CN101819884B - Method for preparing porous carbon thin film material used for supercapacitor electrode - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 38
- 239000000463 material Substances 0.000 title claims abstract description 25
- 239000010409 thin film Substances 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 title claims description 6
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 33
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 33
- 239000004215 Carbon black (E152) Substances 0.000 claims abstract description 30
- 230000008021 deposition Effects 0.000 claims abstract description 24
- 239000010408 film Substances 0.000 claims abstract description 17
- 238000006722 reduction reaction Methods 0.000 claims abstract description 12
- 239000000758 substrate Substances 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 230000001681 protective effect Effects 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims description 85
- 239000010453 quartz Substances 0.000 claims description 53
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 53
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 24
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 24
- 238000000151 deposition Methods 0.000 claims description 23
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 15
- 229910001220 stainless steel Inorganic materials 0.000 claims description 13
- 239000010935 stainless steel Substances 0.000 claims description 13
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 12
- 239000001294 propane Substances 0.000 claims description 12
- 229910052786 argon Inorganic materials 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims description 6
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 6
- 239000005977 Ethylene Substances 0.000 claims description 6
- 239000003990 capacitor Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 229910052759 nickel Inorganic materials 0.000 claims description 6
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 6
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 6
- 238000005229 chemical vapour deposition Methods 0.000 claims description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims 2
- 239000004743 Polypropylene Substances 0.000 claims 1
- 239000004372 Polyvinyl alcohol Substances 0.000 claims 1
- 229910000831 Steel Inorganic materials 0.000 claims 1
- 239000003513 alkali Substances 0.000 claims 1
- 239000002131 composite material Substances 0.000 claims 1
- 238000005336 cracking Methods 0.000 claims 1
- 239000003792 electrolyte Substances 0.000 claims 1
- 239000012528 membrane Substances 0.000 claims 1
- 239000003595 mist Substances 0.000 claims 1
- 229910052697 platinum Inorganic materials 0.000 claims 1
- -1 polypropylene Polymers 0.000 claims 1
- 229920001155 polypropylene Polymers 0.000 claims 1
- 229920002451 polyvinyl alcohol Polymers 0.000 claims 1
- 238000007789 sealing Methods 0.000 claims 1
- 239000010959 steel Substances 0.000 claims 1
- 238000003466 welding Methods 0.000 claims 1
- 238000004321 preservation Methods 0.000 abstract 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 16
- 239000001257 hydrogen Substances 0.000 description 16
- 229910052739 hydrogen Inorganic materials 0.000 description 16
- 239000007772 electrode material Substances 0.000 description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000012495 reaction gas Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000004518 low pressure chemical vapour deposition Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
用于超级电容器电极的多孔碳薄膜材料的制备方法,其步骤为:首先在750~800℃沉积温度下在容器内的沉积位置处放入基片;用真空泵将容器中的空气抽出,使容器内达到高真空,即1-7~10-8Pa的真空状态;向容器内通入惰性保护气体,用质量流量计控制惰性保护气体的流量为70~80mL/s;向容器内通入还原气体,用质量流量计控制气体流量为70~80mL/s;然后向容器内通入烃类混合气体,用质量流量计控制气体流量为50~80mL/s;将容器加热,加热到900~1000℃时进行保温,时间持续1~2小时,混合烃类气体的还原反应使得基底上沉积出多孔碳,即得多孔碳薄膜材料。The preparation method of the porous carbon thin film material used for supercapacitor electrodes comprises the following steps: firstly put the substrate at the deposition position in the container at a deposition temperature of 750-800°C; use a vacuum pump to extract the air in the container to make the container The inside reaches a high vacuum, that is, a vacuum state of 1 -7 ~ 10 -8 Pa; pass an inert protective gas into the container, and use a mass flow meter to control the flow rate of the inert protective gas to 70 ~ 80mL/s; Gas, use a mass flow meter to control the gas flow rate to 70-80mL/s; then pass hydrocarbon mixed gas into the container, use a mass flow meter to control the gas flow rate to 50-80mL/s; heat the container to 900-1000 The heat preservation is carried out at ℃ for 1 to 2 hours, and the reduction reaction of the mixed hydrocarbon gas causes the deposition of porous carbon on the substrate, that is, the porous carbon film material.
