CN110534555A - 基于r面Al2O3图形衬底的β-Ga2O3薄膜制作方法 - Google Patents
基于r面Al2O3图形衬底的β-Ga2O3薄膜制作方法 Download PDFInfo
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- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 claims abstract description 46
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 45
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- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 11
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- 229910052760 oxygen Inorganic materials 0.000 claims description 11
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Abstract
本发明公开了一种基于r面Al2O3衬底的β‑Ga2O3薄膜，主要解决现有技术薄膜位错密度高，薄膜质量差，器件迁移率低的问题。其自下而上包括：200‑500um厚的Al2O3衬底层(1)、30‑110nm厚的β‑Ga2O3成核层(2)、200‑3000nm厚的(‑201)面β‑Ga2O3层(3)，其中衬底层采用r面Al2O3衬底且该衬底表面设有通过金刚石砂纸打磨形成的锯齿状条纹。本发明降低了β‑Ga2O3薄膜位错密度，减小极化效应，有效提升了器件迁移率，改善了制备的Ga2O3薄膜质量，可用于制作高电子迁移率晶体管，发光二极管半导体器件。
Description
技术领域
本发明属于微电子技术领域，特别涉及一种β-Ga2O3薄膜的制作方法，可用于制作高电子迁移率晶体管，发光二极管半导体器件。
技术背景
作为第三代半导体材料的Ga203因其独特的电学和光学性质已成为当前研究的热点。Ga203含有五种同分异构体，其中β-Ga203是五种同分异构体中最为稳定的一种。β-Ga2O3的光学带隙区间为4.2-4.9eV，其吸收边处在240-280nm的区间内，在可见光波段及紫外光波段，β-Ga2O3具有较高透射率，相比与传统的透明导电薄膜材料，β-Ga2O3在深紫外波段更具优势，是制作紫外发光器件最佳的透明导电电极材料，同时在半导体功率器件领域，相比于近些年研究相对热门的氮化镓和碳化硅材料，Ga2O3在带隙、击穿电场和巴利加优值参数上都更具备优势，相应的研究也取得了巨大进展。但是高质量的Ga2O3薄膜极其难生长，许多研究者采用了不同的方法进行技术处理，Alema等人报道了提供不同Ga源在c面Al2O3衬底上外延生长β-Ga2O3薄膜，Zhou等人研究通过调整成核层温度改善在c面Al2O3上生长的β-Ga2O3薄膜的质量。参见Fast growth rate of epitaxialβ–Ga2O3by close coupledshowerhead MOCVD,J.Cryst.Growth 475,77(2017)和Structural properties of Si-dopedβ-Ga2O3layers grown by MOVPE，,J.Cryst.Growth 401,665(2014)。但是这些技术处理得到的薄膜位错密度依然较高，导致制备出的器件迁移率较低，距离实际应用的要求差距较大，限制了高性能器件的发展。
发明内容
