CN114408886A - 一种贵金属掺杂的多孔磷化铁镍的制备 - Google Patents
一种贵金属掺杂的多孔磷化铁镍的制备 Download PDFInfo
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- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 229910000510 noble metal Inorganic materials 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 28
- 239000011780 sodium chloride Substances 0.000 claims abstract description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000001257 hydrogen Substances 0.000 claims abstract description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 13
- 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 12
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 239000002086 nanomaterial Substances 0.000 claims abstract description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 5
- 239000006260 foam Substances 0.000 claims description 29
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 229910052786 argon Inorganic materials 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 11
- 238000011144 upstream manufacturing Methods 0.000 claims description 11
- 238000001291 vacuum drying Methods 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 3
- 229910000000 metal hydroxide Inorganic materials 0.000 abstract description 5
- 239000002243 precursor Substances 0.000 abstract description 5
- 150000004692 metal hydroxides Chemical class 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 2
- 229910000863 Ferronickel Inorganic materials 0.000 description 17
- 239000003054 catalyst Substances 0.000 description 6
- 229910019891 RuCl3 Inorganic materials 0.000 description 5
- 238000005868 electrolysis reaction Methods 0.000 description 4
- 239000010411 electrocatalyst Substances 0.000 description 3
- 239000002135 nanosheet Substances 0.000 description 3
- 229910052723 transition metal Inorganic materials 0.000 description 3
- 150000003624 transition metals Chemical class 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 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 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910002621 H2PtCl6 Inorganic materials 0.000 description 1
- 229910021638 Iridium(III) chloride Inorganic materials 0.000 description 1
