CN112058286A - 一种二维普鲁士蓝类似物@MXene复合电催化剂的原位制备方法 - Google Patents
一种二维普鲁士蓝类似物@MXene复合电催化剂的原位制备方法 Download PDFInfo
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- CN112058286A CN112058286A CN202010863888.7A CN202010863888A CN112058286A CN 112058286 A CN112058286 A CN 112058286A CN 202010863888 A CN202010863888 A CN 202010863888A CN 112058286 A CN112058286 A CN 112058286A
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- Prior art keywords
- mxene
- dimensional
- prussian blue
- blue analogue
- chloride
- Prior art date
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- 238000002360 preparation method Methods 0.000 title claims abstract description 40
- 239000002131 composite material Substances 0.000 title claims abstract description 39
- 239000010411 electrocatalyst Substances 0.000 title claims abstract description 38
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 43
- 238000003756 stirring Methods 0.000 claims abstract description 34
- 239000002243 precursor Substances 0.000 claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 25
- 239000007787 solid Substances 0.000 claims abstract description 17
- 239000003446 ligand Substances 0.000 claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000001509 sodium citrate Substances 0.000 claims abstract description 12
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 9
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical class [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000005530 etching Methods 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 229910009819 Ti3C2 Inorganic materials 0.000 claims description 14
- 229910052751 metal Inorganic materials 0.000 claims description 14
- 239000002184 metal Substances 0.000 claims description 14
- 150000003839 salts Chemical class 0.000 claims description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 7
- -1 potassium ferricyanide Chemical compound 0.000 claims description 7
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 6
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 5
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 4
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 4
