CN112007666A - 一种镍铁硒纳米片阵列材料及其应用 - Google Patents
一种镍铁硒纳米片阵列材料及其应用 Download PDFInfo
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- 239000002135 nanosheet Substances 0.000 title claims abstract description 32
- UHVZOSVJPDWNHJ-UHFFFAOYSA-N [Se].[Fe].[Ni] Chemical compound [Se].[Fe].[Ni] UHVZOSVJPDWNHJ-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 239000000463 material Substances 0.000 title claims abstract description 21
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 67
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 33
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910018162 SeO2 Inorganic materials 0.000 claims abstract description 13
- 229910052603 melanterite Inorganic materials 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 10
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 10
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 10
- 238000002791 soaking Methods 0.000 claims abstract description 10
- 238000004140 cleaning Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000012535 impurity Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 5
- 239000011669 selenium Substances 0.000 claims description 12
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 10
- 229910052711 selenium Inorganic materials 0.000 claims description 10
- 229910000863 Ferronickel Inorganic materials 0.000 claims description 9
- JPJALAQPGMAKDF-UHFFFAOYSA-N selenium dioxide Chemical compound O=[Se]=O JPJALAQPGMAKDF-UHFFFAOYSA-N 0.000 claims description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 4
- 239000004094 surface-active agent Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 abstract description 6
- 239000010935 stainless steel Substances 0.000 abstract description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 9
- 229910052739 hydrogen Inorganic materials 0.000 description 9
- 239000001257 hydrogen Substances 0.000 description 9
- 239000006260 foam Substances 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910021607 Silver chloride Inorganic materials 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 230000010287 polarization Effects 0.000 description 5
- 230000002441 reversible effect Effects 0.000 description 5
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000011031 large-scale manufacturing process Methods 0.000 description 3
- 150000003346 selenoethers Chemical class 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- DUIOKRXOKLLURE-UHFFFAOYSA-N 2-octylphenol Chemical compound CCCCCCCCC1=CC=CC=C1O DUIOKRXOKLLURE-UHFFFAOYSA-N 0.000 description 1
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- PYHYDDIOBZRCJU-UHFFFAOYSA-N [Ni]=[Se].[Co] Chemical compound [Ni]=[Se].[Co] PYHYDDIOBZRCJU-UHFFFAOYSA-N 0.000 description 1