- 229910021604 Rhodium(III) chloride Inorganic materials 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000009510 drug design Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000001493 electron microscopy Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- HTXDPTMKBJXEOW-UHFFFAOYSA-N iridium(IV) oxide Inorganic materials O=[Ir]=O HTXDPTMKBJXEOW-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(IV) oxide Inorganic materials O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/08—Other phosphides
- C01B25/088—Other phosphides containing plural metal
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Abstract
本发明涉及一种贵金属掺杂的多孔磷化铁镍的制备,其特征在于,在常温下利用NaCl和贵金属氯化物腐蚀泡沫镍铁合成金属氢氧化物前驱体,与次亚磷酸钠一起低温焙烧得到贵金属掺杂的多孔磷化铁镍纳米材料。本发明所述制备方法简单、温和、成本低廉和材料结构新颖,该贵金属掺杂的多孔磷化铁镍纳米材料在室温下表现出高效的电催化析氢反应性能。
Description
技术领域
本发明涉及一种贵金属掺杂的多孔磷化铁镍的制备,属于材料的制备领域。
背景技术
随着经济的快速发展,大量的化石能源被消耗,造成一系列的环境问题,以及能源的短缺,寻找替代化石能源成了当今亟需解决的问题。氢能被认为在未来可以取代化石燃料,电解水是目前制取氢气最好的一种方法,然而在电解水过程中动力学迟滞过程,需要较大的过电位,进一步降低了水电解的效率。虽然Pt基纳米材料和IrO2/RuO2被认为是分别析氢反应和析氧反应的高性能电催化剂,但是由于其高昂的价格和稀少的含量使得无法广泛应用。对此,合理设计高性能、低成本的电催化剂已成为催化研究的热门课题之一,在全球范围内引发了更多的兴趣。
近些年来,人们在制造催化剂方面做了很多的努力,非贵金属基催化剂,例如碳化物、硫化物等,可以加快水电解效率并最大限度地减少成本。特别是过渡金属磷化物(TMPs)被认为在析氢反应中可以取代贵金属的催化剂。最近研究表明过渡金属磷化物也可用于析氧反应。尽管取得了重大进展,但大多数报道的催化剂的电催化活性并不理想,并不优于商用Pt和Ru。因此,开发具有较高活性的TMPs基电化学水分解催化剂仍是迫切需要的有效策略,而掺杂少量的贵金属可以有效的提升催化剂的催化性能。中国专利CN107376958B以镍铁化合物、氟化铵和尿素为原料,在基底保温生长NiFe-LDH纳米片,通过低温磷化,得到NiFeP过渡金属磷化物纳米片。中国专利CN109174162B通过水热反应合成的氢氧化物前驱体,进一步在低温磷化反应下得到Ni1CoxFeyP纳米片阵列电催化剂。以上专利都是通过水热合成的金属氢氧化物前驱体,进而进行低温磷化得到最终产物,然而这些方法受到到温度、阴离子和pH值的影响比较大,而且能耗较高。因此,非常需要开发一种制备多金属氢氧化物然后通过低温磷化得到金属磷化物高效电催化剂的新方法。
发明内容
本发明旨在提供一种贵金属掺杂的多孔磷化铁镍的制备方法和在电催化反应中的应用。
基于以上目的,本发明所涉及的技术方案如下:
1)将泡沫镍铁切割成1.5cm×1cm的小片,然后将其浸入到含有NaCl和贵金属氯化物的溶液中并搅拌12h,取出泡沫镍铁用去离子水洗涤数次,在60℃的真空干燥箱中干燥3h;最后将干燥的泡沫镍铁和次亚磷酸钠分别放在管式炉下游和上游;然后,将管式加热炉加热到350℃,升温速率5℃/min,在氩气中保温2h。自然冷却后,得到了贵金属掺杂的多孔磷化铁镍。
2)将贵金属掺杂的多孔磷化铁镍用于室温电催化析氢反应。在析氢反应中电流密度为10mA cm-2和50mA cm-2时的电位分别为18mV和75mV。
本发明具有以下优点:
1)本发明利用NaCl和贵金属氯化物腐蚀泡沫镍铁合成金属氢氧化物前驱体,进而一步磷化合成贵金属掺杂的多孔磷化铁镍有效的拓展了双金属氢氧化物纳米材料的制备方法。
2)本发明所述制备方法具有简单高效、温和、成本低廉的特点。
附图说明
图1是金属掺杂的多孔磷化铁镍的表征结果,(a-b)电镜图片,(c)XPS图和(d)XRD图。
具体实施方式
下面结合实施例对本发明进行近一步说明,但是本发明不仅限于以下实施例。
实施例1
贵金属掺杂的多孔磷化铁镍具体制备过程如下:将一块泡沫镍铁放入含有50mMNaCl和10mg RuCl3的烧杯中在室温下搅12h。取出泡沫镍铁,用去离子水洗涤数次,在60℃的真空干燥箱中干燥3h;最后将干燥的泡沫镍铁和0.4g次亚磷酸钠分别放在管式炉下游和上游;然后,将管式加热炉加热到250℃,升温速率5℃/min,在氩气中保温2h。自然冷却后,得到了贵金属掺杂的多孔磷化铁镍。
