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CN-121976168-A - Method for preparing porous carbon substrate by combining chemical vapor deposition with template method

CN121976168ACN 121976168 ACN121976168 ACN 121976168ACN-121976168-A

Abstract

The invention discloses a method for preparing a porous carbon substrate by combining chemical vapor deposition with a template method, which comprises the following steps of S1, selecting a template material, pretreating the surface of the template, S2, placing the pretreated template in a chemical vapor deposition reactor, and depositing a carbon layer on the surface of the template under a protective atmosphere by taking carbon source gas as a precursor, wherein the deposition reaction temperature is 600-900 ℃, the deposition reaction time is 30-120 min, the carbon source gas flow is 50-200 mL/min, S3, carrying out template removal treatment on the composite material to obtain the porous carbon substrate, and carrying out carbon deposition by adopting a template and a CVD technology, wherein the carbon layer can accurately replicate the internal and external surface morphology of the template, so that the problem of uneven filling by a traditional liquid phase method is avoided.

Inventors

  • MENG FANCHANG
  • WANG MENG
  • CHEN WEIDONG

Assignees

  • 浙江嘉兴星汉纳米科技有限公司

Dates

Publication Date
20260505
Application Date
20251225

Claims (7)

  1. 1. A method for preparing a porous carbon substrate by combining chemical vapor deposition with a template method, which is characterized by comprising the following steps: S1, selecting a template material, and preprocessing the surface of the template; S2, placing the pretreated template in a chemical vapor deposition reactor, and depositing a carbon layer on the surface of the template under a protective atmosphere by taking carbon source gas as a precursor, wherein the deposition reaction temperature is 600-900 ℃, the deposition reaction time is 30-120 min, and the flow rate of the carbon source gas is 50-200 mL/min; S3, performing template removal treatment on the composite material to obtain a porous carbon substrate; The template material is one or more of SiO 2 nanospheres, MOFs or polymer gel, in the step S3 of template removal treatment, a hydrofluoric acid solution is adopted for etching and removing the SiO 2 nanosphere template, high-temperature calcination and removal are adopted for the MOFs template, and an organic solvent is adopted for extraction and removal for the polymer gel template.
  2. 2. The method for preparing the porous carbon substrate by combining the chemical vapor deposition with the template method according to claim 1 is characterized in that in the step S1, in the pretreatment of the template surface, a mixed solution of dilute hydrochloric acid and ethanol is adopted for ultrasonic cleaning of a SiO 2 nanosphere template for 10-30 min, then the template is dried in a nitrogen atmosphere, in the MOFs template, the mixed solvent of methanol and acetone is adopted for soaking and cleaning for 2-4 times for 30-60 min each time, then the template is dried in a vacuum condition, in the polymer gel template, deionized water is adopted for soaking and cleaning for 3-5 times, and in the vacuum drying box at 40-60 ℃ each time.
  3. 3. The method for preparing a porous carbon substrate by combining chemical vapor deposition with a template method according to claim 1, wherein in the step S2, the protective atmosphere is one or more of argon or nitrogen, the gas flow is 100-500 mL/min, and the carbon source gas is one or more of methane, ethylene or acetylene.
  4. 4. The method for preparing the porous carbon substrate by combining chemical vapor deposition with the template method according to claim 1, wherein in the step S2 of deposition reaction, the deposition reaction pressure is 10-100 Pa, and the heating rate is 5-10 ℃ per minute.
  5. 5. The method for preparing the porous carbon substrate by combining the chemical vapor deposition with the template method according to claim 1, wherein the SiO 2 nanosphere template has a particle size of 200-500 nm and a monodispersity coefficient of less than 0.1, the MOFs template is one of ZIF-8, HKUST-1 or MIL-100 (Fe), and the polymer gel template is polyacrylamide gel or polyvinyl alcohol gel.
  6. 6. The method for preparing the porous carbon substrate by combining chemical vapor deposition with the template method according to claim 1, wherein the pore size distribution range of the porous carbon substrate is 10-1000 nm, the specific surface area is 500-2000 m < 2 >/g, and the pore volume is 0.5-2.0 cm < 3 >/g.
  7. 7. The porous carbon substrate is characterized in that the porous carbon substrate is prepared by adopting the method for preparing the porous carbon substrate by combining chemical vapor deposition with a template method according to any one of claims 1-6, the porous carbon substrate has an ordered pore structure which is highly re-carved with the shape of the template, the thickness of a pore wall is 5-50 nm, and the graphitization degree of a carbon layer is 60-90%.

