CN102811809A - 纳米活性材料的具有抑制的迁移性的催化剂的形成方法 - Google Patents

纳米活性材料的具有抑制的迁移性的催化剂的形成方法 Download PDF

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CN102811809A
CN102811809A CN2010800638277A CN201080063827A CN102811809A CN 102811809 A CN102811809 A CN 102811809A CN 2010800638277 A CN2010800638277 A CN 2010800638277A CN 201080063827 A CN201080063827 A CN 201080063827A CN 102811809 A CN102811809 A CN 102811809A
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particle
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Q·尹
X·齐
M·A·比博格
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SDC Materials Inc
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Abstract

形成催化剂的方法，包括：提供多个载体颗粒和多个移动-抑制颗粒，其中多个载体颗粒中的每个载体颗粒附着在其自己的催化颗粒上；以及将多个移动-抑制颗粒附着到多个载体颗粒上，其中通过至少一个移动-抑制颗粒将每个载体颗粒与多个载体颗粒中每个其它颗粒分隔开，其中设置移动-抑制颗粒以阻止催化颗粒从一个载体颗粒转移到另一个载体颗粒上。

Description

纳米活性材料的具有抑制的迁移性的催化剂的形成方法
相关申请的交互参考
本申请要求序列号为61/284,329、提交日为2009年12月15日、名称为“材料加工”的美国临时专利申请的优先权，由此将其全文引入作为参考，如同在文中阐明那样。
发明领域
本发明涉及催化剂领域。具体而言，本发明涉及催化剂的形成方法，其中活性催化颗粒的迁移性被抑制。
发明背景
催化剂用于促进和加速发应。在某些应用中，希望采用小尺寸的催化剂材料，如纳米级的催化颗粒。此外，也常常希望采用担载结构体来提供催化颗粒可在其上留驻的子结构。
附图1A中，催化剂100包括多个载体颗粒110a-d，每个具有至少一个相应的催化颗粒120a-d。尽管附图1A-C仅显示四个载体颗粒110，可以认为催化剂100可含有任何数量的载体颗粒110。催化颗粒120a-d可化学吸附或附着在载体颗粒110a-d的表面。然而，催化颗粒120a-d不会一成不变地固定在其附着的载体颗粒110a-d上。相反，其可从一个载体颗粒110移动到另一个上。例如，附图1A-B显示了催化颗粒120b和120c从其各自的载体颗粒110b和110c分别移动到相邻的载体颗粒110a和110d，这样催化颗粒120a和120b负载在载体颗粒110a上、催化颗粒120c和120d负载在载体颗粒110d上。在高温应用中，这些催化颗粒的移动更为明显。如附图1C所示，当催化颗粒120b和120c移动到临近的载体颗粒110a和110d时，它们开始和那些临近载体颗粒上的其他催化颗粒120a和120d结合，得到更大的催化颗粒120ab和120cd。
可以理解催化剂的效果和活性直接与载体颗粒表面的催化颗粒的尺寸成比例。当催化颗粒结合成更大的团块时，催化颗粒颗粒度增大，催化颗粒的表面积减小，催化剂的效力受到负面影响。
发明内容
本发明抑制了催化颗粒的移动、减少它们的结合，因此可以减少它们各自的大小并提高它们的总表面积。为了阻止催化颗粒从一个载体颗粒移动到另一个上，本发明通过在载体颗粒之间提供一个或多个移动-抑制颗粒来达到这样的结果。