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 4
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 4
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 4
- UCFIGPFUCRUDII-UHFFFAOYSA-N [Co](C#N)C#N.[K] Chemical compound [Co](C#N)C#N.[K] UCFIGPFUCRUDII-UHFFFAOYSA-N 0.000 claims description 3
- DQRBSSNRRYZPJZ-UHFFFAOYSA-N [Co](C#N)C#N.[Na] Chemical compound [Co](C#N)C#N.[Na] DQRBSSNRRYZPJZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910000361 cobalt sulfate Inorganic materials 0.000 claims description 3
- 229940044175 cobalt sulfate Drugs 0.000 claims description 3
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 3
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 3
- DCXPBOFGQPCWJY-UHFFFAOYSA-N trisodium;iron(3+);hexacyanide Chemical compound [Na+].[Na+].[Na+].[Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] DCXPBOFGQPCWJY-UHFFFAOYSA-N 0.000 claims description 3
- 229910021555 Chromium Chloride Inorganic materials 0.000 claims description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 2
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims description 2
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 claims description 2
- QSWDMMVNRMROPK-UHFFFAOYSA-K chromium(3+) trichloride Chemical compound [Cl-].[Cl-].[Cl-].[Cr+3] QSWDMMVNRMROPK-UHFFFAOYSA-K 0.000 claims description 2
- GRWVQDDAKZFPFI-UHFFFAOYSA-H chromium(III) sulfate Chemical compound [Cr+3].[Cr+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRWVQDDAKZFPFI-UHFFFAOYSA-H 0.000 claims description 2
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 2
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 2
- 229960002089 ferrous chloride Drugs 0.000 claims description 2
- 239000011790 ferrous sulphate Substances 0.000 claims description 2
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 2
- 150000004677 hydrates Chemical class 0.000 claims description 2
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 2
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 claims description 2
- YHGPYBQVSJBGHH-UHFFFAOYSA-H iron(3+);trisulfate;pentahydrate Chemical compound O.O.O.O.O.[Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O YHGPYBQVSJBGHH-UHFFFAOYSA-H 0.000 claims description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 2
