CN101785999B - 一种燃料电池用电催化剂Pt1Bi1金属间化合物的制备方法 - Google Patents
一种燃料电池用电催化剂Pt1Bi1金属间化合物的制备方法 Download PDFInfo
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- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 8
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- 238000006243 chemical reaction Methods 0.000 claims description 3
- FBEIPJNQGITEBL-UHFFFAOYSA-J tetrachloroplatinum Chemical compound Cl[Pt](Cl)(Cl)Cl FBEIPJNQGITEBL-UHFFFAOYSA-J 0.000 claims description 3
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- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 2
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Abstract
本发明公开了一种质子交换膜燃料电池用电催化剂Pt1Bi1金属间化合物的制备方法,分为两步:1)按铂与铋的原子比为1∶1将含铋前驱体和含铂的前驱体各0.1mmol及碳粉加入200mL 1mol L-1的盐酸溶液中,水浴搅拌下通过5mol L-1氢氧化钠溶液调节pH至3,然后加入还原剂,90℃下反应10小时后过滤得到Pt1Bi1金属间化合物前驱体;2)将1)过程中制得的前驱体在还原气氛下低温300-600℃热处理2-6小时后得到金属间化合物Pt1Bi1电催化剂。本发明所制备得到的Pt1Bi1金属间化合物颗粒粒径为3nm左右,具有很好抗甲醇中毒的氧还原活性及电催化氧化甲酸活性,本方法制备简单,适合大规模制备。
Description
技术领域
本发明涉及一种燃料电池用电催化剂Pt1Bi1金属间化合物的制备方法,属于燃料电池材料科学技术领域和电催化领域。
背景技术
燃料电池是一种将化学能转换为电能的装置,由于其不受卡诺循环的限制,能量转化效率高,且环境友好而被受到广泛关注,其被认为是21世纪首选的高效清洁的发电方式。
根据所选用的电解质不同,燃料电池可以分为五类(碱性燃料电池、质子交换膜燃料电池、磷酸燃料电池、熔融碳酸盐燃料电池、固体氧化物燃料电池),其中,质子交换膜膜燃料电池由于具有可室温快速启动、寿命长、比功率和比能量高等特点而特别适合用作电动汽车及便携式电子设备的电源。
目前,质子交换膜燃料电池使用的电催化剂主要有Pt/C及PtRu两种,由于Pt价格昂贵及资源有限,因此欲实现质子交换膜燃料电池商业化,必须进一步降低铂的使用量并提高其催化性能,Pt基合金化是其中一种主要选择。Pt基合金中的金属间化合物一类由于具有有序的结构及其他特点而较其他无序的Pt基固溶相合金具有更好的催化选择性及催化活性和稳定性。
发明内容
本发明的目的是提供一种质子交换膜燃料电池用电催化剂Pt1Bi1金属间化合物的制备方法。
本发明提出Pt1Bi1金属间化合物的制备方法,技术方案分为两步:
1)按铂与铋的原子比为1∶1将含铋前驱体和含铂的前驱体各0.1mmol及碳粉加入200mL 1mol L-1的盐酸溶液中,水浴搅拌下通过5molL-1氢氧化钠溶液调节pH至3,然后加入还原剂,90℃下反应10小时后过滤得到Pt1Bi1金属间化合物前驱体;
2)将1)过程中制得的前驱体在还原气氛下低温300-600℃热处理2-6小时后得到金属间化合物Pt1Bi1电催化剂。
上述含铋前驱体为氯化铋或硝酸铋,含铂前驱体为氯铂酸、四氯化铂,碳粉的质量根据需制备催化剂中铂的载量来确定,还原剂为次亚磷酸二氢钠或硼氢化钠,其加入次亚磷酸二氢钠与金属原子总量的摩尔比为100-120或硼氢化钠与金属原子总量的摩尔比为50-60,热处理的还原气氛为氢气体积比大于2%的配气,配气中的另一组分为惰性气氛,为氮气或氩气,如95%Ar+5%H2。
本发明所制备得到的Pt1Bi1金属间化合物颗粒粒径为3nm左右,具有很好抗甲醇中毒的氧还原活性及电催化氧化甲酸活性,本方法制备简单,适合大规模制备。
附图说明
图1为本发明“二步法”制备燃料电池用电催化剂Pt1Bi1金属间化合物的流程图;