Description
技术领域 technical field
本发明涉及一种用于超级电容器电极的多孔碳薄膜材料的制备方法。The invention relates to a preparation method of a porous carbon film material used for supercapacitor electrodes.
背景技术 Background technique
超级电容器由于具有广泛的应用前景和巨大的潜在市场而成为国际能源领域的研究热点。超级电容器主要分为双电层型超级电容器和氧化还原型超级电容器。双电层型超级电容器的比容量主要由材料的表面积决定,其理论容量与电极材料的比表面积成正比。目前主要是通过采用活性炭或者碳纳米管做电极材料,其比容量大约为50~150F/g。对于用纯活性炭或者碳纳米管作为电极的超级电容器,由于碳材料比表面积较低,其低比容问题已成为制约其作为超级电容器电极材料的瓶颈。Due to its broad application prospects and huge potential market, supercapacitors have become a research hotspot in the international energy field. Supercapacitors are mainly divided into electric double layer supercapacitors and redox supercapacitors. The specific capacity of an electric double layer supercapacitor is mainly determined by the surface area of the material, and its theoretical capacity is proportional to the specific surface area of the electrode material. At present, activated carbon or carbon nanotubes are mainly used as electrode materials, and their specific capacity is about 50-150F/g. For supercapacitors using pure activated carbon or carbon nanotubes as electrodes, due to the low specific surface area of carbon materials, the problem of low specific volume has become a bottleneck restricting them as electrode materials for supercapacitors.
发明内容 Contents of the invention
本发明的目的是提供一种用于超级电容器电极的多孔碳薄膜材料的制备方法。The purpose of the present invention is to provide a method for preparing a porous carbon film material used for supercapacitor electrodes.
本发明是这样来实现的,其制备步骤为:The present invention is achieved like this, and its preparation steps are:
(1)首先在750-800℃沉积温度下在容器内的沉积位置处放入基片;(1) First put the substrate at the deposition position in the container at a deposition temperature of 750-800°C;
(2)用真空泵将容器中的空气抽出,使容器内达到高真空,即10-7~10-8Pa的真空状态;(2) Use a vacuum pump to pump out the air in the container to make the container reach a high vacuum, that is, a vacuum state of 10 -7 ~ 10 -8 Pa;
(3)向容器内通入惰性保护气体,用质量流量计控制惰性保护气体的流量为70~80mL/s;(3) Pass inert protective gas into the container, and use a mass flow meter to control the flow rate of the inert protective gas to 70-80mL/s;
(4)向容器内通入还原气体,用质量流量计控制气体流量为70~80mL/s;(4) Feed reducing gas into the container, and use a mass flow meter to control the gas flow to 70-80mL/s;
(5)然后向容器内通入烃类混合气体,用质量流量计控制气体流量为50~80mL/s;(5) Then feed the hydrocarbon mixture gas into the container, and use a mass flow meter to control the gas flow to 50-80mL/s;
(6)将容器加热,加热到900~1000℃时进行保温,时间持续1~2小时,混合烃类气体的还原反应使得基底上沉积出多孔碳,即得多孔碳薄膜材料。(6) Heating the container to 900-1000° C. for 1-2 hours. The reduction reaction of the mixed hydrocarbon gas causes porous carbon to be deposited on the substrate, namely the porous carbon film material.
本发明的有益之处在于:本发明的制备方法制备多孔碳薄膜材料,其化学气相沉积过程是在高温低压条件下进行的,高沉积温度会大幅度改善多孔碳晶体的结晶完整性,沉积过程可以在大尺寸基片或多基片上进行;低压化学气相沉积导致反应气体的扩散系数提高了约三个数量级,因而提高了反应气体和反应产物的扩散能力,总的结果是将多孔碳薄膜的沉积速率提高了一个数量级以上,薄膜厚度均匀性好、气相形核引起颗粒污染的几率小、薄膜较为致密。The benefit of the present invention is that: the preparation method of the present invention prepares porous carbon thin film materials, and its chemical vapor deposition process is carried out under high temperature and low pressure conditions, and the high deposition temperature can greatly improve the crystalline integrity of porous carbon crystals, and the deposition process It can be carried out on large-scale substrates or multi-substrates; low-pressure chemical vapor deposition leads to an increase of the diffusion coefficient of the reaction gas by about three orders of magnitude, thereby improving the diffusion ability of the reaction gas and reaction products, and the overall result is that the porous carbon film The deposition rate is increased by more than an order of magnitude, the film thickness uniformity is good, the probability of particle contamination caused by gas phase nucleation is small, and the film is denser.