- 239000011565 manganese chloride Substances 0.000 claims description 2
- 235000002867 manganese chloride Nutrition 0.000 claims description 2
- 229940099607 manganese chloride Drugs 0.000 claims description 2
- 229940099596 manganese sulfate Drugs 0.000 claims description 2
- 239000011702 manganese sulphate Substances 0.000 claims description 2
- 235000007079 manganese sulphate Nutrition 0.000 claims description 2
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 2
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 2
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 claims description 2
- GTSHREYGKSITGK-UHFFFAOYSA-N sodium ferrocyanide Chemical compound [Na+].[Na+].[Na+].[Na+].[Fe+2].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] GTSHREYGKSITGK-UHFFFAOYSA-N 0.000 claims description 2
- 239000000264 sodium ferrocyanide Substances 0.000 claims description 2
- 235000012247 sodium ferrocyanide Nutrition 0.000 claims description 2
- 239000011592 zinc chloride Substances 0.000 claims description 2
- 235000005074 zinc chloride Nutrition 0.000 claims description 2
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 2
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 2
- 229960001763 zinc sulfate Drugs 0.000 claims description 2
- 229910000365 copper sulfate Inorganic materials 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 19
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 10
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 10
- 239000001257 hydrogen Substances 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 238000005868 electrolysis reaction Methods 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 description 12
- DCYOBGZUOMKFPA-UHFFFAOYSA-N iron(2+);iron(3+);octadecacyanide Chemical class [Fe+2].[Fe+2].[Fe+2].[Fe+3].[Fe+3].[Fe+3].[Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] DCYOBGZUOMKFPA-UHFFFAOYSA-N 0.000 description 10
- 238000001291 vacuum drying Methods 0.000 description 10
- 239000000047 product Substances 0.000 description 9
- 239000011521 glass Substances 0.000 description 6
