CN110227549B - 一种空心立方体结构阳极催化剂及其制备方法 - Google Patents
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- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 description 3
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- 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 1
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Abstract
本发明公开一种空心立方体结构阳极催化剂及其制备方法,采用沉淀法合成PBA立方体;采用水热法,利用无水乙醇对PBA立方体进行刻蚀,最终得到空心PBA立方体,即为电解水和电解尿素用阳极催化剂;本发明的制备方法反应受热均匀,易控制,所使用原料成本低、易得到目标产物、操作简单易行,所得空心结构的PBA的形貌好、易调控,具有优异的电解水OER性能和电解尿素UOR性能。
Description
技术领域
本发明涉及电催化领域,具体涉及一种空心立方体结构阳极催化剂及其制备方法。
背景技术
普鲁士蓝类似物(Prussian Blue Analogue,简称PBA),是典型的面心立方结构的晶体,是由功能性有机配体连接的金属中心/簇组成的典型多孔多功能材料,具有氧化还原性、高表面积和均匀孔隙率的独特性能,应用于催化、传感器、电池电极材料和储存离子等领域,近年来受到越来越多的关注。PBA的合成方法有电化学沉积法和化学合成法。
在电化学能源存储与转换领域,较高的比表面积能提供更多的电化学活性位点以及更大的与电解液的接触面积;较薄而同时具有渗透性的壳层结构极大的加快电子与离子的传输;内部中空结构能有效的缓解离子循环穿梭带来的体积膨胀问题等。将提高PBA纳米材料的固有特性以及进一步赋予其新的功能,使其表现出增强的电解水阳极反应(OER)活性和电解尿素阳极反应(UOR)的优异稳定性。
发明内容
本发明目的在于提供一种空心立方体结构阳极催化剂及其制备方法,制得的催化剂为中空的纳米立方体结构,具有优异的电催化活性和电解尿素阳极反应稳定性。
为实现上述目的,本发明采用的技术方案是:
一种空心立方体结构阳极催化剂的制备方法,包括以下步骤:
S1、称取0.5-1 mmol的镍金属盐、0.5-2 mmol的柠檬酸钠水合物,溶解在20 ml去离子水中,边搅拌边加入金属氰化钾水溶液,得到混合溶液;S2、将上述混合溶液静置20-48h,将产物进行离心、用去离子水和无水乙醇洗涤、真空干燥,得到PBA立方体粉末;
S3、将将PBA立方体粉末分散在乙醇中,然后在连续搅拌下倒入100-500mg/20ml的PVP乙醇溶液中搅拌均匀,将混合溶液转移至水热釜中,160-200 ℃下反应6-48 h,待冷却至室温后离心,用去离子水和无水乙醇洗涤、真空干燥,得到空心PBA立方体。
进一步,所述镍金属盐为硝酸盐、硫酸盐、醋酸盐、氯化物中的一种或几种。
进一步,所述金属氰化钾水溶液为铁氰化钾水溶液或钴氰化钾水溶液。
空心立方体结构阳极催化剂,其为中空的纳米立方体结构。
与现有技术相比,本发明具有以下有益的技术效果:
本发明的制备方法反应受热均匀,易控制,所使用原料成本低、易得到目标产物、操作简单易行,所得空心结构的PBA的形貌好、易调控,具有优异的电催化产氧性能,且相对于未被刻蚀的PBA立方体纳米材料,本发明经过乙醇的化学刻蚀作用得到的空心立方体PBA具有更大的比表面积以及暴露更多的活性位点,因此具有更加优异的电催化活性和优异的电解水OER、电解尿素UOR性能。
本发明采用水热法对PBA立方体结构进行化学刻蚀,使其成为具有中空结构的纳米立方体结构,实心的PBA纳米立方体的不均匀表面反应性是形成中空结构的主要原因,PBA立方体上的蚀刻优先发生在顶点处,并且蚀刻速率沿立方体的体对角线方向逐渐加快,最终形成中空的纳米立方体结构,使PBA材料的结构和功能的优势最大化,扩展了金属有机骨架在电催化方面的应用。
