GaN单晶的HVPE生长及其应力和晶体取向研究
摘要
GaN晶体材料因其具有较高的电子迁移率和热导率,高化学稳定性,耐腐蚀等优点,被广泛应用于光电子器件和高频微波器件,但是由于缺乏GaN单晶衬底材料,目前器件大多是在蓝宝石、SiC等单晶衬底上进行异质外延制备而成,由于衬底材料和外延生长的器件之间存在较大的晶格失配和热失配,造成了在经过高温生长的器件中残余有较大的应力,大大降低了器件的性能,而获得自支撑GaN单晶衬底材料可以在根本上解决这些问题。氢化物气相外延(Hydride Vapor Phase Epitaxy-HVPE)方法生长GaN单晶,具有生长速率高,设备相对简单,所需成本较低等优点,因此被认为是生长GaN晶体最具有前景的生长方法。
本文采用HVPE方法生长GaN晶体,并通过使用图形衬底、腐蚀衬底等技术降低位错密度和残余应力,利用EBSD技术分析异质外延系统中的晶体取向和晶格失配,并提出了一种由晶体取向计算应力的方法,得到了异质衬底外延生长GaN中的应力分布。论文主要取得了以下成果：
1.研究了GaCl载气流量对GaN晶体质量的影响,发现在GaCl载气流量为1.3slm时(0002)和(10-12)衍射峰半峰宽最小,说明此时生长的晶体位错密度最低质量最好。室温PL测试发现每个样品都具有很强的带边发射峰,仅在GaCl载气流量较高时生长的GaN单晶样品处2.26-2.29eV处存在一个很弱的黄光发射峰,说明样品质量较好；通过拉曼光谱E2(high)峰位的移动,发现当GaCl载气流量为1.3slm时样品具有最低的残余压应力为0.36GPa; AFM表征样品的表面形貌发现GaN单晶的生长都是台阶流生长模式。六方GaN晶体的A1(LO)峰是LOPC模式,对峰形进行了拟合,得到了不同GaCl载气流量下生长GaN单晶样品的载流子浓度和迁移率。
2.研究了磷酸腐蚀对MOCVD-GaN腐蚀坑形貌的影响,并利用腐蚀衬底生长出自支撑GaN晶体。首先研究了腐蚀时间对腐蚀坑形貌和大小的影响,利用磷酸短时间对MOCVD-GaN进行腐蚀,会出现常见的六边形腐蚀坑,当延长腐蚀时间到腐蚀坑的深度达到了MOCVD-GaN层厚度时,磷酸能够腐蚀到N面GaN,就会产生了独特的十二面锥形结构。我们根据六方纤锌矿结构对称性和晶体结构参数,计算出该结构出现了两套晶面,其晶面指数分别是(4,-1,-3,-4)和(3,1,-4,-4)。利用这种具有N面腐蚀十二面锥形结构的蓝宝石/MOCVD-GaN衬底进行HVPE生长,在生长GaN厚度较大时能够实现自剥离,获得自支撑GaN晶体,在生长时十二面锥形貌转变为六面锥。通过拉曼光谱对HVPE生长GaN晶体的应力进行了分析,结果显示自支撑GaN晶体中的应力远小于普通衬底生长的样品。
3.研究了在具有六方周期排列Si02图形掩模的蓝宝石/MOCVD-GaN衬底上进行HVPE生长GaN晶体的生长规律。通过EBSD的菊池衍射花样和极图分析,确定了异质外延体系中GaN和蓝宝石衬底之间的晶体取向关系是c面相互平行,GaN晶格在面内相对于蓝宝石衬底晶格发生了30°的旋转。根据这一晶体取向关系和晶格参数,分别使用两种方法计算得到GaN和蓝宝石衬底之间的晶格失配为16.1%和13.8%。由于较大的晶格失配和热失配的存在,蓝宝石衬底上生长GaN的晶体取向偏离理想方向的程度在靠近界面处最大,随着生长厚度增加后逐渐接近理想方向。通过拉曼光谱分析发现图形衬底上生长的GaN晶体的残余应力,比平板衬底上生长的GaN晶体大大下降,说明图形衬底产生空隙的生长模式能够有效的释放GaN晶体中的应力。
4.利用EBSD技术得到的晶体取向信息,分析了蓝宝石衬底上异质外延生长GaN晶体中晶体取向分布情况,提出了一种利用晶体取向信息计算晶体中应力的新方法。我们使用这种方法分析了蓝宝石衬底/GaN异质外延结构GaN晶体的应力分布情况,发现了应力分布的规律是距离衬底越近时应力越大,随着厚度增加应力值减小,达到一定厚度之后应力值保持不变。同时,我们对这一异质外延体系中GaN的应力进行了理论计算,并使用拉曼光谱对应力分布进行了验证。这种利用EBSD分析晶体材料中应力的方法也可以推广到其他晶体材料中。由于EBSD测试具有的独特优势,这种理论的提出为分析晶体材料的性质提供了新的思路。
5.通过EBSD技术分析了6H-SiC衬底上HVPE生长GaN晶体的晶体取向,对外延体系的晶体取向关系进行了分析,并与蓝宝石衬底生长GaN的晶体取向关系进行了比较,发现在6H-SiC衬底上生长的GaN晶体取向没有发生相对衬底的旋转,这和蓝宝石衬底是不同的。根据晶体取向关系和晶格参数,计算了GaN和6H-SiC衬底之间的晶格失配,发现其失配度很小,因此能够有效降低外延生长GaN的位错密度和残余应力。同时还对蓝宝石衬底中产生的小角晶界进行了EBSD分析,研究了小角晶界两侧的晶体取向偏差。
GaN crystal material has a high electron mobility and thermal conductivity, high chemical stability. So it can be widely used in photoelectric devices, high frenquece microwave devices. Due to the lack of GaN single crystal substrate material, devices are mostly epitaxy on foreign substrate, such as sapphire and SiC crystals. There are large lattice mismatch and thermal expansion coefficient mismatch between GaN and substrate. In this case the devices have a larger residual stress and dislocation density after cooling from the growth temperature. In order to solve these problems, free-standing GaN crystal materials need to be grown. Hydride vapor phase epitaxy (HVPE) method growing GaN single crystal is considered to be a suitable way to obtain GaN single crystal substrate materials because of its high growth rate, relatively simple crystal growth system and the low cost of growth sources.