- 239000012621 metal-organic framework Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000009776 industrial production Methods 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 229960003280 cupric chloride Drugs 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910009818 Ti3AlC2 Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- GFHNAMRJFCEERV-UHFFFAOYSA-L cobalt chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Co+2] GFHNAMRJFCEERV-UHFFFAOYSA-L 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910000366 copper(II) sulfate Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 230000005660 hydrophilic surface Effects 0.000 description 1
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000013354 porous framework Substances 0.000 description 1
- 229960003351 prussian blue Drugs 0.000 description 1
- 239000013225 prussian blue Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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- Metallurgy (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
本发明涉及复合材料的合成领域,针对传统方法合成的块体PBA材料电导率低、暴露活性位点有限的问题,提供一种二维普鲁士蓝类似物@MXene复合电催化剂的原位制备方法,包括以下步骤:取MAX相固体,经HF溶液2‑24h刻蚀后,去离子水离心洗涤烘干得到多层MXene粉末;取多层MXene粉末与配体均匀分散在去离子水中,室温搅拌后离心收集,得到MXene前驱体;MXene前驱体中加入含有柠檬酸钠和金属盐的溶液,室温下搅拌0.5‑12 h后离心收集,干燥得粉末状的二维普鲁士蓝类似物@MXene复合电催化剂。本发明工艺高效稳定,工艺流程简单,有效节约能源,能作为电催化剂催化析氢反应及电解水反应。
Description
技术领域
本发明涉及复合材料的合成领域,尤其是涉及一种二维普鲁士蓝类似物@MXene复合电催化剂的原位制备方法。
背景技术
随着科技不断地进步,人们对清洁和可再生能源的需求不断增加,其中最为清洁的氢能源已然成为了目前最理想的新能源。电催化析氢反应(HER)为可持续绿色生产氢能提供了更可行的方案。近年来,一些商业贵金属基催化剂在不同电解液中表现出了优异的电化学析氢活性,但是由于这些贵金属资源稀缺以及高成本,使得这些贵金属基催化剂不能实现广泛地应用。
与贵金属催化剂相比,一些过渡金属氧化物、硫化物、磷化物以及一些金属有机骨架(MOFs)因具有简单的合成工艺、可控的电子结构和低成本的优势,在电催化析氢中展现出优异的电化学活性和稳定性。普鲁士蓝类似物(PBA)作为MOFs的一种,因其具有均匀的孔隙率、高的比表面积以及组分可调,在电催化制氢上得到了广泛地应用。然而传统方法合成的块体PBA材料因自身的低电导率及有限的暴露活性位点严重制约了其在HER中的应用。一篇公告号为CN109928409A的中国专利文献上公开了一种普鲁士蓝类似物及其制备方法、阴极材料和应用, 普鲁士蓝类似物的制备方法包括以下步骤:以水为溶剂,将铁***和硝酸锌进行共沉淀反应,得到反应液;将反应液静置,得到沉淀物;及将沉淀物干燥,得到化学式为K2Zn3[Fe(CN)6]2的普鲁士蓝类似物。上述普鲁士蓝类似物的制备方法操作简单,且能够得到晶粒大小在300 nm左右、循环稳定性较好的普鲁士蓝类似物。但是该发明的普鲁士蓝类似物的形貌结构不可控,性能不够稳定。另一方面MOFs分散性差以及易团聚的问题也会大大降低其催化性能。据此需要一种理想的解决方案。
发明内容
本发明为了克服传统方法合成的块体PBA材料电导率低、暴露活性位点有限的问题,提供一种二维普鲁士蓝类似物@MXene复合电催化剂的原位制备方法,其工艺高效稳定,工艺流程简单,有效节约能源,能作为电催化剂催化析氢反应及电解水反应。
为了实现上述目的,本发明采用以下技术方案:
一种二维普鲁士蓝类似物@MXene复合电催化剂的原位制备方法,包括以下步骤:
