CN104684846A - 碳化硅粉末及其制备方法 - Google Patents

碳化硅粉末及其制备方法 Download PDF

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CN104684846A
CN104684846A CN201380050878.XA CN201380050878A CN104684846A CN 104684846 A CN104684846 A CN 104684846A CN 201380050878 A CN201380050878 A CN 201380050878A CN 104684846 A CN104684846 A CN 104684846A
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silicon carbide
carbide powder
powder
phase
precursors
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CN104684846B (zh
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闵庚皙
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S-tech Co.,Ltd.
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LG Innotek Co Ltd
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Abstract

提供了一种制备碳化硅粉末的方法，该方法包括：将第一碳化硅粉末与液态碳化硅前体混合；在第一温度下对该混合物进行退火并且将碳化硅前体转化为β相碳化硅颗粒物质；以及在第二温度下对该物质进行退火并且利用β相碳化硅颗粒物质将第一碳化硅粉末晶粒生长为第二碳化硅粉末。

Description

碳化硅粉末及其制备方法
技术领域
本发明涉及碳化硅粉末及其制备方法，更具体地，涉及利用细碳化硅粉末来制备颗粒状碳化硅粉末的方法。
背景技术
碳化硅(SiC)具有高温度强度和优异的耐磨性、抗氧化性、抗腐蚀性和抗蠕变性。碳化硅存在具有立方晶体结构的β相和具有六方晶结构的α相。β相在1400℃至1800℃的温度下是稳定的，并且α相在2000℃以上形成。
碳化硅广泛用于工业结构，并且近来已应用于半导体行业。为了在单晶生长中使用碳化硅，需要具有均匀粒径分布的颗粒状碳化硅粉末。可以通过在预定条件下对细碳化硅粉末进行退火来获得颗粒状碳化硅粉末。
然而，当在低于2000℃的温度下对细碳化硅粉末进行退火时，可以获得具有均匀粒径分布的β相碳化硅粉末，但难以获得具有40μm或更大的粒径的颗粒状碳化硅粉末。
然而，当在2000℃以上对细碳化硅粉末进行退火时，可以获得具有100μm或更大的粒径的α相碳化硅粉末，但其因在其中混合有细碳化硅粉末而具有非均匀粒径分布。
发明内容
技术问题
本发明涉及提供具有均匀粒径分布的颗粒状碳化硅粉末及其制备方法。
问题的解决方案
本发明的一个方面提供了一种具有1至10的分散度(D90/D10)和40μm至150μm的粒径(D50)的碳化硅粉末。
碳化硅粉末可以含0.1ppm至10ppm的杂质。
碳化硅粉末可以是β相。
本发明的另一方面提供了一种制备碳化硅粉末的方法，该方法包括：将第一碳化硅粉末与液态碳化硅前体混合；通过在第一温度下对该混合物进行退火来将碳化硅前体转化为β相碳化硅颗粒物质；以及通过在第二温度下对β相碳化硅颗粒物质进行退火、利用β相碳化硅颗粒物质来将第一碳化硅粉末晶粒生长为第二碳化硅粉末。
第一碳化硅粉末的粒径(D50)可以为0.2μm至9μm。
碳化硅前体可以包括碳化硅陶瓷先驱体(preceramic)聚合物系列。
碳化硅前体可以包括选自硅氮烷和聚碳硅烷中的至少一种。
碳化硅前体可以以相对于第一碳化硅粉末和碳化硅前体的总重量的5wt％至20wt％被添加。