本发明的目的在于克服上述已有技术的不足，提供一种基于r面Al2O3图形衬底的Ga2O3薄膜及其制备方法，以降低位错密度，，有效提升器件迁移率，提升制备的Ga2O3薄膜质量。
为实现上述目的，本发明基于r面Al2O3图形衬底的Ga2O3薄膜，自下而上包括：衬底层、β-Ga2O3成核层和(-201)面β-Ga2O3层，
进一步，所述β-Ga2O3成核层的厚度为30-110nm。
进一步所述(-201)面β-Ga2O3层的厚度为200-1500nm。
进一步所述r面Al2O3衬底的厚度为200-500um。
为实现上述目的，本发明基于r面Al2O3图形衬底的β-Ga2O3薄膜的制备方法，包括如下步骤：
1)将r面Al2O3衬底水平放置，将金刚石砂纸放置在衬底表面，在金刚石砂纸上施加5-15牛顿的力对r面Al2O3衬底进行平行打磨，打磨出平行于Al2O3衬底基准边的条纹图案或垂直于Al2O3衬底基准边的锯齿状条纹图案；
2)将打磨后的r面Al2O3衬底先放入HF酸或HCl酸中超声波清洗3-15min，然后依次放入丙酮溶液、无水乙醇溶液和离子水中超声清洗3-15min，最后用氮气吹干；
3)将清洗后的r面Al2O3衬底置于金属有机物化学气相淀积MOCVD反应室中，再抽真空将反应室的真空度降低到小于2×10-2Torr；然后向反应室通入氢气，在MOCVD反应室压力达到为20-780Torr条件下，将衬底加热到温度为950-1150℃，并保持6-11min，完成对衬底基片的热处理；
4)在经过热处理后的r面Al2O3衬底上采用金属有机物化学气相淀积MOCVD工艺生长厚度为30-110nm的β-Ga2O3成核层；
5)在β-Ga2O3成核层上采用金属有机物化学气相淀积MOCVD工艺生长厚度为200-3000nm的(-201)面β-G2O3层，完成薄膜制作。
本发明具有如下优点：
1.本发明由于在r面Al2O3衬底上通过金刚石砂纸上打磨出平行基准边方向或垂直基准边方向的条纹图案来制备图形衬底，提高了材料质量、简化了工艺、缩短了制作周期并且降低了成本。
2.本发明由于采用了r面Al2O3衬底，可以最大程度减小Ga2O3薄膜的面内各向异性，相较于传统的c面Al2O3衬底优势巨大。
附图说明
图1是本发明Ga2O3薄膜剖面示意图；
图2是本发明中金刚石砂纸打磨r面Al2O3图形衬底示意图；
图3是本发明制作Ga2O3薄膜的实现流程图。
具体实施方式
以下结合附图对本发明作进一步详细描述：
参照图1，本发明的Ga2O3薄膜，包括：r面Al2O3衬底层1、β-Ga2O3成核层2、和(-201)面β-Ga2O3层3。
所述r面Al2O3衬底层1，厚度为200-500um，其表面有通过金刚石砂纸打磨形成的锯齿状衬底条纹，如图2所示，该衬底条纹为平行于Al2O3衬底基准边或垂直于Al2O3衬底基准边，以利于后续β-Ga2O3的成核过程，有效降低β-Ga2O3成核层2位错密度，提升β-Ga2O3成核层2质量；
所述成核层2，用于为后续(-201)面β-Ga2O3层3提供良好的基础，其位于r面Al2O3衬底层1之上，厚度为30-110nm；
所述(-201)面β-Ga2O3层3，其位于β-Ga2O3成核层2之上，厚度为200-3000nm。
参照图3，本发明给出制备Ga2O3薄膜的三种实施例。
实施例1，制备β-Ga2O3成核层厚度为30nm，(-201)面β-Ga2O3层厚度为200nm的基于r面Al2O3图形衬底的Ga2O3薄膜。
步骤1，对r面Al2O3衬底进行磨制。
将r面Al2O3衬底水平放置，选择颗粒直径为5um石砂纸，将其放置在衬底表面，并施加5牛顿的力，使砂纸沿平行于Al2O3衬底的基准边打磨，在Al2O3衬底上磨出锯齿状的条纹图案，如图2所示。
步骤2，对磨制好的Al2O3衬底进行清洗。
将经过打磨的r面Al2O3衬底先放入HF酸中超声波清洗3min，然后依次在丙酮溶液、无水乙醇溶液和离子水中分别进行超声波清洗3min，最后用氮气吹干。
步骤3，对衬底基片进行热处理。