In this work we grow GaN crystals by HVPE method and optimized the growth parameter. The patterned substrate and etching process are used to reduce the dislocation density and residual stress of HVPE growth GaN and obtain free-standing GaN crystal. The growth modes on these substrates are researched. EBSD technology is used to analyze the heteroepitaxy system crystallographic orientation relationship between GaN and substrate. The lattice mismatch and stress are calculated from the crystallographic orientation. The mainly research achievements are as follows:
1. The influence of GaCl carrier gas flow rate was studied to obtain optimal condition for high crystalline quality GaN film. The1.3slm GaCl carrier gas flow rate sample with low FWHM of both (0002) and (10-12) reflection was demonstrated to have high crystalline quality and low dislocation density. Room temperature photoluminescence results showed a strong band-edge emission (NBE) peak with a FWHM of20-30meV which was detected in each sample. GaN films grown by high GaCl carrier gas flow rate had a very weak yellow luminescence (YL) peak at2.26-2.29eV. The HVPE GaN films grown with1.3slm GaCl carrier gas flow rate were found to have the lowest the residual compressive stress0.36GPa, which corresponded to the wave number of E2Raman mode at567.7cm-1. The surface morphology of all films showed a clear step flow growth model in AFM images. The carrier concentration and mobility of these GaN crystals are obtained by fitting of the A1(LO) Raman peak which is a LOCP mode.
2. Hexagonal etch pits formed in the MOCVD grown GaN on sapphire after being etched in hot phosphoric acids. With long etching time the etch pits reached the sapphire substrate and kept extending etching time the etch pits connected with each other to form large irregularly shaped etch pits. There were some pyramid structures in the N-polar face of GaN clustered around the etch pits reached the sapphire substrate. These pyramids have twelve facets. The crystallographic plane indexes of the facets were identified as (4,-1,-3,-4) and (3,1,-4,-4) according to the symmetry of wurtzite structure GaN. This kind of structures reduced the contact area between epitaxial GaN and sapphire substrate and was beneficial to self-separated process. This wet etching method provided a possible facile method to obtain free-standing GaN using HVPE growth.
