CN114122433A - 一种银铜锰核壳结构纳米线氧还原催化剂 - Google Patents
一种银铜锰核壳结构纳米线氧还原催化剂 Download PDFInfo
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Abstract
本发明的目的在于提供一种银铜锰核壳结构纳米线氧还原催化剂。其结构特征在于其核为Ag纳米线，外包覆Cu、Mn氧化物纳米片壳层，该核壳结构纳米线中Ag核的平均直径为1～100nm，而其整体的直径为10～1000nm，该核壳结构纳米线的长度可达数百纳米至数微米。其制备方法先采用液相还原法制备银铜锰核壳结构纳米线，随后将银铜锰核壳结构纳米线负载到碳粉上即可得到最终的催化剂。该制备工艺操作简单、易于控制，所得催化剂能够持续、高效、稳定地催化氧还原反应的进行，并且其在碱性膜燃料电池中也具有较好的性能。
Description
技术领域
本发明属于微纳米材料制备技术领域，具体涉及一种银铜锰核壳结构纳米线氧还原催化剂的制备。
背景技术
在过去的三十年中，随着纳米催化剂和质子交换膜领域的最新进展，质子交换膜燃料电池成为现在研究和应用较为广泛的一种燃料电池。但是，Pt金属的高成本和有限的储量是阻碍燃料电池技术广泛使用的商业化的主要问题。由于低酸碱度***中的高腐蚀性酸性条件使得必须使用昂贵的铂族金属和合金才能实现质子交换膜燃料电池等燃料电池的长期稳定性。而碱性膜燃料电池中则可以使用廉价的非铂材料作为氧还原的催化剂，如银及其合金、掺杂碳、过渡金属大分子以及过渡金属氧化物(包括尖晶石和钙钛矿)。此外，在碱性条件下进行氧还原最显著的优点是更快的动力学和更低的过电位，这些优势使得碱性膜燃料电池成为一种有前景的电池***。
Ag的价格不到Pt的3％，并且在碱性的条件下，Ag的氧还原性能相较于酸性条件而言，得到了显著的提升，这就使得Ag成为碱性膜燃料电池中一种有前景的低成本替代品。然而目前研究出的Ag基催化剂大多还是无法与Pt等贵金属相比，同时性能相对优异的Ag基催化剂合成步骤较为繁琐。因此，Ag基电催化剂性能还需要进行很大程度的优化。研究发现，Ag与其他金属元素的复合、调控Ag基材料的形貌有利于促进其氧还原性能，因此现在的研究方向主要朝着开发具有特定形貌的多元Ag基催化剂的方向发展。
发明内容
本发明通过一步法得合成得到银铜锰核壳结构纳米线，其结构特征在于其核为Ag纳米线，外包覆Cu、Mn氧化物纳米片壳层，该核壳结构纳米线中Ag核的平均直径为1～100nm，而其整体的直径为10～1000nm，该核壳结构纳米线的长度可达数百纳米至数微米。并将其负载与碳粉得到碳载银铜锰核壳结构纳米线氧还原电催化剂。该合成方法简单易操作，易于控制。具体包括如下步骤：
步骤1：液相还原法制备银铜锰核壳结构纳米线。
(01)将一定浓度的柠檬酸钠和硝酸银溶解在超纯水中，在搅拌的条件下加入一定浓度的氯化铜和硝酸锰。
步骤(01)中，所述柠檬酸钠的一定浓度选自1mmol/L～100mmol/L。
步骤(01)中，所述硝酸银的一定浓度选自0.1mmol/L～100mmol/L。
步骤(01)中，所述氯化铜的一定浓度选自0.1mmol/L～80mmol/L。
步骤(01)中，所述硝酸猛的一定浓度选自0.1mmol/L～80mmol/L。
(02)加热至一定温度，滴加一定浓度的氨水，反应一定时间后冷却至室温。将溶液离心后取产物置于有机溶剂中保存，得到银铜锰核壳结构纳米线的分散液。
步骤(02)中，所述一定温度选自10～℃90。℃
步骤(02)中，所述氨水的一定浓度选自0.01mmol/L～50mmol/L。
步骤(02)中，所述一定时间选自0.1h～10h。
步骤(02)中，所述有机溶剂为甲醇、乙醇、戊烷、己烷、环己烷、环己酮、异丙醇、丙酮、甲苯、二甲苯、***中的一种或几种。
步骤2：将银铜锰核壳结构纳米线负载到碳粉上
(03)向步骤(02)得到的分散有银铜锰核壳结构纳米线的有机溶剂中加入一定质量的高比表面积碳粉，经过超声、抽滤、干燥，即得到负载在碳粉上的银铜锰核壳结构纳米线。
步骤(03)中，所述高比表面积碳粉的一定质量为银铜锰核壳结构纳米线质量的5％～50％。
本发明的技术原理是：利用阴离子效应，在Ag基催化剂的合成过程中引入Cl-，使其形成线状结构。同时在合成的过程中加入Cu盐、Mn盐，以Ag纳米线为模板，原位生长Cu、Mn氧化物壳层，促进氧还原反应进行。
本发明的有益效果是：
液相还原法的实验条件精确可控，得到的催化剂的尺寸形貌完整粒径均一。本发明将液相还原法应用于银铜锰核壳结构纳米线的合成，是一种新型银铜锰核壳结构纳米线的制备方法。该催化剂独特的纳米线外包覆纳米片的结构使得其氧还原性能以及稳定性得到了较大的提升。该合成方法简单易操作、原料价格较低，有效降低了催化剂的成本。最终将该催化剂作为碱性膜燃料电池的阴极侧催化剂进行测试，也展现出较好的性能，说明其具有实用性。