将r面Al2O3衬底置于金属有机物化学气相淀积MOCVD反应室中，先抽真空将反应室的真空度降低到小于2×10-2Torr，然后向反应室通入氢气，使反应室压力为20Torr，将衬底加热到950℃，对衬底基片进行6min的热处理。
步骤4，生长30nm厚的β-Ga2O3成核层。
将热处理后的衬底温度保持在1100℃，再同时向反应室通入不同流量的镓源、氧源。在保持压力为20Torr的条件下，生长厚度为30nm的β-Ga2O3成核层，其中镓源TMGa的流量为30μmol/min、氧气的流量为1500sccm。
步骤5，生长200nm厚的Ga2O3层。
将已经生长了β-Ga2O3成核层的衬底温度保持在1000℃，向反应室同时通入流量为10μmol/min的镓源、流量为1500sccm的氧气，在保持压力为20Torr的条件下生长200nm厚的(-201)面β-Ga2O3层。
步骤6，将通过上述过程生长的Ga2O3薄膜从MOCVD反应室中取出，完成Ga2O3薄膜的制备。
实施例2，制备β-Ga2O3成核层厚度为70nm，(-201)面β-Ga2O3层厚度为1000nm的基于r面Al2O3图形衬底的Ga2O3薄膜。。
步骤一，对r面Al2O3衬底进行磨制。
将r面Al2O3衬底水平放置，选择颗粒直径为7um的金刚石砂纸，将其放置在衬底表面，并施加的10牛顿的力，使砂纸沿垂直于Al2O3衬底的基准边打磨，在Al2O3衬底上磨出锯齿状的条纹图案，如图2所示。
步骤二，对磨制好的Al2O3衬底进行清洗。
本步骤具体实施与实施例一的步骤2相同。
步骤三，对衬底基片进行热处理。
3.1)将r面Al2O3衬底置于金属有机物化学气相淀积MOCVD反应室中，抽真空将反应室的真空度降低到小于2×10-2Torr；
3.2)向反应室通入氢气，使反应室压力达到60Torr，再将衬底加热到1000℃，对衬底基片进行时间为10min的热处理。
步骤四，生长70nm厚的β-Ga2O3成核层。
4.1)将热处理后的衬底温度升高到1050℃，保持反应室压力为60Torr；
4.2)向反应室通入不同流量的铝源、氢气和氧气，其中镓源的流量为30μmol/min、氢气的流量为1150sccm和氧气的流量为2500sccm，生长厚度为70nm的β-Ga2O3成核层。
步骤五，在β-Ga2O3成核层上生长1000nm厚的(-201)面β-Ga2O3层。
5.1)将已经生长了β-Ga2O3成核层的衬底温度降低为1050℃；
5.2)在保持压力为20Torr的条件下，向反应室同时通入流量为60μmol/min的源镓，流量为1150sccm的氢气和流量为2500sccm的氧气，在β-Ga2O3成核层上生长出厚度为1000nm的(-201)面β-Ga2O3层。
步骤六，将通过上述过程生长的Ga2O3薄膜从MOCVD反应室中取出，完成Ga2O3薄膜的制备。
实施例3，制备β-Ga2O3成核层厚度为110nm，(-201)面β-Ga2O3厚度为3000nm的基于r面Al2O3图形衬底的Ga2O3薄膜。
步骤A，将r面Al2O3衬底水平放置，选择颗粒直径为15um的金刚石砂纸，将其放置在衬底表面，并施加的15牛顿的力，使砂纸沿平行于Al2O3衬底的基准边打磨，在Al2O3衬底上磨出锯齿状的条纹图案，如图2所示。
步骤B，将经过打磨的r面Al2O3衬底先放入HCl酸中超声波清洗15min，然后依次在丙酮溶液、无水乙醇溶液和离子水中分别超声波清洗15min，最后用氮气吹干。
步骤C，将r面Al2O3衬底置于金属有机物化学气相淀积MOCVD反应室中，先抽真空将反应室的真空度降低到小于2×10-2Torr，然后向反应室通入氢气与氨气的混合气体，使反应室压力为780Torr，再将衬底加热到1150℃，对衬底基片进行11min的热处理。
