CN113871493A - 基于原子层沉积技术的铝掺杂氧化钛薄膜及其制备方法 - Google Patents

基于原子层沉积技术的铝掺杂氧化钛薄膜及其制备方法 Download PDF

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CN113871493A
CN113871493A CN202111083954.XA CN202111083954A CN113871493A CN 113871493 A CN113871493 A CN 113871493A CN 202111083954 A CN202111083954 A CN 202111083954A CN 113871493 A CN113871493 A CN 113871493A
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宋晓敏
刘莹
黄增光
童锐
尹海鹏
顾裕华
张颖
钱宇昂
程浩
张丽娟
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Abstract

本发明公开了一种基于原子层沉积技术的铝掺杂氧化钛薄膜及其制备方法，该方法将原硅片进行RCA标准工艺清洗；将硅片放入ALD腔室中，基底温度150℃，腔室抽真空；ALD腔室通入三甲基铝，开阀时间16ms，抽真空25s后通入H2O，开阀时间8ms，抽真空30s，硅片表面形成1层Al2O3；向腔室通入四（二甲胺基）钛，开阀时间180ms，抽真空25s后通入H2O，开阀时间8ms，抽真空30s，硅片表面形成1层Al2O3和5层TiO2薄膜。本发明利用ALD技术，将Al引入TiO2薄膜中，这种薄膜同时具有优异的导电性和钝化性，将其应用在PERC太阳电池上，获得的转化效率优于应用了未掺杂的TiO2薄膜。

Description

基于原子层沉积技术的铝掺杂氧化钛薄膜及其制备方法
技术领域
本发明涉及新能源技术领域，特别涉及一种基于原子层沉积技术的铝掺杂氧化钛薄膜及其制备方法。
背景技术
晶硅表面有大量由于晶体周期性被破坏而产生的悬挂键，使硅片表面存在大量的缺陷能级；并且位错，表面金属污染，化学残留物都会引入缺陷能级，因此硅表面会成为复合中心。为了减少表面悬挂键，降低表面复合速率，引入了各种各样的钝化层。研究最多的硅表面钝化介质是。目前，适用于光伏的电介质包括二氧化硅(SiO2)，氮化硅(SiNx)1，非晶氮化硅(a-SiNx:H)2,3，SiO2/a-SiNx:H叠层4，氧化铝(Al2O3)薄膜5–7或AlOx/SiNx叠层8,9等。目前，市场主流的钝化发射极和背面（PERC）太阳电池背面叠层钝化膜以Al2O3/SiNx叠层为主，但由于两层膜皆是绝缘膜，所以需要通过激光开窗，将钝化膜破开，再进行丝网印刷或者蒸镀电极，形成局域线或点接触。
但是背面需要局部开孔的PERC电池在金属接触区仍有复合损失，为解决这一问题，并去除背面开孔工艺，一种新型的技术：载流子选择性接触（CSCs）技术成为近年来研究的热点。CSCs的本质是利用载流子电导率的强不对称性，选择性地通过一种载流子并对硅提供钝化。最常见的方法是使用高度掺杂的硅结合界面钝化层，该钝化层足够薄以允许多数载流子传输。传统载流子选择性接触技术方案是：以单晶硅为基底，利用硝酸湿法氧化出一层1~2 nm左右的极薄氧化硅层，再利用PECVD（等离子体加强的化学气相沉积）在氧化层表面沉积一层20 nm掺杂的微晶非晶混合Si薄膜。这层混合Si薄膜需通过850℃退火，由微晶非晶转变为多晶以激活其钝化性能。但是这种方法容易造成俄歇复合和寄生吸收等问题。主要原因是，掺杂的多晶硅会吸收一部分的光子，即寄生吸收；掺杂剂扩散到下面的硅衬底中导致俄歇复合，且期间用到的PECVD危险性高，需高温退火。
