CN114481204B - 一种磷化钴负载贵金属纳米材料的制备 - Google Patents
一种磷化钴负载贵金属纳米材料的制备 Download PDFInfo
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 30
- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 19
- 239000010941 cobalt Substances 0.000 title claims abstract description 19
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 229910000510 noble metal Inorganic materials 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002243 precursor Substances 0.000 claims abstract description 14
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 11
- XFZRQAZGUOTJCS-UHFFFAOYSA-N phosphoric acid;1,3,5-triazine-2,4,6-triamine Chemical compound OP(O)(O)=O.NC1=NC(N)=NC(N)=N1 XFZRQAZGUOTJCS-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 11
- 239000003513 alkali Substances 0.000 claims abstract description 9
- 239000003792 electrolyte Substances 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 230000003197 catalytic effect Effects 0.000 claims abstract description 4
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 4
- 239000003795 chemical substances by application Substances 0.000 claims abstract 2
- 239000000843 powder Substances 0.000 claims description 17
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000000967 suction filtration Methods 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 4
- 230000002378 acidificating effect Effects 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims 3
- 238000005119 centrifugation Methods 0.000 claims 2
- 229910021580 Cobalt(II) chloride Inorganic materials 0.000 claims 1
- 238000003287 bathing Methods 0.000 claims 1
- 230000005611 electricity Effects 0.000 claims 1
- 239000011148 porous material Substances 0.000 claims 1
- 239000011592 zinc chloride Substances 0.000 claims 1
- 235000005074 zinc chloride Nutrition 0.000 claims 1
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 4
- 238000000643 oven drying Methods 0.000 description 4
- 238000009210 therapy by ultrasound Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000011865 Pt-based catalyst Substances 0.000 description 1
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910021397 glassy carbon Inorganic materials 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
本发明涉及一种磷化钴负载贵金属(Pt,Ru,Ir等)纳米材料的制备方法,以Pt为例,其特征在于,所述纳米材料以CoCl2·6H2O以及磷酸三聚氰胺为前驱体,ZnCl2作为造孔剂,低温搅拌干燥结合高温焙烧,碱洗涤得到磷化钴纳米材料。经油浴还原铂、醇和丙酮洗涤得到磷化钴负载贵金属的纳米材料(CoP‑Pt),该磷化钴纳米材料在全pH电解液中表现出高的催化活性,并且具有四功能,本发明所述制备方法简单可控、易于实施,该磷化钴纳米材料在室温下可用于高效电催化反应。
Description
技术领域
本发明涉及一种磷化钴负载贵金属纳米材料的制备,属于材料的制备领域。
背景技术
化石能源的急速消耗及不可再生性,促使清洁能源设备的发展。其中电解水备受关注,主要涉及析氢反应(HER),析氧反应(OER),氧还原反应(ORR),但是这些反应自身动力学缓慢,这就需要一种高效的催化剂来提高催化反应。目前,Pt基催化剂被认为是最有效的催化剂,但面临着价格高,资源少等问题,因此开发多功能的催化剂迫在眉睫。其中CoP作为Co基过渡金属磷化物(TMPs),因其在地壳中含量丰富,具有良好的导电性、机械强度、耐化学腐蚀等优点而备受关注,在能源转化和存储方面也得到了深入研究。
近年来金属磷化物由于其出色的物理化学特性,如天然丰度高,成本低,催化性能稳定等而受到了广泛关注。但导电性差,本征活性低等阻碍了磷化物催化剂的发展。引入空位缺陷是调控过渡金属磷化物催化性能的有效方法,空位缺陷的存在改变了居于的原子结构,从而引起电子结构的改变,增加活性位点。特别是负载贵金属到Co基框架中,不仅可以调节CoP的微观电子结构来改变其性能,还可以显著改良CoP纳米材料的导电性以及增加反应活性位点数量,从而增强材料电催化性能,具有至关重要的现实意义。