步骤D，将热处理后的衬底温度保持在1150℃，再同时向反应室通入镓源、氢气和氧气，在保持压力为780Torr的条件下生长厚度为110nm的β-Ga2O3成核层，其中镓源的流量为60μmol/min、氢气的流量为1150sccm和氧气的流量为4500sccm。
步骤E，将已经生长了β-Ga2O3成核层的衬底温度降低为1100℃，在保持压力为780Torr的条件下，向反应室同时通入流量为150μmol/min的镓源、流量为1150sccm氢气和流量为5500sccm的氧气，在保持压力为780Torr的条件下，生长厚度为3000nm的(-201)面β-Ga2O3层。
步骤F，将通过上述过程生长的Ga2O3材料从MOCVD反应室中取出，完成Ga2O3薄膜的制备。
以上描述仅是本发明的三个具体实例，不构成对本发明的任何限制，显然对于本领域的专业人员来说，在了解本发明内容和原理后，都可能在不背离本发明的原理、结构的情况下，进行形式和细节上的各种修正和改变，但是这些基于本发明思想的修正和改变仍在本发明的权利要求保护范围之内。
Claims (8)
1.一种基于r面Al2O3图形衬底的β-Ga2O3薄膜，自下而上包括：衬底层(1)、β-Ga2O3成核层(2)和(-201)面β-Ga2O3层(3)，其特征在于：
衬底层(1)采用r面Al2O3衬底，用以减小β-Ga2O3薄膜的面内各向异性，提高Ga2O3薄膜材料的质量；该r面Al2O3衬底表面设有通过金刚石砂纸打磨形成的锯齿状衬底条纹，用以提高β-Ga2O3成核层(2)的质量。
2.根据权利要求1所述的薄膜，其特征在于：所述β-Ga2O3成核层(2)的厚度为30-110nm。
3.根据权利要求1所述的薄膜，其特征在于：所述(-201)面β-Ga2O3层(3)的厚度为200-1500nm。
4.根据权利要求1所述的薄膜，其特征在于：r面Al2O3衬底的厚度为200-500um。
5.一种基于r面Al2O3图形衬底的β-Ga2O3薄膜制备方法，其特征在于，包括如下步骤：
1)将r面Al2O3衬底水平放置，将金刚石砂纸放置在衬底表面，在金刚石砂纸上施加5-15牛顿的力对r面Al2O3衬底进行平行打磨，打磨出平行于Al2O3衬底基准边的条纹图案或垂直于Al2O3衬底基准边的锯齿状条纹图案；
2)将打磨后的r面Al2O3衬底先放入HF酸或HCl酸中超声波清洗3-15min，然后依次放入丙酮溶液、无水乙醇溶液和离子水中超声清洗3-15min，最后用氮气吹干；
3)将清洗后的r面Al2O3衬底置于金属有机物化学气相淀积MOCVD反应室中，再抽真空将反应室的真空度降低到小于2×102Torr；然后向反应室通入氢气，在MOCVD反应室压力达到为20-780Torr条件下，将衬底加热到温度为950-1150℃，并保持6-11min，完成对衬底基片的热处理；
4)在经过热处理后的r面Al2O3衬底上采用金属有机物化学气相淀积MOCVD工艺生长厚度为30-110nm的β-Ga2O3成核层；
5)在β-Ga2O3成核层上采用金属有机物化学气相淀积MOCVD工艺生长厚度为200-3000nm的(-201)面β-G2O3层，完成薄膜制作。
6.根据权利要求5所述的方法，其中步骤(1)的金刚石砂纸，采用颗粒直径为5-15um的砂纸。
7.根据权利要求5所述的方法，其中步骤4中采用MOCVD工艺生长β-Ga2O3成核层的工艺条件如下：
反应室压力为20-780Torr，
温度为1050-1150℃，
镓源流量为30-60μmol/min，
氢气流量为1150sccm，
氧气流量为1500-4500sccm。
8.根据权利要求5所述的方法，其中步骤5采用MOCVD工艺生长(-201)面β-Ga2O3层的工艺条件如下：
反应室压力为20-780Torr，
温度为1000-1100℃，
镓源流量为10-150μmol/min，
氧气流量为1500-5500sccm。
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