CN111430218A - 一种自分离制备GaN单晶衬底的方法 - Google Patents
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Abstract
本发明涉及一种自分离制备GaN单晶衬底的方法,其在GaN复合衬底的异质衬底上制造穿孔,将带有穿孔的GaN复合衬底浸没在金属镓与金属助溶剂的混合溶液中、并采用液相外延工艺生长得到GaN厚膜材料,生长过程中,金属助溶剂通过异质衬底的穿孔与GaN外延层界面层接触,一方面通过所述穿孔孔洞腐蚀与异质衬底相连的GaN外延层界面层,促使生长形成的GaN厚膜材料与异质衬底缓慢自分离,得到高质量和大尺寸的GaN单晶衬底,另一方面,金属助溶剂与氮形成中间体,该中间体为金属镓提供氮元素而促使GaN单晶生长,应用于钠流法技术制备时,改善钠流法制备技术中氮的溶解度低及不均匀的问题,提高GaN单晶的晶体质量与生长速率。
Description
技术领域
本发明涉及半导体光电材料制备技术领域,特别是涉及一种自分离制备GaN单晶衬底的方法。
背景技术
作为重要的直接带隙宽禁带半导体材料,GaN基III-V族氮化物在发光二极管(LED)、激光二极管(LD)和紫外光探测器等光电子器件,以及微波、电力电子等微电子功率器件领域中有着广泛的应用前景。
目前的GaN单晶衬底的制备方法一般以蓝宝石衬底、SiC、Si等为异质衬底材料制成复合衬底,再通过该复合衬底进行异质外延得到GaN厚膜材料,然后采用激光剥离技术或自分离技术去除异质衬底而获得GaN单晶衬底,但异质衬底与GaN材料间存在晶格与热胀参数的失配往往使GaN厚膜存在较大的残余应力,在激光剥离时受到GaN分解产生的冲击力而容易出现碎裂的问题,影响产品的良率与制造成本;而现有技术也有存在有如中国发明专利申请说明书CN201710691390.5提出的一种采用在异质衬底上制备GaN/氧化镓纳米柱阵列缓冲层,生长GaN厚膜后采用化学方法腐蚀缓冲层,从而去除异质衬底获得GaN单晶衬底的方法,但这种方法存在纳米柱的均匀性难以控制的问题,不适应大尺寸GaN单晶衬底的制备;如中国发明专利申请说明书CN201110134149.5提出在异质衬底上制备一层纳米薄膜,采用退火方式得到纳米颗粒,然后在其上外延生长GaN厚膜,采用机械方法去除异质衬底而得到GaN单晶衬底,但这种方法由于纳米颗粒的存在难以得到高质量的GaN单晶。
发明内容
为解决上述问题,本发明提出一种自分离制备GaN单晶衬底的方法,其通过在GaN复合衬底的异质衬底上制造穿孔,实现GaN单晶衬底和异质衬底自分离,可制备大尺寸高质量GaN单晶衬底。
为解决上述目的,本发明采用的如下技术方案。
一种自分离制备GaN单晶衬底的方法,包括以下步骤:S1,在异质衬底上制备GaN外延层,以获得GaN复合衬底;S2,在上述GaN复合衬底的异质衬底上穿孔,所述穿孔连接至GaN外延层;S3,将步骤S2中有穿孔的GaN复合衬底置于装有金属镓与金属助溶剂混合溶液的坩埚中,坩埚置于高压反应釜内;S4,在步骤S3中的高压反应釜内通入高纯氮气,调整高压反应釜内温度和压强,采用外延生长工艺生长GaN厚膜材料,金属助溶剂通过所述穿孔与GaN外延层接触,异质衬底和GaN厚膜材料自分离,最终得到GaN单晶衬底。
优选地,在步骤S2的异质衬底上穿孔的步骤中,所述穿孔的深度需穿透异质衬底直至GaN外延层。
优选地,在步骤S2的异质衬底上穿孔的步骤中,可采用激光辐射穿孔和机械化学穿孔的一种或多种的组合。
优选地,在步骤S2的异质衬底上穿孔的步骤中,所述穿孔的形状包括圆形、方形、六角形、三角形、十字形、米字型和不规则形状的一种或多种的组合。
优选地,在步骤S3的金属助溶剂可为碱金属或碱土金属溶剂。
优选地,在步骤S1的GaN复合衬底的制备可采用MOCVD工艺或HVPE工艺的一种或多种的组合。
