CN100424899C - MOCVD法超低温制备高电导率、绒面未掺杂ZnO薄膜 - Google Patents
MOCVD法超低温制备高电导率、绒面未掺杂ZnO薄膜 Download PDFInfo
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Abstract
一种MOCVD技术超低温制备高电导率、绒面未掺杂ZnO薄膜的方法。首先利用电子束蒸发技术或者溅射方法在玻璃衬底上沉积一层50-100nm高电导的ITO薄膜作为种子诱导层，其通常具有很好的电导率(～10-4Ωcm)；然后利用MOCVD技术低温生长未掺杂的ZnO薄膜。该方法在很低的温度下即可制备具有良好光散射能力的绒面结构ZnO薄膜；其次在不需要B2H6掺杂的情况下，可大幅度降低MOCVD系统生长ZnO薄膜的电阻率(可降至～10-3Ωcm)。通过后续H2低压退火可使薄膜的电子迁移率从～18.6cm2/Vs提高到～32.5cm2/Vs(提高～30%)。该方法特别适合大面积ZnO薄膜的制备。
Description
【技术领域】：
本发明属于透明导电氧化物薄膜领域，特别是适合薄膜太阳电池应用的透明导电薄膜的制备方法。
【背景技术】：
近年来，在Si薄膜太阳电池(Solar cell)应用方面，由于SnO2膜具有极好的电学和光学特性，被广泛用作太阳电池的透明导电膜。然而，它们在氢等离子体氛围环境下光学特性发生恶化，限制了其在薄膜太阳电池中作为透明导电薄膜的应用。而ZnO薄膜不仅可以在氢等离子体环境中具有高的稳定性，并且能够实现优良光电特性(低电阻率、绒面结构，高透过率)的薄膜生长，从而成为薄膜太阳电池中极具竞争力的透明导电薄膜。对于硅(Si)薄膜太阳电池来说，陷光(light trapping)作用(即相应的绒面结构)可增加入射光的光程，对提高器件性能尤为重要。
目前生长ZnO薄膜的方法很多，包括脉冲激光沉积(PLD)，分子束外延(MBE)，金属有机物化学气相沉积(MOCVD)，射频/直流溅射(RF/DCSputtering)，电子束反应蒸发(EBRE)，喷雾热分解(Spray Pyrolysis)和溶胶-凝胶法(Sol-gel)等。在用于太阳电池及其组件的ZnO薄膜制备中，国际上主要是磁控溅射和MOCVD技术。利用磁控溅射法制备薄膜太阳电池应用的ZnO薄膜，通常采用Al掺杂得到较低电阻率(～10-4Ωcm)的镜面结构。Jin Yoo等人利用射频溅射法在Corning 1737玻璃衬底上生长出了高透过率(T400-800nm＞85％)低电阻率(ρ～1.9×10-4Ωcm)的ZnO:Al薄膜(参见JinsuYoo，Jeonghul Lee，Seokki Kim，etc.High transmittance and low resistive ZnO:Al films for thin film solar cells，ThinSolid Films，2005，480-481：213)，其薄膜特性最优的生长工艺：射频功率100W，衬底温度573K，Ar分压0.27Pa。为适应薄膜太阳电池前电极的陷光作用，溅射后的ZnO薄膜须采取湿法刻蚀才能形成绒面结构，以期获得良好的光散射能力。调制绒面结构时，湿法腐蚀起关键作用，因此，在大面积腐蚀ZnO薄膜形成绒面结构时具有高的风险性和造成材料浪费(腐蚀后薄膜厚度减少)。
然而，MOCVD技术可直接生长出绒面结构的ZnO薄膜(参见Baosheng Sang，Akira Yamada，Makoto Konagai，Growth of Boron doped ZnO thin films by atomiclayer deposition，Solar Energy Materials and Solar cells，1997，46：19)。目前MOCVD生长低电阻率、绒面结构ZnO-TCO薄膜的衬底温度一般在423K以上，并且需要B2H6掺杂(剧毒气体)才能获得低电阻率的薄膜。
【发明内容】：
本发明的目的是解决现有方法制备ZnO薄膜需要B2H6掺杂(一种剧毒气体)而造成环境污染的问题，提供一种“绿色”环保型MOCVD法超低温制备高电导率、绒面未掺杂ZnO薄膜的方法。
本发明提供的金属有机物化学气相沉积(MOCVD)超低温制备高电导率、绒面未掺杂ZnO薄膜的方法，由以下步骤实现：
(a)利用电子束蒸发技术或者溅射方法先在玻璃衬底上沉积一层50-100nm高电导的ITO薄膜作为种子诱导层；
(b)在上述诱导层上，利用金属有机物化学气相沉积法生长600-3000nm的未掺杂ZnO薄膜：反应气源二乙基锌DEZn和水H2O分别装在鼓泡器中并放置于温控水浴罐中，经由Ar气鼓泡源进入真空室；DEZn和H2O的温控水浴罐分别稳定在293-318K和313-353K；二乙基锌和水的流量分别设定为100-300μmol/min和300-600μmol/min，真空室反应气压为100-600Pa，衬底温度变化范围为398-413K，沉积薄膜时间为20-60min。
然后，对(b)步中获得沉积的ZnO薄膜用H2气低压退火。其退火温度为443-503K，可有效提高ZnO薄膜的电子迁移率。
本发明的优点及效果：此方法一方面可以低温条件下获得具有光散射特征的绒面结构，提高生长速率；其次在不需要B2H6掺杂的情况下可以大幅度降低MOCVD系统生长ZnO薄膜的电阻率(可降至～10-3Ωcm)；通过后续H2退火可使薄膜的电子迁移率从～18.6cm2/Vs提高到～32.5cm2/Vs(提高～30％)。另外，本发明提供的方法对环境不会造成污染，属于“绿色”环保型技术。该方法可适合大面积(例如S＝20cm*20cm)ZnO透明导电薄膜的制备。
【附图说明】：