本发明的一个方面在于，提供了催化剂的形成方法。该方法包括提供多个载体颗粒和多个移动-抑制颗粒。多个载体颗粒中的每个载体颗粒附着在其自己的催化颗粒上。然后将多个移动-抑制颗粒附着在载体颗粒上。通过至少一个移动-抑制颗粒，将每个载体颗粒与多个载体颗粒的每个其它的载体颗粒分离开。设置移动-抑制颗粒以阻止催化颗粒从一个载体颗粒移动到另一个载体颗粒上。
本发明的另一方面是在于，提供了催化剂的形成方法。该方法包括提供多个载体颗粒和多个移动-抑制颗粒。多个载体颗粒中的每个载体颗粒附着在其自己的催化颗粒上。多个载体颗粒分散在分散液体中，从而形成载体颗粒的分散体。多个移动-抑制颗粒分散在分散液体中，从而形成移动-抑制颗粒的分散体。将载体颗粒的分散体与移动-抑制颗粒的分散体相混合，从而形成湿混合物。将湿混合物冷冻干燥后形成干燥混合物。然后煅烧干燥混合物，形成多个载体颗粒和多个移动-抑制颗粒的簇。经由至少一个移动-抑制颗粒将每个载体颗粒与多个载体颗粒中的每个其它载体颗粒分离开。设置移动-抑制颗粒以阻止催化颗粒从一个载体颗粒移动到另一个载体颗粒上。
本发明的另一个方面在于，提供了一种催化剂。催化剂包括多个载体颗粒。多个载体颗粒中的每个载体颗粒附着在其自己的催化颗粒上。催化剂还包括多个附着在多个载体颗粒上的移动-抑制颗粒。经由至少一个移动-抑制颗粒，每个载体颗粒与多个载体颗粒中的每个其它载体颗粒相分离。设置移动-抑制颗粒以阻止催化颗粒从一个载体颗粒移动到另一个载体颗粒上。
附图说明
附图1A-C表示容易移动的催化剂和催化颗粒的结合的一个实施方式。
附图2表示根据本发明的原理的形成催化剂的方法的一个实施方式的流程图。
附图3表示根据本发明的原理的颗粒生产系统的一个实施方式。
附图4表示根据本发明的原理的颗粒生产系统的另一个实施方式。
附图5A表示根据本发明的原理的连接有相应催化颗粒的多个载体颗粒的一个实施方式。
附图5B表示根据本发明的原理的多个移动-抑制颗粒的一个实施方式。
附图6A表示根据本发明的原理的带有相关催化颗粒的载体颗粒分散体的一个实施方式。
附图6B表示根据本发明的原理的移动-抑制颗粒的分散体的一个实施方式。
附图7表示根据本发明的原理的附图6A的载体/催化颗粒的分散体和附图6B的移动-抑制颗粒的分散体的混合物的一个实施方式。
附图8表示根据本发明的原理的附着在载体/催化颗粒之间的移动-抑制颗粒的簇的一个实施方式。
实施方式
下述内容可使所属领域技术人员生产和使用本发明以及提供专利申请的内容和必要条件。所述实施方式的多种变形方式对于所属领域技术人员是显然的，并且所述的一般原则可应用到其他实施方式。这样，本发明不仅限于所示的实施方式，而是在于同在此所述的原理和特征相一致的最大范围。
本公开内容涉及颗粒和粉末。这两种术语是等同的，除了强调单一的“粉末”是指颗粒的集合。本发明可应用于多种粉末和颗粒。落入本发明范围的粉末可包括、但不限于下述的任一种：(a)纳米结构粉末(纳米粉末)，其具有小于250纳米的平均颗粒尺寸和1至1百万的长径比；(b)亚微米颗粒，其具有小于1微米的平均颗粒尺寸和1至1百万的长径比；(c)超细粉末，其具有小于100微米的平均颗粒尺寸和1至1百万的长径比；以及(d)细粉末，其具有小于500微米的平均颗粒尺寸和1至1百万的长径比。
附图2是流程图，其表示根据本发明的原理的形成催化剂的方法200的一个实施方式。
在步骤210，提供多个载体颗粒和移动-抑制颗粒。优选地，每个载体颗粒附着在其自己各自的催化颗粒上(也就是，载体颗粒与催化颗粒以1：1比例)。然而，可以认为一些载体颗粒上没有任何催化颗粒。本文所用术语“载体/催化颗粒”是指载体颗粒和与之结合的催化颗粒。设置移动-抑制颗粒以阻止催化颗粒从一个载体颗粒移动到另一个载体颗粒上。在优选的实施方式中，移动-抑制颗粒包括一种或多种催化颗粒不会经过或停留其上的材料，从而降低了催化颗粒的移动性。
在优选的实施方式中，载体颗粒具有非催化组成，其与催化颗粒相反。在这种情况下，理想的载体颗粒具有不同于催化颗粒的化学组成。类似地，优选移动-抑制颗粒具有非催化化学组成，其不同于载体颗粒和微化颗粒。然而，可以认为颗粒化学组成可在实施方式和实施方式之间进行变化。在一个示范的实施方式中，载体颗粒包括或由氧化铝和包含或含有铂族金属的催化颗粒组成，其中铂族金属可为铂、钌、铑、钯、锇、或铱。在一些实施方式中，移动-抑制颗粒包含或由金属氧化物(优选过渡金属氧化物)组成，其包括但不限于氧化铈、氧化镧和氧化钛。在其他的实施方式中，移动-抑制颗粒包括或由玻璃或陶瓷组成，包括但不限于氮化硼、碳化钛和二硼化钛。优选地，移动-抑制颗粒不包含任何贵金属。