附图说明
图1为本发明实施例1所得银铜锰核壳结构纳米线的XRD图；
图2为本发明实施例1所得银铜锰核壳结构纳米线的TEM图；
图3为本发明实施例1所得银铜锰核壳结构纳米线的极化曲线图；
图4为本发明实施例1所得银铜锰核壳结构纳米线在碱性膜燃料电池中的电流-电压图；
图5为本发明实施例2所得银铜锰核壳结构纳米线的TEM图；
图6为本发明实施例2所得银铜锰核壳结构纳米线的极化曲线图。
具体实施方式
以下结合附图及实施例对本发明作进一步说明。
实施例1
(01)将150mg的柠檬酸钠和85mg硝酸银溶解在超纯水中，在搅拌的条件下加入36mg的氯化铜和11.6μL的硝酸锰溶液(50wt％)。
(02)加热至50，℃滴加0.15mL的氨水，反应5h后冷却至室温。将溶液离心后取产物置于乙醇中保存，得到银铜锰核壳结构纳米线的分散液。
(03)向步骤(02)得到的分散有银铜锰核壳结构纳米线的乙醇中加入38mg的高比表面积碳粉，经过超声、抽滤、干燥，即得到负载在碳粉上的银铜锰核壳结构纳米线。
如图1所示，实施例1所得银铜锰核壳结构纳米线的主要组成成分为Ag。
如图2所示，实施例1所得银铜锰核壳结构纳米线呈现Ag纳米线外包覆Cu、Mn氧化物纳米片的结构，该核壳结构纳米线的Ag核的平均直径约为39nm，而其整体的平均尺寸大约为130nm，该核壳结构纳米线的长度可达数百纳米至数微米。
如图3所示，实施例1所得银铜锰核壳结构纳米线催化氧还原反应极化曲线的半波电位达0.837V。
如图4所示，实施例1所得银铜锰核壳结构纳米线在碱性膜燃料电池中应用于阴极催化剂，电池峰值功率密度可达1.4W/cm2。
实施例2
(01)将150mg的柠檬酸钠和85mg硝酸银溶解在超纯水中，在搅拌的条件下加入36mg的氯化铜和17.4μL的硝酸锰溶液(50wt％)。
(02)加热至50，℃滴加0.15mL的氨水，反应5h后冷却至室温。将溶液离心后取产物置于乙醇中保存，得到银铜锰核壳结构纳米线的分散液。
(03)向步骤(02)得到的分散有银铜锰核壳结构纳米线的乙醇中加入38mg的高比表面积碳粉，经过超声、抽滤、干燥，即得到负载在碳粉上的银铜锰核壳结构纳米线。
如图5所示，实施例2所得银铜锰核壳结构纳米线也呈现出直径约为45nm的Ag纳米线外包覆Cu、Mn氧化物纳米片以及纳米颗粒的结构。
如图6所示，实施例2所得银铜锰核壳结构纳米线催化氧还原反应极化曲线的半波电位达0.810V。
Claims (10)
1.一种银铜锰核壳结构纳米线氧还原催化剂，其结构特征在其核为Ag纳米线，外包覆Cu、Mn氧化物纳米片壳层。
2.银铜锰核壳结构纳米线的制备方法，其特征在于，包括如下步骤：
步骤(01)：将一定浓度的柠檬酸钠和硝酸银溶解在超纯水中，在搅拌的条件下加入一定浓度的氯化铜和硝酸锰。加热至一定温度，滴加一定浓度的氨水，反应一定时间后冷却至室温。将溶液离心后取产物置于有机溶剂中保存，得到银铜锰核壳结构纳米线的分散液。
步骤(02)：向步骤(01)得到的分散有银铜锰核壳结构纳米线的乙醇中加入一定质量的高比表面积碳粉，经过超声、抽滤、干燥，即得到负载在碳粉上的银铜锰核壳结构纳米线。
3.根据权利要求1所述的一种银铜锰核壳结构纳米线的制备方法，其特征在于，所述步骤(01)中，所述柠檬酸钠的一定浓度选自1mmol/L～100mmol/L。
4.根据权利要求1所述的一种银铜锰核壳结构纳米线的制备方法，其特征在于，所述步骤(01)中，所述硝酸银的一定浓度选自0.1mmol/L～100mmol/L。
5.根据权利要求1所述的一种银铜锰核壳结构纳米线的制备方法，其特征在于，所述步骤(01)中，所述氯化铜的一定浓度选自0.1mmol/L～80mmol/L。
6.根据权利要求1所述的一种银铜锰核壳结构纳米线的制备方法，其特征在于，所述步骤(01)中，所述硝酸猛的一定浓度选自0.1mmol/L～80mmol/L。
7.根据权利要求1所述的一种银铜锰核壳结构纳米线的制备方法，其特征在于，所述步骤(01)中，所述一定温度选自10℃～90℃。
8.根据权利要求1所述的一种银铜锰核壳结构纳米线的制备方法，其特征在于，所述步骤(01)中，所述氨水的一定浓度选自0.01mmol/L～50mmol/L。
9.根据权利要求1所述的一种银铜锰核壳结构纳米线的制备方法，其特征在于，所述步骤(01)中，所述一定时间选自0.1h～10h。
10.根据权利要求1所述的一种银铜锰核壳结构纳米线的制备方法，其特征在于，所述步骤(01)中，所述有机溶剂为甲醇、乙醇、戊烷、己烷、环己烷、环己酮、异丙醇、丙酮、甲苯、二甲苯、***中的一种或几种。
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