CN103687683B - 从钯纳米颗粒除去表面活性剂 - Google Patents

从钯纳米颗粒除去表面活性剂 Download PDF

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CN103687683B
CN103687683B CN201180071441.5A CN201180071441A CN103687683B CN 103687683 B CN103687683 B CN 103687683B CN 201180071441 A CN201180071441 A CN 201180071441A CN 103687683 B CN103687683 B CN 103687683B
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M.邵
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Abstract

从钯纳米颗粒除去表面活性剂的方法，其包括将钯纳米颗粒暴露于氢气并从钯纳米颗粒除去表面活性剂。方法包括使用表面活性剂合成钯纳米颗粒。所述表面活性剂影响钯纳米颗粒的几何性质并结合至钯纳米颗粒。所述方法也包括将钯纳米颗粒暴露于氢气以从钯纳米颗粒除去表面活性剂。

Description

从钯纳米颗粒除去表面活性剂
背景技术
钯和钯合金纳米颗粒可用作催化剂，具体地在燃料电池中用以产生电场能。例如，在氢燃料电池中，在燃料电池的阳极可用钯催化剂氧化氢气成质子和电子。在燃料电池的阴极，钯催化剂引发氧还原反应（ORR），导致水的形成。
燃料电池的性能部分取决于钯纳米颗粒的可用表面积。当钯纳米颗粒的表面积增大时，燃料电池的性能一般增强。除了尺寸，也可选择钯纳米颗粒的形状以进一步增强氧还原反应（ORR）的活性。在纳米颗粒形成期间通常使用表面活性剂以控制颗粒尺寸和形状。在纳米颗粒成形和成尺寸（size）时表面活性剂结合至纳米颗粒。
一旦形成纳米颗粒，需要将用于使颗粒成形和成尺寸的表面活性剂除去。一些表面活性剂可通过洗涤和低温热处理除去。但是，其它表面活性剂需要长洗涤时间（在特定溶剂中长达几周）或在高于300°C的温度下高温处理。对于一些催化剂纳米颗粒，高温处理存在问题。例如，在300°C，立方钯纳米颗粒可能失去它们的形状并粒度增大。结果，使用高温处理从纳米颗粒除去表面活性剂消除了所述表面活性剂意在提供的益处。
发明综述
从钯纳米颗粒除去表面活性剂的方法包括，将钯纳米颗粒暴露于氢气并从钯纳米颗粒除去表面活性剂。
方法包括使用表面活性剂合成钯纳米颗粒。表面活性剂影响钯纳米颗粒的几何性质并结合至钯纳米颗粒。所述方法也包括将钯纳米颗粒暴露于氢气以从钯纳米颗粒除去表面活性剂。
附图简述
图1是从钯纳米颗粒除去表面活性剂的方法的简化图。
图2用电势将表面活性剂和钯纳米颗粒之间的结合暴露于氢气的方法的简化图。
图3用氢气将表面活性剂和钯纳米颗粒之间的结合暴露于氢气的方法的简化图。
图4是从钯纳米颗粒除去表面活性剂的方法的简化图。
图5是制备钯纳米颗粒的方法的简化图。
发明详述
本发明提供从钯纳米颗粒除去表面活性剂的简单有效的方法。电化学和化学方法使用氢气弱化表面活性剂在钯纳米颗粒上的吸附。该方法提供从钯纳米颗粒除去表面活性剂的简单有效的方式而不使用高温。
表面活性剂经常被用于改变用作燃料电池催化剂的钯纳米颗粒的尺寸和形状。在钯纳米颗粒形成期间存在的表面活性剂胶束影响纳米颗粒的几何形状。可使用特定的表面活性剂和表面活性剂浓度以形成具有满足燃料电池性能要求所需的特定尺寸和形状的钯纳米颗粒。使钯纳米颗粒成尺寸和成形的适合的表面活性剂包括聚乙烯吡咯烷酮(PVP)、和氯基和溴基盐。表面活性剂在它们使得纳米颗粒成形时结合至钯纳米颗粒。在钯纳米颗粒用作催化剂之前，这些表面活性剂必须从钯纳米颗粒除去，以使所述纳米颗粒能和反应物完全接近。
如上文提示的，典型地，通过（有或没有低温处理）洗涤纳米颗粒或高温处理除去表面活性剂。这些表面活性剂的除去方法中的各种均有缺点。一些表面活性剂只有在特别长的洗涤时间后才能除去。用于洗涤纳米颗粒的长时间段增加了生产最终的纳米颗粒催化剂所需的时间和成本。高温处理典型地需要高于300°C的温度并可能对钯纳米颗粒有不利作用。如上文提示的，在300°C钯纳米颗粒可能失去它们的形状并尺寸增大。高温处理以从纳米颗粒除去表面活性剂可能消除用表面活性剂提供的尺寸和形状改性。
