CN114574891A - 一种双金属共掺杂磷化镍纳米片的制备方法及用途 - Google Patents
一种双金属共掺杂磷化镍纳米片的制备方法及用途 Download PDFInfo
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- 239000002135 nanosheet Substances 0.000 title claims abstract description 33
- FBMUYWXYWIZLNE-UHFFFAOYSA-N nickel phosphide Chemical compound [Ni]=P#[Ni] FBMUYWXYWIZLNE-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 65
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 29
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000001301 oxygen Substances 0.000 claims abstract description 15
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 15
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims abstract description 11
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 8
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000007772 electrode material Substances 0.000 claims abstract description 7
- 230000007062 hydrolysis Effects 0.000 claims abstract description 7
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims abstract description 7
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims abstract description 6
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims abstract description 6
- 239000012300 argon atmosphere Substances 0.000 claims abstract description 6
- 239000004202 carbamide Substances 0.000 claims abstract description 6
- 235000003891 ferrous sulphate Nutrition 0.000 claims abstract description 6
- 239000011790 ferrous sulphate Substances 0.000 claims abstract description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 6
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 6
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims abstract description 6
- 235000002867 manganese chloride Nutrition 0.000 claims abstract description 6
- 239000011565 manganese chloride Substances 0.000 claims abstract description 6
- 229940099607 manganese chloride Drugs 0.000 claims abstract description 6
- 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 6
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 6
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- 239000003755 preservative agent Substances 0.000 claims abstract description 3
- 230000002335 preservative effect Effects 0.000 claims abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 229910052748 manganese Inorganic materials 0.000 claims description 7
- 239000011572 manganese Substances 0.000 claims description 7
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 10
- 239000001257 hydrogen Substances 0.000 description 10
- 229910052739 hydrogen Inorganic materials 0.000 description 10
- 239000006260 foam Substances 0.000 description 9
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- 239000003792 electrolyte Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 239000010411 electrocatalyst Substances 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 238000000634 powder X-ray diffraction Methods 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
