CN115196696A - 一种钌酸钇纳米催化剂及其制备方法和应用 - Google Patents
一种钌酸钇纳米催化剂及其制备方法和应用 Download PDFInfo
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Abstract
Description
技术领域
本发明属于能源材料领域,尤其是电化学材料制备技术领域,具体涉及一种钌酸钇纳米催化剂及其制备方法和应用。
背景技术
全球能源变革加速推进,清洁能源替代是大势所趋。可再生能源发电技术具有时效性和地域性与实际情况不匹配的缺点,将间隙式可再生能源发电与电转气技术紧密结合,即利用可再生能源所产生的间断性电力通过电解水的方式转化为氢气,是近年来兴起的一种新型大规模工业化储能技术,被称为氢储能。在其中的关键步骤—电解水过程中,主要的过电位来源于氧气析出反应(Oxygen evolution reaction, OER),其缓慢的动力学过程造成额外的电能消耗,因此,需要开发高效的OER催化剂。目前,钌基烧绿石类的高温复杂金属氧化物被作为OER催化剂被广泛研究,以钌酸钇为例,其具有较低的贵金属含量,且在酸性介质中具有优异的稳定性,有望替代商业的IrO2成为质子交换膜电解水装置的阳极催化材料。但这类材料通常涉及到高温制备(1100℃),因此具有高结晶度、较大的颗粒尺寸、较少的缺陷位点,而在金属氧化物基催化剂中,以氧空位为例的缺陷位点可显著改善催化剂的物理化学性质,如对反应中间物质的吸附能力,或作为活性位点提高催化活性,因此,如何在这类高温氧化物中引入大量缺陷位点是提升其OER性能的关键问题。
发明内容
本发明的目的在于解决现有技术问题,提供了一种钌酸钇纳米催化剂及其制备方法和应用,所得催化剂在酸性介质中表现出优异的OER催化活性。且制备方法工艺简单,对于各类高温氧化物的制备具有普适性,有望实现大规模生产。
更进一步的,所述的制备方法包括如下步骤:
(1)将金属盐溶于水,再加入柠檬酸得到澄清溶液,将溶液烘干陈化后,得到干燥的凝胶中间物质;
(2)将步骤(1)中得到的凝胶中间物质置于800-1100℃空气中进行24 h以上的煅烧;
(3)通过一步淬火工艺得到所述的催化剂。
在本发明的优选实施方式中,所述的金属盐为氯化钌和硝酸钇,两者的摩尔比为1:1。
在本发明的优选实施方式中,金属盐和柠檬酸的摩尔比介于1:1~1:2之间。
在本发明的优选实施方式中,金属盐浓度为0.05~1 mol/L。
在本发明的优选实施方式中,煅烧结束后的淬火工艺中的冷却介质为0~20摄氏度的水或盐溶液,即保温结束后立即置于水中或盐水中冷却;所述的盐溶液选自氯化钠、氯化钾、硫酸钠、硫酸钾水溶液中的一种或几种。
在本发明的优选实施方式中,煅烧结束后的淬火工艺中的冷却介质为0~20摄氏度的空气或惰性气,即保温结束后立即置于相应气氛中进行吹扫冷却;所述的惰性气选自氮气、氩气、二氧化碳中的一种或几种。
在本发明的优选实施方式中,煅烧结束后的淬火工艺中的冷却介质为干冰或液氮,即保温结束后立即置于干冰或液氮中进行冷却。
在本发明还保护上述催化剂在酸性介质中电催化氧气析出反应中的应用。
与现有技术相比,本发明具有如下优点:
(1)制备工艺简单,相比与传统制备方法仅多一步淬火处理工艺便可得到具有高浓度缺陷结构的钌酸钇催化材料。高温煅烧过程中原子运动剧烈,急速的冷却过程可将高温下的高浓度缺陷结构瞬间保留至室温,无需引入额外的缺陷原子,且对于各类高温氧化物的合成具有普适性。
(2)制备所得到的钌酸钇纳米材料作为酸性介质的析氧反应催化剂在等同情况下极大的降低了反应过电位,显著降低了能耗,具有优异的析氧催化性能。
附图说明
下面结合附图对本发明进一步说明:
图1是实施例1中得到的催化剂的XRD图;
图2是实施例1中所得到的催化剂的SEM图;
图3是实施例1中所得到的催化剂的TEM图;
图4是实施例1中所得到的催化剂的EPR图;
图5是实施例1中所得到的催化剂在 0.1 M HClO4溶液中的极化曲线;
