CN117410374A - 一种溶液-凝胶法生长SiO2薄膜钝化GaAs纳米阵列的方法及应用 - Google Patents
一种溶液-凝胶法生长SiO2薄膜钝化GaAs纳米阵列的方法及应用 Download PDFInfo
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Abstract
本发明提供一种溶液‑凝胶法生长SiO2薄膜钝化GaAs纳米阵列的方法及应用，包括：步骤S1、将GaAs纳米阵列浸没至HF溶液中一段时间；步骤S2、将步骤S1处理后的GaAs纳米阵列浸入到一定浓度(NH4)2S溶液中一段时间，然后取出并用气体吹干；步骤S3、向步骤S2处理后的GaAs纳米阵列加入一定浓度的(NH4)2S溶液及溶液‑凝胶法生长SiO2薄膜的原料，搅拌下反应一段时间后洗涤干净。本发明的方法能保护表面原有的S端键，而且有利于缺陷的减少和悬空键的钝化。
Description
技术领域
本发明涉及半导体材料表面钝化技术领域，特别涉及一种溶液-凝胶法生长SiO2薄膜钝化GaAs纳米阵列的方法及应用。
背景技术
III-V族半导体材料凭借其卓越的电学和光学特性，在电子设备中发挥着关键且不可或缺的作用。其中，砷化镓(GaAs)凭借其高电子迁移率、直接带隙、高电子迁移率、高能带隙等独特性能，被广泛应用于光电器件、集成电路、太阳能电池、导航和通信***等各个领域。然而，GaAs表面往往表现出高密度的非辐射复合中心，尤其是对纳米尺寸器件更需要进行表面钝化。
常用的GaAs表面钝化方式包括使用含S和N的化学物质进行溶液钝化。其中，硫化已被证明通过形成S-端基键在去除半导体表面的本征氧化物和富含As元素方面非常有效。然而，当暴露在空气或水中时，这种终端仍不够稳定。因此，硫化之后通常通过沉积钝化薄膜来封装GaAs表面。此外，在沉积过程中，将洁净的GaAs表面暴露于热能和氧气等的等离子体中可能会破坏S-端基键，并再次对侧壁表面造成损害，对器件性能造成很大损伤。因此，如果没有适当封装的钝化薄膜，可能导致化学钝化稳定性急剧降低。
SiO2溶液-凝胶法制备薄膜已被证明在纳米柱阵列的钝化中非常有效，然而由于现有技术中样品长时间经S化处理后长时间暴露在水溶液中且经过不断搅拌使得原本生成的S端键断裂，样品表面重新被氧化，态密度增加，钝化效果变差。因此，当样品暴露于空气或水时，这种终端更加不稳定。因此需要对这种传统的溶液-凝胶法进行进一步优化。
发明内容
为克服现有技术中SiO2溶液-凝胶法所生长的薄膜在S溶液处理后会破坏原有表面，导致GaAs钝化效果不佳的问题，本发明提出一种溶液-凝胶法生长SiO2薄膜钝化GaAs纳米阵列的方法。
具体而言，本发明提供如下技术方案：
一种溶液-凝胶法生长SiO2薄膜钝化GaAs纳米阵列的方法，包括：
步骤S1、将GaAs纳米阵列浸没至HF溶液中一段时间；
步骤S2、将步骤S1处理后的GaAs纳米阵列浸入到一定浓度(NH4)2S溶液中一段时间，然后取出并用气体吹干；
步骤S3、向步骤S2处理后的GaAs纳米阵列加入一定浓度的(NH4)2S溶液及溶液-凝胶法生长SiO2薄膜的原料，搅拌下反应一段时间后洗涤干净。
可选地，步骤S1中，HF溶液浓度为3-10wt％，优选5wt％；浸没时间为5-15s，优选10s。通过HF溶液能去除GaAs纳米阵列表面的污渍，同时通过控制HF浓度与浸没时间，也能避免HF对GaAs纳米阵列造成破坏。
可选地，步骤S2具体为：取出步骤S1得到的GaAs纳米阵列，用去离子水洗涤，N2吹干后，浸入8-12wt％(NH4)2S溶液中5-15min，然后将GaAs纳米阵列取出并用N2吹干；(NH4)2S溶液浓度优选为10wt％，浸入时间优选为10min。
