CN104755421A - 碳化硅粉末和其制备方法 - Google Patents

碳化硅粉末和其制备方法 Download PDF

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CN104755421A
CN104755421A CN201380054592.9A CN201380054592A CN104755421A CN 104755421 A CN104755421 A CN 104755421A CN 201380054592 A CN201380054592 A CN 201380054592A CN 104755421 A CN104755421 A CN 104755421A
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silicon carbide
carbide powder
phase silicon
powder
alpha
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金柄淑
申东根
韩姃恩
闵庚皙
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LG Innotek Co Ltd
Sungkyunkwan University Foundation for Corporate Collaboration
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Abstract

根据本发明的一个实施方案,用于制备碳化硅粉末的方法包括以下步骤:将晶种加入β碳化硅粉末中;并且通过热处理该β碳化硅粉末来形成α碳化硅粉末。

Description

碳化硅粉末和其制备方法
技术领域
本发明涉及碳化硅粉末和其制备方法,更具体而言,涉及使用碳化硅细粉末的碳化硅粉末制备方法。
背景技术
碳化硅(SiC)在高温下强度高并且抗蠕变性以及抗磨损性、抗氧化性和抗腐蚀性等优异。碳化硅以具有立方晶体结构的β相和具有六方晶体结构的α相存在。β相在1400℃至1800℃的温度范围内稳定,而α相在高于2000℃稳定。
碳化硅广泛用作工业结构材料并且近来已应用于半导体工业。由于此原因,期望在高温下稳定的高纯度碳化硅粉末。
碳化硅粉末可以通过例如艾奇逊(Acheson)法、碳热还原法、化学气相沉积(CVD)法等来制备。根据艾奇逊法,可以通过硅源和碳源在高温(例如2200℃至2400℃)下的碳热还原来获得α相碳化硅粉末。然而,由于根据上述方法制备的碳化硅粉末的纯度低,因而需要另外的纯化过程。
相比之下,可以通过在相对低的温度下合成纯化的材料来获得高纯度的碳化硅粉末。然而,在低温下容易获得β相碳化硅细粉末,其导致在高温下的不稳定性。
另一方面,β相碳化硅具有比α相碳化硅更低的蒸气压。因此,当β相碳化硅粉末在高温下热处理时,β相碳化硅挥发并且聚集成α相碳化硅粉末。在这种情况下,问题在于当热处理时间短时,β相和α相共存,并且虽然当热处理时间长时,可以获得高纯度的α相碳化硅粉末,但是颗粒生长至大于数百微米的大小。
发明内容
技术问题
本发明的技术问题涉及提供在高温下稳定的高纯度碳化硅粉末和其制备方法。
本发明的另一个技术问题涉及提供各种粒径的碳化硅粉末的制备方法。
技术解决方案
根据本发明的一个方面,碳化硅粉末的制备方法包括:将晶种加入β相碳化硅粉末,并且热处理该β相碳化硅粉末以形成α相碳化硅粉末。
热处理可以在2000℃至2200℃下进行多于4小时。
α碳化硅粉末的粒径可以根据加入的晶种的量调节。