优选地,所述异质衬底为蓝宝石、SiC、硅或金刚石材料的一种或多种。
优选地,GaN外延层可为GaN单层结构或GaN与InGaAlN缓冲层结合的多层结构。
优选地,在高压反应釜中可外延生长单片GaN厚膜材料或多片GaN厚膜材料同时生长,以得到单片或多片GaN单晶衬底。
本发明的有益效果如下:
与现有技术相比,本发明在GaN复合衬底的异质衬底上制造穿孔,然后将带有穿孔的GaN复合衬底浸没在金属镓与金属助溶剂的混合溶液中、并采用液相外延工艺生长得到GaN厚膜材料,在生长过程中,金属助溶剂通过异质衬底的穿孔与GaN外延层底面接触,一方面通过所述穿孔孔洞腐蚀与异质衬底相连的GaN外延层一面,促使生长形成的GaN厚膜材料与异质衬底缓慢分离,实现自分离,可制得高质量和大尺寸的GaN单晶衬底,另一方面,金属助溶剂与氮形成中间体,该中间体为金属镓提供氮元素而促使GaN单晶生长,应用于钠流法技术制备时,可有效改善钠流法制备技术中氮的溶解度低及不均匀的问题,从而提高GaN单晶的晶体质量与生长速率,减低工艺难度,易于控制及重复可靠性高。
附图说明
图1为本发明的制备流程结构示意图。
附图标记说明:1.GaN复合衬底,2.异质衬底,3.GaN外延层、31.界面层、4.穿孔、5.坩埚、6.金属镓与金属助溶剂的混合溶液、7.高压反应釜,8.GaN厚膜材料、9.GaN外延层与异质衬底界面层。
具体实施方式
下面将结合附图对本发明作进一步的说明。
参考图1,一种自分离制备GaN单晶衬底的方法,包括以下步骤:S1,在异质衬底2上制备GaN外延层3,以获得GaN复合衬底1;S2,在上述GaN复合衬底1的异质衬底2上穿孔4,所述穿孔4连接至GaN外延层3;S3,将步骤S2中有穿孔4的GaN复合衬底1置于装有金属镓与金属助溶剂的混合溶液6的坩埚5中,坩埚5置于高压反应釜7内;S4,在步骤S3中的高压反应釜7内通入高纯氮气,调整高压反应釜7内温度和压强,采用外延生长工艺生长GaN厚膜材料8,金属助溶剂通过所述穿孔4与GaN外延层3接触,异质衬底2和GaN厚膜材料8自分离,最终得到GaN单晶衬底;通过上述制备步骤,本实施例在GaN复合衬底1的异质衬底2上制造穿孔4,然后将带有穿孔4的GaN复合衬底1浸没在金属镓与金属助溶剂的混合溶液6中、并采用液相外延工艺生长得到GaN厚膜材料8,在晶体材料生长过程中,金属助溶剂通过异质衬底2的穿孔4与GaN外延层3底面接触,一方面通过穿孔4孔洞腐蚀与异质衬底2相连的GaN外延层3的界面层31,促使生长的GaN厚膜材料8与异质衬底2缓慢分离,实现自分离,得到高质量和大尺寸的GaN单晶衬底,另一方面,金属助溶剂与氮形成中间体,该中间体为金属镓与金属助溶剂混合溶液6提供氮元素而促使GaN单晶生长,应用钠流法技术制备时,可有效改善钠流法制备技术中氮的溶解度低及不均匀的问题,从而提高GaN单晶的晶体质量与生长速率。
图1示出,本实施例制备的GaN单晶衬底的流程为(a)到(d),其中图(a)中通过MOCVD工艺技术制备GaN复合衬底1,在异质衬底2为蓝宝石衬底上制备GaN外延层3,本实施例中的GaN外延层3为单层结构,GaN外延层3厚度为1-4微米;图(b)中采用激光辐射方式对异质衬底2进行穿孔4,所述穿孔4的形状为十字形,所述穿孔4的宽度设置为1毫米,所述穿孔4的深度穿透异质衬底2直至GaN外延层3,GaN外延层3与异质衬底2相连的界面层31刚好通过穿孔4裸露出;图(c)中将进行穿孔4加工后的GaN复合衬底1放入坩埚5中,坩埚5中充满金属镓和金属助溶剂的混合溶液6,金属助溶剂可为碱金属或碱土金属溶剂,优选地,金属助溶剂为金属钠助溶剂;图(d)中,坩埚5置于高压反应釜7中后,充入高纯氮气,密封后升温至900度,在继续补充氮气,使高压反应釜7腔内压力达到6MPa,并保持40小时,GaN外延层3外延生长,使GaN外延层3不断加厚得到GaN厚膜材料8,在晶体材料生长过程中,GaN外延层3与异质衬底2的界面层31的GaN材料通过所述穿孔4接触到金属镓和金属助溶剂的混合溶液6、并缓慢地被腐蚀分解,促使GaN厚膜材料8与异质衬底2慢慢地分离,从而最终得到高质量大尺寸的GaN单晶衬底,本实施例在高压反应釜7中可同时生长多片GaN厚膜材料8,生产效率以及源材料的利用率高,能有效降低生产成本,可实现产业化量产。