此外,最大的益处在于该种多孔碳薄膜材料可直接制作电极,不需要添加石墨、水和粘结剂等添加剂,提高了电极的导电率,同时也提高了碳材料的比表面积,电容器输出比容量明显提高,该方法在提高碳电极的比容上具有非常显著的效果。In addition, the biggest benefit is that this kind of porous carbon film material can be directly used to make electrodes without adding additives such as graphite, water and binders, which improves the conductivity of the electrode, and also increases the specific surface area of the carbon material, and the output ratio of the capacitor. The capacity is obviously improved, and this method has a very significant effect on increasing the specific capacity of the carbon electrode.
具体实施方式 Detailed ways
实施例1:Example 1:
(1)首先在750℃的沉积温度下在石英管内沉积位置处放入不锈钢网;(1) At first, a stainless steel mesh is placed at the deposition position in the quartz tube at a deposition temperature of 750°C;
(2)利用真空泵将石英管中的空气抽出,使石英管内达到高真空,即10-7~10-8Pa的真空状态;(2) Use a vacuum pump to extract the air in the quartz tube, so that the inside of the quartz tube reaches a high vacuum, that is, a vacuum state of 10 -7 ~ 10 -8 Pa;
(3)向石英管内通入氮气,用质量流量计控制氮气的流量为70mL/s;(3) feed nitrogen into the quartz tube, and control the flow of nitrogen with a mass flow meter to be 70mL/s;
(4)向石英管内通入氢气,用质量流量计控制氢气的流量为75mL/s;(4) feed hydrogen into the quartz tube, and the flow rate of hydrogen controlled with a mass flow meter is 75mL/s;
(5)然后用质量流量计控制甲烷气体的流量为52mL/s、乙烯气体的流量为60mL/s、丙烷气体的流量为70mL/s将这三种烃类气体混合均匀,将烃类混合气体通入石英管内;(5) Then use a mass flow meter to control the flow rate of methane gas to be 52mL/s, the flow rate of ethylene gas to be 60mL/s, and the flow rate of propane gas to be 70mL/s to mix these three kinds of hydrocarbon gases evenly, and the hydrocarbon mixed gas into the quartz tube;
(6)对石英管加热并在950℃的温度下保温,时间持续1小时,混合烃类气体的还原反应使得不锈钢网上沉积出多孔碳,即得多孔碳薄膜材料。(6) Heating the quartz tube and keeping it at a temperature of 950° C. for 1 hour, the reduction reaction of the mixed hydrocarbon gas causes porous carbon to be deposited on the stainless steel net, that is, the porous carbon film material.
实施例2:Example 2:
(1)首先在780℃的沉积温度下在石英管内沉积位置处放入镍网;(1) At first, a nickel mesh is placed at the deposition position in the quartz tube at a deposition temperature of 780°C;
(2)利用真空泵将石英管中的空气抽出,使石英管内达到高真空,即(10-710-8Pa的真空状态;(2) Use a vacuum pump to extract the air in the quartz tube, so that the inside of the quartz tube reaches a high vacuum, that is, a vacuum state of (10 −7 10 −8 Pa;
(3)向石英管内通入氮气,用质量流量计控制氮气的流量为75mL/s;(3) feed nitrogen into the quartz tube, and control the flow of nitrogen with a mass flow meter to be 75mL/s;
(4)向石英管内通入氢气,用质量流量计控制氢气的流量为70mL/s;(4) feed hydrogen into the quartz tube, and use a mass flow meter to control the flow of hydrogen to be 70mL/s;
(5)然后用质量流量计控制甲烷气体的流量为55mL/s、乙烯气体的流量为65mL/s、丙烷气体的流量为70mL/s将三种烃类气体混合均匀,将烃类混合气体通入石英管内;(5) Then use a mass flow meter to control the flow of methane gas to be 55mL/s, the flow of ethylene gas to be 65mL/s, and the flow of propane gas to be 70mL/s to mix the three kinds of hydrocarbon gases evenly, and pass the hydrocarbon mixture gas into the quartz tube;
(6)对石英管加热并在950℃的温度下保温,时间持续1.5小时,混合烃类气体的还原反应使得镍网上沉积出多孔碳,即得多孔碳薄膜材料。(6) Heating the quartz tube and keeping it warm at a temperature of 950° C. for 1.5 hours, the reduction reaction of the mixed hydrocarbon gas causes porous carbon to be deposited on the nickel grid, that is, a porous carbon film material.
