CN111804308B - Ag-Co薄膜/纳米颗粒/薄膜催化剂及其制备方法 - Google Patents

Ag-Co薄膜/纳米颗粒/薄膜催化剂及其制备方法 Download PDF

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CN111804308B
CN111804308B CN202010603616.3A CN202010603616A CN111804308B CN 111804308 B CN111804308 B CN 111804308B CN 202010603616 A CN202010603616 A CN 202010603616A CN 111804308 B CN111804308 B CN 111804308B
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孙浩亮
吕源江
张灏戈
史鹏
王广欣
刘元昊
孙纪航
魏明
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Abstract

Ag‑Co薄膜/纳米颗粒/薄膜催化剂及其制备方法，在Mo‑Ag合金膜的一个表面制备出蠕虫状Ag颗粒，之后在蠕虫状Ag颗粒表面溅射沉积一层Ag‑Co合金膜，在制备时，通过在聚酰亚胺基体上溅射沉积Mo‑Ag合金膜时形成蠕虫状Ag颗粒，之后在形成蠕虫状Ag颗粒的表面溅射沉积Ag‑Co合金膜，使聚酰亚胺基体保持与基片台呈5‑10°夹角的悬垂状态进行溅射，且保证所溅射形成的Mo‑Ag合金膜的厚度为100‑200nm，Ag的含量为22‑29at%。本发明的催化剂通过在Mo‑Ag合金膜的表面制备出蠕虫状Ag颗粒后再溅射沉积Ag‑Co合金膜，从而形成了薄膜、颗粒和薄膜的协同催化效果，大大提升了催化性能。

