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CN105543967B - 一种稳定pvt法生长4h高纯碳化硅单晶晶型的原料处理方法 - Google Patents

一种稳定pvt法生长4h高纯碳化硅单晶晶型的原料处理方法 Download PDF

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CN105543967B
CN105543967B CN201610072172.9A CN201610072172A CN105543967B CN 105543967 B CN105543967 B CN 105543967B CN 201610072172 A CN201610072172 A CN 201610072172A CN 105543967 B CN105543967 B CN 105543967B
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张云伟
靳丽婕
韩金波
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Abstract

本发明公开了一种稳定PVT法生长4H高纯碳化硅单晶晶型的原料处理方法包括：步骤1将合成好的碳化硅粉源放置在石墨坩埚内，用CVD炉加热至1000‑1300℃；步骤2向所述CVD炉内通入Ar（氩）和CH4（甲烷）的混合气体，调节调节Ar与CH4质量流比在1000‑1之间，压力控制在30000‑300pa之间，裂解后的碳沉积在碳化硅粉料表面，旋转翻动粉料使其在表面均匀沉积，根据沉积量需求增加反映时间；步骤3停止通入CH4气体后进行降温停炉，最终得到带有裂解碳镀层的碳化硅粉料。本发明通过增加原料中活性高的沉积碳来调节碳化硅生长中Si/C组分，使升华组分中Si与原料表面上的碳进行反应，最终降低生长组分中Si/C比来实现生长4H‑SiC高纯碳化硅晶型的稳定控制。