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- 229910052697 platinum Inorganic materials 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004832 voltammetry Methods 0.000 description 2
- 238000001075 voltammogram Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000002253 acid Substances 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
- 238000005349 anion exchange Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
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- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000002791 soaking Methods 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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Abstract
本发明公开了一种双金属共掺杂磷化镍纳米片的制备方法和用途,在本发明中,将一定量的氯化锰、硝酸镍、硫酸亚铁、氟化铵和尿素溶解在一定体积的去离子水中,用保鲜膜封口后搅拌,得到澄清透明的溶液,接着将一片泡沫镍放入其中,随后转移到具有聚四氟乙烯内衬的水热反应釜中,进行水热反应,然后冷却,洗涤,烘干,得到干燥后的泡沫镍;将干燥后的泡沫镍与次磷酸钠放入管式炉中,在氩气氛围下烧结退火,冷却后,得到一种双金属共掺杂磷化镍纳米片。电化学验测试表明本方法制备的双金属共掺杂磷化镍纳米片作为电催化水解析氧反应的电极材料具有广阔的应用前景。在整个制备过程中,操作简单,原料成本低,设备投资少,适合批量生产。
Description
技术领域
本发明属于材料化学领域,具体涉及到一种用于提升电解水析氧反应性能的双金属共掺杂磷化镍纳米片的制备方法。
背景技术
随着能源需求和化石燃料消耗的增加,氢能被认为是未来经济中最基本的能源载体之一。然而,如何以一种既环保又方便的方法大规模制氢气是一个极其紧迫的问题。水的电催化分解已成为最有前景的制氢策略之一,因为其环保、高纯度并且无碳排放。水分解由两个半反应组成分别是:析氢反应(HER:2H++2e-→H2)和析氧反应(OER:4OH-→O2+2H2O+4e-)。对于HER或OER反应而言,需要具有高活性、良好选择性和长期稳定性的电催化剂,以降低过电位从而降低生产成本。铂在酸性电解质溶液(0.5M H2SO4)中对HER表现出优良的电催化性能,其起始过电位接近零,而Ir/Ru氧化物在碱性电解质溶液(1.0M KOH)中表现出优异的OER活性。然而,稀有的储量和高昂的成本限制了其在工业中的实际应用。因此,为HER和OER反应制备廉价、高效和稳定的电催化剂仍然是一个巨大的挑战。除了电催化剂的关键热力学和动力学要求外,更重要的是强调一些其他基本要求,以使电催化剂在大规模水电解中经济实惠。第一个问题是催化剂材料资源的可用性,因为我们不能再依赖贵金属(铂、铱和钌)来进行简单的电解水。第二个问题涉及健康和环境危害,催化剂应至少对使用它的人员和环境的危害较小。第三个问题是需要长期稳定性的催化剂,这将会减少催化剂的消耗。
鉴于以上问题,过渡金属磷化物(TMPs)作为全解水电催化剂因其成本低、丰度丰富、价态可调、催化性能好而备受关注,迄今已取得显著进展。其中,Xu及其同事发表了关于她对FeP电催化作用的第一份报告,他们通过阴离子交换法合成了FeP多孔纳米片(Xu,Y.;Wu,R.;Zhang,J.;Shi,Y.;Zhang,B.Chem.Commun.2013,49,6656-6658.)。Du及其同事提出了一种使用氧化铝作为所需硬模板方法,通过简单模板法制备FeP NRs,通过一系列浸泡和干燥过程将Fe3+前体装载到其上,然后在350℃下在管式炉中用次磷酸钠进行磷化(Xu,Y.;Wu,R.;Zhang,J.;Shi,Y.;Zhang,B.Chem.Commun.2013,49,6656-6658.)。Liang等人通过溶剂热处理,在CC上获得FeP NRs纳米阵列(NAs),以形成Fe2O3/CC前驱体,然后在相对较低的温度下使用hypo对其进行磷化处理(Liang,Y.;Liu,Q.;Asiri,A.M.;Sun,X.;Luo,Y.ACSCatal.2014,4,4065-4069)使用类似的合成路线,Tian及其同事在CC上获得了3D FeP NP薄膜,该薄膜在酸性和中性电解质中表现出比其他磷化物更好的性能(Liang,Y.;Liu,Q.;Asiri,A.M.;Sun,X.;Luo,Y.ACS Catal.2014,4,4065-4069)。
发明内容
本发明所要解决的技术问题是针对现有技术,提供一种双金属共掺杂磷化镍纳米片的制备方法。
本发明为解决上述技术问题所采取的技术方案为:一种双金属共掺杂磷化镍纳米片的制备方法,具体包括以下步骤:
1)称取一定量的氯化锰(MnCl2·4H2O)、硝酸镍(Ni(NO3)·6H2O)、硫酸亚铁(FeSO4·4H2O)、氟化铵(NH4F)和尿素(CH4N2O)溶解在一定体积的去离子水中,用保鲜膜封口后搅拌1h,得到澄清的溶液;
2)将泡沫镍放入步骤1所得到的溶液中,随后转移到具有聚四氟乙烯内衬的水热反应釜中,进行水热反应,然后冷却至室温,取出泡沫镍,用去离子水、乙醇先后洗涤后,放入恒温鼓风烘箱进行烘干处理,得到干燥后的泡沫镍;
3)将干燥后的泡沫镍与次磷酸钠放入管式炉中,在氩气氛围下烧结退火,冷却后,得到锰、铁共掺杂磷化镍纳米片,即一种双金属共掺杂磷化镍纳米片,化学表示式Mn、Fe-Ni2P;