在优选的实施方式中，载体颗粒、催化颗粒、和移动-抑制颗粒是纳米颗粒。优选地，载体颗粒和移动-抑制颗粒具有500纳米的最大直径和1~5纳米的最小直径，而催化颗粒具有0.5~5纳米范围的直径。在一些实施方式中，载体颗粒和移动-抑制颗粒的直径在10~15纳米范围内，催化颗粒直径在2~5纳米范围内。然而，可以认为能使用其它的微直径。
可以认为能通过多种方法实现颗粒的纳米尺寸结构。在优选的实施方式中，在等离子枪的最热区使载体颗粒和催化颗粒气化。然后将气化的颗粒进行快速骤冷以使其得以冷凝。这种气化和冷凝的结果即是形成具有附着在其上的纳米尺寸催化颗粒的纳米尺寸的载体颗粒。
申请系列号为No.12/151,935、提交日为2008年5月8日、名称为“高湍流骤冷室”的美国专利公开了使用等离子反应器的颗粒生产系统来生产纳米级颗粒的实例，在此全文引入其内容。一种此类的颗粒生产系统300示于附图3中。系统300包括一个前体供应装置310和工作气体供应装置320，两个装置都流体连通到等离子生产室330，该室具有在其中形成的能量传递区335。等离子生产室330与压缩骤冷室345的注射口340流体连通，从而允许能量传递区335与骤冷室345流体连通。一个或多个口390也允许与装有控制环境系统370(由虚线标注)的骤冷室345流体连通。骤冷室345也与注射口365流体连通。
通常，等离子生产室330作为反应器运行，产生包含在气流中的颗粒的产物。颗粒生产包括结合、反应和调节的步骤。工作气体由气体源供应到等离子反应器。在等离子反应器内，能量由工作气体传送，从而产生等离子。可使用多种不同的方法传送能量，包括但不限于DC耦合器、电容耦合器、电感耦合器和谐振耦合器。一个或更多材料分配装置优选以粉末形式将至少一种材料引入等离子反应器。由材料分配装置引入等离子反应器的等离子和一种或多种材料结合生成具有高反应活性和能量的混合物，在此可将粉末气化。被气化的粉末的混合物在工作气体的流动方向上流过等离子反应器。在移动过程中，混合物冷却并形成颗粒。仍富含能量的输出混合物，其包含热气体和富含能量的颗粒，从等离子反应器注射出来。
在典型的实施方式中，等离子生产室330将由前体供应装置310供应的前体材料(优选以粉末的形式)和由位于能量传送区335内的工作气体供应装置320提供的工作气体相结合，在此工作气体被能量化以形成等离子。等离子被施加到位于能量传送区335内的前体材料以形成富含能量的、有反应活性的混合物。混合物包含以多种相态的至少一个存在的一种或多种材料，相态可包括蒸气态、气体和等离子。
通过注射口340将反应活性混合物从能量传送区335传送至压缩骤冷室345。随着热混合物从能量传送区335移动，其在骤冷室345内快速膨胀并冷却。当混合物流入骤冷室345时，口390沿着骤冷室345的内表面供应调节流体。至少在某种程度上，调节流体与混合物结合，并从骤冷室345流过排出口365。
在进入骤冷室345之后立刻形成颗粒。此外，沿着骤冷室345的内表面供应的调节流体调节反应性混合物以保持对颗粒的夹带，并且阻止骤冷室345内表面上材料的沉积。
仍然见附图3，骤冷室345的结构可由相对薄壁的组件构成，该组件能够大量散热。例如，薄壁组件可引导室内的热量和将热辐射到周围。骤冷室345包含基本为圆柱形的表面350，类锥状(截头圆锥体)表面355，连接注射口340和圆柱表面350的环形表面360。圆柱表面350，其具有相对于注射口340的尺寸更大的直径，为流入骤冷室345后产生的反应性混合物的膨胀提供场地。类锥表面355从远离注射口340的圆柱表面350向排出口365延伸。类锥表面355足够光滑变化从而不会过度地压缩流经骤冷室345至排出口365的流体。
从经过入口流入骤冷室345的混合物排出大量的热，大多是以辐射的形式。优选骤冷室345设计为可有效散发该热。例如，优选将骤冷室345的表面暴露于冷却装置(未显示)。