实施例3:Example 3:
(1)首先在750℃的沉积温度下在石英管内沉积位置处放入不锈钢网;(1) At first, a stainless steel mesh is placed at the deposition position in the quartz tube at a deposition temperature of 750°C;
(2)利用真空泵将石英管中的空气抽出,使石英管内达到高真空,即10-7~10-8Pa的真空状态;(2) Use a vacuum pump to extract the air in the quartz tube, so that the inside of the quartz tube reaches a high vacuum, that is, a vacuum state of 10 -7 ~ 10 -8 Pa;
(3)向石英管内通入氩气,用质量流量计控制氩气的流量为70mL/s;(3) feed argon into the quartz tube, and use a mass flow meter to control the flow of argon to be 70mL/s;
(4)向石英管内通入氢气,用质量流量计控制氢气的流量为75mL/s;(4) feed hydrogen into the quartz tube, and the flow rate of hydrogen controlled with a mass flow meter is 75mL/s;
(5)然后用质量流量计控制甲烷气体的流量为52mL/s、乙烯气体的流量为60mL/s、丙烷气体的流量为70mL/s将三种烃类气体混合均匀,然后将烃类混合气体通入石英管内;(5) Then use a mass flow meter to control the flow rate of methane gas to be 52mL/s, the flow rate of ethylene gas to be 60mL/s, and the flow rate of propane gas to be 70mL/s to mix the three hydrocarbon gases evenly, and then mix the hydrocarbon gas mixture into the quartz tube;
(6)对石英管加热并在950℃的温度下保温,时间持续2小时,混合烃类气体的还原反应使得不锈钢网上沉积出多孔碳,即得多孔碳薄膜材料。(6) Heating the quartz tube and keeping it warm at a temperature of 950° C. for 2 hours, the reduction reaction of the mixed hydrocarbon gas causes porous carbon to be deposited on the stainless steel net, that is, the porous carbon film material.
实施例4:Example 4:
(1)首先在780℃的沉积温度下在石英管内沉积位置处放入镍网;(1) At first, a nickel mesh is placed at the deposition position in the quartz tube at a deposition temperature of 780°C;
(2)利用真空泵将石英管中的空气抽出,使石英管内达到高真空,即10-7~10-8Pa的真空状态;(2) Use a vacuum pump to extract the air in the quartz tube, so that the inside of the quartz tube reaches a high vacuum, that is, a vacuum state of 10 -7 ~ 10 -8 Pa;
(3)向石英管内通入氩气,用质量流量计控制氩气的流量为75mL/s;(3) feed argon gas in the quartz tube, and the flow rate of argon gas controlled with a mass flow meter is 75mL/s;
(4)向石英管内通入氢气,用质量流量计控制氢气的流量为70mL/s;(4) feed hydrogen into the quartz tube, and use a mass flow meter to control the flow of hydrogen to be 70mL/s;
(5)然后用质量流量计控制甲烷气体的流量为55mL/s、乙烯气体的流量为65mL/s、丙烷气体的流量为70mL/s将三种烃类气体混合均匀,然后将烃类混合气体通入石英管内;(5) Then use a mass flow meter to control the flow rate of methane gas to be 55mL/s, the flow rate of ethylene gas to be 65mL/s, and the flow rate of propane gas to be 70mL/s to mix the three hydrocarbon gases evenly, and then mix the hydrocarbon gas mixture into the quartz tube;
(6)对石英管加热并在950℃温度下保温,时间持续1小时,混合烃类气体的还原反应使得镍网上沉积出多孔碳,即得多孔碳薄膜材料。(6) Heating the quartz tube and keeping it warm at 950° C. for 1 hour, the reduction reaction of the mixed hydrocarbon gas causes porous carbon to be deposited on the nickel grid, that is, the porous carbon film material.