实施例2
贵金属掺杂的多孔磷化铁镍具体制备过程如下:将一块泡沫镍铁放入含有50mMNaCl和10mg RuCl3的烧杯中在室温下搅拌12h。取出泡沫镍铁,用去离子水洗涤数次,在60℃的真空干燥箱中干燥3h;最后将干燥的泡沫镍铁和0.5g次亚磷酸钠分别放在管式炉下游和上游;然后,将管式加热炉加热到250℃,升温速率5℃/min,在氩气中保温2h。自然冷却后,得到了贵金属掺杂的多孔磷化铁镍。
实施例3
贵金属掺杂的多孔磷化铁镍具体制备过程如下:将一块泡沫镍铁放入含有50mMNaCl和10mg RuCl3的烧杯中在室温下搅拌12h。取出泡沫镍铁,用去离子水洗涤数次,在60℃的真空干燥箱中干燥3h;最后将干燥的泡沫镍铁和0.6g次亚磷酸钠分别放在管式炉下游和上游;然后,将管式加热炉加热到250℃,升温速率5℃/min,在氩气中保温2h。自然冷却后,得到了贵金属掺杂的多孔磷化铁镍。
实施例4
贵金属掺杂的多孔磷化铁镍具体制备过程如下:将一块泡沫镍铁放入含有50mMNaCl和10mg RuCl3的烧杯中在室温下搅拌12h。取出泡沫镍铁,用去离子水洗涤数次,在60℃的真空干燥箱中干燥3h;最后将干燥的泡沫镍铁和0.5g次亚磷酸钠分别放在管式炉下游和上游;然后,将管式加热炉加热到350℃,升温速率5℃/min,在氩气中保温2h。自然冷却后,得到了贵金属掺杂的多孔磷化铁镍。
实施例5
贵金属掺杂的多孔磷化铁镍具体制备过程如下:将一块泡沫镍铁放入含有50mMNaCl和10mg RuCl3的烧杯中在室温下搅拌12h。取出泡沫镍铁,用去离子水洗涤数次,在60℃的真空干燥箱中干燥3h;最后将干燥的泡沫镍铁和0.5g次亚磷酸钠分别放在管式炉下游和上游;然后,将管式加热炉加热到450℃,升温速率5℃/min,在氩气中保温2h。自然冷却后,得到了贵金属掺杂的多孔磷化铁镍。
实施例6
贵金属掺杂的多孔磷化铁镍具体制备过程如下:将一块泡沫镍铁放入含有50mMNaCl和10mg IrCl3的烧杯中在室温下搅拌12h。取出泡沫镍铁,用去离子水洗涤数次,在60℃的真空干燥箱中干燥3h;最后将干燥的泡沫镍铁和0.5g次亚磷酸钠分别放在管式炉下游和上游;然后,将管式加热炉加热到350℃,升温速率5℃/min,在氩气中保温2h。自然冷却后,得到了贵金属掺杂的多孔磷化铁镍。
实施例7
贵金属掺杂的多孔磷化铁镍具体制备过程如下:将一块泡沫镍铁放入含有50mMNaCl和10mg RhCl3的烧杯中在室温下搅拌12h。取出泡沫镍铁,用去离子水洗涤数次,在60℃的真空干燥箱中干燥3h;最后将干燥的泡沫镍铁和0.5g次亚磷酸钠分别放在管式炉下游和上游;然后,将管式加热炉加热到350℃,升温速率5℃/min,在氩气中保温2h。自然冷却后,得到了贵金属掺杂的多孔磷化铁镍。
实施例8
贵金属掺杂的多孔磷化铁镍具体制备过程如下:将一块泡沫镍铁放入含有50mMNaCl和10mg H2PtCl6的烧杯中在室温下搅拌12h。取出泡沫镍铁,用去离子水洗涤数次,在60℃的真空干燥箱中干燥3h;最后将干燥的泡沫镍铁和0.5g次亚磷酸钠分别放在管式炉下游和上游;然后,将管式加热炉加热到350℃,升温速率5℃/min,在氩气中保温2h。自然冷却后,得到了贵金属掺杂的多孔磷化铁镍
实施例9
贵金属掺杂的多孔磷化铁镍具体制备过程如下:将一块泡沫镍铁放入含有50mMNaCl和10mg PdCl3的烧杯中在室温下搅拌12h。取出泡沫镍铁,用去离子水洗涤数次,在60℃的真空干燥箱中干燥3h;最后将干燥的泡沫镍铁和0.5g次亚磷酸钠分别放在管式炉下游和上游;然后,将管式加热炉加热到350℃,升温速率5℃/min,在氩气中保温2h。自然冷却后,得到了贵金属掺杂的多孔磷化铁镍
实施例10
将实施例4制备的产物测试电催化析氢性能,将所制泡沫镍固定在电极夹上做工作电极,然后采用三电极法(可逆氢为参比电极,碳棒为辅助电极)在电化学工作站上测试析氢性能,电解液为1mol/L KOH溶液。电流密度为10mA cm-2和50mA cm-2时的电位分别为18mV和75mV。
Claims (2)
1.一种贵金属掺杂的多孔磷化铁镍的制备,所述纳米材料通过室温下与NaCl和贵金属氯化物搅拌,然后通过低温磷化得到,在室温下可高效电催化析氢反应;贵金属掺杂的多孔磷化铁镍由如下步骤制得:将泡沫镍铁切割成1.5cm×1cm的小片,然后将其浸入到含有NaCl和贵金属氯化物的溶液中并搅拌12h,取出泡沫镍铁用去离子水洗涤数次,在60℃的真空干燥箱中干燥3h;最后将干燥的泡沫镍铁和次亚磷酸钠分别放在管式炉下游和上游;然后,将管式加热炉加热到350℃,升温速率5℃/min,在氩气中保温2h。自然冷却后,得到了贵金属掺杂的多孔磷化铁镍。
2.按照权利要求1所述的方法,其特征在于:
将贵金属掺杂的多孔磷化铁镍用于室温电催化析氢反应。在析氢反应中电流密度为10mA cm-2和50mA cm-2时的电位分别为18mV和75mV。
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