仍然见附图3，优选控制环境系统370包含室385，可将调节流体从储槽375通过导管380引入其中。优选调节流体含有氩气。然而，其它惰性气体但相对重的气体也同样优选。并且，将调节流体引入骤冷室345的优选机制是在骤冷室345和出口365之间形成压力差。这样的压力差可将调节流体通过口390引入骤冷室345。其它提供调节流体的次优选方法包括但不限于在室385内形成正压。
骤冷室345的截头圆锥形状可在骤冷区内提供适量的湍流，以促进调节流体和反应性混合物的混合，从而增加骤冷率超越现有系统。然而，在一些情形下，可预期骤冷率的甚至更大的增加。所述骤冷率的增加可通过在骤冷室区域内制造调节流体和反应性混合物相混合的较高的湍流来实现。
附图4表示具有高湍流骤冷室445的颗粒生产系统400。系统400包括前体供应装置410，其直接连接到等离子产生和反应室430的工作气体供应装置420，与如上所述的附图3的等离子生产室330近似。能量传送系统425也连接到等离子产生和反应室430上。等离子产生和反应室430包括注射口440，其流体连通压缩骤冷室445。一个或多个口490也可允许在骤冷室445和控制环境系统470之间流体连通，与附图3的控制环境系统近似。骤冷室445也流体连通出口465。
通常，室430作为反应器运转，与附图3的室330近似，产生含有包含夹带在气流内的颗粒的产物。生产过程包括下述的结合、反应和调节步骤。系统在室430的能量传递区将供应自前体供应装置410的前体材料和供应自工作气体供应装置420的工作气体结合。系统通过产自能量供应系统490的能量将室430内的工作气体能量化，从而获得等离子。将等离子应用到室430内的前体材料以形成富含能量的、具有反应活性的混合物。混合物包含一种或多种以多种相态的至少一个存在的材料，相态可含有蒸气相、气相、和等离子。反应性混合物从等离子产生和反应室430通过注射口440流入骤冷室445。
优选骤冷室445包含基本为圆柱形的表面450，截头圆锥体表面455、和连接圆柱表面450和注射口440的环形表面460。截头圆锥形表面460变窄以配合出口465。等离子生产和反应室430包括末端的扩大部分，在此设置有注射口440。该扩大部分缩短了注射口440和出口465间的距离，减少了反应性混合物和调节流体混合区域的体积，该区域被称为骤冷区。在优选的实施方式中，注射口440与出口465同轴设置。注射口的中心与出口465的距离为第一距离d1。注射口的周边与截头锥形体表面455的部分的距离为第二距离d2。注射口440和截头锥体形表面455之间形成前述骤冷区。在注射口440周边和截头锥形体表面455之间的空间形成间隙，其作为将调节流体供应到骤冷区的通道。截头锥形体表面455作为漏斗状表面，通过该间隙引导流体并进入骤冷区。
当反应性混合物流入骤冷室445，口490将调节流体供应进入骤冷室445。然后调节流体沿截头锥形体表面455流动，通过注射口440和截头锥形体455之间的间隙、并进入骤冷区。在一些实施方式中，设置控制环境系统470以控制供应到骤冷区的调节流体的体积流速或质量流速。
随着反应性混合物移出注射口440，其发生膨胀并与调节流体相混合。优选地，在供应调节流体的角度产生了高度湍流并促进反应性混合物的混合。湍流可依赖于很多参数。在优选的实施方式中，可调节一个或多个这样的参数以控制湍流水平。这些因素包括调节流体的流速、截头锥形体表面455的温度、截头锥形体表面455的角度(可影响调节流体进入骤冷区的角度)、以及骤冷区的大小。例如，截头锥形体表面455和注射口440的相对位置可调，这可用于调节骤冷区的体积。可以多种不同的方式、使用多种不同的机理进行这些调节，包括但不限于自动方法或人工方法。
在进入骤冷室445后立刻形成颗粒。颗粒聚集的程度取决于冷却速率。冷却速率依赖于骤冷区内的流动湍流。优选地，对系统进行调节以形成高湍流，从而形成非常分散的颗粒。例如，在优选的实施方式中，骤冷区内的湍流具有至少1000的雷诺数。
仍然见附图4，优选骤冷室445的结构由相对薄壁的组件构成，该组件能够大量散热。例如，薄壁组件可引导室内的热量和将热辐射到周围。
从经由入口流入骤冷室445的反应性混合物释放大量的热，大多是以辐射的形式。骤冷室445设计为可有效散发该热。优选将骤冷室245的表面暴露于冷却装置(未显示)。在优选的实施方式中，设置冷却系统以控制截头锥形体表面455的温度。