附图说明
图1为实施例1制备得到的NiFe-PBA的XRD图;
图2为实施例1制备得到的NiFe-PBA的SEM图;
图3为实施例1制备得到的Hollow NiFe-PBA的SEM表征图;
图4为实施例1制备得到的NiFe -PBA和Hollow NiFe -PBA在1 M的KOH电解液中的LSV曲线图;
图5为实施例1制备得到的NiFe -PBA和Hollow NiFe -PBA在1 M的KOH和0.5 M尿素电解液中的LSV曲线图;
具体实施方式
下面结合具体实施例对本发明作进一步详细描述,但不作为对本发明的限定。
空心立方体结构阳极催化剂的制备方法,具体步骤如下:
称取0.5-1 mmol的镍金属盐、0.5-2 mmol的柠檬酸钠水合物,溶于20 ml去离子水中,边搅拌边加入金属氰化钾水溶液,得到混合溶液,静置一段时间,将产物进行离心、洗涤、干燥得到PBA立方体。
称取一定量的PBA立方体粉末,分散在乙醇中,然后在连续搅拌下倒入100-500mg/20 ml的PVP乙醇溶液中,搅拌15 min后,将混合溶液转移到50 mL水热釜中,160-200 ℃下反应6-48 h,待冷却至室温后离心,用去离子水和无水乙醇洗涤、真空干燥,得到空心PBA立方体;
下面通过具体实施例来对本发明进行更详细的说明:
实施例1
将175 mg的六水合硝酸镍和265 mg的二水合柠檬酸钠溶于20 mL去离子水中,边搅拌边加入20 mL铁氰化钾水溶液,得到混合溶液,静置20 h,将产物进行离心、洗涤、真空干燥24 h得到NiFe-PBA。
称取20 mg上述NiFe-PBA粉末,分散在20 mL乙醇中,然后在连续搅拌下倒入100mg/20 mL的PVP乙醇溶液中,搅拌15 min后,将混合溶液转移到50 mL水热釜中,180 ℃下反应48 h,待冷却至室温后离心,用去离子水和无水乙醇洗涤、真空干燥24 h,得到空心NiFe-PBA。
图1分别是NiFe-PBA的XRD图谱。可以看出大约在14.9,17.4,24.6和30.2,35.1,39.4,43.3,50.4,53.7,56.9处分别显示衍射峰,分别对应于NiFe-PBA的(111),(200),(220),(222),(400),(420),(422),(440),(600)和(620)面,表明NiFe-PBA的形成。
图2是NiFe-PBA在100 nm放大倍数下的SEM表征图,可以看出所合成的NiFe-PBA具有实心立方体结构,且尺寸均一,分布均匀。
图3是经过乙醇刻蚀后的NiFe-PBA的SEM表征图,可以看出经过刻蚀,NiFe-PBA立方体从顶点处被刻蚀,呈空心立方体结构。
图4中分别是NiFe-PBA、Hollow NiFe-PBA、贵金属催化剂IrO2的LSV曲线图,可以看出所制备的空心NiFe -PBA在碱性溶液中具有良好的电解水OER性能,相对于NiFe-PBA,其产氧性能明显提升,在达到10 mA/cm2时,过电位大约为293 mV。
图5中分别是NiFe-PBA、Hollow NiFe-PBA、贵金属催化剂IrO2的LSV曲线图,可以看出所制备的空心NiFe -PBA在尿素溶液中具有良好的电解尿素UOR性能,相对于NiFe-PBA,其产氧性能明显提升,在达到10 mA/cm2时,过电位大约为130 mV。
实施例2
将78 mg的无水氯化镍和265 mg的二水合柠檬酸钠溶于20 mL去离子水中,边搅拌边加入20 mL铁氰化钾水溶液,得到混合溶液,静置48 h,将产物进行离心、洗涤、真空干燥24 h得到NiFe-PBA。
称取20 mg上述NiFe-PBA粉末,分散在20 mL乙醇中,然后在连续搅拌下倒入100mg/20 mL的PVP乙醇溶液中,搅拌15 min后,将混合溶液转移到50 mL水热釜中,200 ℃下反应48 h,待冷却至室温后离心,用去离子水和无水乙醇洗涤、真空干燥24 h,得到空心NiFe-PBA。
实施例3
