CN110548525B - 一种碳纳米管复合镍硒纳米片电催化剂的制备方法 - Google Patents
一种碳纳米管复合镍硒纳米片电催化剂的制备方法 Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 26
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 26
- 239000002135 nanosheet Substances 0.000 title claims abstract description 23
- QHASIAZYSXZCGO-UHFFFAOYSA-N selanylidenenickel Chemical compound [Se]=[Ni] QHASIAZYSXZCGO-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 239000002131 composite material Substances 0.000 title claims abstract description 16
- 239000010411 electrocatalyst Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 27
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims abstract description 5
- 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
- 239000000843 powder Substances 0.000 claims abstract description 5
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 5
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 13
- 239000011669 selenium Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 239000002244 precipitate Substances 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 241000282414 Homo sapiens Species 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 229940075397 calomel Drugs 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000002447 crystallographic data Methods 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical compound Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910021397 glassy carbon Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000005464 sample preparation method Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/057—Selenium or tellurium; Compounds thereof
- B01J27/0573—Selenium; Compounds thereof
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Abstract
本发明公开一种碳纳米管复合镍硒纳米片电催化剂的制备方法,包括以下步骤:将Se粉、硼氢化钠、碳纳米管和硝酸镍溶于乙腈和乙二醇的混合溶液中,在180℃微波辅助反应24小时。
Description
技术领域
本发明涉及一种碳纳米管复合镍硒纳米片电催化剂的制备方法。
技术背景
人类社会的快速发展,造成了常规能源的过度消耗和自然资源的浪费,环境污染越来越严重,进而影响了人类的长期发展。因此,清洁能源的利用近来引起了广泛关注。其中,氢燃料因其出色的燃烧性能以及高的能量密度而被认为是最有前途的绿色能源。此外,氢的来源非常广泛,通过很多方式可以获得氢能源。其中,通过电解水制氢被认为是最有效的方式。目前,效率最高的析氢催化剂是Pt基金属。但是,由于这些极高成本的贵金属相对缺乏,因此未在电催化领域广泛使用。探索廉价且性能优异的电催化剂来替代贵金属至关重要。
