CN110634749B - 一种BaSi2薄膜的外延生长方法 - Google Patents
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Abstract
本发明一种BaSi2薄膜的外延生长方法，具体指一种利用磁控共溅射技术在单晶Si衬底上外延生长BaSi2薄膜的方法，涉及BaSi2薄膜制作方法技术领域。一种BaSi2薄膜的外延生长方法，所述单晶硅衬底晶向为<111>或<100>，电阻率0.01～10000Ω.cm。还包括如下步骤：I.单晶硅衬底清洗；II.单晶硅衬底退火；III.BaSi2种子层生长；IV.Ba、Si共溅射生长得到BaSi2外延薄膜。综上所述，本发明一种BaSi2薄膜的外延生长方法，与现有技术相比，具有可以实现薄膜的化学计量比的精确控制，提高薄膜的质量，有较好的外延特性及比分子束外延技术有生长速率快、成本低等优点。
Description
技术领域：
本发明涉及BaSi2薄膜制作方法技术领域，具体指一种利用磁控共溅射技术在单晶 Si衬底上外延生长BaSi2薄膜的方法
背景技术：
随着能源和环境问题的日趋严峻，清洁、高效的可再生能源越来越受到人们的瞩目。太阳能电池作为一种新能源，一直是人们的研究的热点。目前，以晶硅(单晶硅、多晶硅)为主的太阳能电池占据了绝大部分的市场份额，主要归功于成熟的硅提纯工艺和晶硅太阳能电池生产工艺。近年来，薄膜太阳能电池如碲化镉(CdTe)和铜铟镓硒 (CIGS)太阳能电池也加入了竞争行列，其优势在于它们低的制造成本，较高的效率，灵活的应用场景，柔性等特点。钙钛矿太阳能电池由于其高效和简单灵活的制造工艺，成为太阳能电池家族的又一有力竞争者。然而昂贵元素如In、Ga的使用，造成了电池成本的上升，而且电池材料中所含的有毒元素如Cd、Pb等容易造成对环境的污染，这些因素限制了该类薄膜太阳能电池的进一步发展。因此，发展环境友好型薄膜太阳能电池，进一步提高薄膜太阳能电池的转换效率，降低制造成本，一直是太阳能电池研究领域中的热点问题。
二硅化钡(BaSi2)作为一种新型半导体材料，与常见太阳能电池材料相比，主要有两大特点：1，对环境友好，BaSi2中不含有污染环境的元素；2，原材料丰富廉价，使得制备低成本太阳能电池成为可能。此外，该材料具有合适的禁带宽度(1.3eV)，在可见光区有着很高的吸收系数(105cm-1)，在薄膜太阳能电池方面具有广阔的应用前景。
目前已公开的BaSi2薄膜的制备方法主要有三种(Suemasu T，UsamiN.Exploringthe potential of semiconducting BaSi2 for thin-film solar cellapplications[J].Journal of Physics D：Applied Physics，2016，50(2)： 023001.)：分子束外延，磁控溅射和热蒸发。分子束外延法制备BaSi2薄膜通常在超高真空下进行，通过Si和Ba的慢速率共沉积到加热的Si衬底上，得到BaSi2外延薄膜。该方法制备的BaSi2薄膜具有结晶性高、少子寿命长，光电响应强等优点，但其生长速率较慢(1～1.5nm/min)，设备昂贵，造成较高的制备成本，不适于工业化应用。
磁控溅射法利用BaSi2靶材在Si、石英或玻璃衬底上，直接溅射沉积BaSi2薄膜，其生长速率在每分钟数十纳米，适合大规模生产，但目前该方法得到的BaSi2薄膜一般为多晶性质，需要进一步提高结晶质量。
热蒸发法通过在真空中利用钨舟加热BaSi2粉末，快速沉积到衬底上得到BaSi2薄膜，该方法对实验条件依赖较低，生长速率很快，达到每分钟数百纳米，但结晶质量较差，尚不能与分子束外延或溅射得到的薄膜质量相比。
从目前已公开的BaSi2薄膜的制备技术来说，其主要的问题是如何在获得高质量的基础上，提高薄膜生长速率。