3. GaN crystal was grown using a MOCVD-GaN/sapphire substrate with hexagonally distributed SiO2masks. GaN epitaxial grown on the maskless area underwent lateral overgrowth and coalesced on the top of the masks. Voids were formed on the masks because of this growth mode. The orientation relationship was examined by EBSD Kikuchi diffraction patterns and pole figures of GaN and sapphire. The cross-sectional plane was1-210for GaN and10-10for sapphire, respectively. The in-plane orientation relationship between the two materials constitutes an angular rotation of30°. The lattice mismatch calculated from the orientation relationship and the lattice parameters was16.1%and13.8%between GaN and the sapphire substrate, according to different evaluation methods. As a result of the large lattice mismatch, the disorientation of GaN was largest at the interface and decreased as the GaN grew. The crystallographic orientation approached the ideal growth direction as the GaN was growing. The EBSD mapping analysis also confirmed this result. The Raman spectrum measurements confirmed reduced residual stress values in the HVPE grown GaN on the substrate with masks.
4. The method of calculating stress in the crystal materials directly from the deformation of lattice identified by EBSD was provided. The stress of crystal materials at each mapping point was obtained from EBSD by this method. Stress distribution in large area was obtained efficiently and exactly by this method. Wurtzite structure GaN crystals grown by HVPE on foreign substrate was used as the example of hexagonal crystal system. Stress obtained from Raman spectroscopy confirmed the distribution identified by EBSD. We think that the stress distribution of other crystal materials also can be calculated by this method depends on changing the form of elasticity tensor. Other properties related to the lattice deformation were also analyzed by this way.
5. The GaN crystal HVPE grown on the6H-SiC substrate was researched by EBSD. The cross-sectional plane was10-10for GaN and6H-SiC substrate. It was different from the in-plane orientation relationship of sapphire/GaN heteroepitaxy system. The lattice mismatch calculated from the orientation relationship and the lattice parameters was3.7%and3.5%between GaN and the sapphire substrate, according to different evaluation methods. The lattice mismatch was much smaller than the GaN on sapphire substrate. The use of6H-SiC substrate reduced the dislocation density and residual stress values in the HVPE grown GaN. The small angle grain boundary of sapphire was also researched by the EBSD.