Description

Ag-Co薄膜/纳米颗粒/薄膜催化剂及其制备方法
技术领域
本发明涉及到负载型金属纳米催化剂领域，具体的说是一种Ag-Co薄膜/纳米颗粒/薄膜催化剂及其制备方法。
背景技术
近年来，负载型金属纳米催化剂具有良好的活性，稳定性等催化性能，在催化研究及应用领域中受到了广泛关注和研究。在影响负载型金属纳米催化剂催化效果的因素中颗粒尺寸和形态是最终的因素，金属颗粒的尺寸成为决定负载型金属催化剂催化性能及选择性的关键因素。为提升催化剂的性能，2011年，张涛课题组首次报道单原子催化剂的合成与表征，研究发现其中Pt原子在催化剂表面呈原子级分散，导致该催化剂表现出优异的一氧化碳氧化及选择性氧化的反应活性。同时，单原子催化剂还表现出许多新颖的特性，例如，具有更高不饱和的配位环境，量子尺寸效应，与衬底相互作用，已成为连接多相催化与均相催化的桥梁。当然，单原子催化剂同样也存在不足，尺寸的减小导致表面自由能急剧增加，使得单原子催化剂在制备和反应过程中易于团聚生长，为了避免颗粒的形成，单原子催化剂的负载量均较低。
发明内容
为了提升负载型金属纳米催化剂的催化性能，本发明提供了一种Ag-Co薄膜/纳米颗粒/薄膜催化剂及其制备方法，该催化剂通过在Mo-Ag合金膜的表面制备出蠕虫状Ag颗粒后再溅射沉积上Ag-Co合金膜，从而形成了薄膜、颗粒和薄膜的协同催化效果，明显提升了催化性能。
本发明为实现上述技术目的所采用的技术方案为： Ag-Co薄膜/纳米颗粒/薄膜催化剂，其主体为Mo-Ag合金膜，在所述Mo-Ag合金膜的一个表面制备出蠕虫状Ag颗粒，之后在蠕虫状Ag颗粒表面溅射沉积一层Ag-Co合金膜。
作为上述Ag-Co薄膜/纳米颗粒/薄膜催化剂的一种优化方案，所述蠕虫状Ag颗粒的尺寸为50-180nm。
作为上述Ag-Co薄膜/纳米颗粒/薄膜催化剂的另一种优化方案，所述Mo-Ag合金膜的厚度为80-200nm，其中Ag的含量为22-29at%。
作为上述Ag-Co薄膜/纳米颗粒/薄膜催化剂的另一种优化方案，所述Mo-Ag合金膜是以聚酰亚胺为基体，并使其保持与基片台呈5-10°夹角的悬垂状态后，溅射沉积获得。
作为上述Ag-Co薄膜/纳米颗粒/薄膜催化剂的另一种优化方案，所述Ag-Co合金膜的厚度为15-26nm。
上述Ag-Co薄膜/纳米颗粒/薄膜催化剂的制备方法，通过在聚酰亚胺基体上溅射沉积Mo-Ag合金膜时形成蠕虫状Ag颗粒，之后在形成蠕虫状Ag颗粒的表面溅射沉积Ag-Co合金膜即可得到，在溅射沉积Mo-Ag合金膜时，使聚酰亚胺基体保持与基片台呈5-10°夹角的悬垂状态进行溅射，且保证所溅射形成的Mo-Ag合金膜的厚度为80-200nm，Ag的含量为22-29at%。
上述Ag-Co薄膜/纳米颗粒/薄膜催化剂的制备方法，所述Ag-Co合金膜溅射沉积时，采用由Ag靶与其表面覆盖的Co片构成复合靶材，施以射频溅射工艺，功率为100w，沉积时间为1-2min。
本发明的具体制备工艺为：首先，将清洗好的聚酰亚胺（PI）基体倾斜固定到磁控溅射镀膜机基片台上，并且使PI基体保持与基片台之间呈5-10°夹角的悬垂状态。然后在PI基体上溅射沉积Mo-Ag合金膜，即可室温制备出蠕虫状Ag颗粒/Mo-Ag合金膜/PI基体的膜基体系；
其次，在已经制备的蠕虫状Ag颗粒/Mo-Ag合金膜/PI基体表面再次用磁控溅射沉积Ag-Co合金膜。沉积工艺为采用射频溅射，功率100W，沉积时间1-2min，即可制备出Ag-Co合金膜/蠕虫状Ag颗粒/Mo-Ag合金膜复合结构催化剂，即为本发明的产品。
为了获得蠕虫状纳米Ag颗粒，本发明的核心是采用倾斜溅射，并且严格控制Mo-Ag合金膜Ag含量（22-29at%）、薄膜厚度（80-200nm），最终在室温下获得蠕虫状Ag颗粒/Mo-Ag合金膜复合结构催化剂。如果Ag含量和膜厚超出本发明设计范围，则不会获得蠕虫状Ag颗粒，可能获得球状多面体结构或者薄膜表面没有Ag颗粒形成。
本发明中的镀膜设备为JCP-350高真空磁控溅射镀膜机，制备Mo-Ag合金膜/聚酰亚胺基体的参数为：首先将聚酰亚胺基体倾斜固定到磁控溅射镀膜机基片台上，然后对真空室抽真空，使真空度达到6×10-4 Pa，然后，通入高纯氩气使真空室的气压达到0.5Pa。接下来采用射频磁控溅射法制备Mo-Ag合金膜，溅射靶材是由99.95at%Mo靶和覆盖在Mo靶上的99.99at%的Ag片组成的复合靶材，基片为375μm厚的聚酰亚胺薄膜，溅射过程中基片不加热。溅射功率100W，溅射时间5-12分钟；
本发明制备的纯银颗粒形态均为蠕虫状，颗粒平均尺寸在50-180nm之间。可通过改变Mo-Ag合金膜中的Ag含量或薄膜厚度的工艺参数调控Ag颗粒的尺寸。