Description

Method for preparing porous carbon substrate by combining chemical vapor deposition with template method Technical Field The invention relates to the technical field of porous carbon material preparation, in particular to a method for preparing a porous carbon substrate by combining chemical vapor deposition with a template method. Background The porous carbon material has wide application in the fields of super capacitor, catalyst carrier, adsorption separation and the like due to high specific surface area, excellent conductivity and chemical stability. The traditional porous carbon preparation method such as an activation method has the problems of uncontrollable pore structure, uneven specific surface area distribution and the like. The template method can prepare porous carbon with an ordered pore structure through the shape guidance of the template, but in the prior art, the pore structure collapse is easily caused by the template removing step, the carbon layer deposition efficiency is low, and high-precision shape re-etching is difficult to realize. Disclosure of Invention The invention aims to provide a method for preparing a porous carbon substrate by combining chemical vapor deposition with a template method, which aims to solve the problems that in the prior art, the template removing step is easy to cause collapse of a pore structure, high-precision morphology re-etching is difficult to realize and the like. In order to achieve the aim, the invention provides the following technical scheme that the method for preparing the porous carbon substrate by combining chemical vapor deposition with a template method comprises the following steps: S1, selecting a template material, and preprocessing the surface of the template; S2, placing the pretreated template in a chemical vapor deposition reactor, and depositing a carbon layer on the surface of the template under a protective atmosphere by taking carbon source gas as a precursor, wherein the deposition reaction temperature is 600-900 ℃, the deposition reaction time is 30-120 min, and the flow rate of the carbon source gas is 50-200 mL/min; S3, performing template removal treatment on the composite material to obtain a porous carbon substrate; The template material is one or more of SiO 2 nanospheres, MOFs or polymer gel, in the step S3 of template removal treatment, a hydrofluoric acid solution is adopted for etching and removing the SiO 2 nanosphere template, high-temperature calcination and removal are adopted for the MOFs template, and an organic solvent is adopted for extraction and removal for the polymer gel template. Preferably, in the step S1, the SiO 2 nanosphere template is subjected to ultrasonic cleaning by adopting a mixed solution of dilute hydrochloric acid and ethanol for 10-30 min and then is subjected to drying treatment in a nitrogen atmosphere, the MOFs template is soaked and cleaned for 2-4 times by adopting a mixed solvent of methanol and acetone for 30-60 min each time and then is subjected to drying treatment under a vacuum condition, and the polymer gel template is soaked and cleaned for 3-5 times by adopting deionized water each time for 1-2 h and then is subjected to drying treatment by adopting a 40-60 ℃ vacuum drying oven. Preferably, in the step S2, the protective atmosphere is one or more of argon and nitrogen, the gas flow is 100-500 ml/min, and the carbon source gas is one or more of methane, ethylene and acetylene. Preferably, in the step S2 deposition reaction, the deposition reaction pressure is 10-100 Pa, and the heating rate is 5-10 ℃ per minute. Preferably, the SiO 2 nanosphere template has a particle size of 200-500 nm and a monodispersity coefficient of less than 0.1, the MOFs template is one of ZIF-8, HKUST-1 or MIL-100 (Fe), and the polymer gel template is polyacrylamide gel or polyvinyl alcohol gel. Preferably, the porous carbon substrate has a pore size distribution range of 10-1000 nm, a specific surface area of 500-2000 m2/g, and a pore volume of 0.5-2.0 cm3/g. The porous carbon substrate is provided with an ordered pore structure which is highly re-carved with the shape of a template, the thickness of a pore wall is 5-50 nm, and the graphitization degree of a carbon layer is 60-90%. The invention has the beneficial effects that: the template and the CVD technology are adopted for carbon deposition, the carbon layer can accurately copy the internal and external surface morphology of the template, the problem of uneven filling in the traditional liquid phase method is avoided, the prepared porous carbon has complete and ordered structure and narrow pore size distribution, and the accurate regulation and control of the pore structure are realized. For different templates (such as SiO 2 nanospheres, various MOFs, polymer gels and other templates), different template removal treatment modes are adopted, the template removal efficiency is high, the damage rate of a carbon structure is low, and the damage of