衡量电催化剂性能好坏的指标之一即为过电位。过电位太高则会导致在采用电催化生产氢气的过程中浪费过多的能源。因此探索出具有较低过电位的非贵金属电催化剂是亟待解决的问题。
发明内容
本发明的目的在于提供一种具有低过电位的一种碳纳米管复合镍硒纳米片电催化剂的制备方法。
本发明的实现包括以下步骤:将0.4mmolSe粉和1mmol硼氢化钠添加至60mL乙腈和乙二醇的混合溶液中,其中乙腈和乙二醇各30mL,磁力搅拌1小时;再将50mg碳纳米管和0.35mmol硝酸镍添加至上述溶液中,磁力搅拌1小时;再将上述溶液密封于100mL的反应釜中,将反应釜放置在微波辅助加热马弗炉中保持24小时,其中马弗炉温度设置为180℃,微波频率设置为1500兆赫兹,微波功率设置为140瓦;冷却到室温;将溶液中的沉淀物用酒精清洗3次后,放置于50℃的烘箱中保温24小时。
与现有技术相比,本发明所述的样品制备方法具有以下的优点:制备的样品呈纳米片结构,暴露的活性位点较多,过电位较低;成本较低。
附图说明
图1是碳纳米管复合镍硒纳米片电催化剂的X射线衍射图谱。
图2是碳纳米管复合镍硒纳米片电催化剂的扫描电镜图谱。
图3是镍硒纳米片电催化剂的扫描电镜图谱。
图4是碳纳米管的扫描电镜图谱。
图5是碳纳米管复合镍硒纳米片电催化剂和镍硒纳米片电催化剂的过电位曲线图。
具体实施方式
以下结合具体实施例对本发明的实现进行详细的描述。
本实施例的具体步骤如下:将0.4mmolSe粉和1mmol硼氢化钠添加至60mL乙腈和乙二醇的混合溶液中,其中乙腈和乙二醇各30mL,磁力搅拌1小时;再将50mg碳纳米管和0.35mmol硝酸镍添加至上述溶液中,磁力搅拌1小时;再将上述溶液密封于100mL的反应釜中,将反应釜放置在微波辅助加热马弗炉中保持24小时,其中马弗炉温度设置为180℃,微波频率设置为1500兆赫兹,微波功率设置为140瓦;冷却到室温;将溶液中的沉淀物用酒精清洗3次后,放置于50℃的烘箱中保温24小时。
为了说明不添加碳纳米管时的技术效果,还按以下步骤制备了镍硒纳米片样品:将0.4mmolSe粉和1mmol硼氢化钠添加至60mL乙腈和乙二醇的混合溶液中,其中乙腈和乙二醇各30mL,磁力搅拌1小时;再将0.35mmol硝酸镍添加至上述溶液中,磁力搅拌1小时;再将上述溶液密封于100mL的反应釜中,将反应釜放置在微波辅助加热马弗炉中保持24小时,其中马弗炉温度设置为180℃,微波频率设置为1500兆赫兹,微波功率设置为140瓦;冷却到室温;将溶液中的沉淀物用酒精清洗3次后,放置于50℃的烘箱中保温24小时。
为了说明本实施例的技术效果,对按实施例的方法步骤制备的样品进行了表征。图1是X射线衍射方法测得的衍射数据,样品的衍射峰位分别与标准数据库中的Ni0.85Se和碳纳米管的衍射峰位一致,说明合成的样品为Ni0.85Se和碳纳米管的复合物。对样品做扫描电镜表征,结果如图2-4所示,Ni0.85Se为纳米片结构的形貌,碳纳米管为纳米管的形貌,碳纳米管复合镍硒纳米片的形貌呈现为Ni0.85Se纳米片分散于碳纳米管中。过电位表征的条件为:以0.5M硫酸溶液作为电解液,样品涂覆在玻碳电极上作为工作电极,甘汞电极作为参考电极,石墨电极作为对电极。样品的过电位曲线如图5所示。通常采用-10mA/cm2时的过电位来评价电催化性能的好坏,碳纳米管复合镍硒纳米片的过电位为-161mV,表现出优异的电催化性能。为了和文献中报道的Ni0.85Se纳米晶的结果进行对比(文献中给出的数据是-30mA/cm2时的过电位为-275mV),如图5所示,本申请的Ni0.85Se纳米片的过电位为-254mv,过电位更低。此外,碳纳米管复合镍硒纳米片在-30mA/cm2时的过电位为-233mV,性能更加优异。
本发明还公开了一种碳纳米管复合镍硒纳米片电催化剂,其采用如实施例所述的方法制备而成。
需要声明的是,以上所述的仅是本发明的优选实施方式,本发明不限于以上实施例。可以理解,本领域技术人员在不脱离本发明的基本构思的前提下直接导出或联想到的其他改进和变化,均应认为包含在本发明的保护范围之内。
Claims (2)
1.一种碳纳米管复合镍硒纳米片电催化剂的制备方法,包括如下步骤:将0.4mmolSe粉和1mmol硼氢化钠添加至60mL乙腈和乙二醇的混合溶液中,其中乙腈和乙二醇各30mL,磁力搅拌1小时;再将50mg碳纳米管和0.35mmol硝酸镍添加至所得溶液中,磁力搅拌1小时;再将所得溶液密封于100mL的反应釜中,将反应釜放置在微波辅助加热马弗炉中保持24小时,其中马弗炉温度设置为180℃,微波频率设置为1500兆赫兹,微波功率设置为140瓦;冷却到室温;将溶液中的沉淀物用酒精清洗3次后,放置于50℃的烘箱中保温24小时。
2.一种碳纳米管复合镍硒纳米片电催化剂,其特征在于,所述电催化剂采用如权利要求1中的方法制备而成。
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