Description

一种稳定PVT法生长4H高纯碳化硅单晶晶型的原料处理方法
技术领域
本发明涉及半导体生长技术领域，特别是一种稳定PVT（物理气相沉积）法生长4H高纯碳化硅单晶晶型的原料处理方法。
背景技术
SiC是第三代宽带隙半导体材料之一，相对于常见Si和GaAs等半导体材料，SiC在带隙、介质击穿电压、电子饱和速率、导热率等方面具有优良的性能。因此，SiC有望成为超越Si极限的下一代能源器件和高温器件材料，伴随于此，广泛进行着衬底材料的发展。特别是在极端条件和恶劣条件下应用时，SiC器件的特性远远超过了Si器件和GaAs器件。在光电子领域，也较相对传统衬底材料Si 与蓝宝石优越很多。
碳化硅生长方式有PVT（物理气相沉积）法、CVD（化学气相沉积）法等，大尺寸高纯半绝缘碳化硅的生长多采用PVT法进行生长，生长的晶型多已4H-SiC或6H-SiC为主要晶型衬底材料。碳化硅晶型有3C-SiC、2H-SiC、4H-SiC、6H-SiC、15R-SiC等多型，一定条件下晶体的几种多型结构可以共存共融，2H-SiC多型一般在1300-1600℃形成；4H-SiC多型在1900-2500℃温度范围生成；15R-SiC多型在2300-2700℃范围内形成。而3C-SiC和6H-SiC多型生成温度范围则很宽，3C-SiC多型生成温度范围1000-2750℃几乎涵盖了其他多型的生成温度范围；6H-SiC多型生成范围为1800-3000℃，涵盖了4H-SiC、15R-SiC多型生成范围。因此在生长过程容易产生多型，多型带来的位错、微管等缺陷大大降低了其制备的器件性能。
根据4H-SiC的生长特点，适宜的温度范围和底的生长组分Si/C比有利于提高4H-SiC生长稳定性，适宜的温度范围其采用测温可以满足控制，但与其矛盾的条件SiC的升华特性，底的Si/C比一般要求较高的生长温度，根据4H-SiC、6H-SiC、15R-SiC的形成温度范围，控制在2100-2300℃之间较为适宜4H-SiC生长。这样其生长组分的Si/C比又较高，因此如何降低碳化硅生长气氛中Si/C是解决晶型稳定的关键技术。
发明内容
针对现有技术存在的问题，本发明的目的在于提供一种稳定PVT法生长4H高纯碳化硅单晶晶型的原料处理方法。
为实现上述目的本发明一种稳定PVT法生长4H高纯碳化硅单晶晶型的原料处理方法，该方法包括如下步骤：
步骤1将合成好的碳化硅粉源放置在石墨坩埚内，用CVD炉加热至1000-1300℃；
步骤2向所述CVD炉内通入Ar（氩）和CH4（甲烷）的混合气体，调节调节Ar与CH4质量流比在1000-1之间，压力控制在30000-300pa之间，裂解后的碳沉积在碳化硅粉料表面，旋转翻动粉料使其在表面均匀沉积，根据沉积量需求增加反映时间；
步骤3停止通入CH4气体后进行降温停炉，最终得到带有裂解碳镀层的碳化硅粉料。
进一步，所述带有裂解碳镀层的碳化硅粉料的表面镀层碳与碳化硅粉料的质量比在1/500-1/5000之间。
本发明通过增加原料中活性高的沉积碳来调节碳化硅生长中Si/C组分，使升华组分中Si与原料表面上的碳进行反应，最终降低生长组分中Si/C比来实现生长4H-SiC高纯碳化硅晶型的稳定控制。
附图说明
图1为实例1中利用本发明进行生长的4H-SiC晶型的晶体的光谱分析图；
图2为实例2中利用本发明进行生长的4H-SiC晶型的晶体的光谱分析图；
图3为实例3中利用本发明进行生长的4H-SiC晶型的晶体的光谱分析图。
具体实施方式
下面结合附图和具体实施方式对本发明作进一步详细说明。
本发明的一种稳定PVT法生长4H高纯碳化硅单晶晶型的原料处理方法，该方法包括如下步骤：
步骤1将合成好的碳化硅粉源放置在石墨坩埚内，利用CVD炉加热至1000-1300℃；
步骤2向CVD炉内通入Ar（氩）和CH4（甲烷）的混合气体，调节调节Ar与CH4质量流比在1000-1之间，石墨坩埚内压力控制在30000-300pa之间，裂解后的碳沉积在碳化硅粉料表面，旋转翻动粉料使其在表面均匀沉积，根据沉积量需求增加反映时间；
步骤3停止通入CH4气体后进行降温停炉，最终得到带有活性高的裂解碳镀层的高纯碳化硅粉料。
优选的，将通过上述方法处理的碳化硅粉料的表面镀层碳与碳化硅粉料的质量比在1/500-1/5000之间。
下面选取三组生长实例说明本发明的效果：
实例1：CVD炉反应温度1150℃，Ar/CH4：800/50（sccm/min）,石墨坩埚内压力控制在3000pa，反应20分钟。将得到的碳化硅粉料放置在石墨坩埚中，将4H-SiC籽晶固定在粉料上方的坩埚盖上，向单晶炉中通入Ar气体或混有H2的气体充至4-8万帕，温度控制在2100-2300℃之间进行4H-SiC晶型的晶体生长。将晶体切片后使用拉曼光谱分析进行晶型测试，如图1所示，晶型稳定95%。
实例2：CVD炉反应温度1200℃，Ar/CH4：800/50（sccm/min）,石墨坩埚内压力控制在2000pa，反应20分钟。将得到的碳化硅粉料放置在石墨坩埚中，将4H-SiC籽晶固定在粉料上方的坩埚盖上，向单晶炉中通入Ar气体或混有H2的气体充至4-8万帕，温度控制在2100-2300℃之间进行4H-SiC晶型的晶体生长。将晶体切片后使用拉曼光谱分析进行晶型测试，如图2所示，晶型稳定100%。
实例3：CVD炉反应温度1150℃，Ar/CH4：500/50（sccm/min）, 石墨坩埚内压力控制在2000pa，反应20分钟。将得到的碳化硅粉料放置在石墨坩埚中，将4H-SiC籽晶固定在粉料上方的坩埚盖上，向单晶炉中通入Ar气体或混有H2的气体充至4-8万帕，温度控制在2100-2300℃之间进行4H-SiC晶型的晶体生长。将晶体切片后使用拉曼光谱分析进行晶型测试，如图3所示，晶型稳定100%。
上述示例只是用于说明本发明，本发明的实施方式并不限于这些示例，本领域技术人员所做出的符合本发明思想的各种具体实施方式都在本发明的保护范围之内。

Claims (1)

1.一种稳定PVT法生长4H高纯碳化硅单晶晶型的原料处理方法，其特征在于，该方法包括如下步骤：
步骤1将合成好的碳化硅粉源放置在石墨坩埚内，用CVD炉加热至1150～1200℃；
步骤2向所述CVD炉内通入Ar和CH4的混合气体，调节Ar与CH4质量流比在1000～1之间，压力控制在30000～300pa之间，裂解后的碳沉积在碳化硅粉料表面，旋转翻动粉料使其在表面均匀沉积，根据沉积量需求增加反应时间；
步骤3停止通入CH4气体后进行降温停炉，最终得到带有裂解碳镀层的碳化硅粉料；
所述带有裂解碳镀层的碳化硅粉料的表面镀层碳与碳化硅粉料的质量比在1/500-1/5000之间。
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