第一温度和第二温度可以为2000℃以下。
β相碳化硅颗粒物质可以比第一碳化硅粉末的粒径(D50)小。
根据在第二温度下的退火时间，可以控制第二碳化硅粉末的粒径。
混合操作可以包括用液态碳化硅前体来涂覆第一碳化硅粉末的表面。
发明的有益效果
根据本发明的示例性实施方案，可以获得可以在单晶生长中使用的、具有均匀粒径分布的颗粒状碳化硅粉末。
特别地，当在低于2000℃的温度下处理细碳化硅粉末时，由于粉末没有被相转移为α相，所以可以获得具有均匀粒径分布和40μm或更大的粒径的碳化硅粉末。
附图说明
图1是示出了制备根据本发明的示例性实施方案的碳化硅粉末的方法的流程图。
图2至图6是示出了制备根据本发明的示例性实施方案的碳化硅粉末的方法的图。
具体实施方式
本发明将以各种形式被修改并且具有数个示例性实施方案，但是仅参照附图描述特定实施方案。然而，可以理解，本发明不限于以下公开的特定实施方案，而是包括本发明的范围和技术范围内的所有修改方案、等效方案或替代方案。
虽然可以使用表述“第一、第二”等来描述各种元件，但是这些元件不限于这些表述。这些表述仅用于将一个元件与另一元件进行区分。例如，在不脱离示例性实施方案的范围的情况下，第一元件可以被表述为第二元件，并且类似地，第二元件可以被表述为第一元件。表述“和/或”包括一个或更多个所列有关项的任意组合和所有组合。
本文中使用的术语只是为了描述具体实施方案的目的，而无意于对示例性实施方案进行限制。单数形式也意在包括复数形式，除非上下文另有明确说明。还应当理解的是，表述“包括”和/或“包含”在本说明书中使用时，表示所陈述的特征、整体、步骤、操作、要素、成分和/或其组合的存在，但不排除存在或添加一个或更多个其他特征、整体、步骤、操作、要素、成分和/或其组合。
除非另有定义，否则本文中使用的所有术语(包括技术术语或科学术语)具有与本发明所属技术领域中的一个普通技术人员所通常理解的含义相同的含义。在通常使用的字典中定义的这样的术语应被理解为具有与相关技术中的上下文含义等效的含义，并且除非在说明书中明确定义，否则不应被理解为具有理想或过于形式化的含义。
参照附图，下面将详细描述本发明的示例性实施方案。为了帮助理解本发明，在整个附图的描述中，类似的附图标记指代类似的元件，并且将不重复相同元件的描述。
图1是示出了制备根据本发明的示例性实施方案的碳化硅粉末的方法的流程图。图2至图6是示出了制备根据本发明的示例性实施方案的碳化硅粉末的方法的图。
参照图1至图6，制备根据示例性实施方案的碳化硅粉末的方法包括：将细碳化硅粉末与液态碳化硅前体混合(ST100)；将液态碳化硅前体转化为β相碳化硅颗粒物质(ST200)；以及利用β相碳化硅颗粒物质将细碳化硅粉末晶粒生长为颗粒状碳化硅粉末(ST300)。
首先，参照图2和图3，可以制备细碳化硅粉末100用于将细碳化硅粉末与液态碳化硅前体混合的操作(ST100)。细碳化硅粉末100的粒径(D50)可以为0.2μm至9μm。根据本发明的示例性实施方案，可以由具有0.2μm至9μm的粒径(D50)的细碳化硅粉末100获得具有40μm至150μm的粒径(D50)的颗粒状碳化硅粉末(图6的300)。在本说明书中，细碳化硅粉末可以与第一碳化硅粉末一起使用，并且颗粒状碳化硅粉末可以与第二碳化硅粉末一起使用。
可以通过将提供硅的硅源与提供碳的碳源混合并且对混合物加热而获得细碳化硅粉末100。硅源可以是选自例如热解法二氧化硅、二氧化硅溶胶、二氧化硅凝胶、细二氧化硅、石英粉及其混合物中的至少之一。固体碳源可以是例如选自石墨、炭黑、碳纳米管(CNT)、富勒烯及其混合物中的至少之一。有机碳化合物可以是选自酚醛树脂、法郎树脂、二甲苯树脂、聚酰亚胺、聚氨酯、聚乙烯醇、聚丙烯腈、聚乙酸乙烯酯、纤维素及其混合物中的至少之一。为了获得细碳化硅粉末100，可以在1700℃至1800℃下对混合的硅源和碳源进行加热。
同时，如图3所示，可以通过将细碳化硅粉末100与液态碳化硅前体210混合来用液态碳化硅前体210涂覆细碳化硅粉末100的表面。因此，可能有助于在细碳化硅粉末100与碳化硅前体210之间的物质转移。