可选地，步骤S3具体为：将无水乙醇和去离子水的混合溶液倒入放置有GaAs纳米阵列的容器中，然后加入一定量CTAB并搅拌一段时间，随后依次加入NH4OH、(NH4)2S溶液和TEOS，室温下搅拌一段时间后，用去离子水和无水乙醇洗涤干净。步骤S2中(NH4)2S作用为钝化剂，而在步骤S3中则用作提供S氛围，防止溶胶-凝胶反应过程破坏S端键，因此步骤S2中所用(NH4)2S浓度要低于步骤S3的浓度。通过步骤S3，能避免现有技术中将样品长时间S化处理后长时间暴露于水溶液中且由于不断搅拌导致的S端键断裂，使得钝化效果变差。
可选地，步骤S3中原料比例为：无水乙醇∶去离子水∶NH4OH∶(NH4)2S∶TEOS＝40-45∶55-60∶0.2-0.4∶0.2-0.4∶0.04-0.08，优选比例为42∶58∶0.3∶0.3∶0.3∶0.06，以上比例为体积比。CTAB用量为原料总质量的0.1-0.3％。
可选地，NH4OH浓度为28-30wt％；(NH4)2S溶液为14wt％；步骤S3的反应条件为500rpm下搅拌1.5h。
进一步的，本发明还提供了一种SiO2薄膜钝化的GaAs纳米阵列。
进一步的，本发明还提供了SiO2薄膜钝化的GaAs纳米阵列在光电器件、集成电路、太阳能电池、导航和通信***领域的应用。
本发明提供的技术方案带来的有益效果至少包括：
本发明在S溶液钝化的基础上进一步在GaAs纳米阵列表面生长SiO2薄膜，有效去除表面氧化物并减少表面态；在SiO2溶液-凝胶法生长过程中加入硫化铵溶液以维持稳定氛围，采用这种方法制备的SiO2封装壳层，可以规避原有SiO2溶液-凝胶法的弊端，保护表面原有的S端键，而且SiO2的非晶化有利于缺陷的减少和悬空键的钝化。以溶液法生长替代干法镀膜，成本低，生长温度低，厚度均匀，PL提升效果明显。
附图说明
为了更清楚地说明本发明实施例中的技术方案，下面将对实施例描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。
图1为本发明溶液-凝胶法生长SiO2薄膜的原理示意图；
图2为GaAs纳米线上未添加(NH4)2S溶液时采用溶液-凝胶法生长的SiO2壳的形态和结构图，其中(a)为GaAs纳米线SEM图，(b)为GaAs纳米线生长SiO2壳后SEM图，(c)为生长时间为10分钟，标尺为100nm下的SiO2壳的纳米线TEM图像，(d)为生长时间为10分钟，标尺为50nm下的SiO2壳的纳米线TEM图像，(e)为生长时间为10分钟，标尺为20nm下的SiO2壳的纳米线TEM图像，(f)为SiO2与GaAs交界处的TEM图，(g)为生长时间为30分钟，标尺为200nm下的SiO2壳的纳米线TEM图像，(h)为生长时间为30分钟，标尺为100nm下的SiO2壳的纳米线TEM图像，(i)为生长时间为30分钟，标尺为50nm下的SiO2壳的纳米线TEM图像，(j)为生长时间为30分钟，EDS面扫图；
图3(a)为直径为1.8μm的GaAs纳米阵列经HF、钝化S处理和添加(NH4)2S溶液的SiO2溶胶-凝胶法生长钝化膜后，在室温下的PL光谱图；图3(b)为直径为1.8μm的GaAs纳米阵列经HF、钝化S处理和添加(NH4)2S溶液的SiO2溶胶-凝胶法生长钝化膜后的TRPL衰减曲线；图3(c)为直径分别为0.5μm、0.75μm、1μm和1.8μm的GaAs纳米柱阵列的归一化积分PL强度；图3(d)为直径分别为0.5μm、0.75μm、1μm和1.8μm的GaAs纳米柱阵列的载流子转移寿命直方图；
图4为为不同处理方式下的Ga 3d XPS光谱；其中(a)为ICP蚀刻后的GaAs晶片；(b)为仅经HF和(NH4)2S钝化处理后的样品；(c)为使用HF和(NH4)2S处理后采用未添加(NH4)2S的溶胶-凝胶法生长SiO2壳后的样品；(d)为使用HF和(NH4)2S处理后采用添加(NH4)2S的溶胶-凝胶法生长SiO2壳后的样品。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚，下面将结合附图及具体实施例对本发明的技术方案进行详细的描述。