加入的晶种的量按β相碳化硅粉末计可以是1wt%至7wt%。
加入的晶种可以是α碳化硅。
根据本发明的另一方面,碳化硅粉末包含α相碳化硅粉体,该α相碳化硅粉体具有45μm至110μm的粒径(D50)并且包括小于10ppm的杂质。
根据本发明的另一方面,碳化硅粉末包括选自以下中的至少一组:第一组,其包括粒径(D50)大于0μm且小于45μm、杂质小于10ppm的α碳化硅粉体;第二组,其包括粒径大于45μm且小于75μm、杂质小于10ppm的α碳化硅粉体;和第三组,其包括粒径大于75μm且小于110μm、杂质小于10ppm的α碳化硅粉体。
第一组、第二组和第三组可以根据在α碳化硅粉体的制备中加入的晶种的量来相互区分。
有益效果
根据本发明的示例性实施方案,可以获得在高温下稳定的高纯度碳化硅粉末。此外,所获得的碳化硅粉末的粒径可以通过调节热处理条件和晶种比率等来调节。
附图说明
图1示出表示根据本发明的示例性实施方案的碳化硅粉末制备方法的流程图。
图2示出比较例1的结果,图3示出比较例2的结果,图4示出比较例3的结果,并且图5示出表示根据比较例3的粒径分布的图。
图6示出示例性实施方案1的结果,图7示出示例性实施方案2的结果,图8示出示例性实施方案3的结果,并且图9示出示例性实施方案4的结果。
图10示出表示示例性实施方案1的粒径分布的图,图11示出表示示例性实施方案2的粒径分布的图,图12示出表示示例性实施方案3的粒径分布的图,并且图13示出表示示例性实施方案4的粒径分布的图。
具体实施方式
本发明可以具有各种示例性实施方案,并且可以采用各种修改,因而在附图中示出并且描述具体的示例性实施方案。然而,具体的示例性实施方案无意于限制本发明,并且应理解包括在本发明的精神和范围内的所有修改方案、等效方案和替代方案。
虽然包括序数词例如“第二”、“第一”等的术语可以用于描述各种要素,但是这些要素不受这些术语限制。这些术语仅用于将一个要素与另一个要素区分开。例如,第二要素可以被称为第一要素,并且相似地,第一要素可以被称为第二要素,而不偏离本发明的范围。术语“和/或”包括相关所列项目中一种或更多种的任意组合和所有组合。
本文所使用的术语仅用于描述具体实施方案的目的并且无意限制本发明。如本文中所使用,单数形式旨在也包括复数形式,除非上下文另行明确指出。还应理解当在本文中使用时,术语“包含”和/或“包括”表明所述的特征、整体、步骤、操作、要素、组分和/或其组的存在,但不排除存在或加入一种或更多种其他特征、整体、步骤、操作、要素、组分和/或其组。
除非另有限定,否则本文中所使用的所有术语(包括技术术语和科学术语)具有与本发明所属领域的普通技术人员通常的理解相同的含义。还应理解,例如在常用字典中定义的术语应当解读为具有与其在相关领域背景中的含义一致的含义,并且不解释为理想化或过于形式化的意义,除非本文明确地如此定义。
下文中将参照附图详细描述示例性实施方案,其中贯穿附图,相同或相应的要素用相同的附图标记指代,并且省略了要素的重复说明。
高纯度的α相碳化硅粉末可以通过在高温下热处理高纯度的β相碳化硅粉末来获得。然而,在β相碳化硅挥发并且聚集成α相碳化硅的过程期间,存在α相碳化硅和β相碳化硅共存的阶段。因此,为了获得高纯度的α相碳化硅粉末,需要将热处理保持期望的时间。然而,如果热处理保持期望的时间,那么会获得过度生长的α相碳化硅颗粒(例如大于150μm)。
另一方面,在市场中对具有各种粒径(例如数十微米)的α相碳化硅粉末的需求日益增长。
根据本发明的示例性实施方案,β相碳化硅粉末在高温下经热处理以获得在高温下稳定的α相碳化硅粉末。在这种情况下,将晶种加入β相碳化硅中以调节由此形成的α相碳化硅粉末的粒径。
