CN101521282A - 一种金属电极催化剂及其制备方法 - Google Patents
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Abstract
本发明公开了一种金属电极催化剂，化学式为MxA1－x，其中M选自Ag、Pt、Pd、Ru和Rh中的一种或其组合；A选自Mn、Cr、Fe、Co、Ni、Cu、Nb、Mo、V、Ti、Zn、Zr、Ce、Y、Pb中的一种或其组合；其中0.70≤x≤0.99。本发明还提供了制备上述催化剂的方法，将含元素M和A的混合盐溶液，浸渍注入多孔层，烘干，焙烧直到多孔层内形成纳米催化颗粒，即得电极催化剂。本发明制备的催化剂在工作时不易烧结，可长时间稳定操作，广泛应用于各种燃料电池电极。
Description
技术领域
本发明属于能源领域，具体涉及一种金属电极催化剂及其制备方法，尤其适用于固体氧化物燃料电池阴极。
背景技术
固体氧化物燃料电池(SOFC)作为一种高温燃料电池可以直接以碳氢化合物或其内重整气为燃料，不仅具有高能效和低污染等突出特点，还具有低温燃料电池所不具备的燃料选择范围大的优点，除了纯氢外，CO、醇、烃、煤气、甚至氨都可以作为其燃料，另外，SOFC具有较高的功率密度。SOFC在固定电站、移动电源、移动运输以及军事等领域都有着广泛的应用前景。其成功应用对于缓解我国能源危机，满足人们对电力数量与质量的不断提升的要求，保护人类的居住环境及保障我国的能源安全具有重大意义。
目前SOFC商业化的主要障碍是其居高不下的成本，而降低SOFC的工作温度被视为降低成本的关键。当燃料电池的操作温度降至800℃以下，就可以采用金属连接体，从而大大降低电池的材料成本，降低电池组件之间的相反应，同时电池组件热膨胀系数不匹配对电池稳定性的影响也变小，使得密封变得容易。
然而，随着温度的下降，阴极对氧气的催化还原活性也随之急剧降低，使阴极电阻迅速增大。贵金属与电解质材料组成的复合阴极在800℃温度下显示了优越的氧气催化还原性能，同时贵金属催化剂与电解质不存在相反应，也不会发生CO2中毒。这些优点使贵金属阴极成为固体氧化物燃料电池阴极材料领域的研究热点之一。但该电极经长时间操作后会使贵金属催化剂烧结，颗粒聚集长大，导致催化性能下降。因此，提高阴极贵金属催化剂纳米颗粒的稳定性是使该类电极成功应用的关键。
发明内容
本发明的目的在于提供一种金属电极催化剂，该催化剂纳米颗粒在工作时不易烧结，可长时间稳定操作。
本发明的另一目的在于提供制备上述催化剂的方法，制备的催化剂纳米颗粒不易烧结，可长时间稳定操作。
一种金属电极催化剂，其化学式为MxA1-x，其中元素M选自Ag、Pt、Pd、Ru和Rh中的一种或其组合；元素A选自Mn、Cr、Fe、Co、Ni、Cu、Nb、Mo、V、Ti、Zn、Zr、Ce、Y、Pb中的一种或其组合，0.70≤x≤0.99。
一种制备上述电极催化剂的方法，具体为：将含元素M的贵金属盐和含元素A的金属盐充分溶解制备成均一透明的混合盐溶液，然后将其浸渍注入多孔层，烘干，焙烧直到多孔层内形成纳米催化颗粒，即得电极催化剂。
所述焙烧温度为500～1000℃，焙烧时间为1～5h，升温速率1～10℃/min。
本发明的技术效果体现在：
(1)在现有技术中，经过长时间操作，纳米颗粒贵金属催化剂会发生颗粒的烧结长大使阴极性能下降，而本发明制备的催化剂通过实验验证，经过长时间操作后，性能以及微观形貌没有发生明显变化。这是因为本发明中的贵金属合金较单纯的贵金属稳定，不容易发生纳米颗粒的聚集长大，长期保持贵金属一陶瓷复合阴极的催化活性和稳定性。