- CPYJQJCFBJRNQD-UHFFFAOYSA-N [Se].[Mn].[Ni] Chemical compound [Se].[Mn].[Ni] CPYJQJCFBJRNQD-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 1
- 239000010411 electrocatalyst Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- HTXDPTMKBJXEOW-UHFFFAOYSA-N iridium(IV) oxide Inorganic materials O=[Ir]=O HTXDPTMKBJXEOW-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 description 1
- 229910000357 manganese(II) sulfate Inorganic materials 0.000 description 1
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002060 nanoflake Substances 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229940051841 polyoxyethylene ether Drugs 0.000 description 1
- 229920000056 polyoxyethylene ether Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(IV) oxide Inorganic materials O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- QHASIAZYSXZCGO-UHFFFAOYSA-N selanylidenenickel Chemical compound [Se]=[Ni] QHASIAZYSXZCGO-UHFFFAOYSA-N 0.000 description 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 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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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
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Abstract
本发明公开了一种镍铁硒纳米片阵列材料及其应用。本发明的镍铁硒纳米片阵列材料通过以下方法制备:将泡沫镍置于1~5mol/L的盐酸中浸泡5~20min,去除表面杂质,将处理后的泡沫镍置于装有水热溶液的聚四氟乙烯内胆中,所述水热溶液的组成为:1~10mmol/L FeSO4·7H2O和2~20mmol/L SeO2,将内胆放入不锈钢高压反应釜中,控制水热温度100~180℃和水热时间2~16h,反应完成后冷却至室温,取出后用去离子水和乙醇洗净、冷风吹干后即得到镍铁硒纳米片阵列覆盖的泡沫镍。本发明以镍铁硒纳米片作为活性位点,可有效提高活性组分的比表面积,而且具有良好的循环稳定性。
Description
技术领域
本发明涉及材料领域,具体地说是一种镍铁硒纳米片阵列材料及其作为电催化析氧电极的应用。
背景技术
氢能被认为是最有希望替代化石燃料的清洁能源,相对于其它清洁能源,其受自然条件制约少,有利于大规模生产。电解水制氢方法简单且制得的氢气纯度高,有着广阔的工业前景。但由于其成本较高和效率较低,限制了进一步的发展。这是由于析氧反应(OER)缓慢的动力学导致水的实际分解电压远大于1.23V。IrO2和RuO2是目前商用的贵金属析氧催化剂,它们具有优异的析氧催化剂性能,但是其储量稀缺且价格昂贵不能用于大规模生产。因需要寻找价格低廉且性能优异的催化剂。
铁、钴、镍等过渡金属具有分布广泛和成本较低等优点。然而,单一的廉价金属材料电子电导率和催化稳定性较差,不能满足能源领域的需求。因此需要对廉价金属进行改性以调高其催化性能。镍基硫化物作为析氧催化剂已经被广泛研究。相对硫元素而言,硒元素具有更强的金属性能,因而,开发具有更强电子传输能力的镍基硒化物作为析氧电催化剂材料对于水分解的实际应用具有重要意义。
发明内容
本发明所要解决的技术问题是克服上述现有技术存在的缺陷,提供一种具有较低过电位和良好循环稳定性的镍铁硒纳米片阵列材料。
为实现上述目的,本发明采用如下技术方案:一种镍铁硒纳米片阵列材料,其通过以下方法制备:
将泡沫镍置于1-5mol/L的盐酸中浸泡5-20min,去除表面杂质,将处理后的泡沫镍置于装有水热溶液的聚四氟乙烯内胆中,所述水热溶液的组成为:1-10mmol/L FeSO4·7H2O和2-20mmol/L SeO2,将聚四氟乙烯内胆放入反应釜中,控制水热温度100-180℃和水热时间2-16h,反应完成后冷却至室温,取出后用去离子水和乙醇洗净、冷风吹干后即得到镍铁硒纳米片阵列覆盖的泡沫镍。
作为优选,所述的盐酸浓度为2-4mol/L,浸泡时间为10-20min。
作为优选,所述水热溶液的组成为:5-10mmol/L FeSO4·7H2O和10-15mmol/LSeO2。
更优选地,所述水热溶液的组成为:10mmol/L FeSO4·7H2O和10mmol/L SeO2。
作为优选,所述的水热温度为120-160℃,水热时间为8-12h。
最优选地,所述的水热温度为140℃,水热时间为12h。
作为优选,所述的水热溶液中还有表面活性剂。所述的表面活性剂可采用十二烷基苯磺酸钠、十六烷基三甲基溴化铵、辛基酚的聚氧乙烯醚等。
