CN111455455A - 具有在线监测功能的晶体生长装置 - Google Patents

具有在线监测功能的晶体生长装置 Download PDF

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CN111455455A
CN111455455A CN202010132322.7A CN202010132322A CN111455455A CN 111455455 A CN111455455 A CN 111455455A CN 202010132322 A CN202010132322 A CN 202010132322A CN 111455455 A CN111455455 A CN 111455455A
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刘胜
东芳
高冰
周振
甘志银
王诗兆
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Wuhan University WHU
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Abstract

公开了一种具有在线监测功能的晶体生长装置,包括:生长坩埚,其上具有至少两个检测窗口,所述检测窗口通过阀门密封;透明密封腔,罩在所述检测窗口上在所述阀门打开时使所述生长坩埚处于密闭状态;光谱仪,位于所述生长坩埚外,其中光谱仪发射器对准所述至少两个检测口中的一个,光谱仪接收器对准所述至少两个检测口中的另一个;和/或XRD衍射仪,位于所述生长坩埚外,其中XRD发射器对准所述至少两个检测口中的一个,XRD接收器对准所述至少两个检测口中的另一个;和/或质谱仪,其探头位于所述生长坩埚内;和/或检测所述生长坩埚侧壁温度的测温仪。本发明装置可以在晶体生长过程中对元素、物质、晶格等与缺陷直接相关的信息进行监测。

