CN113629263A - 一种采用化学螯合吸附法合成的质子交换膜燃料电池铂合金催化剂 - Google Patents
一种采用化学螯合吸附法合成的质子交换膜燃料电池铂合金催化剂 Download PDFInfo
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Abstract
本发明涉及一种采用化学螯合吸附法合成的质子交换膜燃料电池铂合金催化剂,所述的铂合金催化剂其特征为催化金属纳米颗粒为铂‑银‑铜三种元素的合金,具有高氧还原催化活性,能够大幅降低质子交换膜燃料电池中的铂用量。其合成方法的特征为采用经过表面基团处理后的多孔碳基底与金属前驱体的进行化学螯合,再经简单的一步焙烧即可制备该合金催化剂。该制备方法工序简单,批次稳定性高适合批量生产,合成的催化剂氧还原性能高,具有良好的应用前景。
Description
技术领域
本发明涉及一种质子交换膜燃料电池合金催化剂及其制备方法,属于燃料电池催化剂技术领域。
背景技术
质子交换膜燃料电池(PEMFC)具有环境友好、能量转化效率高、燃料气体来源广泛、结构简单且维护方便、应用领域广泛等优点,被认为是21世纪解决能源和环境问题最具潜力的发电技术之一。然而,PEMFC中最关键的反应是阴极氧还原反应(ORR),受限于缓慢的化学动力学,往往需要使用大量的贵金属Pt。由于Pt资源稀缺、价格昂贵且本身存在降解失活的问题,开发具有高活性,低铂用量的新型ORR催化剂成为了产业界的热点技术之一。
通常情况下,合金催化剂比单一组分能表现出更优越的性能。目前,降低铂载量、提高铂活性的主要研究方向是将过渡金属M与Pt合金化形成二元或多元合金电催化剂。形成合金后,Pt的电子结构得到了优化,Pt-Pt间距缩短,这将有利于氧的双位解离吸附,从而使催化剂的活性大幅度提高。比如研究发现Pt3Ni合金通过改变Pt表面原子的电子结构来提高ORR活性,相对于Pt/C催化剂,其活性提高了两个数量级。关于铂基合金催化剂ORR活性提高的机理解释包括以下几种:Pt-Pt间距缩短引起压缩应变,过渡金属溶解产生更高的表面粗糙度、应力效应和配位效应导致Pt的d带中心下移或d带空位的改变、氧化物种类的延迟形成等。此外,由于合金中M对于Pt具有“锚定效应”,可以将Pt原子更好的嵌入或锚定在载体表面防止其聚集或流失,从而在提高铂合金催化剂的ORR活性同时,也能够增强其化学稳定性。
发明内容
本发明所要解决的技术问题是:质子交换膜燃料电池铂碳催化剂中铂纳米颗粒与碳基底之间的相互作用较弱,铂纳米颗粒催化活性较低并且在长时间的ORR过程中化学稳定性弱,容易团聚失活的问题。本发明采用了一种经过氧化和氮化官能团表面处理的高比表面碳基底,通过化学螯合金属盐中的金属离子,制备具有良好合金化程度和与碳基底具有锚定作用的铂合金/碳复合催化剂,有效提高催化剂的电化学活性和稳定性。
一种采用化学螯合吸附法合成的质子交换膜燃料电池铂合金催化剂,其通过以下方法制备得到:
第1步,将多孔碳基底在浓硝酸中进行处理,再在氨气气氛下焙烧处理,得到碳基底材料;
第2步,将第1步中得到的碳基底与铂、银、铜的前驱体在有机溶剂中进行混合,干燥后,进行焙烧,得到催化剂。
在一个实施方式中,第1步中浓硝酸中进行处理是在40-68 wt%浓硝酸中化学处理2-5 h,处理温度为60-90 ℃。
在一个实施方式中,第1步中焙烧处理温度为300-600 ℃,时间为1-5 h。
在一个实施方式中,在第2步中,焙烧过程是在还原性气氛下700 ℃焙烧1-5 h。
在一个实施方式中,在第2步中,有机溶剂是乙醇。
有益效果
本发明的优点在于:通过对碳基底的氧化和氮化改性,使金属前驱体与碳吸附复合过程中,不仅能够使多孔碳基底能够牢牢螯合住铂,银,铜等金属离子,从而提高煅烧制备的铂合金纳米颗粒的分散度和合金化程度;并且由于化学螯合的特性,提高了铂合金颗粒-碳载体之间的相互作用力,进一步锚定贵金属纳米粒子,以增强催化剂的电化学稳定性。
附图说明
图1是本发明采用的化学螯合吸附法合成铂合金催化剂的示意图。
图2是实施例1制备得到的Pt3AgCu3/ON-EC-600J样品与商业Pt/C对比的LSV性能曲线。
图3是对照例1制备得到的Pt3AgCu3/EC-600J样品的LSV性能图样品与商业Pt/C对比的LSV性能曲线。
图4是实施例1制备得到的Pt3AgCu3/ON-EC-600J样品与商业Pt/C对比的ECSA曲线。
图5是实施例2制备得到的PtAgCu/ON-XC-72R样品的XRD晶体结构图。