图1示出表示本发明的碳化硅粉末的制备方法的流程图。
参照图1,首先制备β相碳化硅粉末(S100)。β相碳化硅粉末可以通过混合硅源(Si源)和碳源(C源)然后热处理经混合的粉末来获得。
硅源是能够提供硅的各种材料之一。硅源可以是,例如,选自气相法二氧化硅(fumed silica)、细二氧化硅、二氧化硅溶胶、二氧化硅凝胶、石英粉末和其混合物的多于一种。
碳源可以是固体碳源或有机碳化合物。固体碳源可以是,例如,选自石墨、炭黑、碳纳米管(CNT)、富勒烯和其混合物中的多于一种。有机碳化合物可以是,例如,选自酚树脂、法郎(franc)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、纤维素和其混合物中的多于一种。
硅源和碳源可以通过湿法或干法混合。硅源和碳源可以例如通过使用球磨机、磨碎机、3辊磨机等来混合。经混合的粉末可以例如使用筛来收集。
经混合的粉末的热处理过程可以分成碳化过程和合成过程。碳化过程可以例如在600℃至1000℃的条件下进行,而合成过程可以例如在1300℃至1700℃的条件下进行期望的时间(例如3小时)。
上述β相碳化硅粉末的制备方法仅用于示例性目的,并且β相碳化硅粉末可以根据各种方法来制备。
接下来,将α相碳化硅粉末作为晶种加入β相碳化硅粉末(S110),并且通过对其热处理,形成碳化硅颗粒(S120)。
热处理可以例如在高于2000℃(例如2000℃至2200℃)的高温下进行。如果β相碳化硅粉末在高温下经热处理,由于在β相碳化硅和α相碳化硅之间的高蒸气压差而发生挥发-聚集,并且由于再结晶,颗粒可以快速生长。另一方面,在由β相碳化硅至α相碳化硅的相变中存在β相碳化硅和α相碳化硅共存的阶段。为了仅获得α相碳化硅,热处理可以保持多于4小时。
然而,如果β相碳化硅保持多于4小时,可能获得粒径(D50)大于150μm的过度生长的碳化硅颗粒。因此,为了调节碳化硅粉末的粒径,可以在热处理β相碳化硅之前加入晶种。
在这种情况下,作为晶种加入的α相碳化硅粉末进行成核作用。即,β相碳化硅在高温下挥发并且在作为晶种加入的α相碳化硅粉末的表面上聚集。根据进行成核作用的晶种的量,所形成的碳化硅粉末的粒径可以变化。例如,随作为晶种加入的α相碳化硅粉末的量变大,所形成的颗粒的尺寸减小。因此,作为晶种加入的α相碳化硅粉末的量可以根据期望的粒径调节。
因此,即使为获得高纯度的α相碳化硅粉末而将β相碳化硅保持多于4小时的时候,也可以防止形成过度生长的碳化硅颗粒。
根据本发明的示例性实施方案,可以获得包含至少一组选自以下的碳化硅粉末:第一组,其包括粒径(D50)大于0μm且小于45μm的α碳化硅粉体;第二组,其包括粒径大于45μm且小于75μm的α碳化硅粉体;和第三组,其包括粒径大于75μm且小于110μm的α碳化硅粉体。此外,根据本发明的示例性实施方案,由于可以调节粒径而没有研磨过程,因而可以获得杂质少于10ppm(99.999%纯)的α碳化硅颗粒。此处,杂质可以表示在α碳化硅颗粒中包含的氧或氮等。
下文中,根据比较例和示例性实施例详细说明了根据本发明的示例性实施方案的碳化硅粉末的制备方法。
表1
<比较例1>
将平均粒径为1.7μm的β相碳化硅粉末置于石墨坩埚中,并且在真空环境下将温度升高至1450℃,在氩气气氛下升高至2150℃,保持1小时,然后自然冷却。
<比较例2>
将平均粒径为1.7μm的β相碳化硅粉末置于石墨坩埚中,并且在真空环境下将温度升高至1450℃,在氩气气氛下升高至2150℃,保持3小时,然后自然冷却。
<比较例3>
将平均粒径为1.7μm的β相碳化硅粉末置于石墨坩埚中,并且在真空环境下将温度升高至1450℃,在氩气气氛下升高至2150℃,保持5小时,然后自然冷却。