将106 mg的醋酸镍和265 mg的二水合柠檬酸钠溶于20 mL去离子水中,边搅拌边加入20 mL铁氰化钾水溶液,得到混合溶液,静置48 h,将产物进行离心、洗涤、真空干燥24h得到NiFe-PBA。
称取20 mg上述NiFe-PBA粉末,分散在20 mL乙醇中,然后在连续搅拌下倒入200mg/20 mL的PVP乙醇溶液中,搅拌15 min后,将混合溶液转移到50 mL水热釜中,160 ℃下反应24 h,待冷却至室温后离心,用去离子水和无水乙醇洗涤、真空干燥24 h,得到空心NiFe-PBA。
实施例4
将143 mg的六水合氯化镍和265 mg的二水合柠檬酸钠溶于20 mL去离子水中,边搅拌边加入20 mL铁氰化钾水溶液,得到混合溶液,静置48 h,将产物进行离心、洗涤、真空干燥24 h得到NiFe-PBA。
称取20 mg上述NiFe-PBA粉末,分散在20 mL乙醇中,然后在连续搅拌下倒入100mg/20 mL的PVP乙醇溶液中,搅拌15 min后,将混合溶液转移到50 mL水热釜中,200 ℃下反应24 h,待冷却至室温后离心,用去离子水和无水乙醇洗涤、真空干燥24 h,得到空心NiFe-PBA。
实施例5
将291 mg的六水合硝酸镍和353 mg的二水合柠檬酸钠溶于20 mL去离子水中,边搅拌边加入20 mL钴氰化钾水溶液,得到混合溶液,静置20 h,将产物进行离心、洗涤、真空干燥24 h得到NiCo-PBA。
称取20 mg上述NiCo-PBA粉末,分散在20 mL乙醇中,然后在连续搅拌下倒入400mg/20 mL的PVP乙醇溶液中,搅拌15 min后,将混合溶液转移到50 mL水热釜中,160 ℃下反应48 h,待冷却至室温后离心,用去离子水和无水乙醇洗涤、真空干燥24 h,得到空心NiCo-PBA。
实施例6
将291 mg的六水合硝酸镍和353 mg的二水合柠檬酸钠溶于20 mL去离子水中,边搅拌边加入20 mL铁氰化钾水溶液,得到混合溶液,静置48 h,将产物进行离心、洗涤、真空干燥24 h得到NiFe-PBA。
称取20 mg上述NiFe-PBA粉末,分散在20 mL乙醇中,然后在连续搅拌下倒入500mg/20 mL的PVP乙醇溶液中,搅拌15 min后,将混合溶液转移到50 mL水热釜中,200 ℃下反应6 h,待冷却至室温后离心,用去离子水和无水乙醇洗涤、真空干燥24 h,得到空心NiFe-PBA。
最后应该说明的是:以上实施例仅用于说明本发明的技术方案而非对其限制,尽管参照上述实施例对本发明进行了详细说明,所属领域的普通技术人员应当理解:依然可以对本发明的具体实施方式进行修改或者等同替换,而未脱离本发明精神和范围的任何修改或者等同替换,其均应涵盖在本权利要求范围当中。
Claims (5)
1.一种空心立方体结构阳极催化剂的制备方法,其特征在于包括以下步骤:
S1、称取0.5-1 mmol的镍金属盐、0.5-2 mmol的柠檬酸钠水合物,溶解在20 mL 去离子水中,边搅拌边加入金属氰化钾水溶液,得到混合溶液;
S2、将上述混合溶液静置20-48 h,将产物进行离心、用去离子水和无水乙醇洗涤、真空干燥,得到PBA立方体粉末;S3、将PBA立方体粉末分散在乙醇中,然后在连续搅拌下倒入100-500mg/20mL 的PVP乙醇溶液中搅拌均匀,将混合溶液转移至水热釜中,160-200 ℃下反应6-48 h,待冷却至室温后离心,用去离子水和无水乙醇洗涤、真空干燥,得到空心PBA立方体。
2.根据权利要求1所述的空心立方体结构阳极催化剂的制备方法,其特征在于:所述镍金属盐为硝酸盐、硫酸盐、醋酸盐、氯化物中的一种或几种。
3.根据权利要求1所述的空心立方体结构阳极催化剂的制备方法,其特征在于:所述金属氰化钾水溶液为铁氰化钾水溶液或钴氰化钾水溶液。
4.一种根据权利要求1-3任一项方法制备的空心立方体结构阳极催化剂。
5.根据权利要求4所述的空心立方体结构阳极催化剂,其特征在于:其为中空的纳米立方体结构。
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