注射进入骤冷区，冷却，形成颗粒之后，混合物从骤冷室445经由出口465流动。由发生器495产生的抽吸使混合物和调节流体从骤冷区进入导管492。混合物经由导管492从出口465流向抽吸发生器495。优选地，在到达抽吸发生器495之前，颗粒由收集或采样系统(未显示)从混合物中分离。
仍然见附图4，控制环境系统470包括室485，通过一个或多个口490与骤冷区流体连通，调节流体从例如附图3中的储槽375的储槽引出后通过导管480进入该室。如上所述，优选调节流体包含氩气。然而，其它惰性但相对重的气体也同样优选。并且，将调节流体引入骤冷室445的优选机制是在骤冷室445和出口465之间形成压力差。这样的压力差可将调节流体通过口490引入骤冷室445。其它提供调节流体的方法包括但不限于在室485内形成正压。
截头锥形体表面的角度影响调节流体供应到骤冷区的角度，这可影响骤冷区内的湍流水平。优选调节流体沿多个动量矢量流入骤冷区。动量矢量之间的角度越大，产生的湍流水平越高。在优选的实施方式中，高湍流骤冷室包含截头锥形体表面，其设置使进入骤冷区的至少两个调节流体动量矢量形成漏斗状，在两个动量矢量之间的角度至少为90度。可以认为其它的角度极限可如上使用。例如，也可注意至少一个调节流体动量矢量和反应性混合物的动量矢量之间形成的角度。在高湍流骤冷室的一个实施方式中，设置反应性混合物入口以将反应性混合物沿着第一动量矢量供入骤冷区，设置截头锥形体表面以将调节流体沿着第二动量矢量供入骤冷区，第二动量矢量具有相对于第一动量矢量大20度的倾斜角度。
骤冷区的大小也会影响骤冷区的湍流水平。骤冷区越小，产生的湍流水平越高。可以通过缩小注射口440中心和出口465的距离来减小骤冷区的大小。
根据本发明的实施方式产生的高湍流降低了形成的颗粒之间可聚集的时间，从而产生更加均一尺寸的颗粒，在一些情形下，产生小尺寸的颗粒。这些因素共同导致产生增加了分散性和增加了表面积与体积比率的颗粒。
回顾附图2的方法200，可使用颗粒生产系统200或300(或相应的变形)以提供一种或多种纳米级形态的载体颗粒、催化颗粒和移动-抑制颗粒。例如，这些颗粒可作为微米级的前体材料引入颗粒生产系统，在此这些颗粒被气化然后冷凝形成纳米尺寸级颗粒。在优选的实施方式中，形成载体/催化颗粒并独立于移动-抑制颗粒提供，这样可避免移动-抑制颗粒和载体/催化颗粒之间提前的相互作用(如：附着)。这样的分离可通过多种方式来实现，包括但不限于、对于两类颗粒使用不同的颗粒生产系统，或者对于两种颗粒在不同时间使用同一颗粒生产系统。
附图5A表示由方法200的步骤210提供的多个载体颗粒510的一个实施方式。每个载体颗粒510(优选在其外表面)具有附着在其上的催化颗粒520。尽管在一些实施方式中，某些载体颗粒510上可能没有催化颗粒520。可以认为通过改变提供到颗粒生产系统的催化材料的量、或者调节提供到颗粒生产系统中的催化颗粒与载体颗粒的混合比率来影响载体颗粒510上的催化颗粒520的尺寸。提供到颗粒生产系统的催化颗粒的浓度越大，附着在载体颗粒510上的催化颗粒520的尺寸越大。
附图5B表示由方法200的步骤210提供的多个移动-抑制颗粒530的一个实施方式。提供在移动-抑制颗粒530上的条纹的作用仅是为了帮助将移动-抑制颗粒530与载体颗粒510区分开来。
在方法200的步骤220，载体/催化颗粒和移动-抑制颗粒分散在液体中。附图6A表示载体/催化颗粒的分散体625的一个实施方式。分散体625的放大图表示被液体625a分隔开的载体/催化颗粒、其由具有附着在其上的具有催化颗粒620的载体颗粒610组成。附图6B表示移动-抑制颗粒630的分散体635的一个实施方式。分散体635的放大图表示被液体615b分隔开的分散体630。尽管附图6A-B表示了在分离分散体625和635中的载体/催化颗粒和移动-抑制颗粒，可以认为可在同一时间在同一容器内将其分散形成同一分散体。
分散液体615a和615b可以是用来分别分散载体/催化颗粒和移动-抑制颗粒的任何液体。在一个优选的实施方式中，分散液体包含或由水或任何有机液体比如二醇醚组成。在一些实施方式中，分散体625和635使用同一类型的分散液体。在其他的实施方式中，分散体625和635使用不同类型的分散液体(如分散液体615a是水、分散液体615b是乙二醇)。