实施例1
步骤S1、将刻蚀后的GaAs纳米阵列浸没在5％HF中10s；取出样品，用去离子水洗涤、N2吹干；
步骤S2、在室温条件下浸入使用14％的H2O中的硫化铵溶液制备的，10wt％的(NH4)2S稀释溶液中10分钟，然后将样品直接取出并用N2干燥；
步骤S3、最后将42ml无水乙醇(EtOH)和58ml去离子水的混合液倒入放置了样品的烧杯中，在室温下将0.1g CTAB倒入上述溶液并在500rpm的转速下搅拌5分钟，随后将0.3ml28-30％NH4OH溶液、0.3ml 14％(NH4)2S溶液和0.06ml TEOS溶液依次滴加到反应物中，将所得混合物在室温、500rpm转速下连续搅拌1.5小时。最后用去离子水和EtOH洗涤晶片数次，得到厚度约50nm的SiO2薄膜壳层。
对比例1
样品仅经过实施例1中的S1、S2步骤处理，之后未生长SiO2壳层。结果发现钝化效果虽然相对初始刻蚀后的GaAs样品具有一定钝化效果，但该效果不稳定，还需要进一步处理。
对比例2
其他条件于实施例1相同，不同之处在于步骤S3中在采用溶液-凝胶法生长SiO2壳时未加入(NH4)2S溶液。结果发现钝化效果相对实施例1及对比例1较差。
以上所述，仅为本发明的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，可轻易想到变化或替换，都应涵盖在本发明的保护范围之内。因此，本发明的保护范围应以所述权利要求的保护范围为准。
Claims (8)
1.一种溶液-凝胶法生长SiO2薄膜钝化GaAs纳米阵列的方法，其特征在于，包括：
步骤S1、将GaAs纳米阵列浸没至HF溶液中一段时间；
步骤S2、将步骤S1处理后的GaAs纳米阵列浸入到一定浓度(NH4)2S溶液中一段时间，然后取出并用气体吹干；
步骤S3、向步骤S2处理后的GaAs纳米阵列加入一定浓度的NH4)2S溶液及溶液-凝胶法生长SiO2薄膜的原料，搅拌下反应一段时间后洗涤干净。
2.根据权利要求1所述的方法，其特征在于，步骤S1中，HF溶液浓度为3-10wt％，优选5wt％；浸没时间为5-15s，优选10s。
3.根据权利要求1所述的方法，其特征在于，步骤S2具体为：取出步骤S1得到的GaAs纳米阵列，用去离子水洗涤，N2吹干后，浸入8-12wt％(NH4)2S溶液中5-15min，然后将GaAs纳米阵列取出并用N2吹干；(NH4)2S溶液浓度优选为10wt％，浸入时间优选为10min。
4.根据权利要求1所述的方法，其特征在于，步骤S3具体为：将无水乙醇和去离子水的混合溶液倒入放置有GaAs纳米阵列的容器中，然后加入一定量CTAB并搅拌一段时间，随后依次加入NH4OH、(NH4)2S溶液和TEOS，室温下搅拌一段时间后，用去离子水和无水乙醇洗涤干净。
5.根据权利要求1所述的方法，其特征在于，步骤S3中比例为：无水乙醇∶去离子水∶NH4OH∶(NH4)2S∶TEOS＝40-45∶55-60∶0.2-0.4∶0.2-0.4∶0.04-0.08，优选比例为42∶58∶0.3∶0.3∶0.3∶0.06；CTAB用量为原料总质量的0.1-0.3％。
6.根据权利要求5所述的方法，其特征在于，NH4OH浓度为28-30wt％；(NH4)2S溶液为14wt％；步骤S3中在500rpm下搅拌1.5h。
7.一种权利要求1-6任一项所述方法制备得到的SiO2薄膜钝化的GaAs纳米阵列。
8.权利要求7所述的SiO2薄膜钝化的GaAs纳米阵列在光电器件、集成电路、太阳能电池、导航和通信***领域的应用。
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