实施例5:Example 5:
(1)首先在790℃的沉积温度下在石英管内沉积位置处放入不锈钢网;(1) At first, a stainless steel mesh is placed at the deposition position in the quartz tube at a deposition temperature of 790°C;
(2)利用真空泵将石英管中的空气抽出,使石英管内达到高真空,即10-7~10-8Pa的真空状态;(2) Use a vacuum pump to extract the air in the quartz tube, so that the inside of the quartz tube reaches a high vacuum, that is, a vacuum state of 10 -7 ~ 10 -8 Pa;
(3)向石英管内通入氮气,用质量流量计控制氮气的流量为76mL/s;(3) feed nitrogen into the quartz tube, and control the flow of nitrogen with a mass flow meter to be 76mL/s;
(4)向石英管内通入氢气,用质量流量计控制氢气的流量为75mL/s;(4) feed hydrogen into the quartz tube, and the flow rate of hydrogen controlled with a mass flow meter is 75mL/s;
(5)然后用质量流量计控制甲烷气体的流量为65mL/s、丙烯气体的流量为55mL/s、乙烷的气体流量为75mL/s、丙烷气体的流量为70mL/s将这四种烃类气体混合均匀,然后将烃类混合气体通入石英管内;(5) Control the flow of methane gas with a mass flow meter to be 65mL/s, the flow of propylene gas to be 55mL/s, the flow of ethane gas to be 75mL/s, the flow of propane gas to be 70mL/s with these four kinds of hydrocarbons Mix the hydrocarbon gas evenly, and then pass the hydrocarbon gas mixture into the quartz tube;
(6)对容器加热并在970℃温度下保温,时间持续1.5小时,混合烃类气体的还原反应使得不锈钢片上沉积出多孔碳,即得多孔碳薄膜材料。(6) The container is heated and kept at 970° C. for 1.5 hours. The reduction reaction of the mixed hydrocarbon gas causes porous carbon to be deposited on the stainless steel sheet, that is, a porous carbon film material.
实施例6:Embodiment 6:
(1)首先在800℃的沉积温度下在石英管内沉积位置处放入不锈钢网;(1) At first, a stainless steel mesh is placed at the deposition position in the quartz tube at a deposition temperature of 800°C;
(2)利用真空泵将石英管中的空气抽出,使石英管内达到高真空,即10-7~10-8Pa的真空状态;(2) Use a vacuum pump to extract the air in the quartz tube, so that the inside of the quartz tube reaches a high vacuum, that is, a vacuum state of 10 -7 ~ 10 -8 Pa;
(3)向石英管内通入氮气,用质量流量计控制氮气的流量为80mL/s;(3) feed nitrogen into the quartz tube, and use a mass flow meter to control the flow of nitrogen to be 80mL/s;
(4)向石英管内通入氢气,用质量流量计控制氢气的流量为80mL/s;(4) feed hydrogen into the quartz tube, and use a mass flow meter to control the flow of hydrogen to be 80mL/s;
(5)然后用质量流量计控制甲烷气体的流量为70mL/s、丙烯气体的流量为55mL/s、乙烷的气体流量为75mL/s、丙烷气体的流量为65mL/s将这四种烃类气体混合均匀,然后将烃类混合气体通入石英管内;(5) Then the flow of mass flow meter control methane gas is 70mL/s, the flow of propylene gas is 55mL/s, the flow of ethane gas is 75mL/s, and the flow of propane gas is 65mL/s. Mix the hydrocarbon gas evenly, and then pass the hydrocarbon gas mixture into the quartz tube;
(6)对容器加热并在950℃温度下保温,时间持续2小时,混合烃类气体的还原反应使得不锈钢片上沉积出多孔碳,即得多孔碳薄膜材料。(6) The container is heated and kept at a temperature of 950° C. for 2 hours, and the reduction reaction of the mixed hydrocarbon gas causes porous carbon to be deposited on the stainless steel sheet, that is, a porous carbon film material.