本文采用HVPE方法生长GaN晶体,并通过使用图形衬底、腐蚀衬底等技术降低位错密度和残余应力,利用EBSD技术分析异质外延系统中的晶体取向和晶格失配,并提出了一种由晶体取向计算应力的方法,得到了异质衬底外延生长GaN中的应力分布。论文主要取得了以下成果：
1.研究了GaCl载气流量对GaN晶体质量的影响,发现在GaCl载气流量为1.3slm时(0002)和(10-12)衍射峰半峰宽最小,说明此时生长的晶体位错密度最低质量最好。室温PL测试发现每个样品都具有很强的带边发射峰,仅在GaCl载气流量较高时生长的GaN单晶样品处2.26-2.29eV处存在一个很弱的黄光发射峰,说明样品质量较好；通过拉曼光谱E2(high)峰位的移动,发现当GaCl载气流量为1.3slm时样品具有最低的残余压应力为0.36GPa; AFM表征样品的表面形貌发现GaN单晶的生长都是台阶流生长模式。六方GaN晶体的A1(LO)峰是LOPC模式,对峰形进行了拟合,得到了不同GaCl载气流量下生长GaN单晶样品的载流子浓度和迁移率。
2.研究了磷酸腐蚀对MOCVD-GaN腐蚀坑形貌的影响,并利用腐蚀衬底生长出自支撑GaN晶体。首先研究了腐蚀时间对腐蚀坑形貌和大小的影响,利用磷酸短时间对MOCVD-GaN进行腐蚀,会出现常见的六边形腐蚀坑,当延长腐蚀时间到腐蚀坑的深度达到了MOCVD-GaN层厚度时,磷酸能够腐蚀到N面GaN,就会产生了独特的十二面锥形结构。我们根据六方纤锌矿结构对称性和晶体结构参数,计算出该结构出现了两套晶面,其晶面指数分别是(4,-1,-3,-4)和(3,1,-4,-4)。利用这种具有N面腐蚀十二面锥形结构的蓝宝石/MOCVD-GaN衬底进行HVPE生长,在生长GaN厚度较大时能够实现自剥离,获得自支撑GaN晶体,在生长时十二面锥形貌转变为六面锥。通过拉曼光谱对HVPE生长GaN晶体的应力进行了分析,结果显示自支撑GaN晶体中的应力远小于普通衬底生长的样品。
3.研究了在具有六方周期排列Si02图形掩模的蓝宝石/MOCVD-GaN衬底上进行HVPE生长GaN晶体的生长规律。通过EBSD的菊池衍射花样和极图分析,确定了异质外延体系中GaN和蓝宝石衬底之间的晶体取向关系是c面相互平行,GaN晶格在面内相对于蓝宝石衬底晶格发生了30°的旋转。根据这一晶体取向关系和晶格参数,分别使用两种方法计算得到GaN和蓝宝石衬底之间的晶格失配为16.1%和13.8%。由于较大的晶格失配和热失配的存在,蓝宝石衬底上生长GaN的晶体取向偏离理想方向的程度在靠近界面处最大,随着生长厚度增加后逐渐接近理想方向。通过拉曼光谱分析发现图形衬底上生长的GaN晶体的残余应力,比平板衬底上生长的GaN晶体大大下降,说明图形衬底产生空隙的生长模式能够有效的释放GaN晶体中的应力。
4.利用EBSD技术得到的晶体取向信息,分析了蓝宝石衬底上异质外延生长GaN晶体中晶体取向分布情况,提出了一种利用晶体取向信息计算晶体中应力的新方法。我们使用这种方法分析了蓝宝石衬底/GaN异质外延结构GaN晶体的应力分布情况,发现了应力分布的规律是距离衬底越近时应力越大,随着厚度增加应力值减小,达到一定厚度之后应力值保持不变。同时,我们对这一异质外延体系中GaN的应力进行了理论计算,并使用拉曼光谱对应力分布进行了验证。这种利用EBSD分析晶体材料中应力的方法也可以推广到其他晶体材料中。由于EBSD测试具有的独特优势,这种理论的提出为分析晶体材料的性质提供了新的思路。
5.通过EBSD技术分析了6H-SiC衬底上HVPE生长GaN晶体的晶体取向,对外延体系的晶体取向关系进行了分析,并与蓝宝石衬底生长GaN的晶体取向关系进行了比较,发现在6H-SiC衬底上生长的GaN晶体取向没有发生相对衬底的旋转,这和蓝宝石衬底是不同的。根据晶体取向关系和晶格参数,计算了GaN和6H-SiC衬底之间的晶格失配,发现其失配度很小,因此能够有效降低外延生长GaN的位错密度和残余应力。同时还对蓝宝石衬底中产生的小角晶界进行了EBSD分析,研究了小角晶界两侧的晶体取向偏差。
GaN crystal material has a high electron mobility and thermal conductivity, high chemical stability. So it can be widely used in photoelectric devices, high frenquece microwave devices. Due to the lack of GaN single crystal substrate material, devices are mostly epitaxy on foreign substrate, such as sapphire and SiC crystals. There are large lattice mismatch and thermal expansion coefficient mismatch between GaN and substrate. In this case the devices have a larger residual stress and dislocation density after cooling from the growth temperature. In order to solve these problems, free-standing GaN crystal materials need to be grown. Hydride vapor phase epitaxy (HVPE) method growing GaN single crystal is considered to be a suitable way to obtain GaN single crystal substrate materials because of its high growth rate, relatively simple crystal growth system and the low cost of growth sources.