图6是实施例1中所得到的催化剂在 0.1 M HClO4溶液中进行恒电流测试所得到的电压-时间曲线。
具体实施方式
为了使本发明的目的、技术方案及有益效果更加清楚,本发明用以下具体实施例进行说明,但本发明绝非限于这些例子。
实施例1
(1)将0.840 g柠檬酸溶解于10 mL去离子水中,加入0.38 g硝酸钇,0.21 g三氯化钌,超声溶解均匀,将上述溶液置于80℃热台上加热烘干,陈化,得到蓬松的干燥凝胶;
(2)将上述凝胶置于马弗炉中,升温至1100℃保温24 h。
对所得的样品进行XRD分析,结果见图1,表现为纯相的钌酸钇。一步淬火过程对钌酸钇的相纯度没有影响。其表面形貌用SEM进行观察,如图2。进一步使用透射电子显微镜观察其结构变化,如图3。添加一步淬火工艺后,其表面的粗糙度增加,说明淬火处理对于缺陷的增加有显著作用。使用EPR表征了材料表面的氧空位浓度,淬火处理后钌酸钇表现为氧空位的增多,使材料中氧化学计量比发生变化,如图4所示。该催化剂具有优异的氧析出催化活性,其在酸性介质中的活性表现如图5所示。该催化剂同时具有优异的稳定性,在长时间反应之后活性不产生衰减,如图6所示。
实施例2
(1)将0.42 g柠檬酸溶解于10 mL去离子水中,加入0.19 g硝酸钇,0.10 g三氯化钌,超声溶解均匀,将上述溶液置于80℃热台上加热烘干,陈化,得到蓬松的干燥凝胶;
(2)将上述凝胶置于马弗炉中,升温至1100℃保温24 h。
实施例3
1)将0.42 g柠檬酸溶解于10 mL去离子水中,加入0.19 g硝酸钇,0.10 g三氯化钌,超声溶解均匀,将上述溶液置于80℃热台上加热烘干,陈化,得到蓬松的干燥凝胶;
(2)将上述凝胶置于马弗炉中,升温至1100℃保温24 h。
实施例4
1)将0.42 g柠檬酸溶解于10 mL去离子水中,加入0.19 g硝酸钇,0.10 g三氯化钌,超声溶解均匀,将上述溶液置于80℃热台上加热烘干,陈化,得到蓬松的干燥凝胶;
(2)将上述凝胶置于马弗炉中,升温至1100℃保温24 h。
以上实施例显示和描述了本发明的主要特征和主要优点进行了具体说明,但本发明并不限于所述实施例,熟悉本领域的技术人员在不违背本发明精神的前提下还可作出种种的等同的变型或替换,这些等同的变型或替换均包含在本申请权利要求所限定的范围内。
Claims (10)
2.根据权利要求1所述的钌酸钇纳米催化剂的制备方法,其特征在于,由高温热处理后结合淬火工艺得到。
3.根据权利要求2所述的制备方法,其特征在于,包括如下步骤:
(1)将金属盐溶于水,再加入柠檬酸得到澄清溶液,将溶液烘干陈化后,得到干燥的凝胶中间物质;
(2)将步骤(1)中得到的凝胶中间物质置于800-1100℃空气中进行24 h以上的煅烧;
(3)通过一步淬火工艺得到所述的催化剂。
4.根据权利要求3所述的制备方法,其特征在于,所述的金属盐为氯化钌和硝酸钇,两者的摩尔比为1:1。
5.根据权利要求4所述的制备方法,其特征在于,金属盐和柠檬酸的摩尔比介于1:1~1:2之间。
6.根据权利要求3所述的制备方法,其特征在于,金属盐浓度为0.05~1 mol/L。
7.根据权利要求3所述的制备方法,其特征在于,煅烧结束后的淬火工艺中的冷却介质为0~20摄氏度的水或盐溶液,即保温结束后立即置于水中或盐水中冷却;所述的盐溶液选自氯化钠、氯化钾、硫酸钠、硫酸钾水溶液中的一种或几种。
8.根据权利要求3所述的制备方法,其特征在于,煅烧结束后的淬火工艺中的冷却介质为0~20摄氏度的空气或惰性气,即保温结束后立即置于相应气氛中进行吹扫冷却;所述的惰性气选自氮气、氩气、二氧化碳中的一种或几种。
9.根据权利要求3所述的制备方法,其特征在于,煅烧结束后的淬火工艺中的冷却介质为干冰或液氮,即保温结束后立即置于干冰或液氮中进行冷却。
10.权利要求1所述的钌酸钇纳米催化剂,或是权利要求2-9中任一项所述的制备方法制备得到的钌酸钇纳米催化剂在酸性介质中电催化氧气析出反应中的应用。
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