在其他实施例中,步骤S1中的GaN复合衬底1的制备方法可采用HVPE工艺制备,GaN外延层3可为GaN与InGaAlN缓冲层结合的多层结构,在步骤S2的异质衬底2上穿孔4的步骤中,还可采用机械化学穿孔4方式在异质衬底2上穿孔4,所述穿孔4的深度穿透异质衬底2直至GaN外延层3,使金属镓和金属助溶剂混合溶液6能够穿过异质衬底2与GaN外延层3一面接触,所述穿孔4的形状还可为但不限于圆形、方形、六角形、三角形、米字型和不规则形状的一种或多种,异质衬底2可为但不限于硅、SiC或金刚石材料的一种或多种,在高压反应釜7中可外延生长单片GaN厚膜材料8或多片GaN厚膜材料8同时生长,以得到单片或多片GaN单晶衬底,
上述实施例只是本发明的举例,但依照本发明原理,这还可以衍生出其它各种方案。其中只要涉及采用将GaN复合衬底的异质衬底实施穿孔,从而使GaN外延层加厚生长的同时,通过孔洞腐蚀GaN使其与异质衬底分离而得到GaN单晶衬底的方法与技术方案都包含在本发明范围内,均属于本发明的保护范围。因此,本发明专利的保护范围应以所附权利要求为准。
Claims (9)
1.一种自分离制备GaN单晶衬底的方法,其特征在于,包括以下步骤:
S1,在异质衬底上制备GaN外延层,以获得GaN复合衬底;
S2,在上述GaN复合衬底的异质衬底上穿孔,所述穿孔连接至GaN外延层;
S3,将步骤S2中有穿孔的GaN复合衬底置于装有金属镓与金属助溶剂混合溶液的坩埚中,坩埚置于高压反应釜内;
S4,在步骤S3中的高压反应釜内通入高纯氮气,调整高压反应釜内温度和压强,采用外延生长工艺生长GaN厚膜材料,金属助溶剂通过所述穿孔与GaN外延层接触,异质衬底和GaN厚膜材料自分离,最终得到GaN单晶衬底。
2.根据权利要求1所述的一种自分离制备GaN单晶衬底的方法,其特征在于,在步骤S2的异质衬底上穿孔的步骤中,所述穿孔的深度需穿透异质衬底直至GaN外延层。
3.根据权利要求1所述的一种自分离制备GaN单晶衬底的方法,其特征在于,在步骤S2的异质衬底上穿孔的步骤中,可采用激光辐射穿孔和机械化学穿孔的一种或多种的组合。
4.根据权利要求1所述的一种自分离制备GaN单晶衬底的方法,其特征在于,在步骤S2的异质衬底上穿孔的步骤中,所述穿孔的形状包括圆形、方形、六角形、三角形、十字形、米字型和不规则形状的一种或多种的组合。
5.根据权利要求1所述的一种自分离制备GaN单晶衬底的方法,其特征在于,在步骤S3的金属助溶剂可为碱金属或碱土金属溶剂。
6.根据权利要求1所述的一种自分离制备GaN单晶衬底的方法,其特征在于,在步骤S1的GaN复合衬底的制备可采用MOCVD工艺或HVPE工艺的一种或多种的组合。
7.根据权利要求1所述的一种自分离制备GaN单晶衬底的方法,其特征在于,所述异质衬底为蓝宝石、SiC、硅或金刚石材料的一种或多种。
8.根据权利要求1所述的一种自分离制备GaN单晶衬底的方法,其特征在于,GaN外延层可为GaN单层结构或GaN与InGaAlN缓冲层结合的多层结构。
9.根据权利要求1所述的一种自分离制备GaN单晶衬底的方法,其特征在于,在高压反应釜中可外延生长单片GaN厚膜材料或多片GaN厚膜材料同时生长,以得到单片或多片GaN单晶衬底。
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