与现有技术相比，本发明具有如下有益效果：
1）本发明首次在薄膜表面制备出了蠕虫状纳米尺度Ag颗粒，所获得的蠕虫状纳米尺度Ag颗粒与以往用化学、物理方法制备的多面体或者球形Ag纳米颗粒形态完全不同，为蠕虫状，蠕虫状Ag纳米颗粒具有独特的物理化学性能，以往文献中未见报道；而基于此制备出的Ag-Co合金膜/蠕虫状Ag颗粒/Mo-Ag合金膜复合结构催化剂，以往文献中未见报道，更重要的是，形成了薄膜、颗粒和薄膜的协同催化效果，大大提升了催化性能；
2）本发明方法简单，环境友好，成本低，易于室温制备尺寸均匀的具有大比表面积的Ag-Co合金膜/蠕虫状纳米Ag颗粒/合金薄膜复合催化剂，可用于催化、柔性电子器件及光电显示器件等领域。
附图说明
图1为实施例1所制备的产品表面形貌图；
图2为实施例3所制备的产品表面形貌图。
具体实施方式
下面结合具体实施例对本发明作进一步说明，以使本领域的技术人员可以更好的理解本发明并能予以实施，但所举实施例不作为对本发明的限定。
实施例1
制备Ag-Co薄膜/纳米颗粒/薄膜催化剂的方法，包括以下步骤：
1）将清洗好的聚酰亚胺（PI）基体倾斜固定到磁控溅射镀膜机基片台上，并且使PI基体保持与基片台之间呈5°夹角的悬垂状态。然后对真空室抽真空，使真空度达到6×10-4 Pa，通入高纯氩气使真空室的气压达到0.5Pa。接下来对复合靶材进行10min预溅射，预溅结束后，采用射频磁控溅射法制备Mo-Ag合金膜，溅射过程中基片不加热，溅射功率100W，溅射时间5分钟，即可制备出蠕虫状Ag颗粒/Mo-Ag合金膜复合结构；
2）在已经制备的蠕虫状Ag颗粒/Mo-Ag合金膜复合结构表面再次用磁控溅射沉积Ag-Co合金膜。沉积工艺为采用射频溅射，功率100W，溅射沉积1min，即可制备出Ag-Co合金膜/蠕虫状Ag颗粒/Mo-Ag合金膜复合结构催化剂。
最终在室温下获得Ag-Co合金膜/蠕虫状Ag颗粒/Mo-Ag合金膜复合结构催化剂，其中Mo-Ag膜中Ag含量22%，膜厚80nm，薄膜表面形貌如图1所示，蠕虫状Ag颗粒的平均尺寸约为50nm，Ag-Co薄膜厚度约为15nm。从图1中可以看出，覆盖Ag-Co薄膜后，蠕虫状Ag颗粒的尺寸变大，颗粒之间的间距变小，薄膜表面没有颗粒的区域面积减小了，有助于提升颗粒膜的催化性能。
实施例2
制备Ag-Co薄膜/纳米颗粒/薄膜催化剂的方法，包括以下步骤：
1）将清洗好的聚酰亚胺（PI）基体倾斜固定到磁控溅射镀膜机基片台上，并且使PI基体保持与基片台之间呈7°夹角的悬垂状态。然后对真空室抽真空，使真空度达到6×10-4 Pa，通入高纯氩气使真空室的气压达到0.5Pa。接下来对复合靶材进行10min预溅射，预溅结束后，采用射频磁控溅射法制备Mo-Ag合金膜，溅射过程中基片不加热，溅射功率100W，溅射时间9分钟，即可制备出蠕虫状Ag颗粒/Mo-Ag合金膜复合结构；
2）在已经制备的蠕虫状Ag颗粒/Mo-Ag合金膜复合结构表面再次用磁控溅射沉积Ag-Co合金膜。沉积工艺为采用射频溅射，功率100W，溅射沉积1.5min，即可制备出Ag-Co合金膜/蠕虫状Ag颗粒/Mo-Ag合金膜复合结构催化剂。
最终在室温下获得Ag-Co合金膜/蠕虫状Ag颗粒/Mo-Ag合金膜复合结构，其中Mo-Ag合金膜中Ag含量26%，膜厚150nm，薄膜表面形貌如图2所示，蠕虫状Ag颗粒的平均尺寸约为100nm，蠕虫状Ag颗粒的平均尺寸约为50nm，Ag-Co薄膜厚度约为21 nm。
实施例3
制备Ag-Co薄膜/纳米颗粒/薄膜催化剂的方法，包括以下步骤：
1）将清洗好的聚酰亚胺（PI）基体倾斜固定到磁控溅射镀膜机基片台上，并且使PI基体保持与基片台之间呈10°夹角的悬垂状态。然后对真空室抽真空，使真空度达到6×10-4 Pa，通入高纯氩气使真空室的气压达到0.5Pa。接下来对复合靶材进行10min预溅射，预溅结束后，采用射频磁控溅射法制备Mo-Ag合金膜，溅射过程中基片不加热，溅射功率100W，溅射时间12分钟，即可制备出蠕虫状Ag颗粒/Mo-Ag合金膜复合结构；
2）在已经制备的蠕虫状Ag颗粒/Mo-Ag合金膜复合结构表面再次用磁控溅射沉积Ag-Co合金膜。沉积工艺为采用射频溅射，功率100W，溅射沉积2min，即可制备出Ag-Co合金膜/蠕虫状Ag颗粒/Mo-Ag合金膜复合结构催化剂。
最终在室温下获得Ag-Co合金膜/蠕虫状Ag颗粒/Mo-Ag合金膜复合结构，其中Ag含量29%，膜厚200nm，薄膜表面形貌如图2所示。其中，蠕虫状Ag颗粒的平均尺寸约为180nm，Ag-Co薄膜厚度26nm。从图2中可以看出，覆盖Ag-Co薄膜后，蠕虫状Ag颗粒的尺寸变大，颗粒之间的间距变小，有助于提升颗粒膜的催化性能。