发明内容
本发明旨在提供一种磷化钴负载贵金属(Pt,Ru,Ir等)的纳米材料(以 CoP-Pt为例)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)①将1mol磷酸三聚氰胺,0.167mol CoCl2·6H2O、0.039g ZnCl2,溶解在20mL去离子水中,在75℃下搅拌烘干得到粉末;将粉末置于气体氛围保护下的管式炉中,900℃焙烧2小时,升温速率为10℃/min,冷却至室温,用碱洗12h后抽滤烘干即得到前驱体。
②将4.7mg的氯铂酸,10mg的前驱体溶解在乙二醇溶剂中,超声6min后 65℃油浴5个小时,然后冷却至室温,用乙醇离心三次和丙酮离心四次得到磷化钴负载的贵金属纳米材料(CoP-Pt)。
2)将磷化钴负载贵金属的纳米材料用于室温电催化产氢,达到电流密度为 10mAcm-2时,所述纳米材料在碱性、酸性和中性电解液中的过电位分别为44 mV、6mV和65mV。用于室温电催化析氧,达到电流密度为10mA cm-2时,所述纳米材料在碱性电解液中的过电位为1.55V。用于室温电催化氧还原,所述纳米材料在碱性电解液中半波电位达到0.84V。
本发明具有以下优点:
1)以CoCl2·6H2O、磷酸三聚氰胺,ZnCl2为前驱体,经蒸干煅烧得到CoP,再经由于还原铂得到磷化钴负载贵金属的纳米材料,该方法简单可控、易于实施,可用于高效电催化反应。
附图说明
图1是实施例1所得金属磷化物CoP-Pt的扫描电镜。
图2是实施例1所得金属磷化物CoP-Pt的透射电镜。
图3是实施例1所得金属磷化物CoP-Pt的XRD谱图。
图4是实施例1所得金属磷化物CoP-Pt的XPS谱图。
图5是实施例1所得金属磷化物CoP-Pt在碱性,酸性,中性条件下的线性扫描曲线。
具体实施方式
下面结合实施例对本发明进行进一步说明,但是本发明不仅限于以下实施例。
实施例1
将1mol磷酸三聚氰胺,0.167mol CoCl2·6H2O、0.039g ZnCl2,溶解在20mL 去离子水中,在75℃下搅拌烘干得到粉末;将粉末置于气体氛围保护下的管式炉中,900℃焙烧2小时,升温速率为10℃/min,冷却至室温,用碱洗12h后抽滤烘干即得到前驱体。将4.7mg的氯铂酸,10mg的前驱体溶解在乙二醇溶剂中,超声6min后65℃油浴5个小时,然后冷却至室温,用乙醇离心三次和丙酮离心四次得到磷化钴负载的贵金属纳米材料(CoP-Pt)。
实施例2
将1mol磷酸三聚氰胺,0.167mol CoCl2·6H2O、0.039g ZnCl2,溶解在20 mL去离子水中,在75℃下搅拌烘干得到粉末;将粉末置于气体氛围保护下的管式炉中,900℃焙烧2小时,升温速率为10℃/min,冷却至室温,用碱洗12h 后抽滤烘干即得到前驱体。将9.8mg的氯铂酸,10mg的前驱体溶解在乙二醇溶剂中,超声6min后65℃油浴5个小时,然后冷却至室温,用乙醇离心三次和丙酮离心四次得到磷化钴负载的贵金属纳米材料(CoP-Pt)。
实施例3
将1mol磷酸三聚氰胺,0.167mol CoCl2·6H2O、0.039g ZnCl2,溶解在20 mL去离子水中,在75℃下搅拌烘干得到粉末;将粉末置于气体氛围保护下的管式炉中,900℃焙烧2小时,升温速率为10℃/min,冷却至室温,用碱洗12h 后抽滤烘干即得到前驱体。将1.76mg的氯铂酸,10mg的前驱体溶解在乙二醇溶剂中,超声6min后65℃油浴5个小时,然后冷却至室温,用乙醇离心三次和丙酮离心四次得到磷化钴负载的贵金属纳米材料(CoP-Pt)。
实施例4
将1mol磷酸三聚氰胺,0.167mol CoCl2·6H2O、0.039g ZnCl2,溶解在20 mL去离子水中,在75℃下搅拌烘干得到粉末;将粉末置于气体氛围保护下的管式炉中,900℃焙烧2小时,升温速率为10℃/min,冷却至室温,用碱洗12h 后抽滤烘干即得到前驱体CoP。
实施例5
将1mol磷酸三聚氰胺,0.167mol CoCl2·6H2O、0.013g ZnCl2,溶解在20 mL去离子水中,在75℃下搅拌烘干得到粉末;将粉末置于气体氛围保护下的管式炉中,900℃焙烧2小时,升温速率为10℃/min,冷却至室温,用碱洗12h 后抽滤烘干即得到前驱体CoP。
实施例6
将1mol磷酸三聚氰胺和0.167mol CoCl2·6H2O,溶解在20mL去离子水中,在75℃下搅拌烘干得到粉末;将粉末置于气体氛围保护下的管式炉中,900℃焙烧2小时,升温速率为10℃/min,冷却至室温得到CoP。
实施例7
将实施例1制备的产物进行电催化析氢性能测试,将所制粉末配成溶液涂在玻碳电极上做工作电极,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电化学性能,电解液为1M KOH溶液。电流密度为10mAcm-2和100mAcm-2时的电位分别为44mV和137mV。
Claims (2)
1.一种磷化钴负载贵金属纳米材料的制备方法,以 Pt 为例,所
述纳米材料以 CoCl2·6H2O 以及磷酸三聚氰胺为前驱体,ZnCl2作为造
孔剂,低温搅拌干燥结合高温焙烧,碱洗涤得到磷化钴纳米材料;经
油浴还原铂、醇和丙酮洗涤得到磷化钴负载 Pt 的纳米材料(CoP-Pt),
该磷化钴纳米材料在全 pH 电解液中表现出高的催化活性,磷化钴负
载 Pt 纳米材料的制备由如下步骤制得:
①将 1 mol 磷酸三聚氰胺,0.167 mol CoCl2·6H2O,0.039 g ZnCl2,
溶解在 20 mL 去离子水中,在 75 oC 下搅拌烘干得到粉末;将粉末置
于气体氛围保护下的管式炉中,900 oC 焙烧 2 小时,升温速率为 10
oC/min,冷却至室温,用碱液洗涤,抽滤烘干即得到前驱体;
②将 4.7 mg 的氯铂酸,10 mg 由①所制备的前驱体分散在乙二醇
溶剂中,超声 6 min,然后 65 oC 油浴 5 个小时,冷却至室温,用乙
醇离心三次和丙酮离心四次得到磷化钴负载 Pt 的纳米材料(CoP-Pt)。
2.按照权利要求 1 所述的方法,其特征在于:
将磷化钴负载 Pt 的纳米材料用于室温电催化产氢,达到电流密
度为 10 mAcm-2 时,所述纳米材料在碱性、酸性和中性电解液中的过
电位分别为 44 mV、6 mV 和 65 mV,用于室温电催化析氧,达到电
流密度为 10 mA cm-2 时,所述纳米材料在碱性电解液中的过电位为
1.55 V,用于室温电催化氧还原,所述纳米材料在碱性电解液中半波
电位达到 0.84 V。
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