在一些实施方式中，可将一种或多种表面活性剂或其他分散助剂，如阳离子、阴离子、两性离子、和/或非离子碳基低聚物和/或聚合物加入分散液体。为了调节酸度和使其稳定，可在分散体中加入某些表面活性剂。为了酸化N-氧化物颗粒的表面，可将酸加入分散体。应仔细选择表面活性剂使其不会破坏催化材料。在优选的实施方式中，不在分散体中加入硫酸盐和磷酸盐。能加入分散液体的表面活性剂的实例是羧酸、多胺、聚醚。可以认为也可使用其它的表面活性剂或分散助剂。
可以认为能使用颗粒、分散液体和表面活性剂浓缩物的不同变形。在优选的实施方式中，分散体包括5~25重量%浓度的粉末，也就是载体/催化颗粒和移动-抑制颗粒各自构成它们相应分散体的约5~25重量%。在优选的实施方式中，分散体包括1~10重量%浓度的表面活性剂或其它分散助剂。优选地，表面活性剂或其它分散助剂占分散体的约5%或更少。
在方法200的步骤230，将分散的载体/催化颗粒和移动-抑制颗粒混合得到混合物。如果载体/催化颗粒和移动-抑制颗粒不是最初在一起分散，或者不是随后放入同一个容器以形成单一分散体，那么，可以此时将其放入它们混合在一起的同一容器中。在优选的实施方式中，通过超声、机械混合、和/或剪切混合完成混合。然而，可以认为为了实现混合可以使用多种其它的搅拌方法。
附图7表示在一个容器中分散体的混合物745的一个实施方式。混合物745含有多个载体颗粒710，每个颗粒具有附着在其上的催化颗粒720和移动-抑制颗粒730。颗粒用液体715分离，该液体可含有在前述步骤中使用的任何分散液体和表面活性剂(或其他分散助剂)。
在步骤240，从混合物中除去分散液体以形成干燥混合物。可以认为可以多种方式除去液体。在一个实施方式中，颗粒的分散体是冷冻干燥。将混合物倾倒入适宜冷冻-干燥的容器中。然后用液氮或其它足够冷以冷冻颗粒分散体的介质进行冷冻。在一个实施方式中，液氮、或其它冷冻介质约是-60摄氏度。但是，可以认为也可在其他温度下使用液氮、或其他冷冻介质。然后将混合物放入真空系统，在此颗粒的分散体保持冷冻，如水，或其他分散液体，在真空压力下除去。在一个实施方式中，使用约10微米的真空压力。在其他实施方式中，可以使用约2微米到约5微米之间的真空压力。
真空压力除去混合物中水和具有比水高的蒸气压力的其它液体。然而，在一些实施方式中，表面活性剂留在颗粒的冷冻分散体中。除去水会导致载体/催化颗粒和移动-抑制颗粒的多孔粉末结构，表面活性剂位于孔内。所得粉末处于中间状态，其相互间松散附着，然后摸上去是干燥的，提供机械处理能力。
在步骤250，煅烧干燥后的混合物，从而烘烤表面活性剂、以及形成附着在载体/催化颗粒之间的移动-抑制颗粒的簇。在一些实施方式中，将粉末放置在坩锅中。可以认为坩锅可由陶瓷或多种其它材料制备。然后将坩锅放在煅烧炉中，在设定时间内加热到设定温度。在一些实施方式中，在煅烧炉中在约550摄氏度加热坩锅约2个小时。然而，可以认为也能使用其它温度和加热时间。在一些实施方式中，将坩锅放入已经预热到所需烘烤温度的炉子中。通过在放入坩锅之前预热炉子可以显示测试结果，而不是坩锅在炉子中时将温度逐渐升至所需温度，这样金属颗粒的分散可实现最大化。然而，可以认为，在一些实施方式中，当坩锅在炉子内时逐渐升高炉温。在一些实施方式中，当坩锅治置于炉内时使用1~50摄氏度的升温速率来升高温度。在优选的实施方式中，炉子可以提供周围空气环境，其中坩锅及由此粉末得以加热。可以认为炉内的环境无须包含空气。然而优选含有一定量的氧气。
干燥后的混合物的煅烧可使其从颗粒之间的范德华力或近距离引力变为颗粒间的实际的共价键，这可获得载体/催化颗粒和移动-抑制颗粒的不含表面活性剂的聚集。附图8表示载体颗粒810之间附着的移动-抑制颗粒830的簇的一个实施方式，上述载体颗粒810具有附着其上的催化颗粒820。在一些实施方式中，本发明可得到0.5~50微米范围内的簇。在一些实施方式中，本发明可得到5~10微米范围内的簇。然而，可以认为也能得到其它尺寸的簇。
在一些实施方式中，可调节粉末(载体，催化剂和移动-抑制)的负载百分比以达到所需产物簇的各种类型粉末的粉末浓度。在一些实施方式中，使用0.01~15%负载量的催化剂粉末。然而，可以认为也可使用其它的负载量。
