CN114506842A - Three-dimensional carbon nanotube aggregate material and preparation method thereof - Google Patents
Three-dimensional carbon nanotube aggregate material and preparation method thereof Download PDFInfo
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- CN114506842A CN114506842A CN202210230520.6A CN202210230520A CN114506842A CN 114506842 A CN114506842 A CN 114506842A CN 202210230520 A CN202210230520 A CN 202210230520A CN 114506842 A CN114506842 A CN 114506842A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 57
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 56
- 239000000463 material Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000002243 precursor Substances 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000001354 calcination Methods 0.000 claims abstract description 12
- 239000004005 microsphere Substances 0.000 claims abstract description 7
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims abstract description 7
- 239000004926 polymethyl methacrylate Substances 0.000 claims abstract description 7
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000011261 inert gas Substances 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 238000007598 dipping method Methods 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 7
- 239000012298 atmosphere Substances 0.000 claims description 6
- 239000012159 carrier gas Substances 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 239000012445 acidic reagent Substances 0.000 claims description 2
- 230000004323 axial length Effects 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- 238000005530 etching Methods 0.000 claims 1
- 238000011065 in-situ storage Methods 0.000 claims 1
- 239000002105 nanoparticle Substances 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 3
- 238000001816 cooling Methods 0.000 abstract description 3
- 238000000197 pyrolysis Methods 0.000 abstract description 2
- 239000011259 mixed solution Substances 0.000 abstract 1
- 238000005303 weighing Methods 0.000 description 4
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- 239000012300 argon atmosphere Substances 0.000 description 2
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- 239000000126 substance Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000011144 upstream manufacturing Methods 0.000 description 2
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- 238000001237 Raman spectrum Methods 0.000 description 1
- 241000722270 Regulus Species 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 239000007772 electrode material Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- 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
- C01B32/158—Carbon nanotubes
- C01B32/16—Preparation
- C01B32/162—Preparation characterised by catalysts
Abstract
A three-dimensional carbon nanotube aggregate material and a preparation method thereof belong to the field of carbon nanotubes. The carbon nanotube aggregate material has a continuous three-dimensional network structure, and is composed of randomly oriented and intertwined carbon nanotubes. The material can be prepared in batches by a simple gradient temperature calcination strategy by adopting a self-template method. Specifically, the preparation method comprises the following steps: and (2) taking a polymethyl methacrylate microsphere template filled with a mixed solution of nickel nitrate and citric acid as a precursor, simultaneously placing the precursor in two different calcining temperature zones, calcining the precursor under the protection of inert gas at normal pressure and a certain flow rate, and cooling to room temperature to obtain the carbon nano tube aggregate material. The carbon nano tube provided by the invention does not need to add extra catalyst, has simple preparation method and low cost, can be prepared in a large scale, and provides a new method for preparing the three-dimensional carbon nano tube by a pyrolysis method.
Description
Technical Field
The invention relates to the technical field of carbon materials, in particular to a three-dimensional carbon nanotube aggregate material and a preparation method thereof.
Background
Carbon Nanotubes (CNTs) can be regarded as seamless hollow tubes formed by winding single-layer or multi-layer graphene sheets, exhibit excellent electrical and thermal conductivity and mechanical strength due to their special structure and nano-size, and show great application potential in the fields of energy storage and conversion, field effect transistors, super-strong fibers, biomedicine, and the like. Other advantages, such as good stability, large specific surface area and chemical modifiability, also make it suitable for more applications. In addition, since most practical applications require macroscopic materials, it is necessary to aggregate single carbon nanotubes into a macroscopic structure while maintaining the excellent properties of the carbon nanotubes. Another advantage of such macroscopic states is the ease of handling and use of the carbon nanotube material under a variety of conditions. At present, the carbon nano tube macroscopic body mainly comprises a three-dimensional block material, a two-dimensional film structure, a one-dimensional fiber and the like, wherein the carbon nano tube three-dimensional material has the structural characteristics of a three-dimensional conductive network, a large specific surface area, high porosity and the like, so that the carbon nano tube macroscopic body has wide application prospects in the fields of electrode materials, catalysis, adsorption and the like.
Currently, Chemical Vapor Deposition (CVD) is the primary method of carbon nanotube preparation, which typically involves pyrolysis of hydrocarbon gas at a temperature of 600 ℃. — -1000 ℃ on the surface of an active catalyst supported on a substrate. Even when a proper supporting substrate (such as silicon dioxide, quartz or alumina) is selected, strict process control is required, and the problems of relatively complicated preparation process, high cost and energy consumption and the like still remain to be solved. Therefore, it is very important to develop a method for preparing the carbon nanotube aggregate simply, green and easily on a large scale to facilitate its practical application.