发明内容：
本发明的目的在于克服现有技术存在的缺失和不足，提出一种BaSi2薄膜的生长方法，基于独立的Si靶和Ba靶作为源，通过双靶共溅射的方法，在单晶硅衬底上进行 BaSi2薄膜的外延生长，解决分子束外延生长中速率低下、成本高昂等问题。
本发明的技术方案：
一种BaSi2薄膜的外延生长方法，所述单晶硅衬底晶向为<111>或<100>，电阻率0.01～10000Ω·cm。
还包括如下步骤：
(1)单晶Si衬底分别使用丙酮、无水乙醇、去离子水依次超声清洗5分钟，然后在80℃的盐酸∶双氧水∶水＝1∶1∶5的溶液中清洗5min，之后在80℃的氨水∶双氧水∶水＝1∶1∶5的溶液中清洗5min，最后使用5％的氢氟酸溶液除去表面氧化层，取出用去离子水漂洗干净后用高纯氮气吹干放入磁控溅射腔室。
(2)在真空环境下退火硅衬底，退火温度850℃，退火时间30。
(3)在Si衬底上溅射一层5nm的Ba层，升高Si衬底温度和Ba反应得到BaSi2种子层，或直接在升温的Si衬底上溅射Ba得到BaSi2种子层。
(4)Si、Ba双靶共溅射生长BaSi2薄膜。
所述磁控溅射的背景压强低于5×10-5Pa。
优选地，步骤(3)中氩气流量为6sccm，溅射压强为0.3Pa。
优选地，步骤(3)中衬底温度为500-550℃，优选为500℃。
优选地，步骤(3)中Ba的溅射速率为1-5nm/min，优选为2.5nm/min。
优选地，步骤(3)中溅射时间为1-5min，优选为2min。
优选地，步骤(4)中氩气流量为6sccm，溅射压强为0.3Pa。
优选地，步骤(4)中衬底温度为500-600℃，优选为550℃。
优选地，步骤(4)中Si的溅射速率3～7nm/min，优选为5nm/min；Ba的溅射速率为15～25nm/min，优选为15nm/min；溅射时间1～4h。
如上所述，与现有技术相比，本发明具有如下优势：
具有较好的外延特性，相比分子束外延技术具有生长速率快，成本低等优点。可以实现薄膜的化学计量比的精确控制，提高薄膜的质量。
附图说明
图1为本发明一种BaSi2薄膜的外延生长方法流程框图；
图2为本发明实施例BaSi2种子层的拉曼光谱；
图3为本发明实施例在衬底上BaSi2薄膜的高分辨率X射线衍射图；
图4为本发明实施例在衬底上BaSi2薄膜的(a)表面和(b)截面扫描电镜图。
具体实施方式
以下结合附图和实施例对本发明作进一步描述
本发明一种BaSi2薄膜的外延生长方法步骤流程(如附图1所示)
本发明实施例1：
I步骤，将衬底依次在丙酮、乙醇、去离子水中各超声清洗5min。之后依次放入 80℃盐酸∶双氧水∶水＝1∶1∶5的酸溶液和80℃氨水∶双氧水∶水＝1∶1∶5的碱溶液中清洗5min，最后在5％的稀HF中除去氧化层，用去离子水冲洗并用高纯氮气吹干备用。
II步骤洗净的衬底导入磁控溅射真空腔室，抽取真空到5×10-5Pa以下，将衬底升温至850℃并维持30min，之后降低衬底温度至500℃。
III步骤在500℃的衬底上溅射Ba层，溅射压强为0.3Pa，溅射速率2.5nm/min，溅射时间2min，在该过程中，Ba和加热的Si衬底发生反应，生成BaSi2种子层，通过拉曼光谱检测，在250～300cm-1和350～400cm-1之间，得到代表BaSi2的四个拉曼特征峰(如附图2所示)。
IV步骤将衬底温度升高到550℃，在已经生成BaSi2种子层的衬底上同时溅射Ba和Si，溅射压强0.3Pa，溅射速率分别为15nm/min和5nm/min，溅射时间1h，得到外延生长的BaSi2薄膜，溅射结束后自然降温至室温后取出样品进行结晶性和微观形貌表征。
薄膜的高分辨率X射线衍射图(如附图3所示)，检测到除Si衬底峰之外的代表BaSi2沿<100>方向生长的BaSi2(200)，BaSi2(400)和BaSi2(600)三个峰，表明薄膜的外延特性；