(2)采用贵金属与其它金属合成电极催化剂，减少了贵金属用量，节约了成本。
附图说明
图1为本发明实施例一YSZ多孔层结构示意图。
图2为实施例一多孔YSZ阴极中Pd0.95Mn0.05O合金催化剂的分布示意图。
图3为实施例一Pd+YSZ和Pd0.95Mn0.05+YSZ阴极在750℃测得的阻抗图谱。
图4为实施例一Pd+YSZ和Pd0.95Mn0.05+YSZ阴极极化阻抗与温度的关系图。
图5为实施例一Pd+YSZ和Pd0.95Mn0.05+YSZ阴极极化过电位随测试时间的变化对比示意图。
图6为实施例一长时间测试后Pd催化剂在多孔YSZ中的分布示意图。
图7为实施例一长时间测试后Pd0.95Mn0.05合金催化剂在多孔YSZ中的分布示意图。
图8为本发明实施例二Pd0.95Co0.05+YSZ阴极在750℃测得的阻抗图谱。
图9为实施例二Pd0.95Co0.05+YSZ阴极极化阻抗与温度的关系图。
图10为本发明实施例三Pd0.80Co0.20+YSZ阴极在750℃测得的阻抗图谱。
图11为实施例三Pd0.80Co0.20+YSZ阴极极化阻抗与温度的关系图。
具体实施方式
本发明中的多孔层是指附着在致密基底上的多孔材料层，多孔材料层可采用电解质材料(如：钇稳定的氧化锆(如：Y0.08Zr0.92O1.91(YSZ))、钪稳定的氧化锆(如：Sc0.2Zr0.80O1.9(SSZ))、钐掺杂的氧化铈(如：Sm0.10Ce0.9O1.95(SDC)，Gd0.20Ce0.8O1.9(GDC))、镧镓基钙钛矿型(如：La0.8Sr0.2Ga0.8Mg0.2O3(LSGM))氧化物电解质)中的任意一种，也可采用陶瓷阴极材料(如：La0.6Sr0.4MnO3、La0.6Sr0.4FeO3、Ba0.5Sr0.5Co0.8Fe0.2O3、La0.6Sr0.4Co0.2Fe0.8O3、La0.8Sr0.2MnO3、La0.8Sr0.2Sc0.2Mn0.8O3、La2NiO4、PrBaCo2O5)。通过丝网印刷，流延或喷涂法将上述材料的浆料，沉积在致密电解质的表面，经高温(1100～1300℃)焙烧，得到多孔层。
下面将结合实施例详细说明本发明
实施例一：Pd0.95Mn0.05O注入YSZ的阴极材料制备与应用。
首先是多孔层的制备：将4g YSZ、2.2g乙基纤维素—松油醇配制的粘结剂和0.1g鱼油分散剂混合研磨，制成浆料，通过丝网印刷将该浆料涂于YSZ致密电解质表面，然后在1200℃下经1h烧结后得到多孔YSZ结构，升温速率为5℃/min。图1为该阴极多孔层的SEM电镜照片。
然后，将PdCl2和MnCl2的混合盐溶液(加入少量盐酸)浸渍到上述YSZ多孔层中，经750℃焙烧后得到纳米Pd0.95Mn0.05O合金阴极催化剂。Pd0.95Mn0.05O合金氧化物在阴极的用量为1～1.4mg/cm2。图2为多孔YSZ阴极中Pd0.95Mn0.05O合金催化剂的扫描电子显微镜(SEM)照片。催化剂粒径为20～80nm。为了对比说明实验效果，现将纯PdCl2溶液浸渍到上述YSZ多孔层中，采用相同方式制备得到纳米结构Pd+YSZ阴极。图3为Pd+YSZ和Pd0.95Mn0.05+YSZ阴极在750℃测得的阻抗图谱，Pd+YSZ阴极极化阻抗为0.118Ωcm2，而Pd0.95Mn0.05+YSZ阴极的阻抗值为0.11Ωcm2。图4为阴极极化阻抗与温度的关系图，贵金属催化的Pd+YSZ和Pd0.95Mn0.05+YSZ阴极氧还原催化活化能分别为105和108kJ·mol-1。