因此，一种透明导电薄膜同时能钝化硅基底引起了科研人员的广泛关注。
发明内容
本发明所要解决的技术问题是针对现有技术的不足，提供一种设计合理，提高TiO2薄膜的钝化性和导电性，降低电池制备过程中对激光开窗的依赖，基于原子层沉积技术的铝掺杂氧化钛薄膜。
本发明所要解决的另一技术问题是针对现有技术的不足，提供一种上述铝掺杂氧化钛薄膜的制备方法。
为了实现上述目的，本发明采用了如下技术方案：
一种基于原子层沉积技术的铝掺杂氧化钛薄膜，其特点是，该薄膜包括作为基底的硅片，硅片上方至少设有一层铝掺杂氧化钛层，每层铝掺杂氧化钛层均由Al2O3薄膜层和若干TiO2薄膜层组成，Al2O3薄膜层设在TiO2薄膜层下方。
本发明所要解决的技术问题还可以通过以下技术方案实现，所述硅片采用n型（100）面切割、50×50 mm2尺寸、Fz硅片，硅片厚度285±10 μm，电阻率为3 Ωcm。
一种权利要求1或2所述铝掺杂氧化钛薄膜的制备方法，其特点是，具体步骤如下，
（1）将硅片进行RCA标准工艺清洗；
（2）将清洗好的硅片放入ALD腔室中，基底温度设置在150℃，腔室抽真空；
（3）打开三甲基铝源瓶快阀，向ALD腔室通入三甲基铝，开阀时间10ms-20ms后，关闭三甲基铝源瓶快阀，将ALD腔室抽真空20s-30s后，打开H2O源瓶快阀，开阀时间5ms-10ms，关闭水源瓶快阀，再次将ALD腔室抽真空20s-40s，此时，硅片表面形成1层Al2O3薄膜；
（4）打开四（二甲胺基）钛源瓶快阀，向腔室通入四（二甲胺基）钛，开阀时间150ms-200ms后，关闭四（二甲胺基）钛源瓶快阀，将ALD腔室抽真空20-30s后，打开H2O源瓶快阀，开阀时间8ms，关闭水源瓶快阀，再次将ALD腔室抽真空20-40s，此时，在覆有一层Al2O3薄膜的硅片表面形成有一层TiO2薄膜，从而制得Al掺杂TiO2薄膜。
本发明所要解决的技术问题还可以通过以下技术方案实现，所述Al掺杂TiO2薄膜中的Al : Ti比例为1:5，其制备方法为，先按步骤（1）-（4）制得含有一层Al2O3薄膜和一层TiO2薄膜的产品，接着按步骤（4）重复5次，从而制得含有一层Al2O3薄膜和五层TiO2薄膜的产品，再按步骤（3）-（4）重复40次，制得厚度为16.5nm的比例为1:5的Al掺杂TiO2薄膜。
本发明所要解决的技术问题还可以通过以下技术方案实现，所述三甲基铝源瓶内的温度为常温，所述水源瓶内的温度为42℃，所述四（二甲胺基）钛源瓶内的温度为85℃。
本发明所要解决的技术问题还可以通过以下技术方案实现，具体步骤如下，
（1）将硅片进行RCA标准工艺清洗；
（2）将清洗好的硅片放入ALD腔室中，基底温度设置在150℃，腔室抽真空；
（3）打开三甲基铝源瓶快阀，向ALD腔室通入三甲基铝，开阀时间16ms后，关闭三甲基铝源瓶快阀，将ALD腔室抽真空25s后，打开H2O源瓶快阀，开阀时间8ms，关闭水源瓶快阀，再次将ALD腔室抽真空30s，此时，硅片表面形成1层Al2O3薄膜；
（4）打开四（二甲胺基）钛源瓶快阀，向腔室通入四（二甲胺基）钛，开阀时间180ms后，关闭四（二甲胺基）钛源瓶快阀，将ALD腔室抽真空25s后，打开H2O源瓶快阀，开阀时间8ms，关闭水源瓶快阀，再次将ALD腔室抽真空30s，此时，在覆有一层Al2O3薄膜的硅片表面形成有一层TiO2薄膜，从而制得Al掺杂TiO2薄膜。