实施例7:Embodiment 7:
(1)首先在790℃的沉积温度下在石英管内沉积位置处放入不锈钢网;(1) At first, a stainless steel mesh is placed at the deposition position in the quartz tube at a deposition temperature of 790°C;
(2)利用真空泵将石英管中的空气抽出,使石英管内达到高真空,即10-7~10-8Pa的真空状态;(2) Use a vacuum pump to extract the air in the quartz tube, so that the inside of the quartz tube reaches a high vacuum, that is, a vacuum state of 10 -7 ~ 10 -8 Pa;
(3)向石英管内通入氩气,用质量流量计控制氩气的流量为76mL/s;(3) feed argon gas into the quartz tube, and the flow rate of argon gas controlled with a mass flow meter is 76mL/s;
(4)向石英管内通入氢气,用质量流量计控制氢气的流量为75mL/s;(4) feed hydrogen into the quartz tube, and the flow rate of hydrogen controlled with a mass flow meter is 75mL/s;
(5)然后用质量流量计控制甲烷气体的流量为65mL/s、丙烯气体的流量为55mL/s、乙烷的气体流量为75mL/s、丙烷气体的流量为70mL/s将这四种烃类气体混合均匀,然后将烃类混合气体通入石英管内;(5) Control the flow of methane gas with a mass flow meter to be 65mL/s, the flow of propylene gas to be 55mL/s, the flow of ethane gas to be 75mL/s, the flow of propane gas to be 70mL/s with these four kinds of hydrocarbons Mix the hydrocarbon gas evenly, and then pass the hydrocarbon gas mixture into the quartz tube;
(6)对容器加热并在970℃温度下保温,时间持续1小时,混合烃类气体的还原反应使得不锈钢片上沉积出多孔碳,即得多孔碳薄膜材料。(6) The container is heated and kept at a temperature of 970° C. for 1 hour, and the reduction reaction of the mixed hydrocarbon gas causes porous carbon to be deposited on the stainless steel sheet, that is, a porous carbon film material.
实施例8:Embodiment 8:
(1)首先在800℃的沉积温度下在石英管内沉积位置处放入不锈钢网;(1) At first, a stainless steel mesh is placed at the deposition position in the quartz tube at a deposition temperature of 800°C;
(2)利用真空泵将石英管中的空气抽出,使石英管内达到高真空,即10-7~10-8Pa的真空状态;(2) Use a vacuum pump to extract the air in the quartz tube, so that the inside of the quartz tube reaches a high vacuum, that is, a vacuum state of 10 -7 ~ 10 -8 Pa;
(3)向石英管内通入氩气,用质量流量计控制氩气的流量为80mL/s;(3) feed argon into the quartz tube, and use a mass flow meter to control the flow of argon to be 80mL/s;
(4)向石英管内通入氢气,用质量流量计控制氢气的流量为80mL/s;(4) feed hydrogen into the quartz tube, and use a mass flow meter to control the flow of hydrogen to be 80mL/s;
(5)然后用质量流量计控制甲烷气体的流量为70mL/s、丙烯气体的流量为55mL/s、乙烷的气体流量为75mL/s、丙烷气体的流量为65mL/s将这四种烃类气体混合均匀,然后将烃类混合气体通入石英管内;(5) Then the flow of mass flow meter control methane gas is 70mL/s, the flow of propylene gas is 55mL/s, the flow of ethane gas is 75mL/s, and the flow of propane gas is 65mL/s. Mix the hydrocarbon gas evenly, and then pass the hydrocarbon gas mixture into the quartz tube;
(6)对容器加热并在950℃的温度下保温,时间持续1.5小时,混合烃类气体的还原反应使得不锈钢片上沉积出多孔碳,即得多孔碳薄膜材料。(6) The container is heated and kept at a temperature of 950° C. for 1.5 hours. The reduction reaction of the mixed hydrocarbon gas causes porous carbon to be deposited on the stainless steel sheet, that is, a porous carbon film material.
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