在优选的实施方式中，得到的产品簇中的载体颗粒、催化剂颗粒、和移动-抑制颗粒是纳米颗粒。优选地，载体颗粒和移动-抑制颗粒具有最大500纳米的直径和最小1~5纳米范围的直径，而催化颗粒具有0.5~5纳米范围的直径。在一些实施方式中，载体颗粒和移动-抑制颗粒的直径在5~20纳米范围内。在一些实施方式中，载体颗粒和移动-抑制颗粒的直径在10~15纳米范围内、催化剂颗粒直径在2~5纳米范围内。然而，可以认为能使用其它的颗粒度。
移动-抑制颗粒的引入和附着到载体/催化颗粒上和载体/催化颗粒之间阻止了催化颗粒从一个载体颗粒转移动至另外一个，从而阻止催化颗粒的结合。结果是，单个催化颗粒的尺寸可以尽量小以及簇的总催化表面积的尽量大。
本发明通过引入细节的具体实施方式来描述以促进对本发明的结构和实施的原理的理解。这些对具体实施方式和细节的参考不对要求保护的权利要求的范围构成限制。对实施方式做出其它多种变形方式而不脱离于权利要求所定义的发明的精神和范围对于所属领域技术人员是十分明显的。

Claims (42)

1.催化剂的形成方法，包括：
提供多个载体颗粒和多个移动-抑制颗粒，其中多个载体颗粒中的每个载体颗粒附着在其自己的催化颗粒上；以及
将多个移动-抑制颗粒附着到多个载体颗粒上，
其中通过至少一个移动-抑制颗粒，每个载体颗粒从多个载体颗粒中的每个其它的载体颗粒分离开，以及
其中设置移动-抑制颗粒以阻止催化颗粒从一个载体颗粒移动至另一个载体颗粒上。
2.根据权利要求1的方法，其中提供多个载体颗粒包括：
对具有等于或大于1微米的平均颗粒尺寸的前体载体粉末进行纳米尺寸化；
对具有等于或大于1微米的平均颗粒尺寸的前体催化粉末进行纳米尺寸化；以及
将纳米尺寸催化粉末附着到纳米尺寸载体粉末上，从而形成多个载体颗粒，其中多个载体颗粒中的每个载体颗粒附着在其自己的催化颗粒上。
3.根据权利要求2的方法，其中：
对前体载体粉末和前体催化粉末进行纳米尺寸化包括将等离子流施加到前体载体粉末和前体催化粉末上，从而使前体载体粉末和前体催化粉末气化；以及
使纳米尺寸催化微末附着到纳米尺寸载体粉末包括冷凝气化的载体粉末和气化的催化粉末，从而形成多个载体颗粒，其中多个载体颗粒中的每个载体颗粒附着在其自己的催化颗粒上。
4.根据权利要求1的方法，其中提供多个移动-抑制颗粒包括对具有等于或大于1微米的平均颗粒尺寸的前体移动-抑制粉末进行纳米尺寸化。
5.根据权利要求4的方法，其中对前体移动-抑制粉末进行纳米尺寸化包括：
将等离子流施加到前体移动-抑制粉末以将前体移动-抑制粉末气化；以及冷凝气化的移动-抑制粉末。
6.根据权利要求1的方法，其中提供多个载体颗粒和多个移动-抑制颗粒包括：
将多个载体颗粒分散在分散液体中，其中多个载体颗粒中的每个载体颗粒附着在其自己的催化颗粒上；
将多个移动-抑制颗粒分散在分散液体中；以及
将分散的载体颗粒和分散的移动-抑制颗粒混合，从而得到分散的载体颗粒和分散的移动-抑制颗粒的混合物。
7.根据权利要求6的方法，其中载体颗粒和移动-抑制颗粒的至少一种的分散液体包含水。
8.根据权利要求6的方法，其中载体颗粒和移动-抑制颗粒的至少一种的分散液体包含有机液体。
9.根据权利要求8的方法，其中有机溶液为二醇醚。
10.根据权利要求6的方法，其中多个载体颗粒的分散和多个移动-抑制颗粒的分散中的至少一种包括在分散液体中加入表面活性剂。
11.根据权利要求10的方法，其中表面活性剂选自羧酸、多胺、和聚醚。
12.根据权利要求6的方法，其中通过超声方法混合分散的载体颗粒和分散的移动-抑制颗粒。
13.根据权利要求6的方法，其中至少一个移动-抑制颗粒附着在多个载体颗粒的每个载体颗粒上以及在多个载体颗粒的每个载体颗粒之间的步骤包括冷冻干燥分散的载体颗粒和分散的移动-抑制颗粒的混合物的步骤，从而形成分散的载体颗粒和分散的移动-抑制颗粒的干燥后的混合物。
14.根据权利要求13的方法，其中至少一个移动-抑制颗粒附着在多个载体颗粒的每个载体颗粒上以及在多个载体颗粒的每个载体颗粒之间的步骤包括煅烧分散的载体颗粒和分散的移动-抑制颗粒的干燥混合物的步骤。
15.根据权利要求1的方法，其中多个载体颗粒包括多个氧化铝颗粒。
16.根据权利要求1的方法，其中催化颗粒包括铂。
17.根据权利要求1的方法，其中多个移动-抑制颗粒包括与多个载体颗粒不同的化学组成。