Claims (5)

1.Ag-Co薄膜/纳米颗粒/薄膜催化剂，其主体为Mo-Ag合金膜，其特征在于：通过在聚酰亚胺基体上溅射沉积Mo-Ag合金膜时形成蠕虫状Ag颗粒，之后在蠕虫状Ag颗粒表面溅射沉积一层Ag-Co合金膜；所述Mo-Ag合金膜的厚度为80-200nm，其中Ag的含量为22-29at%；所述Mo-Ag合金膜是以聚酰亚胺为基体，并使其保持与基片台呈5-10°夹角的悬垂状态后，溅射沉积获得。
2.根据权利要求1所述的Ag-Co薄膜/纳米颗粒/薄膜催化剂，其特征在于：所述蠕虫状Ag 颗粒的尺寸为 50-180nm。
3.根据权利要求1所述的Ag-Co薄膜/纳米颗粒/薄膜催化剂，其特征在于：所述Ag-Co合金膜的厚度为15-26nm。
4.根据权利要求1所述的Ag-Co薄膜/纳米颗粒/薄膜催化剂的制备方法，通过在聚酰亚胺基体上溅射沉积Mo-Ag合金膜时形成蠕虫状Ag颗粒，之后在形成蠕虫状Ag颗粒的表面溅射沉积Ag-Co合金膜即可得到，其特征在于：在溅射沉积Mo-Ag合金膜时，使聚酰亚胺基体保持与基片台呈5-10°夹角的悬垂状态进行溅射，且保证所溅射形成的Mo-Ag合金膜的厚度为80-200nm，Ag的含量为22-29at%。
5.根据权利要求4所述的Ag-Co薄膜/纳米颗粒/薄膜催化剂的制备方法，其特征在于：所述溅射沉积Ag-Co合金膜时，采用由Ag靶与其表面覆盖的Co片构成复合靶材，施以射频溅射工艺，功率为100w，沉积时间为1-2min。
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