(1)取MAX相固体,经HF溶液2-24 h刻蚀后,去离子水离心洗涤烘干得到多层MXene粉末;
(2)取步骤(1)制得的多层MXene粉末与配体均匀分散在去离子水中,多层MXene粉末和配体的质量比为(0.2-2):(0.5-5),配体的浓度为0.01-20 mg/mL,室温搅拌5-360 min后离心收集,得到MXene前驱体;
(3)在步骤(2)制得的MXene前驱体中加入含有柠檬酸钠和金属盐的溶液, MXene前驱体和金属盐的投料质量比为(0.2-2):(0.5-5),金属盐在溶液中的浓度为0.01-20 mg/mL,室温下搅拌0.5-12 h后离心收集,干燥得粉末状的二维普鲁士蓝类似物@MXene复合电催化剂。
MXene是一种新型的过渡金属碳/氮化物二维晶体,具有类似石墨烯的片状结构。MXene作为一种典型的二维材料,由于其良好的亲水性表面、较高的化学稳定性和可调的中间层,在催化领域得到了广泛的研究。特别是,即使在表面官能团存在的情况下,MXene也具有很高的金属导电性,这使得它适合组装成各种类异质结复合材料。因此本发明利用上述MXene自身的特点,在MXene上负载超薄二维PBA阵列,来实现高效和稳定地电催化析氢。
本发明利用MXene和配体的简单静电吸附,实现超薄二维PBA在MXene上快速生长,该复合样的制备方法普适、有效、温和、所用试剂仪器来源广泛,能够批量化或工业化生产;本发明技术方案采用静电吸附法,均在室温下即可实现;本发明所用到的溶剂在实验室或工业化生产中都能获得,价格低廉、来源广泛,所用到的实验设备操作方便,无需大功率设备,生产过程节能环保。制备所得的二维普鲁士蓝类似物@MXene复合电催化剂在常规条件下电化学析氢反应中表现出优异的电化学活性和稳定性。
作为优选,步骤(1)所述的MXene为Ti2CTx、Ti3C2Tx、Nb2CTx、Ti3CNTx、V2CTx、Mo2CTx、Ti4N3Tx中的一种。作为进一步优选,步骤(1)所述的MXene为Ti3C2Tx。
作为优选,步骤(1)的HF溶液质量分数为40%,MAX相固体和HF溶液的投料比为1gMAX相固体:(5-20 mL) HF溶液。作为进一步优选,步骤(1)MAX相固体和HF溶液的投料比为1g MAX相固体:10 mL HF溶液。
作为优选,步骤(2)所述的配体为铁***、铁***、钴***、钴***、亚铁***中的一种。作为进一步优选,步骤(2)所述的配体为铁***。
作为优选,步骤(2)所述的配体的浓度为0.8-3 mg/mL。浓度过低无法实现二维片在MXene上的原位生长。作为进一步优选,步骤(2)所述的配体的浓度为1 mg/mL。
作为优选,步骤(3)所述的金属盐为硫酸镍、硝酸镍、氯化镍、硫酸钴、硝酸钴、氯化钴、硫酸锰、硝酸锰、氯化锰、硫酸铁、硫酸亚铁、硝酸铁、硝酸亚铁、氯化铁、氯化亚铁、硫酸铜、硝酸铜、氯化铜、硫酸锌、硝酸锌、氯化锌、硫酸铬、硝酸镉、氯化铬及其水合物中的一种。作为进一步优选,步骤(3)所述的金属盐为氯化镍、氯化钴、氯化铜、氯化铁中的一种。
作为优选,步骤(3)所述柠檬酸钠和金属盐的溶液的溶剂为甲醇、乙醇、乙二醇、水中的一种或多种。作为进一步优选,步骤(3)所述柠檬酸钠和金属盐的溶液的溶剂为水。
作为优选,步骤(3)所述金属盐在溶液中的浓度为0.8-3 mg/mL。金属盐在溶液中的浓度过低,无法实现二维PBA在MXene上的生长,浓度过高则会有颗粒PBA的生成。作为进一步优选,步骤(3)所述金属盐在溶液中的浓度为1 mg/mL。
因此,本发明具有如下有益效果:(1)制备方法操作简单、条件温和、形貌可调、结构可控、组分分布均匀、纳米片尺寸小;(2)能够批量化或工业化生产;(3)制备方法保留了MXene纳米片和普鲁士蓝多孔框架结构类似物的完整性,兼具MXene和普鲁士蓝类似物的优异性能;(4)复合后可实现PBA的二维化,大大提高PBA可暴露的活性位点;(5)复合后HER性能大幅度提升。
附图说明
图1是实施例1制得的2D NiHCF@Ti3C2Tx的扫描电镜图。
图2是实施例1制得的2D NiHCF@Ti3C2Tx 的XRD图。
图3是实施例1制得的2D NiHCF@Ti3C2Tx的OER性能图。
具体实施方式
下面通过具体实施例,对本发明的技术方案做进一步说明。
本发明中,若非特指,所采用的原料和设备等均可从市场购得或是本领域常用的,实施例中的方法,如无特别说明,均为本领域的常规方法。
实施例1
一种二维普鲁士蓝类似物@MXene复合电催化剂的原位制备方法,包括以下步骤:
(1)多层Ti3C2Tx粉末的制备:取50 mL圆底离心管置于水浴锅中,加热至35 ℃,待温度稳定后,加入10 mL质量分数为40%的HF,再加入1 g Ti3AlC2固体,在35 ℃水浴中加热搅拌反应24 h,反应结束后,用去离子水洗涤至pH降到6,所得产物经60℃真空干燥24 h后,可获得多层Ti3C2Tx粉末;
(2)Ti3C2Tx前驱体的制备:在20 mL玻璃瓶中加入100 mg铁***和5 mL水,搅拌均匀,再加入50 mg多层Ti3C2Tx粉末,室温下搅拌2 h,反应结束后,直接离心去除上层溶液,得到Ti3C2Tx前驱体;