In this work we grow GaN crystals by HVPE method and optimized the growth parameter. The patterned substrate and etching process are used to reduce the dislocation density and residual stress of HVPE growth GaN and obtain free-standing GaN crystal. The growth modes on these substrates are researched. EBSD technology is used to analyze the heteroepitaxy system crystallographic orientation relationship between GaN and substrate. The lattice mismatch and stress are calculated from the crystallographic orientation. The mainly research achievements are as follows:
1. The influence of GaCl carrier gas flow rate was studied to obtain optimal condition for high crystalline quality GaN film. The1.3slm GaCl carrier gas flow rate sample with low FWHM of both (0002) and (10-12) reflection was demonstrated to have high crystalline quality and low dislocation density. Room temperature photoluminescence results showed a strong band-edge emission (NBE) peak with a FWHM of20-30meV which was detected in each sample. GaN films grown by high GaCl carrier gas flow rate had a very weak yellow luminescence (YL) peak at2.26-2.29eV. The HVPE GaN films grown with1.3slm GaCl carrier gas flow rate were found to have the lowest the residual compressive stress0.36GPa, which corresponded to the wave number of E2Raman mode at567.7cm-1. The surface morphology of all films showed a clear step flow growth model in AFM images. The carrier concentration and mobility of these GaN crystals are obtained by fitting of the A1(LO) Raman peak which is a LOCP mode.
2. Hexagonal etch pits formed in the MOCVD grown GaN on sapphire after being etched in hot phosphoric acids. With long etching time the etch pits reached the sapphire substrate and kept extending etching time the etch pits connected with each other to form large irregularly shaped etch pits. There were some pyramid structures in the N-polar face of GaN clustered around the etch pits reached the sapphire substrate. These pyramids have twelve facets. The crystallographic plane indexes of the facets were identified as (4,-1,-3,-4) and (3,1,-4,-4) according to the symmetry of wurtzite structure GaN. This kind of structures reduced the contact area between epitaxial GaN and sapphire substrate and was beneficial to self-separated process. This wet etching method provided a possible facile method to obtain free-standing GaN using HVPE growth.
3. GaN crystal was grown using a MOCVD-GaN/sapphire substrate with hexagonally distributed SiO2masks. GaN epitaxial grown on the maskless area underwent lateral overgrowth and coalesced on the top of the masks. Voids were formed on the masks because of this growth mode. The orientation relationship was examined by EBSD Kikuchi diffraction patterns and pole figures of GaN and sapphire. The cross-sectional plane was1-210for GaN and10-10for sapphire, respectively. The in-plane orientation relationship between the two materials constitutes an angular rotation of30°. The lattice mismatch calculated from the orientation relationship and the lattice parameters was16.1%and13.8%between GaN and the sapphire substrate, according to different evaluation methods. As a result of the large lattice mismatch, the disorientation of GaN was largest at the interface and decreased as the GaN grew. The crystallographic orientation approached the ideal growth direction as the GaN was growing. The EBSD mapping analysis also confirmed this result. The Raman spectrum measurements confirmed reduced residual stress values in the HVPE grown GaN on the substrate with masks.
4. The method of calculating stress in the crystal materials directly from the deformation of lattice identified by EBSD was provided. The stress of crystal materials at each mapping point was obtained from EBSD by this method. Stress distribution in large area was obtained efficiently and exactly by this method. Wurtzite structure GaN crystals grown by HVPE on foreign substrate was used as the example of hexagonal crystal system. Stress obtained from Raman spectroscopy confirmed the distribution identified by EBSD. We think that the stress distribution of other crystal materials also can be calculated by this method depends on changing the form of elasticity tensor. Other properties related to the lattice deformation were also analyzed by this way.
5. The GaN crystal HVPE grown on the6H-SiC substrate was researched by EBSD. The cross-sectional plane was10-10for GaN and6H-SiC substrate. It was different from the in-plane orientation relationship of sapphire/GaN heteroepitaxy system. The lattice mismatch calculated from the orientation relationship and the lattice parameters was3.7%and3.5%between GaN and the sapphire substrate, according to different evaluation methods. The lattice mismatch was much smaller than the GaN on sapphire substrate. The use of6H-SiC substrate reduced the dislocation density and residual stress values in the HVPE grown GaN. The small angle grain boundary of sapphire was also researched by the EBSD.
引文
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