Disclosure of Invention
The invention aims to provide a three-dimensional carbon nanotube aggregate material and a preparation method thereof. The method has the advantages of low cost, simple preparation process and the like.
Therefore, the invention provides a three-dimensional carbon nanotube aggregate material which is composed of randomly oriented and wound carbon nanotubes, wherein the carbon nanotubes with small and uniform tube diameters form a continuous three-dimensional network structure, and the outer diameter of a single carbon nanotube is 7-13 nm.
The invention provides a preparation method of a three-dimensional carbon nanotube aggregate material, which comprises the following steps:
s1, dissolving citric acid and nickel nitrate solid in deionized water, and fully stirring to obtain a precursor solution;
s2, putting the polymethyl methacrylate microsphere template into the precursor liquid to be completely soaked, and performing suction filtration and drying to obtain a precursor;
and S3, dividing the precursor obtained in the step S2 into two parts, respectively placing the two parts in two different temperature areas of the same tube furnace, namely a low temperature area and a high temperature area, calcining the two parts under the conditions of normal pressure and inert atmosphere carrier gas, supplying a carbon source to the material in the high temperature area through the carrier gas to the material in the low temperature area, and finally obtaining the three-dimensional carbon nanotube aggregate material in the high temperature area.
Further, the concentration of citric acid in the precursor liquid is 1-2 mol/L; preferably, the concentration of citric acid in the precursor solution is 1 mol/L.
Further, the concentration of nickel nitrate in the precursor liquid is 2-3 mol/L; preferably, the concentration of citric acid in the precursor liquid is 2 mol/L.
Further, the dipping time is 4-8h at room temperature; preferably, the dipping condition is that the dipping time is 4h at room temperature.
Further, the calcination temperatures corresponding to the two different temperature zones in the step S3 are 300-375 ℃ and 450-1000 ℃. Preferably, the calcination temperatures of the two different temperature zones in the step S3 are 300 ℃ and 450-600 ℃ respectively. In some embodiments of the invention, the calcination temperature of the high temperature zone is 450 ℃ and 600 ℃.
Further, the roasting conditions in the step S3 are specifically: the inert atmosphere is argon, the gas flow rate is 20-80sccm, the pressure is normal pressure, the two temperature zones are heated to respective target temperature from room temperature at the same heating rate of 5-10 ℃/min, then the temperature is kept for 40-60min, and the temperature is naturally reduced to the room temperature.
Preferably, the roasting conditions in the step S3 are specifically: the inert atmosphere is argon, the gas flow rate is 80sccm, the pressure is normal pressure, the two temperature zones are heated to respective target temperatures from room temperature at the same heating rate of 10 ℃/min, then the temperature is kept for 60min, and the three-dimensional carbon nano tube aggregate material is obtained in the high temperature zone.
And (3) introducing inert gas carrier gas into the tubular furnace adopted in the step S3 along the axial length direction, wherein the low-temperature area is positioned in front of the high-temperature area along the gas flow direction, and the low-temperature area and the high-temperature area are respectively and independently heated.
In addition, the nickel component in the material can be conveniently etched and removed by an acid reagent according to the application requirement, and the carbon nano tube material is obtained.
The preparation method provided by the invention has the following beneficial effects:
according to the preparation method of the three-dimensional carbon nanotube aggregate material, provided by the invention, the self-template method is adopted, the three-dimensional carbon nanotube aggregate material can be prepared at a lower temperature through simple operations such as dipping, two-stage gradient calcination and the like without adding an additional catalyst, and the prepared carbon nanotubes are uniform in size and are interconnected to form a three-dimensional continuous network. The preparation process is novel, the raw material sources are rich, the cost and the energy consumption are reduced, and the wide application prospect is shown.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a schematic diagram of the preparation of a three-dimensional carbon nanotube aggregate material prepared in example 1-2;
FIG. 2 is an X-ray diffraction pattern (XRD) of the carbon nanotube aggregate material obtained in example 1-2, wherein (a) is a sample prepared at a temperature of 450 ℃ in the high temperature region and (b) is a sample prepared at a temperature of 600 ℃ in the high temperature region;
FIG. 3 is a Raman spectrum of the carbon nanotube aggregate material obtained in example 1-2, wherein (a) is a sample prepared at a temperature of 450 ℃ in the high temperature region and (b) is a sample prepared at a temperature of 600 ℃ in the high temperature region;
FIG. 4 is a scanning electron microscope photograph of the carbon nanotube aggregate material prepared in example 1;
fig. 5 is a scanning electron microscope image and a transmission electron microscope image of the carbon nanotube aggregate material prepared in example 2.