(3)2D NiHCF@Ti3C2Tx复合电催化剂的制备:在100 mL烧杯中,将100 mg柠檬酸钠和50mg六水合氯化镍分散于20 mL水中,再倒入步骤(2)中得到的Ti3C2Tx前驱体,充分搅拌均匀,室温下搅拌6 h后,用水和乙醇低速离心洗涤3次,所得产物经60 ℃真空干燥24 h后,可获得2D NiHCF@Ti3C2Tx。
性能测试
选取实施例1中样品进行表征与分析,测试结果如图所示。图1是实施例1中获得的2DNiHCF@Ti3C2Tx的SEM图,从图中可以看出,获得的2D NiHCF@Ti3C2Tx复合电催化剂横向尺寸为10个微米左右,上面布满了超薄二维PBA。图2是2D NiHCF@Ti3C2Tx的XRD图。图3是2DNiHCF@Ti3C2Tx复合电催化剂的性能对比图。在10 mA/cm2的电流密度下,2D NiHCF@Ti3C2Tx复合电催化剂只有140 mV的过电位,在相同的电流密度下,MXene和PBA的过电位分别为240mV和295 mV,均大于二维普鲁士蓝类似物@MXene的过电位,说明2D NiHCF@Ti3C2Tx的电催化剂性能优于NiHCF和Ti3C2Tx。
实施例2
一种二维普鲁士蓝类似物@MXene复合电催化剂的原位制备方法,包括以下步骤:
(1)多层Ti2CTx粉末的制备:取20 mL圆底离心管置于水浴锅中,加热至35 ℃,待温度稳定后,加入5 mL质量分数为40%的HF,再加入1 g Ti2AlC固体,在35 ℃水浴中加热搅拌反应2 h,反应结束后,用去离子水洗涤至pH降到6,所得产物经60 ℃真空干燥24 h后,可获得多层Ti2CTx粉末;
(2)Ti2CTx前驱体的制备:在玻璃瓶中加入100 mg铁***和100 mL水,搅拌均匀,再加入4 mg多层Ti2CTx粉末,室温下搅拌5 min,反应结束后,直接离心去除上层溶液,得到Ti2CTx前驱体;
(3)2D CoHCF@Ti2CTx复合电催化剂的制备:在100 mL烧杯中,将100 mg柠檬酸钠和100mg六水合氯化钴分散于20 mL甲醇中,再倒入步骤(2)中得到的Ti2CTx前驱体,充分搅拌均匀,室温下搅拌0.5 h后,用甲醇低速离心洗涤3次,所得产物经60 ℃真空干燥24 h后,可获得2D CoHCF@Ti2CTx。
实施例3
一种二维普鲁士蓝类似物@MXene复合电催化剂的原位制备方法,包括以下步骤:
(1)多层Nb2CTx粉末的制备:取50 mL圆底离心管置于水浴锅中,加热至35 ℃,待温度稳定后,加入20 mL质量分数为40%的HF,再加入1 g Nb2AlC固体,在35 ℃水浴中加热搅拌反应10 h,反应结束后,用去离子水洗涤至pH降到6,所得产物经60℃真空干燥24 h后,可获得多层Nb2CTx粉末;
(2)Nb2CTx前驱体的制备:在玻璃瓶中加入100 mg钴***和125 mL水,搅拌均匀,再加入400 mg多层Nb2CTx粉末,室温下搅拌6 h,反应结束后,直接离心去除上层溶液,得到Nb2CTx前驱体;
(3)2D FeHCC@ Nb2CTx复合电催化剂的制备:在100 mL烧杯中,将100 mg柠檬酸钠和100 mg无水氯化铁分散于125 mL乙醇中,再倒入步骤(2)中得到的Nb2CTx前驱体,充分搅拌均匀,室温下搅拌12 h后,用水和乙醇低速离心洗涤3次,所得产物经60 ℃真空干燥24 h后,可获得2D FeHCC@ Nb2CTx。
实施例4
一种二维普鲁士蓝类似物@MXene复合电催化剂的原位制备方法,包括以下步骤:
(1)多层V2CTx粉末的制备:取50 mL圆底离心管置于水浴锅中,加热至35 ℃,待温度稳定后,加入10 mL质量分数为40%的HF,再加入1 g V2AlC固体,在35 ℃水浴中加热搅拌反应24 h,反应结束后,用去离子水洗涤至pH降到7,所得产物经60℃真空干燥24 h后,可获得多层V2CTx粉末;
(2)V2CTx前驱体的制备:在20 mL玻璃瓶中加入100 mg铁***和5 mL水,搅拌均匀,再加入50 mg多层V2CTx粉末,室温下搅拌2 h,反应结束后,直接离心去除上层溶液,得到V2CTx前驱体;
(3)2D NiHCF@ V2CTx复合电催化剂的制备:在100 mL烧杯中,将100 mg柠檬酸钠和100mg无水硝酸镍分散于5 mL水中,再倒入步骤(2)中得到的V2CTx前驱体,充分搅拌均匀,室温下搅拌6 h后,用水和乙醇低速离心洗涤3次,所得产物经60 ℃真空干燥24 h后,可获得2DNiHCF@ V2CTx。
实施例5
一种二维普鲁士蓝类似物@MXene复合电催化剂的原位制备方法,包括以下步骤:
(1)多层Mo2CTx粉末的制备:取50 mL圆底离心管置于水浴锅中,加热至35 ℃,待温度稳定后,加入10 mL质量分数为40%的HF,再加入1 gMo2Ga2C固体,在35 ℃水浴中加热搅拌反应24 h,反应结束后,用去离子水洗涤至pH降到7,所得产物经60℃真空干燥24 h后,可获得多层Mo2CTx粉末;
(2)Mo2CTx前驱体的制备:在20 mL玻璃瓶中加入90 mg铁***和30 mL水,搅拌均匀,再加入50 mg多层Mo2CTx粉末,室温下搅拌2 h,反应结束后,直接离心去除上层溶液,得到Mo2CTx前驱体;