代替使用冗长的洗涤方法或有害的高温方法，本发明使用分子氢弱化纳米颗粒和用于使得所述纳米颗粒成形和/或成尺寸的表面活性剂之间的结合。图1示出从纳米颗粒除去表面活性剂的方法的简化图。方法10包括将纳米颗粒暴露于氢气(步骤12)并从纳米颗粒除去表面活性剂(步骤14)。氢气穿透进钯颗粒并扩大钯-钯点阵间距。钯-钯点阵间距的这种扩大弱化表面活性剂的吸附并促进从纳米颗粒除去表面活性剂。如下文讨论的，氢气暴露步骤12可通过电化学或化学方法进行。
图2示出从纳米颗粒除去表面活性剂的电化学方法16的简化图。在步骤18中，施加电势至纳米颗粒。适合的电势在或低于氢气吸附/吸收和氢气释放发生的电势。在示例性实施方式中，相对可逆的氢电极电势测量在约-0.2V和约0.35V之间。在甚至更示例性的实施方式中，相对可逆的氢电极电势测量在约-0.2V和约0.1V之间。在一个具体实施方式中，相对可逆的氢电极电势测量在约-0.05V。
在步骤20中，保持电势足以使得氢穿透进纳米颗粒的一段时间。所述纳米颗粒作为电极，并且氢气作为多步反应的结果而形成。首先，吸附的氢原子形成在纳米颗粒的表面上
H3O++e-→H· ads+H2O(1)
其中H· ads是在纳米颗粒表面吸附的原子。吸附的氢原子组合形成分子氢
H· ads+H· ads→H2(2)
或进一步的电化学反应生成分子氢
H· ads+H3O++e-→H2+H2O(3)
取决于电势。所形成的氢气穿透进入钯纳米颗粒，形成一氢化二钯并扩大钯纳米颗粒点阵。一氢化二钯是在其晶格中含有大量氢的金属钯。在室温下和大气压力下，钯能吸收高达900倍其自身体积的氢气。表面活性剂的吸附变弱，并且由于点阵扩大所述表面活性剂能从钯表面轻易脱附。在一些情况下，分子氢是不必要的。在反应(1)中形成的原子氢也能被钯吸收和引起点阵扩大。
在示例性实施方式中，保持电势少于约5分钟。在一个具体实施方式中，保持电势不多于约1分钟。典型地，步骤18和20在室温下进行（约15°C和约30°C之间）。在步骤18和20中使用电解质。适合的电解质包括稀释的水性酸，例如0.1M高氯酸(HClO4)。
图3示出除去在钯纳米颗粒上的表面活性剂的化学方法22的简化图。代替在钯纳米颗粒表面形成氢，不涉及电化学反应的情况下，分子氢被递送到钯纳米颗粒。在步骤24中，将成尺寸的和成形的含表面活性剂的钯纳米颗粒放入容器中。在步骤26中，将氢气加入容器中使得钯纳米颗粒吸收分子氢，导致钯纳米颗粒的点阵扩大。吸收的氢气弱化钯纳米颗粒和表面活性剂之间的结合，使得表面活性剂易于除去。
一旦钯纳米颗粒已吸收足量的氢气，表面活性剂和钯纳米颗粒之间的结合将足够弱化使得表面活性剂只从纳米颗粒脱附（即表面活性剂从纳米颗粒“掉落”）。在钯纳米颗粒表面或钯晶格中存在的氢气也不需要进一步的处理。任何存在的氢气将在用作燃料电池催化剂之前或期间离开。
图4示出从纳米颗粒除去表面活性剂的具有后处理步骤的方法的简化图。方法28包含方法10的步骤（将钯纳米颗粒暴露于氢气并从纳米颗粒除去表面活性剂）以及洗涤步骤30和过滤步骤32。用水洗涤所述钯纳米颗粒。洗涤步骤30提供杂质以及在步骤18和20中期间使用的任何溶剂的去除。根据上述方法处理的钯纳米颗粒也可在步骤32中过滤以进一步纯化纳米颗粒。
图5示出制备钯纳米颗粒的方法的简化图。方法34包括将钯纳米颗粒与表面活性剂(步骤36)组合。在步骤36中，所述表面活性剂改变纳米颗粒的几何性质（例如，尺寸、形状等）。作为步骤36的几何改性的结果，所述表面活性剂与所述纳米颗粒结合。一旦纳米颗粒的几何性质被改变，纳米颗粒暴露于步骤38的氢气中以从纳米颗粒除去表面活性剂。步骤38根据上述方法16或方法22进行。步骤38之后，表面活性剂不再结合至纳米颗粒，可以使用该纳米颗粒。
总之，用氢气弱化钯纳米颗粒和用于使得纳米颗粒成形和成尺寸的表面活性剂之间的结合。可使用电化学方法在钯纳米颗粒表面上形成氢气，使其被纳米颗粒吸收。也可将氢气加至纳米颗粒的环境使其被纳米颗粒吸收。将钯纳米颗粒暴露于氢气扩大了纳米颗粒的点阵结构并弱化了表面活性剂和纳米颗粒之间的结合，使得所述表面活性剂易于被去除。本文中描述的方法使得简单、快速和有效的表面活性剂去除，而不使用不利的高温或不需要长处理时间。
虽然提及优选的实施方式来描述本发明，本领域技术人员将认识到可以在形式和细节上进行改变而不背离本发明的精神和范围。

