying treatment. Shooting is carried out under the condition of accelerating voltage of 25kV and magnification factor of 8000 times (the size of a scale is 2 mu m), and the same area is selected for shooting in different time periods through the steps of focusing, adjusting contrast, brightness, eliminating astigmatism and the like, and 4 images are shot in each area. The imaging effect of the calibration standard sample is described as follows: (1) whether the image is clearly visible, (2) whether the sphere is deviated or distorted, and (3) whether the brightness and contrast of the image are moderate, and carrying out particle size statistics on the same nanospheres.
The scanned image of fig. 5 shows that at the high acceleration voltage and magnification described above, the obtained image is excellent in sharpness, moderate in contrast, moderate in brightness, free from distortion and lateral stripes due to poor conductivity. Meanwhile, the same nanospheres photographed in different time periods have smaller particle size statistical error ranges, and the prepared conductive carbon coated silica nanospheres are proved to have good calibration imaging level.
Application example 3:
the conductive carbon coated silica nanospheres prepared in example 1 were fixed on a sample-carrying stage of a (environmental) scanning electron microscope, and scanning photographic imaging calibration was directly performed without any metal spraying treatment. Shooting is carried out under the condition of accelerating voltage of 25kV and magnification factor of 15000 times (the size of a scale is 1 mu m), and the same area is selected for shooting in different time periods through the steps of focusing, adjusting contrast, brightness, eliminating astigmatism and the like, and 4 images are shot in each area. The imaging effect of the calibration standard sample is described as follows: (1) whether the image is clearly visible, (2) whether the sphere is deviated or distorted, and (3) whether the brightness and contrast of the image are moderate, and carrying out particle size statistics on the same nanospheres.
The scanned image of fig. 6 shows that at the high acceleration voltage and magnification described above, the obtained image is excellent in sharpness, moderate in contrast, moderate in brightness, free from distortion and lateral stripes due to poor conductivity. Meanwhile, the same nanospheres photographed in different time periods have smaller particle size statistical error ranges, and the prepared conductive carbon coated silica nanospheres are proved to have good calibration imaging level.
The above-described embodiments are provided to illustrate the gist of the present invention, but are not intended to limit the scope of the present invention. It will be understood by those skilled in the art that various modifications and equivalent substitutions may be made to the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention.
Claims (5)
1. A preparation method of a conductive nano carbon sphere is characterized in that: the method comprises the following steps:
s1, providing spherical nano silicon dioxide;
s2, forming a polydopamine compact layer on the surface of the spherical silicon dioxide;
and S3, performing heat treatment on the polydopamine compact layer to obtain the conductive nano carbon spheres.
2. The method of manufacturing according to claim 1, wherein: in step S1, the specific preparation method is as follows: weighing 1-4ml of 25% ammonia water, 12-48ml of 99.5% absolute ethyl alcohol and 80-100ml of deionized water, vigorously stirring for 20-40min, dropwise adding 1-3ml tetraethoxysilane, and continuously vigorously stirring for 15-45min.
3. The method of manufacturing according to claim 1, wherein: in step S2, the specific preparation method is as follows: adding 50mg/ml dopamine hydrochloride 6-12ml into the spherical nano silicon dioxide solution prepared in the step S1 for self-polymerization for 12-36 hours to obtain brown mixed solution, washing with deionized water to be neutral, and carrying out suction filtration to obtain a brown black solid, namely the spherical nano silicon dioxide coated with polydopamine.
4. The method of manufacturing according to claim 1, wherein: in step S3, the conductive carbon nanospheres are required to be obtained by high-temperature pyrolysis under the atmosphere of inert gas, wherein the inert gas can be selected from nitrogen, argon and helium; the preparation method comprises the following steps: drying the spherical nano silicon dioxide coated with polydopamine obtained in the step S2 in an oven at 80 ℃ for 12 hours, carbonizing the spherical nano silicon dioxide by using a tube furnace with temperature programming under the protection of nitrogen atmosphere, heating at a speed of 5-10 ℃/min, heating at a temperature of 700-900 ℃ for 120-240min, and finally grinding to obtain the conductive nano carbon spheres.
5. Use of the conductive nanocarbon sphere of any of claims 1-4 for scanning electron microscope calibration.
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