进一步地,所述的FeSO4·7H2O也可采用CoSO4·6H2O、MnSO4·7H2O或NiSO4·7H2O代替,形成镍钴硒、镍锰硒、镍硒纳米片阵列材料。当然,采用FeSO4·7H2O的产品性能最好。
本发明还提供上述镍铁硒纳米片阵列材料作为电催化析氧电极的应用。
与现有技术相比,本发明具有的有益效果在于:
1)以镍铁硒纳米片作为活性位点,可有效提高活性组分的比表面积,而且具有良好的循环稳定性;
2)一般采用水热合成制备硒化物材料时使用Se粉,但Se粉有毒,而且需要将Se先与强还原剂反应后再进行水热。而SeO2可溶于水,不需要与强还原剂反应,有利于水热反应的进行。
3)另一方面,SeO2水溶液呈酸性,在水热过程中会与泡沫镍基体反应生成Ni2+,有利于原位生长镍铁基硒化物。
4)原料可循环利用,工艺流程简单,制备成本低,有利于大规模生产。
附图说明
图1为本发明实施例1所制得的镍铁硒阵列材料的SEM图。
具体实施方式
下面通过实施例对本发明进行进一步的说明,但本发明的保护范围并不仅限于此。
实施例1
将泡沫镍置于1mol/L的盐酸中浸泡20min去除表面杂质,将前处理后的泡沫镍置于装有水热溶液的聚四氟乙烯内胆中,所述水热溶液的组成为:FeSO4·7H2O(10mmol/L)和SeO2(2mmol/L),将内胆放入不锈钢高压反应釜中,控制水热温度100℃和水热时间16h,反应完成后冷却至室温,取出后用去离子水和乙醇洗净、冷风吹干后即得到镍铁硒纳米片阵列覆盖的泡沫镍。
在25℃的1.0mol/L KOH中,以上述有“镍铁硒纳米片阵列”的泡沫镍为工作电极,石墨片为对电极,Ag/AgCl为参比电极,以1.0mV·s-1的扫速进行稳态极化曲线测试,1.5V(相对于可逆氢电极)电位下电流密度能达到42mA·cm-2。
实施例2
将泡沫镍置于5mol/L的盐酸中浸泡5min去除表面杂质,将前处理后的泡沫镍置于装有水热溶液的聚四氟乙烯内胆中,所述水热溶液的组成为:FeSO4·7H2O(1mmol/L)和SeO2(20mmol/L),将内胆放入不锈钢高压反应釜中,控制水热温度180℃和水热时间2h,反应完成后冷却至室温,取出后用去离子水和乙醇洗净、冷风吹干后即得到镍铁硒纳米片阵列覆盖的泡沫镍。
在25℃的1.0mol/L KOH中,以上述有“镍铁硒纳米片阵列”的泡沫镍为工作电极,石墨片为对电极,Ag/AgCl为参比电极,以1.0mV·s-1的扫速进行稳态极化曲线测试,1.5V(相对于可逆氢电极)电位下电流密度能达到86mA·cm-2。
实施例3
将泡沫镍置于5mol/L的盐酸中浸泡5min去除表面杂质,将前处理后的泡沫镍置于装有水热溶液的聚四氟乙烯内胆中,所述水热溶液的组成为:FeSO4·7H2O(10mmol/L)和SeO2(10mmol/L),将内胆放入不锈钢高压反应釜中,控制水热温度140℃和水热时间12h,反应完成后冷却至室温,取出后用去离子水和乙醇洗净、冷风吹干后即得到镍铁硒纳米片阵列覆盖的泡沫镍。
在25℃的1.0mol/L KOH中,以上述有“镍铁硒纳米片阵列”的泡沫镍为工作电极,石墨片为对电极,Ag/AgCl为参比电极,以1.0mV·s-1的扫速进行稳态极化曲线测试,1.5V(相对于可逆氢电极)电位下电流密度能达到121mA·cm-2。
实施例4
将泡沫镍置于4mol/L的盐酸中浸泡15min去除表面杂质,将前处理后的泡沫镍置于装有水热溶液的聚四氟乙烯内胆中,所述水热溶液的组成为:FeSO4·7H2O(10mmol/L)和SeO2(10mmol/L),将内胆放入不锈钢高压反应釜中,控制水热温度140℃和水热时间12h,反应完成后冷却至室温,取出后用去离子水和乙醇洗净、冷风吹干后即得到镍铁硒纳米片阵列覆盖的泡沫镍。
在25℃的1.0mol/L KOH中,以上述有“镍铁硒纳米片阵列”的泡沫镍为工作电极,石墨片为对电极,Ag/AgCl为参比电极,以1.0mV·s-1的扫速进行稳态极化曲线测试,1.5V(相对于可逆氢电极)电位下电流密度能达到128mA·cm-2。
实施例5
将泡沫镍置于3mol/L的盐酸中浸泡10min去除表面杂质,将前处理后的泡沫镍置于装有水热溶液的聚四氟乙烯内胆中,所述水热溶液的组成为:FeSO4·7H2O(7mmol/L)和SeO2(7mmol/L),将内胆放入不锈钢高压反应釜中,控制水热温度120℃和水热时间10h,反应完成后冷却至室温,取出后用去离子水和乙醇洗净、冷风吹干后即得到镍铁硒纳米片阵列覆盖的泡沫镍。
在25℃的1.0mol/L KOH中,以上述有“镍铁硒纳米片阵列”的泡沫镍为工作电极,石墨片为对电极,Ag/AgCl为参比电极,以1.0mV·s-1的扫速进行稳态极化曲线测试,1.5V(相对于可逆氢电极)电位下电流密度能达到101mA·cm-2。
Claims (8)
1.一种镍铁硒纳米片阵列材料,其特征在于,通过以下方法制备:
将泡沫镍置于1-5mol/L的盐酸中浸泡5-20min,去除表面杂质,将处理后的泡沫镍置于装有水热溶液的聚四氟乙烯内胆中,所述水热溶液的组成为:1-10mmol/L FeSO4·7H2O和2-20mmol/L SeO2,将聚四氟乙烯内胆放入反应釜中,控制水热温度100-180℃和水热时间2-16h,反应完成后冷却至室温,取出后用去离子水和乙醇洗净、冷风吹干后即得到镍铁硒纳米片阵列覆盖的泡沫镍。
2.如权利要求1所述的镍铁硒纳米片阵列材料,其特征在于,所述的盐酸浓度为2-4mol/L,浸泡时间为10-20min。
3.如权利要求1或2所述的镍铁硒纳米片阵列材料,其特征在于,所述水热溶液的组成为:5-10mmol/L FeSO4·7H2O和10-15mmol/L SeO2。
4.如权利要求3所述的镍铁硒纳米片阵列材料,其特征在于,所述水热溶液的组成为:10mmol/L FeSO4·7H2O和10mmol/L SeO2。
5.如权利要求1或2所述的镍铁硒纳米片阵列材料,其特征在于,所述的水热温度为120-160℃,水热时间为8-12h。
6.如权利要求5所述的镍铁硒纳米片阵列材料,其特征在于:所述的水热温度为140℃,水热时间为12h。
7.如权利要求1或2所述的镍铁硒纳米片阵列材料,其特征在于,所述的水热溶液中还有表面活性剂。
8.权利要求1-7任一项所述镍铁硒纳米片阵列材料作为电催化析氧电极的应用。
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