Detailed Description
The present invention will be further described with reference to the following examples, which are not intended to limit the invention to the preferred embodiments described herein, nor to limit the invention to the following examples. Any product that is identical or similar to the present invention, whether made in accordance with the teachings of the present invention or combined with other features of the prior art, is within the scope of the present invention.
The specific operation method and test method adopted by the invention are conventional methods in the field, and if no special description is given, the operation or conditions can be determined according to the conventional experiment described in the literature in the field. The reagents related to the invention are all conventional commercial products.
Example 1
The present embodiment provides a three-dimensional carbon nanotube aggregate material, which is composed of randomly oriented and wound carbon nanotubes, and the carbon nanotubes with small and uniform tube diameters form a continuous three-dimensional network structure.
The preparation method of the three-dimensional carbon nanotube aggregate material comprises the following steps:
s1, weighing citric acid and Ni (NO)3)2·6H2Dissolving O solid in deionized water, stirring thoroughly to obtain precursor solution containing citric acid 1mol/L and Ni (NO)3)2·6H2The concentration of O is 2 mol/L;
s2, weighing a polymethyl methacrylate microsphere template, adding the polymethyl methacrylate microsphere template into the precursor liquid, soaking for 4 hours, and then carrying out vacuum filtration and natural drying to obtain a precursor;
s3, placing the precursor into two different temperature areas of the same tube furnace, heating the upstream low-temperature area from room temperature to 300 ℃, heating the downstream high-temperature area from room temperature to 450 ℃ at a heating rate of 10 ℃/min under the conditions of normal pressure and 80sccm argon atmosphere, keeping the two temperature areas at the same temperature for 60min, and then naturally cooling to room temperature to obtain the three-dimensional carbon nanotube aggregate material;
example 2
The present embodiment provides a three-dimensional carbon nanotube aggregate material, which is composed of randomly oriented and entangled carbon nanotubes, and the carbon nanotubes with fine and uniform diameters form a continuous three-dimensional network structure.
The preparation method of the three-dimensional carbon nanotube aggregate material comprises the following steps:
s1, weighing citric acid and Ni (NO)3)2·6H2Dissolving O solid in deionized water, stirring thoroughly to obtain precursor solution containing citric acid 1mol/L and Ni (NO)3)2·6H2The concentration of O is 2 mol/L;
s2, weighing a polymethyl methacrylate microsphere template, adding the polymethyl methacrylate microsphere template into the precursor liquid, soaking for 4 hours, and then carrying out vacuum filtration and natural drying to obtain a precursor;
s3, placing the precursor into two different temperature areas of the same tube furnace, heating the upstream low-temperature area from room temperature to 300 ℃, heating the downstream high-temperature area from room temperature to 600 ℃, keeping the two temperature areas at the same temperature for 60min at the heating rate of 10 ℃/min under the conditions of normal pressure and 80sccm argon atmosphere, and then naturally cooling to room temperature to obtain the three-dimensional carbon nanotube aggregate material;
test example 1
Physical properties such as a crystal structure, morphology, chemical components and the like of the aggregate material consisting of the obtained carbon nanotubes are measured by using instruments such as a D8-Focus type X-ray diffractometer (XRD), a Regulus 8100 type Scanning Electron Microscope (SEM), a JEM F200 type high-resolution electron projection microscope (TEM), a LabRam HR Evolution type Raman spectrometer (Raman) and the like.
It should be understood that the above examples are only examples for helping understanding the method of the present invention and the core idea thereof, and are not intended to limit the embodiments. It should be noted that various changes and modifications in other forms can be made by those skilled in the art without departing from the principle of the present invention, and these changes and modifications are still within the scope of the appended claims.
Claims (10)
1. The three-dimensional carbon nanotube aggregate material is characterized by consisting of randomly oriented and wound carbon nanotubes, wherein the carbon nanotubes with small and uniform tube diameters form a continuous three-dimensional network structure, and the outer diameter of a single carbon nanotube is 7-13 nm.