图2示出比较例1的结果,图3示出比较例2的结果,图4示出比较例3的结果,并且图5示出表示根据比较例3的粒径分布的图。
参照表1和图2至图4,可以看出当热处理中的保持时间短时,β相碳化硅和α相碳化硅共存,而随热处理中的保持时间变长,α相碳化硅的比率增加。
然而,如图5所示,如果热处理中的保持时间变长,粒径(D50)大幅增加至大于150μm。因此,为了获得粒径小于150μm的高纯度α相碳化硅,可以将α相碳化硅粉末作为晶种加入β相碳化硅粉末。
<示例性实施例1>
将1wt%α相碳化硅粉末加入平均粒径为1.7μm的β相碳化硅粉末,将其置于石墨坩埚中,并且在真空环境下将温度升高至1450℃,在氩气气氛下升高至2150℃,保持5小时,然后自然冷却。
<示例性实施例2>
将3wt%α相碳化硅粉末加入平均粒径为1.7μm的β相碳化硅粉末,将其置于石墨坩埚中,并且在真空环境下将温度升高至1450℃,在氩气气氛下升高至2150℃,保持5小时,然后自然冷却。
<示例性实施例3>
将5wt%α相碳化硅粉末加入平均粒径为1.7μm的β相碳化硅粉末,将其置于石墨坩埚中,并且在真空环境下将温度升高至1450℃,在氩气气氛下升高至2150℃,保持5小时,然后自然冷却。
<示例性实施例4>
将7wt%α相碳化硅粉末加入平均粒径为1.7μm的β相碳化硅粉末,将其置于石墨坩埚中,并且在真空环境下将温度升高至1450℃,在氩气气氛下升高至2150℃,保持5小时,然后自然冷却。
图6示出示例性实施方案1的结果,图7示出示例性实施方案2的结果,图8示出示例性实施方案3的结果,并且图9示出示例性实施方案4的结果,图10示出表示示例性实施方案1的粒径分布的图,图11示出表示示例性实施方案2的粒径分布的图,图12示出表示示例性实施方案3的粒径分布的图,并且图13示出表示示例性实施方案4的粒径分布的图。
参照表1和图6至图13,可以看出随着加入更多的α相碳化硅粉末,粒径减小。即,当α相碳化硅粉末的量按β相碳化硅粉末计为1wt%时,在最终粉末中粒径为75μm至150μm的粉末的比率是最高的。相比之下,当α相碳化硅粉末的量按β相碳化硅粉末计为3wt%时,在最终粉末中粒径为45μm至75μm的粉末的比率是最高的,并且当α相碳化硅粉末的量按β相碳化硅粉末计大于5wt%时,在最终粉末中粒径小于45μm的粉末的比率是最高的。这是因为当更多大小的晶种用于成核作用时,粒径减小。
根据本发明的示例性实施方案,可以通过在高温下热处理高纯度的β相碳化硅粉末来获得高纯度的α相碳化硅颗粒。在这种情况下,所获得的α相碳化硅颗粒的品质可以通过延长热处理时间来改善。此外,所获得的碳化硅粉末的粒径可以通过用向其加入的晶种的量来调节。因此,可以满足对具有各种粒径的α相碳化硅粉末的市场需求,并且由于未进行研磨过程以调节粒径,可以提高材料的纯度。
虽然上文描述了本发明优选的示例性实施方案,但本领域技术人员将理解,本发明可以进行各种修改和变化,而不偏离在以上权利要求中所描述的本发明的精神和范围。

Claims (2)

1.一种碳化硅粉末,其包含选自以下中的至少一组:第一组,其包含粒径(D50)大于0μm且小于45μm、杂质少于10ppm的α相碳化硅粉体;第二组,其包含粒径大于45μm且小于75μm、杂质少于10ppm的α相碳化硅粉体;和第三组,其包含粒径大于75μm且小于110μm、杂质少于10ppm的α相碳化硅粉体。
2.根据权利要求1所述的碳化硅粉末,其中所述第一组、所述第二组和所述第三组根据在所述α相碳化硅粉体的制备中加入的晶种的量来相互区分。
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