与现有技术相比，本发明通过ALD沉积技术，将Al引入TiO2薄膜中，这种新型的Al掺杂TiO2（ATO）薄膜应用在单晶硅上，最终成功获得了 1.9 ms 超高有效少数载流子寿命(τeff) 和 0.1Ω•cm2 的低接触电阻率 (ρc)，这意味着Al的掺杂同时提高了薄膜的钝化和导电性。得益于该薄膜光学和电学性能的改进，将其应用的PERC太阳电池的发光面上，获得的冠军电池转换效率21.4%，短路电流密度39.2 mA·cm-2，开路电压0.679V，填充因子80.5%，明显优于应用了未掺杂TiO2的PERC电池。
附图说明
图1中，a) 横截面 TEM 图像；
b) EDS 元素映射（Si、Ti、Al 和 P 元素）；
c) HAADF-STEM 显微镜图像以及 c-Si/SiOx/ATO(Al:Ti=1:5)/Pt 界面的 EDS线扫描；
图2为应用ATO薄膜的PERC太阳电池示意图；
图3为应用ATO或TiO2薄膜的 PERC 太阳电池的 I-V 和 P-V 曲线图；
图4为应用ATO薄膜，效率为21.4%的冠军太阳电池的I-V 和 P-V 曲线，（c）照片和（d）PL 图像图。
具体实施方式
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。
在本发明的描述中，需要理解的是，术语“上”、“下”、“前”、“后”、“左”、“右”、“顶”、“底”、“内”、“外”等指示的方位或位置关系为基于附图所示的方位或位置关系，仅是为了便于描述本发明和简化描述，而不是指示或暗示所指的装置或元件必须具有特定的方位、以特定的方位构造和操作，因此不能理解为对本发明的限制。
实施例1，参照图1-4，一种基于原子层沉积技术的铝掺杂氧化钛薄膜，该薄膜包括作为基底的硅片，硅片上方至少设有一层铝掺杂氧化钛层，每层铝掺杂氧化钛层均由Al2O3薄膜层和若干TiO2薄膜层组成，Al2O3薄膜层设在TiO2薄膜层下方，以Al : Ti比例为1:5，每层铝掺杂氧化钛层由一层Al2O3薄膜层和五层TiO2薄膜层组成，再根据铝掺杂氧化钛薄膜的厚度要求，在硅片上方连续设置40层铝掺杂氧化钛层，采用n型（100）面切割的、50×50 mm2尺寸（赝平方）、Fz硅片，硅片厚度285±10 μm，电阻率大约在3 Ωcm；
参照图2，应用本发明所述铝掺杂氧化钛薄膜的PERC太阳电池的结构为，从下至上依次设置有背接触板、SiNX覆盖层、AlOX纯化层、P型硅、n+发射极、本发明所述铝掺杂氧化钛薄膜、SiNX减反膜、前表面接触层。
实施例2，一种上述铝掺杂氧化钛薄膜的制备方法，具体步骤如下，
（1）将硅片进行RCA标准工艺清洗；
（2）将清洗好的硅片放入ALD腔室（指原子层沉积设备中的腔室）中，基底温度设置在150℃，腔室抽真空；
（3）三甲基铝源瓶内的温度为常温，打开三甲基铝源瓶快阀，向ALD腔室通入三甲基铝，开阀时间16ms后，关闭三甲基铝源瓶快阀，将ALD腔室抽真空25s后，打开H2O源瓶快阀，开阀时间8ms，关闭水源瓶快阀，再次将ALD腔室抽真空30s，此时，硅片表面形成1层Al2O3薄膜，所述水源瓶内的温度为42℃；
（4）打开四（二甲胺基）钛源瓶快阀，向腔室通入四（二甲胺基）钛，开阀时间180ms后，关闭四（二甲胺基）钛源瓶快阀，将ALD腔室抽真空25s后，打开H2O源瓶快阀，开阀时间8ms，关闭水源瓶快阀，再次将ALD腔室抽真空30s，此时，在覆有一层Al2O3薄膜的硅片表面形成有一层TiO2薄膜，从而制得Al掺杂TiO2薄膜，所述四（二甲胺基）钛源瓶内的温度为85℃。