图1是衬底温度为408K时ZnO薄膜的典型形貌图；
图2是衬底温度为408K时ZnO/ITO薄膜的表面形貌图(其中ITO薄膜为50nm)。
【具体实施方式】：
实施例1
本发明提出两部生长“绿色”环保型ZnO-TCO薄膜的方法。
首先，利用电子束蒸发技术或者溅射方法先在玻璃衬底上沉积一层100nm高电导的ITO薄膜作为种子诱导层(Seed layer)，其通常具有很好的电导率(～10-4Ωcm)；然后利用MOCVD技术低温生长未掺杂的ZnO薄膜。这种方法一方面可以获得具有光散射特征的绒面结构，另一方面，可以大幅度降低MOCVD系统生长ZnO薄膜的电阻率(可降至～10-3Ωcm)。
薄膜具体制造过程：
1、电子束蒸发设备中沉积一层100nm高电导的ITO薄膜；
2、MOCVD生长1.2μm左右的未掺杂ZnO薄膜。
典型的生长条件如下：实验中，反应气源二乙基锌DEZn和水H2O分别装在鼓泡器中并放置于温控水浴罐中，经由Ar气鼓泡源进入反应室；DEZn和H2O的温控水浴罐分别稳定在313K和333K；二乙基锌和水的流量分别设定为202.1μmol/min和447.75μmol/min，真空室反应气压为200Pa，衬底温度变化范围为398-413K，沉积薄膜时间为30min。另外，H2气退火(～473K)可提高ZnO薄膜的电子迁移率从18.6到32.5cm2/Vs。表1是制备的ZnO薄膜和ZnO/ITO薄膜的电学特性比较。
表1ZnO薄膜和ZnO/ITO薄膜的电学特性比较
ITO：d＝100nm，ρ＝3.5×10-4Ωcm，μ＝12.21cm2/Vs，n＝1.62×1021cm-3，T＞85％(in VIS-NIR region).
实施例2
薄膜具体制造过程：
1、利用电子束蒸发技术或者溅射方法先在玻璃衬底上沉积一层50nm高电导 的ITO薄膜作为种子诱导层；
2、MOCVD生长1.0μm左右的未掺杂ZnO薄膜。
典型的生长条件如下：实验中，反应气源二乙基锌DEZn和水H2O分别装在鼓泡器中并放置于温控水浴罐中，经由Ar气鼓泡源进入反应室；DEZn和H2O的温控水浴罐分别稳定在313K和333K；二乙基锌和水的流量分别设定为202.1μmol/min和447.75μmol/min，真空室反应气压为200Pa，衬底温度变化范围为398-413K，沉积薄膜时间为30min。图1和图2分别为直接玻璃衬底上生长的ZnO薄膜和ITO上低温生长的绒面ZnO薄膜。ZnO/ITO薄膜的电阻率为～4.5×10-3Ωcm。
Claims (2)
1. 一种金属有机物化学气相沉积法超低温制备高电导率、绒面未掺杂ZnO薄膜的方法，其特征是该方法由以下步骤实现：
(a)利用电子束蒸发技术或者溅射方法先在玻璃衬底上沉积一层50-100nm高电导的ITO薄膜作为种子诱导层；
(b)在上述诱导层上，利用金属有机物化学气相沉积法生长600-3000nm的未掺杂ZnO薄膜：反应气源二乙基锌DEZn和水H2O分别装在鼓泡器中并放置于温控水浴罐中，经由Ar气鼓泡源进入真空室；DEZn和H2O的温控水浴罐分别稳定在293-318K和313-353K；二乙基锌和水的流量分别设定为100-300μmol/min和300-600μmol/min，真空室反应气压为100-600Pa，衬底温度变化范围为398-413K，沉积薄膜时间为20-60min。
2. 根据权利要求1所述的方法，其特征在于(b)步中最后沉积薄膜用H2气低压退火，温度443-503K以提高ZnO薄膜的电子迁移率。
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| CN100494486C (zh) * | 2007-05-08 | 2009-06-03 | 中国科学院上海光学精密机械研究所 | 金属有机化学气相沉积生长m面或a面ZnO薄膜的方法 |
| KR100870837B1 (ko) * | 2008-03-04 | 2008-11-28 | 한국철강 주식회사 | 산화아연 박막의 수분 제거 방법 |
| CN105349966A (zh) * | 2015-10-15 | 2016-02-24 | 南开大学 | 一种绒面复合结构ZnO-TCO薄膜的制备方法及应用 |
| CN106968015B (zh) * | 2016-08-17 | 2019-08-06 | 佛山市中山大学研究院 | 一种紫外透明导电薄膜及其制造方法 |
| CN114032525B (zh) * | 2021-11-04 | 2023-09-12 | 西南科技大学 | 金刚石-多层石墨烯复合阴极材料及其制备方法 |
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| JPH07283430A (ja) * | 1994-04-12 | 1995-10-27 | Matsushita Electric Ind Co Ltd | 太陽電池の製造方法 |
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| US20160192480A1 (en) * | 2014-12-30 | 2016-06-30 | Clemson University Research Foundation | Electronic device including transparent and flexible mica substrate and method for manufacturing the same |
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