图2为实施例1中制得的燃料电池用电催化剂金属间化合物Pt1Bi1的X射线衍射图;
图3为实施例2中制得的燃料电池用电催化剂金属间化合物Pt1Bi1的X射线衍射图;
图4为实施例1制得的燃料电池用电催化剂金属间化合物Pt1Bi1的投射电镜照片;
图5为实施例1制得的燃料电池用催化剂金属间化合物Pt1Bi1在0.5mol L-1 H2SO4中的电化学循环伏安曲线,其中1为氮气,2为氧气。
图6为本发明实施例1和实施例2制得的金属间化合物Pt1Bi1在0.5mol L-1 H2SO4+0.5mol L-1 HCOOH中的电化学循环伏安曲线,其中1为实施例1的循环伏安曲线,2为实施例2的循环伏安曲线。
具体实施方式
实施例1
合成过程参见图1:将51.8mg氯铂酸(H2PtCl6 6H2O)和48.5mg硝酸铋(Bi(NO3)35H2O)加入200mL 1mol L-1盐酸中,待溶解后加入50mg碳粉(Vulcan XC-72),在90℃恒温水浴搅拌的条件下用5mol L-1NaOH调节pH至3后加入次亚磷酸钠3g,反应10小时后抽滤出样品,干燥后置于具有还原性的混合气氛(95%Ar+5%H2)中350℃热处理3小时后得碳载金属间化合物Pt1Bi1电催化剂。其X射线衍射照片如图2所示,投射电子显微镜照片如图4所示。将所得的碳载金属间化合物Pt1Bi1电催化剂制成工作电极,采用传统三电极体系,标准氢电极为参比电极,玻碳片作为辅助电极,进行电化学测试,图5给出了其在0.5mol L-1H2SO4中氮气饱和(图5中的1)和氧气饱和(图5中的2)条件下的循环伏安曲线,扫描速度为20mV s-1,图6中1给出了其在0.5mol L-1H2SO4+0.5MHCOOH中的循环伏安曲线,扫描速度为50mV s-1。
实施例2
合成过程参见图1:将51.8mg氯铂酸(H2PtCl6 6H2O)和48.5mg硝酸铋(Bi(NO3)35H2O)加入200mL 1mol L-1盐酸中,待溶解后加入50mg碳粉(Vulcan XC-72),在90℃恒温水浴搅拌的条件下用5mol L-1NaOH调节pH至3后加入次亚磷酸钠3g,反应10小时后抽滤出样品,干燥后置于具有还原性的混合气氛(95%Ar+5%H2)中500℃热处理3小时后得碳载金属间化合物Pt1Bi1电催化剂。X射线衍射照片如图3示。图6中2给出了在0.5mol L-1 H2SO4+0.5MHCOOH中的循环伏安曲线,扫描速度为50mV s-1。
实施例3
合成过程参见图1:将34.0mg四氯化铂(PtCl4)和31.5mg氯化铋(BiCl3)加入200mL 1mol L-1盐酸中,待溶解后加入50mg碳粉(VulcanXC-72),在90℃恒温水浴搅拌的条件下用5mol L-1NaOH调节pH至3后加入硼氢化钠(NaBH4)0.4g,反应10小时后抽滤出样品,干燥后置于具有还原性的混合气氛(95%Ar+5%H2)中600℃热处理3小时后得碳载金属间化合物Pt1Bi1电催化剂。
Claims (5)
1.一种质子交换膜燃料电池用电催化剂Pt1Bi1金属间化合物的制备方法,其特征在于,包括以下步骤:
1)按铂与铋的原子比为1∶1将含铋前驱体和含铂的前驱体各0.1mmol及碳粉加入200mL 1mol L-1的盐酸溶液中,水浴搅拌下通过5mol L-1氢氧化钠溶液调节pH至3,然后加入还原剂,90℃下反应10小时后过滤得到Pt1Bi1金属间化合物前驱体;
2)将1)过程中制得的前驱体在还原气氛下低温300-600℃热处理2-6小时后得到金属间化合物Pt1Bi1电催化剂;
所述还原剂为次亚磷酸二氢钠或硼氢化钠;所述还原气氛为氢气体积
比大于2%的配气,配气中的另一组分为惰性气氛。
2.按照权利要求1的制备方法,其特征在于,所述含铋前驱体为氯化铋或硝酸铋。
3.按照权利要求1的制备方法,其特征在于,所述含铂前驱体为氯铂酸、四氯化铂。
4.按照权利要求1的制备方法,其特征在于,次亚磷酸二氢钠与金属原子总量的摩尔比为100-120。
5.按照权利要求1的制备方法,其特征在于,硼氢化钠与金属原子总量的摩尔比为50-60。
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CN103551147B (zh) * | 2013-10-10 | 2015-07-29 | 北京工业大学 | 一种快速、可控的PtBi金属间化合物电催化剂的合成方法 |
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