实施例3，一种上述铝掺杂氧化钛薄膜的制备方法，具体步骤如下，
（1）将硅片进行RCA标准工艺清洗；
（2）将清洗好的硅片放入ALD腔室中，基底温度设置在150℃，腔室抽真空；
（3）打开三甲基铝源瓶快阀，向ALD腔室通入三甲基铝，开阀时间10ms后，关闭三甲基铝源瓶快阀，将ALD腔室抽真空20s后，打开H2O源瓶快阀，开阀时间5ms，关闭水源瓶快阀，再次将ALD腔室抽真空20s，此时，硅片表面形成1层Al2O3薄膜；
（4）打开四（二甲胺基）钛源瓶快阀，向腔室通入四（二甲胺基）钛，开阀时间150ms后，关闭四（二甲胺基）钛源瓶快阀，将ALD腔室抽真空20s后，打开H2O源瓶快阀，开阀时间5ms，关闭水源瓶快阀，再次将ALD腔室抽真空20-40s，此时，在覆有一层Al2O3薄膜的硅片表面形成有一层TiO2薄膜，从而制得Al掺杂TiO2薄膜。
实施例4，一种上述铝掺杂氧化钛薄膜的制备方法，具体步骤如下，
（1）将硅片进行RCA标准工艺清洗；
（2）将清洗好的硅片放入ALD腔室中，基底温度设置在150℃，腔室抽真空；
（3）打开三甲基铝源瓶快阀，向ALD腔室通入三甲基铝，开阀时间10ms-20ms后，关闭三甲基铝源瓶快阀，将ALD腔室抽真空30s后，打开H2O源瓶快阀，开阀时间10ms，关闭水源瓶快阀，再次将ALD腔室抽真空20s-40s，此时，硅片表面形成1层Al2O3薄膜；
（4）打开四（二甲胺基）钛源瓶快阀，向腔室通入四（二甲胺基）钛，开阀时间200ms后，关闭四（二甲胺基）钛源瓶快阀，将ALD腔室抽真空30s后，打开H2O源瓶快阀，开阀时间10ms，关闭水源瓶快阀，再次将ALD腔室抽真空40s，此时，在覆有一层Al2O3薄膜的硅片表面形成有一层TiO2薄膜，从而制得Al掺杂TiO2薄膜。
以Al : Ti比例为1:5，其制备方法为，先按步骤（1）-（4）制得含有一层Al2O3薄膜和一层TiO2薄膜的产品，接着按步骤（4）重复5次，从而制得含有一层Al2O3薄膜和五层TiO2薄膜的产品，再按步骤（3）-（4）重复40次，制得厚度为16.5nm的比例为1:5的Al掺杂TiO2薄膜。
由于氧化钛（TiO2）薄膜与硅之间存在小导带带阶和大价带带阶，使TiO2有望成为选择性接触薄膜。但是，目前还没有同时具有优异的导电性和钝化性的TiO2薄膜。而向半导体内引入掺杂剂以改变该材料特性（例如，带隙，功函数，电荷载流子复合率和电导率）是较为常见的改性方式10,11。为了提高TiO2薄膜的性能，考虑引入金属离子掺杂，在TiO2的晶格中引入缺陷，形成缺陷能级，形成光生电子-空穴的浅势捕获阱，从而延长电子空穴对的复合时间，并且使TiO2的带隙宽度变窄，提高长波段可见光的吸收。
原子层沉积（Atomic layer deposition，ALD）是一种基于气态前驱体在基底表面发生化学吸附的纳米薄膜沉积技术，通过自限制性的前驱体交替饱和反应获得厚度、组分、形貌及结构在纳米尺度上高度可控的薄膜。该方法将物质以单原子膜的形式一层一层镀在基底表面的方法。采用ALD制备的薄膜具有高致密性（无针孔）、高保形性及大面积均匀性等优异性能，这对薄膜的使用具有重要的实际意义。
以上所述，仅为本发明较佳的具体实施方式，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，根据本发明的技术方案及其发明构思加以等同替换或改变，都应涵盖在本发明的保护范围之内。