18.根据权利要求17的方法，其中多个移动-抑制颗粒包含多个陶瓷颗粒。
19.根据权利要求17的方法，其中多个移动-抑制颗粒包含多个金属氧化物颗粒。
20.根据权利要求1的方法，其中：
多个载体颗粒中的每个载体颗粒具有1纳米至500纳米之间的直径；
每个催化颗粒具有0.5纳米至5纳米之间的直径；以及
多个移动-抑制颗粒中的每个移动-抑制颗粒具有1纳米至500纳米之间的直径。
21.形成催化剂的方法，包括：
提供多个载体颗粒和多个移动-抑制颗粒，其中多个载体颗粒中的每个载体颗粒附着在其自己的催化颗粒上；
将多个载体颗粒分散在分散液体中，从而形成载体颗粒的分散体；
将多个移动-抑制颗粒分散在分散液体中，从而形成移动-抑制颗粒的分散体；
将载体颗粒的分散体和移动-抑制颗粒的分散体混合，从而形成湿混合物；
冷冻干燥该湿混合物，从而形成干燥的混合物；以及
煅烧该干燥的混合物，从而形成多个载体颗粒和多个移动-抑制颗粒的簇，其中通过至少一个移动-抑制颗粒将每个载体颗粒与多个载体颗粒的每个其它载体颗粒分离开，以及其中设置移动-抑制颗粒以阻止催化颗粒从一个载体颗粒移动到另一个载体颗粒上。
22.根据权利要求21的方法，其中提供多个载体颗粒和多个移动-抑制颗粒包括：
将等于或大于1微米的平均颗粒尺寸的前体载体粉末纳米化；
将等于或大于1微米的平均颗粒尺寸的前体催化粉末纳米化；
将纳米化催化粉末附着到纳米化载体粉末上，从而形成具有多个载体颗粒，其中多个载体颗粒中的每个载体颗粒附着在其自己的催化颗粒上；以及
将具有等于或大于1微米的平均颗粒尺寸的前体移动-抑制粉末纳米化。
23.根据权利要求22的方法，其中纳米化前体粉末的步骤包括：
将等离子流施加到前体粉末上，从而使前体粉末气化；以及
冷凝该气化的粉末。
24.根据权利要求21的方法，其中载体颗粒和移动-抑制颗粒的至少一种的分散液体包含水。
25.根据权利要求21的方法，其中载体颗粒和移动-抑制颗粒的至少一种的分散液体包含有机液体。
26.根据权利要求25的方法，其中有机液体是二醇醚。
27.根据权利要求21的方法，其中多个载体颗粒的分散和多个移动-抑制颗粒的分散中的至少一种包括在分散液体中加入表面活性剂。
28.根据权利要求27的方法，其中表面活性剂选自羧酸、多胺、和聚醚。
29.根据权利要求21的方法，其中载体颗粒分散体和移动-抑制颗粒分散体的混合步骤包括使用超声方法。
30.根据权利要求21的方法，其中多个载体颗粒包括多个氧化铝颗粒。
31.根据权利要求21的方法，其中催化颗粒包含铂。
32.根据权利要求21的方法，其中多个移动-抑制颗粒包含与多个载体颗粒不同的化学组成。
33.根据权利要求32的方法，其中多个移动-抑制颗粒包含多个陶瓷颗粒。
34.根据权利要求32的方法，其中多个移动-抑制颗粒包含多个金属氧化物颗粒。
35.根据权利要求21的方法，其中：
多个载体颗粒中的每个载体颗粒具有1纳米至500纳米之间的直径；
每个催化颗粒具有0.5纳米至5纳米之间的直径；以及
多个移动-抑制颗粒中的每个移动-抑制颗粒具有1纳米至500纳米之间的直径。
36.催化剂包含：
多个载体颗粒，其中多个载体颗粒中的每个载体颗粒附着在其自己的催化颗粒上；以及
多个移动-抑制颗粒附着在多个载体颗粒上，
其中通过至少一个移动-抑制颗粒将每个载体颗粒与多个载体颗粒中的每个其它载体颗粒相分离，以及
其中设置移动-抑制颗粒以阻止催化颗粒从一个载体颗粒移动到另一个载体颗粒上。
37.根据权利要求36的催化剂，其中多个载体颗粒包括多个氧化铝颗粒。
38.根据权利要求36的催化剂，其中催化颗粒包含铂。
39.根据权利要求36的催化剂，其中多个移动-抑制颗粒含有同多个载体颗粒不同的化学组成。
40.根据权利要求39的催化剂，其中多个移动-抑制颗粒包含多个陶瓷颗粒。
41.根据权利要求39的催化剂，其中多个移动-抑制颗粒包含多个金属氧化物颗粒。
42.根据权利要求36的催化剂，其中
多个载体颗粒中的每个载体颗粒具有1纳米至500纳米之间的直径；
每个催化颗粒具有0.5纳米至5纳米之间的直径；以及
多个移动-抑制颗粒中的每个移动-抑制颗粒具有1纳米至500纳米之间的直径。
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