Claims (20)

1.从钯纳米颗粒除去表面活性剂的方法，所述方法包括：
暴露所述钯纳米颗粒于氢气，和
从所述钯纳米颗粒除去所述表面活性剂。
2.权利要求1所述的方法，其中所述钯纳米颗粒包含选自钯、钯合金及其组合的化学物质。
3.权利要求1所述的方法，其中暴露所述钯纳米颗粒于氢气包括：
施加电势至所述钯纳米颗粒，其中施加至所述钯纳米颗粒的所述电势不高于氢气吸附/吸收所需的电势且不高于氢气释放所需的电势；和
保持所述电势足以让氢气穿透入钯纳米颗粒的时间。
4.权利要求3所述的方法，其中施加至所述钯纳米颗粒的所述电势测量从约-0.2V至约0.1V。
5.权利要求4所述的方法，其中施加至所述钯纳米颗粒的所述电势测量为约-0.05V。
6.权利要求3所述的方法，其中将所述电势施加至所述钯纳米颗粒少于约5分钟。
7.权利要求6所述的方法，其中将所述电势施加至所述钯纳米颗粒不多于约1分钟。
8.权利要求3所述的方法，其中当所述钯纳米颗粒在约15°C和约30°C之间的温度时，将所述电势施加至所述钯纳米颗粒。
9.权利要求3所述的方法，其中在稀酸存在下将所述电势施加至所述钯纳米颗粒。
10.权利要求3所述的方法，其进一步包括：
施加所述电势至所述钯纳米颗粒之后，用水洗涤所述钯纳米颗粒。
11.权利要求3所述的方法，其进一步包括：
施加所述电势至所述钯纳米颗粒之后，过滤所述钯纳米颗粒。
12.权利要求2所述的方法，其中暴露所述钯纳米颗粒于氢气包括：
将所述钯纳米颗粒放入容器中；和
将氢气加至所述容器中使得所述钯纳米颗粒吸收氢气。
13.用于形成和处理钯纳米颗粒的方法，其包括：
使用表面活性剂合成钯纳米颗粒，其中所述表面活性剂影响所述钯纳米颗粒的几何性质并结合至所述钯纳米颗粒；和
暴露所述钯纳米颗粒于氢气以从所述钯纳米颗粒除去所述表面活性剂。
14.权利要求13所述的方法，其中所述钯纳米颗粒包含选自钯、钯合金及其组合的化学物质。
15.权利要求13所述的方法，其中暴露所述钯纳米颗粒于氢气包括：
施加电势至所述钯纳米颗粒，其中施加至所述钯纳米颗粒的所述电势不高于氢气吸附/吸收所需的电势且不高于氢气释放所需的电势；和
保持所述电势足以让氢气穿透入钯纳米颗粒以弱化所述表面活性剂和所述钯纳米颗粒之间的结合的时间。
16.权利要求15所述的方法，其中施加至所述钯纳米颗粒的所述电势测量从约-0.2V至约0.1V。
17.权利要求16所述的方法，其中施加至所述钯纳米颗粒的所述电势测量为约-0.05V。
18.权利要求15所述的方法，其中将所述电势施加至所述钯纳米颗粒少于约5分钟。
19.权利要求18所述的方法，其中将所述电势施加至所述钯纳米颗粒不多于约1分钟。
20.权利要求14所述的方法，其中暴露所述表面活性剂和所述钯纳米颗粒之间的结合于分子氢包括：
将所述钯纳米颗粒放入容器中；和
将氢气加至所述容器中使得所述钯纳米颗粒吸收氢气。
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