将上述Pd+YSZ和Pd0.95Mn0.05+YSZ阴极的稳定性通过3电极法极化测试，测试电流密度为-200mA/cm2，温度为750℃。图5为两阴极极化过电位随测试时间的变化对比示意图，Pd催化电极经30h测试后Pd电极过电位增加7mV，而Pd0.95Mn0.05合金催化电极性能没有明显的衰减，阴极过电位保持为70mV。测试后Pd和Pd0.95Mn0.05合金催化剂在多孔YSZ中的分布分别如图6和7所示。结果表明经测试后，Pd催化电极形貌发生了明显的改变，电极中纳米Pd颗粒发生熔融长大，而PdMn合金催化的电极形貌没有明显改变。说明阴极催化剂中引入Mn不仅改善了催化剂的催化效果，也提高了阴极热稳定性。
实施例二：Pd0.95Co0.05O注入YSZ的阴极材料制备与应用。
多孔层的制备同实施例一，将PdCl2和Co(NO3)2的混合盐溶液(加入少量盐酸)同上述方法浸渍到YSZ多孔层中，750℃焙烧后得到纳米结构Pd0.95Co0.05O合金氧化物阴极催化剂。Pd0.95Co0.05O合金氧化物在阴极的用量为1～1.4mg/cm2。图8为Pd0.95Co0.05+YSZ阴极在750℃测得的阻抗图谱，极化阻抗为0.10Ωcm2。图9为阴极极化阻抗与温度的关系图，Pd0.95Co0.05合金催化的阴极氧还原催化活化能为103kJ·mol-1。
实施例三：Pd0.80Co0.20O注入YSZ的阴极材料制备与应用。
多孔层的制备同实施例一和二，PdCl2和Co(NO3)2的混合盐溶液(加入少量盐酸)同上述方法分别浸渍到YSZ多孔层中，750℃焙烧后得到纳米结构Pd0.80Co0.20O合金氧化物阴极催化剂。Pd0.80Co0.20O合金氧化物在阴极的用量为1～1.4mg/cm2。图10为Pd0.80Co0.20+YSZ阴极在750℃测得的阻抗图谱，极化阻抗为0.105Ωcm2。图11为Pd0.80Co0.20+YSZ阴极极化阻抗与温度的关系图，贵金属催化的阴极氧还原催化活化能为104kJ·mol-1。
本发明还分别将Pd0.95Ni0.05O、Pd0.80Ni0.20O、Pd0.95Cu0.05O、Pd0.80Cu0.20O、Pd0.95Feo0.05O和Pd0.80Fe0.20O注入YSZ形成阴极材料。除了选用材料不同，其余合成过程与测试手段均与实施例一相同，实验结果均表明按照本发明制备的催化剂具有较好的催化能力和抗烧结性能。
本发明中的金属电极催化剂不仅适用于固体氧化物燃料电池阴极，同样适用于其阳极，还可将该催化剂应用于其它燃料电池电极。
Claims (3)
1、一种金属电极催化剂，化学式为MxA1-x，其中元素M选自Ag、Pt、Pd、Ru和Rh中的一种或其组合；元素A选自Mn、Cr、Fe、Co、Ni、Cu、Nb、Mo、V、Ti、Zn、Zr、Ce、Y、Pb中的一种或其组合，0.70≤x≤0.99。
2、一种制备权利要求1所述电极催化剂的方法，具体为：将含元素M的贵金属盐和含元素A的金属盐充分溶解制备成混合盐溶液，然后将其浸渍注入多孔层，烘干，焙烧直到多孔层内形成纳米催化颗粒，即得电极催化剂。
3、根据权利要求2所述的电极催化剂制备方法，其特征在于，所述焙烧温度为500～1000℃，焙烧时间为1～5h，升温速率1～10℃/min。
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| CN102762776A (zh) * | 2010-02-10 | 2012-10-31 | 培尔梅烈克电极股份有限公司 | 产氢用活性阴极 |
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