Claims (6)

1.一种基于原子层沉积技术的铝掺杂氧化钛薄膜，其特征在于，该薄膜包括作为基底的硅片，硅片上方至少设有一层铝掺杂氧化钛层，每层铝掺杂氧化钛层均由Al2O3薄膜层和TiO2薄膜层组成。
2.根据权利要求1所述的一种基于原子层沉积技术的铝掺杂氧化钛薄膜，其特征在于，所述硅片采用n型（100）面切割、50×50 mm2尺寸、Fz硅片，硅片厚度285±10 μm，电阻率为3Ωcm。
3.一种权利要求1或2所述铝掺杂氧化钛薄膜的制备方法，其特征在于，具体步骤如下，
（1）将硅片进行RCA标准工艺清洗；
（2）将清洗好的硅片放入ALD腔室中，基底温度设置在150℃，腔室抽真空；
（3）打开三甲基铝源瓶快阀，向ALD腔室通入三甲基铝，开阀时间10ms-20ms后，关闭三甲基铝源瓶快阀，将ALD腔室抽真空20s-30s后，打开H2O源瓶快阀，开阀时间5ms-10ms，关闭水源瓶快阀，再次将ALD腔室抽真空20s-40s，此时，硅片表面形成1层Al2O3薄膜；
（4）打开四（二甲胺基）钛源瓶快阀，向腔室通入四（二甲胺基）钛，开阀时间150ms-200ms后，关闭四（二甲胺基）钛源瓶快阀，将ALD腔室抽真空20-30s后，打开H2O源瓶快阀，开阀时间5-10ms，关闭水源瓶快阀，再次将ALD腔室抽真空20-40s，此时，在覆有一层Al2O3薄膜的硅片表面形成有一层TiO2薄膜，从而制得Al掺杂TiO2薄膜。
4.根据权利要求3所述的一种铝掺杂氧化钛薄膜的制备方法，其特征在于，所述Al掺杂TiO2薄膜中的Al : Ti比例为1:5，其制备方法为，先按步骤（1）-（4）制得含有一层Al2O3薄膜和一层TiO2薄膜的产品，接着按步骤（4）重复5次，从而制得含有一层Al2O3薄膜和五层TiO2薄膜的产品，再按步骤（3）-（4）重复40次，制得厚度为16.5nm的比例为1:5的Al掺杂TiO2薄膜。
5.根据权利要求3所述的一种铝掺杂氧化钛薄膜的制备方法，其特征在于，所述三甲基铝源瓶内的温度为常温，所述水源瓶内的温度为42℃，所述四（二甲胺基）钛源瓶内的温度为85℃。
6.根据权利要求3所述的一种铝掺杂氧化钛薄膜的制备方法，其特征在于，具体步骤如下，
（1）将硅片进行RCA标准工艺清洗；
（2）将清洗好的硅片放入ALD腔室中，基底温度设置在150℃，腔室抽真空；
（3）打开三甲基铝源瓶快阀，向ALD腔室通入三甲基铝，开阀时间16ms后，关闭三甲基铝源瓶快阀，将ALD腔室抽真空25s后，打开H2O源瓶快阀，开阀时间8ms，关闭水源瓶快阀，再次将ALD腔室抽真空30s，此时，硅片表面形成1层Al2O3薄膜；
（4）打开四（二甲胺基）钛源瓶快阀，向腔室通入四（二甲胺基）钛，开阀时间180ms后，关闭四（二甲胺基）钛源瓶快阀，将ALD腔室抽真空25s后，打开H2O源瓶快阀，开阀时间8ms，关闭水源瓶快阀，再次将ALD腔室抽真空30s，此时，在覆有一层Al2O3薄膜的硅片表面形成有一层TiO2薄膜，从而制得Al掺杂TiO2薄膜。
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CN117144333B (zh) * 2023-09-21 2024-05-14 无锡松煜科技有限公司 一种柔性基底ald沉积氧化铝薄膜的方法及应用

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