图6是实施例3制备得到的Pt3AgCu/ON-EC-300J样品的XRD晶体结构图。
具体实施方式
实施例1:
将1.0 g EC-600J碳基底浸泡在50 mL的浓硝酸中(40 wt%),并于70℃下油浴加热搅拌处理3 h。抽滤洗涤后,在氨气(NH3)氛围下焙烧400 ℃,3 h。获得表面官能团氧化和氮化改性处理后的碳基底(ON-EC-600J)。
之后,量取53.3 mg 氯铂酸,17.55 mg 氯化铜,4.92 mg 氯化银,分散于10 mL乙醇溶剂中,与76 mg ON-EC-600J碳基底均匀混合。烘干后,在氢氩气(10% H2)还原气氛的保护下,700 ℃焙烧2 h。冷却至室温后,最后在0.1M HNO3 中80 ℃酸洗去除杂质,获得纯净的产物Pt3AgCu3/ON-EC-600J。电化学测试结果表明,采用Ag,Cu共合金化的三元合金催化剂Pt3AgCu3/ON-EC-600J表现出比商业铂碳更加优越的ORR活性和电化学活性面积,如图2和图4所示。其性能数据对比见表1。
实施例2:
将1.0 g XC-72R碳基底浸泡在50 mL的浓硝酸中(68 wt%),并于60℃下油浴加热搅拌处理5 h。抽滤洗涤后,在氨气(NH3)氛围下焙烧600 ℃,1.0 h。获得表面官能团氧化和氮化改性处理后的碳基底(ON-XC-72R)。
之后,量取53.3 mg 氯铂酸,17.55 mg 氯化铜,14.76 mg 氯化银,分散于10 mL乙醇溶剂中,与76 mg ON-XC-72R碳基底均匀混合。烘干后,在氢氩气(50% H2)还原气氛的保护下,700 ℃焙烧1 h。冷却至室温后,最后在0.1M HNO3 中80 ℃酸洗去除杂质,获得纯净的产物PtAgCu/ON-XC-72R。其XRD晶体结构曲线如图5所示。
实施例3:
将1.0 g EC-300J碳基底浸泡在50 mL的浓硝酸中(50 wt%),并于90℃下油浴加热搅拌处理2 h。抽滤洗涤后,在氨气(NH3)氛围下焙烧300 ℃,5.0 h。获得表面官能团氧化和氮化改性处理后的碳基底(ON-EC-300J)。
之后,量取53.3 mg 氯铂酸,5.85 mg 氯化铜,4.92 mg 氯化银,分散于10 mL乙醇溶剂中,与76 mg ON-EC-300J碳基底均匀混合。烘干后,在氢氮气(70% H2)还原气氛的保护下,700 ℃焙烧3 h。冷却至室温后,最后在0.1M HNO3 中80 ℃酸洗去除杂质,获得纯净的产物Pt3AgCu/ON-EC-300J。其XRD晶体结构曲线如图6所示。
对照例1
与实施例1的区别在于:未对碳基底进行氧化/氮化的处理步骤,制备得到的Pt3AgCu3/EC-600J样品。其LSV性能曲线如图3所示。
表1是实施例1制备得到的Pt3AgCu3/ON-EC-600J样品,和对照例1中的Pt3AgCu3/EC-600J与商业Pt/C的性能对比表格。
从上表中可以看出,本发明中采用的方法对碳基底材料采用了硝酸和氨气气氛焙烧处理后,显著地提高其表面对于金属离子的吸附螯和作用,制备得到的催化材料在应用于PEMFC电池时,表现出更好的催化活性。
Claims (5)
1.一种采用化学螯合吸附法合成的质子交换膜燃料电池铂合金催化剂,其特征在于,其通过以下方法制备得到:
第1步,将多孔碳基底在浓硝酸中进行处理,再在氨气气氛下焙烧处理,得到碳基底材料;
第2步,将第1步中得到的碳基底与铂、银、铜的前驱体在有机溶剂中进行混合,干燥后,进行焙烧,得到催化剂。
2.根据权利要求1所述的采用化学螯合吸附法合成的质子交换膜燃料电池铂合金催化剂,其特征在于,在一个实施方式中,第1步中浓硝酸中进行处理是在40-68 wt%浓硝酸中化学处理2-5 h,处理温度为60-90 ℃。
3.根据权利要求1所述的采用化学螯合吸附法合成的质子交换膜燃料电池铂合金催化剂,其特征在于,在一个实施方式中,第1步中焙烧处理温度为300-600 ℃,时间为1-5 h。
4.根据权利要求1所述的采用化学螯合吸附法合成的质子交换膜燃料电池铂合金催化剂,其特征在于,在一个实施方式中,在第2步中,焙烧过程是在还原性气氛下700 ℃焙烧1-5 h。
5.根据权利要求1所述的采用化学螯合吸附法合成的质子交换膜燃料电池铂合金催化剂,其特征在于,在一个实施方式中,在第2步中,有机溶剂是乙醇。
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