2. The method for preparing the three-dimensional carbon nanotube aggregate material of claim 1, comprising the steps of:
s1, dissolving citric acid and nickel nitrate solid in deionized water, and fully stirring to obtain a precursor solution;
s2, putting the polymethyl methacrylate microsphere template into the precursor liquid to be completely soaked, and performing suction filtration and drying to obtain a precursor;
and S3, dividing the precursor obtained in the step S2 into two parts, respectively placing the two parts in two different temperature areas of the same tube furnace, namely a low temperature area and a high temperature area, calcining the two parts under the conditions of normal pressure and inert atmosphere carrier gas, supplying a carbon source to the material in the high temperature area through the carrier gas to the material in the low temperature area, and finally obtaining the three-dimensional carbon nanotube aggregate material in the high temperature area.
3. The method of claim 2, wherein the concentration of citric acid in the precursor solution is 1-2 mol/L; preferably, the concentration of citric acid in the precursor solution is 1 mol/L.
4. The method according to claim 2, wherein the concentration of nickel nitrate in the precursor solution is 2 to 3 mol/L; preferably, the concentration of citric acid in the precursor liquid is 2 mol/L.
5. The method according to claim 2, wherein the dipping conditions are a dipping time of 4 to 8 hours at room temperature; preferably, the dipping condition is that the dipping time is 4h at room temperature.
6. The method as claimed in claim 2, wherein the calcination temperatures of the two different temperature zones in the S3 step are 300-375 ℃ and 450-1000 ℃, respectively; preferably, the calcination temperatures of the two different temperature zones in the step S3 are 300 ℃ and 450-600 ℃ respectively. In some embodiments of the invention, the calcination temperature of the high temperature zone is 450 ℃ or 600 ℃.
7. The method according to claim 2, wherein the roasting conditions in the step S3 are as follows: the inert atmosphere is argon, the gas flow rate is 20-80sccm, the pressure is normal pressure, the two temperature zones are heated to respective target temperature from room temperature at the same heating rate of 5-10 ℃/min, then the temperature is kept for 40-60min, and the temperature is naturally reduced to the room temperature.
8. The method according to claim 2, wherein the roasting conditions in the step S3 are as follows: the inert atmosphere is argon, the gas flow rate is 80sccm, the pressure is normal pressure, the two temperature zones are heated to respective target temperatures from room temperature at the same heating rate of 10 ℃/min, then the temperature is kept for 60min, and the three-dimensional carbon nano tube aggregate material is obtained in the high temperature zone.
9. The method as set forth in claim 2, wherein said step S3 is performed by introducing an inert gas carrier gas into the tube furnace along the axial length direction, and the low temperature zone is located in front of the high temperature zone in the gas flow direction, thereby separately heating the low temperature zone and the high temperature zone.
10. The method according to claim 2, wherein nickel nanoparticles formed in situ in the high temperature zone during the preparation catalyze the growth of carbon nanotubes on a three-dimensional structure to obtain a carbon nanotube aggregate material; the nickel can be conveniently removed by etching with an acidic reagent according to the application requirements, and a pure carbon nanotube material is obtained.
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Citations (4)
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| CN106129410A (en) * | 2016-07-18 | 2016-11-16 | 吉科猛 | The class Graphene Carbon Materials of three-dimensional ordered macroporous structure, prepare and apply |
| KR20210031074A (en) * | 2019-09-11 | 2021-03-19 | 한국교통대학교산학협력단 | Cathode active material of hollow structure prepared by using a surfactant, preparation method thereof and lithium secondary battery comprising the same |
| CN113213452A (en) * | 2021-06-11 | 2021-08-06 | 天津大学 | Three-dimensional ordered macroporous carbon material composed of carbon nanotubes and preparation method thereof |
| CN113410459A (en) * | 2021-06-11 | 2021-09-17 | 天津大学 | Embedded MoSxThree-dimensional ordered macroporous graphene carbon material of nanosheet, preparation and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106129410A (en) * | 2016-07-18 | 2016-11-16 | 吉科猛 | The class Graphene Carbon Materials of three-dimensional ordered macroporous structure, prepare and apply |
| KR20210031074A (en) * | 2019-09-11 | 2021-03-19 | 한국교통대학교산학협력단 | Cathode active material of hollow structure prepared by using a surfactant, preparation method thereof and lithium secondary battery comprising the same |
| CN113213452A (en) * | 2021-06-11 | 2021-08-06 | 天津大学 | Three-dimensional ordered macroporous carbon material composed of carbon nanotubes and preparation method thereof |
| CN113410459A (en) * | 2021-06-11 | 2021-09-17 | 天津大学 | Embedded MoSxThree-dimensional ordered macroporous graphene carbon material of nanosheet, preparation and application |
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