Description

具有在线监测功能的晶体生长装置
技术领域
本公开涉及具有在线监测功能的晶体生长装置,可用于碳化硅生长的监控。
背景技术
碳化硅作为第三代半导体材料具有宽带隙、高临界击穿电场、高热导率、高载流子饱和浓度、化学性能稳定、高硬度、抗磨损等特点,使得它在军用和航天领域的高温、高频、大功率光电器件方面具有优越的应用价值,成为当今最受关注的新型半导体材料。
建立在碳化硅基础上的整个产业和技术的发展,离不开高质量的碳化硅晶片。目前,碳化硅晶体材料的制备方法有“溶液生长法”、“升华再结晶”法、“改进升华”法、外延生长法。“升华再结晶”法是把碳化硅晶体颗粒置于石墨坩埚内,在Ar气氛中升温到2500℃以上进行热解升华,并将其输送到低温处进行有序再结晶成为高纯的碳化硅单晶体。不管是溶液生长,还是气相生长,都涉及到下面4个现象:1、物质的对流及扩散输运;2、温度场的分布;3、杂质的扩散及输运;4、点缺陷、线缺陷、面缺陷的生成。
碳化硅晶体的缺陷主要包括微管、位错、层错、多型性、异质包裹物、小角度晶界和平面六方空洞等。这些晶体缺陷的存在主要有以下两方面的原因:籽晶自身缺陷在晶体生长过程中进一步的延伸;单晶生长过程中由于偏离化学计量比而形成缺陷。由于一种缺陷的存在会诱发其他缺陷产生,因此对这些缺陷进行研究并且在晶体生长过程中进行有效控制,对提高碳化硅晶体质量非常重要。同时,在目前碳化硅生长过程中存在非常严重的现象为碳化现象,且其形成机理不是很明确,因此,结合多种检测手段监测碳化硅生长过程的演变细节十分重要。在碳化硅生长设备中集成测量仪难度较大,原因在于碳化硅生长炉内部温度在碳化硅晶体处的温度为2500度,并温度成梯度递减,各类监测设备与生长炉集成具有很大挑战。
发明内容
本发明提供一种具有在线监测功能的晶体生长装置,有效监测晶体生长过程。
根据本发明实施例的一方面,提供一种晶体生长装置,包括:
生长坩埚,其上具有至少两个检测窗口,所述检测窗口通过阀门密封;
透明密封腔,罩在所述检测窗口上在所述阀门打开时使所述生长坩埚处于密闭状态;
光谱仪,位于所述生长坩埚外,其中光谱仪发射器对准所述至少两个检测口中的一个,光谱仪接收器对准所述至少两个检测口中的另一个;和/或
XRD衍射仪,位于所述生长坩埚外,其中XRD发射器对准所述至少两个检测口中的一个,XRD接收器对准所述至少两个检测口中的另一个;和/或
质谱仪,其探头位于所述生长坩埚内。
在上述的晶体生长装置,还包括检测所述生长坩埚侧壁温度的测温仪。
在上述的晶体生长装置,所述测温仪位于垂直升降装置上。
本发明的具有在线监测功能的晶体生长装置可以在晶体生长过程中对元素、物质、晶格等与缺陷直接相关的信息进行监测。本发明的晶体生长装置可以在晶体生长过程中,减小位错密度、降低堆积层错,减少微管的形成,实现低缺陷晶体生长。
附图说明
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。
图1示出了根据本发明的一个实施例的具有在线监测功能的晶体生长装置的结构示意图。
附体标记说明:
1-籽晶;
2-线圈;
3-晶体原料;
4-冷却室;
5-移动杆;
6-换气孔;
7-生长坩埚;
8-光谱仪发射器;
9-XRD发射器;
10-质谱仪;
11-质谱仪探头;
12-XRD接收器;
13-光谱仪接收器,
14-测温仪;
15-透明密封腔;
16-密封阀门;
17-密封阀门。
具体实施方式
本发明的具有在线监测功能的晶体生长装置可用于碳化硅、蓝宝石、氮化镓、InGaN、AlGaN、金刚石、氮化铝、硅、Ga2O3、低维材料、或上述多种材料组合的晶体的生长。
如图1,晶体生长装置的生长坩埚7上具有至少两个检测窗口,所述检测窗口通过阀门16,17密封。透明密封腔15罩在所述检测窗口上,以便在所述阀门打开时使生长坩埚7处于密闭状态。透明密封腔15可采用高温石英制成。
生长坩埚7外设有光谱仪,所述光谱仪采用激光诱导发射光谱检测技术。光谱仪发射器8对准所述至少两个检测窗口中的一个,光谱仪接收器13对准所述至少两个检测口中的另一个。所述检测窗口上的阀门16,17打开后,光谱仪发射器8发射的光谱通过透明密封腔15、所述至少两个检测窗口中的所述一个入射到晶体薄膜表面,使材料气化并电离成等离子体与蒸汽混合物,等离子体发出的光信号经过所述至少两个检测窗口中的所述另一个、透明密封腔15被光谱仪接收器13接收,形成对籽晶1上沉积物的物质成分的监测过程。此外,还可使用所述光谱仪对生长坩埚7内升华气体的元素成分进行实时监测。
生长坩埚7外还可设有XRD衍射仪,XRD衍射仪可以实现晶体生长的原位 X射线表征测试,包括X射线衍射,X射线CTR散射(晶体截断面),和X射线反射率等。XRD发射器9对准所述至少两个检测口中的一个,XRD接收器12 对准所述至少两个检测口中的另一个。所述检测窗口上的阀门16,17打开后, XRD发射器9发射的X射线通过透明密封腔15、所述至少两个检测窗口中的所述一个入射到晶体薄膜上,XRD接收器12通过透明密封腔15、所述至少两个检测窗口中的所述另一个获得衍射信息,其中根据生长过程中薄膜表面的反射率的变化来反映晶体薄膜厚度的变化和表面粗糙度,监测生长物质的晶格结构,从而监测缺陷的生长过程,监测晶体的残余应力,为设备优化降低缺陷进行指导。
生长坩埚7外还可设置质谱仪10,质谱仪10的探测头11伸入生长坩埚7 内进行探测,实现对晶体生长过程中升华气体的成分含量的检测。为保持生长坩埚7内的密封度和所需压强,探测头11和坩埚7接触处可采用密封压圈或密封法兰或密封胶来密封。
生长坩埚7外还可设置检测生长坩埚7侧壁温度的测温仪14。测温仪14可安装在垂直升降装置上,实现不同高度处温度的检测。测温仪14发射探测射线从加热线圈2间隙处射向生长坩埚7表面,从而测量生长坩埚7侧壁的温度,并实时将温度反馈给线圈控制系统,调节不同位置处线圈2的温度,保证生长坩埚 7内部温度的恒定。
本发明利用光谱仪和XRD衍射仪对形成的沉积层成分及晶粒结构进行实时检测,以逐层判断沉积的杂质成分和晶粒结构缺陷是否超标,同时利用质谱仪对升华的气体成分进行实时检测,判断气体的成分比例及是否有杂质气体混入,一旦发现杂质成分或晶粒结构缺陷超标,则停机调整设备,优化设备参数,实现晶体生长过程中质量和缺陷的控制。晶体生长完成后,通过移动杆5降至冷却室4 内,对晶体进行降温。

Claims (3)

1.一种晶体生长装置,其特征在于,包括:
生长坩埚,其上具有至少两个检测窗口,所述检测窗口通过阀门密封;
透明密封腔,罩在所述检测窗口上在所述阀门打开时使所述生长坩埚处于密闭状态;
光谱仪,位于所述生长坩埚外,其中光谱仪发射器对准所述至少两个检测口中的一个,光谱仪接收器对准所述至少两个检测口中的另一个;和/或
XRD衍射仪,位于所述生长坩埚外,其中XRD发射器对准所述至少两个检测口中的一个,XRD接收器对准所述至少两个检测口中的另一个;和/或
质谱仪,其探头位于所述生长坩埚内。
2.根据权利要求1所述的晶体生长装置,其特征在于,还包括检测所述生长坩埚侧壁温度的测温仪。
3.根据权利要求2所述的晶体生长装置,其特征在于,所述测温仪位于垂直升降装置上。
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