(3)2D CoHCF@ Mo2CTx复合电催化剂的制备:在100 mL烧杯中,将100 mg柠檬酸钠和90mg无水硫酸钴分散于15 mL乙醇和15 mL水中,再倒入步骤(2)中得到的Mo2CTx前驱体,充分搅拌均匀,室温下搅拌6 h后,用水和乙醇低速离心洗涤3次,所得产物经60 ℃真空干燥24h后,可获得2D CoHCF@ Mo2CTx。
实施例6
一种二维普鲁士蓝类似物@MXene复合电催化剂的原位制备方法,包括以下步骤:
(1)多层Ti3CNTx粉末的制备:取50 mL圆底离心管置于水浴锅中,加热至35 ℃,待温度稳定后,加入10 mL质量分数为40%的HF,再加入1 g Ti3AlCN固体,在35 ℃水浴中加热搅拌反应24 h,反应结束后,用去离子水洗涤至pH降到7,所得产物经60℃真空干燥24 h后,可获得多层Ti3CNTx粉末;
(2)Ti3CNTx前驱体的制备:在玻璃瓶中加入5 mg钴***和500 mL水,搅拌均匀,再加入5 mg多层Ti3CNTx粉末,室温下搅拌2 h,反应结束后,直接离心去除上层溶液,得到Ti3CNTx前驱体;
(3)2D CuHCC@ Ti3CNTx复合电催化剂的制备:在100 mL烧杯中,将100 mg柠檬酸钠和5mg无水氯化铜分散于500 mL乙二醇中,再倒入步骤(2)中得到的Ti3CNTx 前驱体,充分搅拌均匀,室温下搅拌6 h后,用乙醇低速离心洗涤3次,所得产物经60 ℃真空干燥24 h后,可获得2D CuHCC@ Ti3CNTx。
比较实施例1-6,实施例1在本发明的最优选条件下制备得到的2D NiHCF@Ti3C2Tx,电催化性能优于实施例2-6。
以上所述,仅是本发明的较佳实施例而已,并非对本发明作任何形式上的限制,虽然本发明已以较佳实施例揭露如上,然而并非用以限定本发明,任何熟悉本专业的技术人员,在不脱离本发明技术方案范围内,当可利用上述揭示的技术内容作出些许更动或修饰为等同变化的等效实施例,但凡是未脱离本发明技术方案内容,依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与修饰,均仍属于本发明技术方案的范围内。
Claims (9)
1.一种二维普鲁士蓝类似物@MXene复合电催化剂的原位制备方法,其特征在于,包括以下步骤:(1)取MAX相固体,经HF溶液2-24 h刻蚀后,去离子水离心洗涤烘干得到多层MXene粉末;
(2)取步骤(1)制得的多层MXene粉末与配体均匀分散在去离子水中,多层MXene粉末和配体的质量比为(0.2-2):(0.5-5),配体的浓度为0.01-20 mg/mL,室温搅拌5-360 min后离心收集,得到MXene前驱体;
(3)在步骤(2)制得的MXene前驱体中加入含有柠檬酸钠和金属盐的溶液, MXene前驱体和金属盐的投料质量比为(0.2-2):(0.5-5),金属盐在溶液中的浓度为0.01-20 mg/mL,室温下搅拌0.5-12 h后离心收集,干燥得粉末状的二维普鲁士蓝类似物@MXene复合电催化剂。
2.根据权利要求1所述的一种二维普鲁士蓝类似物@MXene复合电催化剂的原位制备方法,其特征在于,步骤(1)所述的MXene为Ti2CTx、Ti3C2Tx、Nb2CTx、Ti3CNTx、V2CTx、Mo2CTx、Ti4N3Tx中的一种。
3.根据权利要求1或2所述的一种二维普鲁士蓝类似物@MXene复合电催化剂的原位制备方法,其特征在于,步骤(1)MAX相固体和HF溶液的投料比为1g MAX相固体:(5-20 mL) HF溶液。
4.根据权利要求1所述的一种二维普鲁士蓝类似物@MXene复合电催化剂的原位制备方法,其特征在于,步骤(2)所述的配体为铁***、铁***、钴***、钴***、亚铁***中的一种。
5.根据权利要求1或4所述的一种二维普鲁士蓝类似物@MXene复合电催化剂的原位制备方法,其特征在于,步骤(2)所述的配体的浓度为0.8-3 mg/mL。
6.根据权利要求1所述的一种二维普鲁士蓝类似物@MXene复合电催化剂的原位制备方法,其特征在于,步骤(3)所述的金属盐为硫酸镍、硝酸镍、氯化镍、硫酸钴、硝酸钴、氯化钴、硫酸锰、硝酸锰、氯化锰、硫酸铁、硫酸亚铁、硝酸铁、硝酸亚铁、氯化铁、氯化亚铁、硫酸铜、硝酸铜、氯化铜、硫酸锌、硝酸锌、氯化锌、硫酸铬、硝酸镉、氯化铬及其水合物中的一种。
7.根据权利要求6所述的一种二维普鲁士蓝类似物@MXene复合电催化剂的原位制备方法,其特征在于,步骤(3)所述的金属盐为氯化镍、氯化钴、氯化铜、氯化铁中的一种。
8.根据权利要求1所述的一种二维普鲁士蓝类似物@MXene复合电催化剂的原位制备方法,其特征在于,步骤(3)所述柠檬酸钠和金属盐的溶液的溶剂为甲醇、乙醇、乙二醇、水中的一种或多种。
9.根据权利要求1或8所述的一种二维普鲁士蓝类似物@MXene复合电催化剂的原位制备方法,其特征在于,步骤(3)所述金属盐在溶液中的浓度为0.8-3 mg/mL。
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