此处，碳化硅前体210可以包括碳化硅陶瓷先驱体聚合物系列。作为示例，碳化硅前体210可以包括硅氮烷或聚碳硅烷。
细碳化硅粉末100和碳化硅前体210可以利用例如球磨机、喷雾干燥机或亨舍尔(Henschel)混合机来混合。
另外，为了涂覆碳化硅前体210，可以使用有机溶剂例如乙醇或异丙基安替比林(isopropylantipyrine，IPA)。
碳化硅前体210可以以相对于细碳化硅粉末100和碳化硅前体210的总重量的5wt％至20wt％被添加。碳化硅前体210的这样的重量是用于适当地涂覆细碳化硅粉末100的表面的量。
接着，参照图4，在预定温度下对涂覆有碳化硅前体210的细碳化硅粉末100进行退火，然后将碳化硅前体210转化为β相碳化硅颗粒物质220(ST200)。可以在例如1500℃至1600℃下对涂覆有碳化硅前体210的细碳化硅粉末100进行退火。
可以在1600℃以下对碳化硅前体210进行热分解，从而将其转化为β相碳化硅颗粒物质220。此处，β相碳化硅颗粒物质220可以具有超细(例如，纳米单元)粒径，并且可以为固相。
接着，参照图5和图6，通过以预定温度加热、利用β相碳化硅颗粒物质将细碳化硅粉末100晶粒生长为颗粒状碳化硅粉末300(ST300)。将β相碳化硅颗粒物质220分散在细碳化硅粉末100中以填充孔。因此，可以通过β相碳化硅颗粒物质220与细碳化硅粉末100的接触来促进物质转移和反应。此处，加热温度可以为2000℃以下。因此，细碳化硅粉末100可以晶粒生长为具有均匀粒径分布的颗粒状碳化硅粉末300，而没有相转移为α相。
同时，退火可以维持1小时至10小时。随着退火时间增加，可以获得具有高粒径的碳化硅粉末。因此，可以利用退火时间来控制碳化硅粉末的粒径。
另外，可以连续地或间歇地执行ST200和ST300。例如，当温度缓慢地从1500℃升高至2000℃时，可以执行到β相碳化硅颗粒物质的转化(ST200)和碳化硅粉末的晶粒生长(ST300)，或者可以在1600℃以下的温度下执行β相碳化硅颗粒物质的转化(ST200)，然后可以在升高的温度下执行碳化硅粉末的晶粒生长(ST300)。
根据本发明的示例性实施方案，如图6所示，可以制备颗粒状碳化硅粉末300。所制备的颗粒状碳化硅粉末300为β相，并且具有均匀粒径分布和40μm至150μm的粒径(D50)。另外，在所制备的碳化硅粉末300中，含0.1ppm至10ppm的杂质。碳化硅粉末300的粒径分布可以通过分散度(D90/D10)表示。根据本发明的示例性实施方案的碳化硅粉末300的分散度为1至10。此处，D10指对应于低的10％处的粉末的粒径。另外，D90指对应于低的90％处的粉末的粒径。
虽然已参照其某些示例性实施方案示出和描述了本发明，但是本领域技术人员应理解，在不脱离由所附权利要求限定的本发明的范围的情况下，可以在其中进行形式和细节的各种变化。

Claims (7)

1.一种β相碳化硅粉末，其具有1至10的分散度(D90/D10)和40μm至150μm的粒径(D50)。
2.根据权利要求1所述的粉末，其包含0.1ppm至10ppm的杂质。
3.一种制备碳化硅粉末的方法，包括：
将第一碳化硅粉末与液态碳化硅前体混合；
在第一温度下对所述混合物进行退火，并且将所述碳化硅前体转化为β相碳化硅颗粒物质；以及在第二温度下对所述物质进行退火，并且利用所述β相碳化硅颗粒物质将所述第一碳化硅粉末晶粒生长为第二碳化硅粉末。
4.根据权利要求3所述的方法，其中，所述第一碳化硅粉末具有0.2μm至9μm的粒径(D50)。
5.根据权利要求3所述的方法，其中，所述第二碳化硅粉末具有1至10的分散度(D90/D10)和40μm至150μm的粒径(D50)，并且为β相。
6.根据权利要求3所述的方法，其中，所述碳化硅前体包括选自由硅氮烷和聚碳硅烷组成的组中的至少之一。
7.根据权利要求3所述的方法，其中，所述碳化硅前体以相对于所述第一碳化硅粉末和所述碳化硅前体的总重量的5wt％至20wt％被添加。
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