进一步的,将上述制备方法制备所得到的双金属共掺杂磷化镍纳米片作为电催化水解析氧反应的电极材料,在1.5M KOH电解液中电流密度为10mA·cm-2下的过电势为222mV,低的过电势有利于提升电解水析氧反应的能耗;在电流密度为50mA cm-2所对应的1.51V(相对标准氢电极电势)电势下,在1.5M KOH电解液中连续测试24小时,电流密度仅下降了1.2%,测试表明该材料具有良好的电化学稳定性。
与现有技术相比,本发明的特点如下:
本发明所制备的双金属共掺杂磷化镍纳米片作为电催化水解析氧反应的电极材料具有优异的电化学反应性能,锰和铁的引入不仅调整了催化材料的电子结构,还为催化材料表面的析氧反应提供了更多可利用的活性中心。另外独特的花状结构具有更大的表面积,也能够为析氧反应提供了更多的活性中心,加速电子的传递。所述制备的双金属共掺杂磷化镍纳米片作为电催化水解析氧反应的电极材料,在1.5M KOH电解液中电流密度为10mAcm-2下过电势为222mV;在电流密度为50mA cm-2所对应的1.51V(相对标准氢电极电势)电势下,连续测试24小时,电流密度仅下降了1.2%,测试表明该材料具有良好的电化学稳定性(图4)。
附图说明
图1为本发明实施例提供的双金属共掺杂磷化镍纳米片的XRD图。
图2为本发明实施例提供的双金属共掺杂磷化镍纳米片的SEM图。
图3为本发明实施例提供的双金属共掺杂磷化镍纳米片作为电催化水解析氧反应的电极材料,在1.5M KOH电解液中的线性伏安曲线图。
图4为本发明实施例提供的双金属共掺杂磷化镍纳米片作为电催化水解析氧反应的电极材料,在50mA cm-2所对应的1.51V(相对标准氢电极电势)电势下,在1.5M KOH电解液中连续测试24h,电流密度仅下降了1.2%的测试图。
具体实施方式
以下结合实施例对本发明作进一步详细描述。
实施例1
称取2.0mmol(0.3g)硫酸亚铁(FeSO4·4H2O),0.5mmol(0.098g)氯化锰(MnCl2·4H2O),2.5mmol(0.72g)硝酸镍(Ni(NO3)2·6H2O),5.0mmol(0.185g)氟化铵(NH4F),10mmol(0.6g)尿素(CH4N2O)加入到35mL去离子水中,然后密封搅拌1h,得到澄清的溶液;将一块泡沫镍(2×4cm)和上述溶液放入具有聚四氟乙烯内衬的反应釜中,在160℃高温下反应8h,然后冷却至室温,取出泡沫镍,用去离子水、乙醇先后洗涤后,放入恒温鼓风烘箱进行烘干处理,得到干燥后的泡沫镍;将干燥后的泡沫镍与次磷酸钠(质量比1:10)放入管式炉中,在氩气氛围下350℃下烧结退火2h,得到锰、铁共掺杂磷化镍纳米片,即一种双金属共掺杂磷化镍纳米片,化学表示式Mn、Fe-Ni2P;将得到的双金属共掺杂磷化镍纳米片进行X射线粉末衍射XRD测试分析其组成结构(图1);用扫描电子显微镜SEM观察材料的形貌(图2);用电化学测试仪测试材料在析氧反应过程中的线性伏安曲线(图3),用电化学测试仪在1.5M KOH电解液中50mA cm-2电流密度所对应的1.51V(相对标准氢电极电势)电势下,连续测试24小时电流密度的变化图,结果显示电流密度仅下降了1.2%(图4)。
实施例2
称取1.5mmol(0.225g)硫酸亚铁(FeSO4·4H2O),1.0mmol(0.196g)氯化锰(MnCl2·4H2O),2.0mmol(0.576g)硝酸镍(Ni(NO3)2·6H2O),5.0mmol(0.185g)氟化铵(NH4F),10mmol(0.6g)尿素(CH4N2O)加入到35mL去离子水中,然后密封搅拌1h,得到澄清的溶液;将一块泡沫镍(2×4cm)和上述溶液放入具有聚四氟乙烯内衬的反应釜中,在160℃高温下反应8h,冷却至室温,取出泡沫镍,用去离子水、乙醇先后洗涤后,放入恒温鼓风烘箱进行烘干处理,得到干燥后的泡沫镍;将干燥后的泡沫镍与次磷酸钠(质量比1:10)放入管式炉中,在氩气氛围下,350℃下烧结退火2h,得到锰、铁共掺杂磷化镍纳米片,即一种双金属共掺杂磷化镍纳米片;将得到双金属共掺杂磷化镍纳米片进行X射线粉末衍射测试分析其组成结构;用扫描电子显微镜SEM观察材料的形貌;用电化学测试仪测试材料在析氧反应过程中的线性伏安曲线,用电化学测试仪在50mA cm-2电流密度所对应的1.51V(相对标准氢电极电势)电势下,测试材料的电化学稳定性能。
实施例3
称取1.0mmol(0.15g)硫酸亚铁(FeSO4·4H2O),1.5mmol(0.294g)氯化锰(MnCl2·4H2O),2.0mmol(0.576g)硝酸镍(Ni(NO3)2·6H2O),5.0mmol(0.185g)氟化铵(NH4F),10mmol(0.6g)尿素(CH4N2O)加入到35mL去离子水中,然后密封搅拌1h,得到澄清的溶液;将一块泡沫镍(2×4cm)和上述溶液放入具有聚四氟乙烯内衬的反应釜中,在160℃高温下反应8h,冷却至室温,取出泡沫镍,用去离子水、乙醇先后洗涤后,放入恒温鼓风烘箱进行烘干处理,得到干燥后的泡沫镍;将干燥后的泡沫镍与次磷酸钠(质量比1:10)放入管式炉中,在氩气氛围下,350℃下烧2h,得到一种双金属共掺杂磷化镍纳米片;将得到的双金属共掺杂磷化镍纳米片进行X射线粉末衍射测试分析其组成结构;用扫描电子显微镜观察材料的形貌;用电化学测试仪测试材料在析氧反应过程中的线性伏安曲线,用电化学测试仪在50mA cm-2电流密度所对应的1.51V(相对标准氢电极电势)电势下,测试材料的电化学稳定性能。
Claims (2)
1.一种双金属共掺杂磷化镍纳米片的制备方法,其特征在于,所述制备方法包括以下步骤:
1)称取氯化锰(MnCl2·4H2O)、硝酸镍(Ni(NO3)2·6H2O)、硫酸亚铁(FeSO4·4H2O)、氟化铵(NH4F)和尿素(CH4N2O)溶解在去离子水中,用保鲜膜封口后搅拌1h,得到澄清的溶液;
2)将泡沫镍放入步骤1)所得到的溶液中,随后转移到具有聚四氟乙烯内衬的水热反应釜中,进行水热反应,然后冷却至室温,取出泡沫镍,用去离子水、乙醇先后洗涤后,放入恒温鼓风烘箱进行烘干处理,得到干燥后的泡沫镍;
3)将干燥后的泡沫镍与次磷酸钠放入管式炉中,在氩气氛围下烧结退火,冷却后,得到锰、铁共掺杂磷化镍纳米片,即双金属共掺杂磷化镍纳米片。
2.一种根据利要求1所叙述制备方法得到的双金属共掺杂磷化镍纳米片的用途,其特征在于,该双金属共掺杂磷化镍纳米片作为电催化水解析氧反应的电极材料,在1.5M KOH电解液中电流密度为10mA cm-2下过电势为222mV。
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