生长1h的BaSi2薄膜的(a)表面和(b)截面形貌图，观察到BaSi2薄膜和Si衬底之间的清晰界面(如附图4所示)。
本发明实施例2(如附图1所示)
I.步骤：将衬底依次在丙酮、乙醇、去离子水中各超声清洗5min。之后依次放入 80℃盐酸∶双氧水∶水＝1∶1∶5的酸溶液和80℃氨水∶双氧水∶水＝1∶1∶5的碱溶液中清洗5min，最后在5％的稀HF中出去氧化层，用去离子水冲洗并用高纯氮气吹干备用。
II.步骤：洗净的衬底导入磁控溅射真空腔室，抽取真空到5×10-5Pa以下，将衬底升温至850℃并维持30分钟，之后降低衬底温度至室温。
III步骤：在衬底上溅射Ba层，溅射压强为0.3Pa，溅射速率2.5nm/min，溅射时间2min，然后缓慢升高衬底温度至500℃并维持该温度30min，形成BaSi2种子层。
IV步骤：共溅射Ba和Si，溅射压强0.3Pa，衬底温度为550℃，溅射速率分别为15nm/min和5nm/min，溅射时间1h，溅射结束后自然降温至室温后取出样品进行结晶性和微观形貌表征。
综上所述，本发明一种BaSi2薄膜的外延生长方法，特别在二硅化钡(BaSi2)作为一种新型半导体材料，与常见太阳能电池材料相比，主要有几大特点：对环境友好， BaSi2中不含有污染环境的元素；原材料丰富廉价，使得制备低成本太阳能电池成为可能；以及该材料具有合适的禁带宽度(1.3eV)，在可见光区有着很高的吸收系数(105cm-1) 基础上，与现有技术相比，具有实现薄膜的化学计量比的精确控制，提高薄膜的质量和具有较好的外延特性，相比分子束外延技术具有生长速率快，成本低等优点，为在硅异质结太阳能电池、薄膜太阳能电池、光电探测器等领域良好的应用前景，提供坚实的技术物质基础。
Claims (5)
1.一种BaSi2薄膜的外延生长方法，基于独立的Si靶和Ba靶作为源，通过双靶共溅射在单晶硅衬底上进行BaSi2薄膜的外延生长，其特征在于，所述单晶硅衬底晶向为<111>或<100>，电阻率0.01～10000Ω·cm；
并包括如下步骤：
I.单晶硅衬底清洗；
II.单晶硅衬底退火；
III.BaSi2种子层生长；
IV.Ba、Si共溅射生长得到BaSi2外延薄膜；
所述III.BaSi2种子层生长，还包括：III.1硅衬底温度至500～550℃，溅射5nm厚Ba原子层至硅衬底上，反应得到BaSi2种子层；
或在室温下溅射5nm厚Ba原子层至硅衬底上，缓慢升高衬底温度至500～550℃，反应得到BaSi2种子层。
2.如权利要求1所述的一种BaSi2薄膜的外延生长方法，其特征在于，所述I.单晶硅衬底的清洗，还包括：I.1在丙酮、乙醇、去离子水中各超声清洗5min；
I.2在80℃的盐酸∶双氧水∶水＝1∶1∶5的溶液中清洗5min；
I.3在80℃的氨水∶双氧水∶水＝1∶1∶5的溶液中清洗5min；
I.4在5％的稀HF中除去氧化层并用高纯氮气吹干。
3.如权利要求1所述的一种BaSi2薄膜的外延生长方法，其特征在于，所述II.单晶硅衬底退火，还包括：退火的温度为850℃，退火时间30min。
4.如权利要求1所述的一种BaSi2薄膜的外延生长方法，其特征在于，所述III.BaSi2种子层生长，其中：
氩气流量为6sccm，溅射压强为0.3Pa；
衬底温度为500-550℃；
Ba的溅射速率为1-5nm/min；
溅射时间为1-5min。
5.如权利要求1所述的一种BaSi2薄膜的外延生长方法，其特征在于，所述IV.Ba、Si共溅射生长得到BaSi2外延薄膜的溅射速率：
其中，Si的溅射速率3～7nm/min；
Ba的溅射速率为15～25nm/min；
溅射时间1～4h；
氩气流量为6sccm；
溅射压强为0.3Pa；
衬底温度为500-600℃。
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