CN105932099A - ZnS纳米带/CdS纳米柱异质结的合成方法 - Google Patents
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Abstract
本发明公开了ZnS纳米带/CdS纳米柱异质结的合成方法，其特征在于：包含以下步骤：首先，利用离子溅射仪在硅基片上沉积金膜，ZnS粉末放置在陶瓷舟里，并将陶瓷舟放置在管式炉的热电偶位置处，然后，将上述的硅基片放置在ZnS粉末的下风向，通入氩气，在氩气的保护下将反应温度升至900±20℃，并在此温度反应2±0.5h，反应结束后硅片上有白色样品生成，最后，打开装置将CdS粉末放置在热电偶位置处，将上述制备的白色样品放置在距离CdS粉末下风口处，在氩气的保护下将反应温度升至800±20℃，并在氩气的保护下在此温度反应1±0.3h，待反应完成并降到室温，在硅基片上得到淡黄色的样品。
Description
技术领域
本发明是一种II-VI族半导体异质结材料（ZnS纳米带/CdS纳米柱异质结）的合成方法。
背景技术
II-VI族化合物半导体因具有较宽的禁带范围、直接跃迁型的能带结构及丰富的发光色彩等显著特点而在激光器、发光二极管、太阳能电池等应用方面一直发挥着重要的作用。纳米尺度的II-VI族半导体材料更因其独特的发光性质、半导体量子化性能以及更能满足器件微型化的需求，在纳米光电子器件领域表现出巨大的应用潜力。因此，II-VI族半导体纳米材料的合成、光电等性能及其应用方面的相关研究在近些年来备受人们的关注。ZnS和CdS作为代表性的II-VI族半导体材料，有关这两种纳米材料的研究成为科研工作者关注的焦点。ZnS是一种具有纤锌矿结构的半导体材料，在室温下禁带宽度约为3.91eV；而CdS的室温禁带宽度约为2.42 eV，两者在可见光范围内具有很好的光电特性。并且，随着尺寸和维度的降低，ZnS 和CdS纳米材料表现出许多不同于块体和薄膜材料的光学、电学及非线性光学等性质。如量子尺寸效应使得CdS的能级改变、能隙变宽，吸收和发射光谱向短波方向移动；表面效应引起CdS纳米微粒的表面原子输运和构型发生变化，同时也引起其表面电子自旋构象和电子能谱发生变化。因而，CdS纳米结构材料在电子、光电子方面具有非常重要的潜在应用前景。目前为止，虽然已经有很多关于不同结构（如纳米带、纳米线等）ZnS 和CdS纳米材料合成工艺的报道。但是有关ZnS/CdS纳米材料异质节的合成很少有报道。
发明内容
本发明要解决的技术问题是：提供一种ZnS纳米带/CdS纳米柱异质结的合成方法，从而为该种先进半导体异质结材料的研发和应用奠定物质基础。
本发明的技术方案是：一种ZnS纳米带/CdS纳米柱异质结的合成方法，包含以下步骤：首先，利用离子溅射仪在硅基片上沉积金膜，ZnS粉末放置在陶瓷舟里，并将陶瓷舟放置在管式炉的热电偶位置处，然后，将上述的硅基片放置在ZnS粉末的下风向，通入氩气，在氩气的保护下将反应温度升至900±20℃，并在此温度反应2±0.5h，反应结束后硅片上有白色样品生成，最后，打开装置将CdS粉末放置在热电偶位置处，将上述制备的白色样品放置在距离CdS粉末下风口处，在氩气的保护下将反应温度升至800±20℃，并在氩气的保护下在此温度反应1±0.3h，待反应完成并降到室温，在硅基片上得到淡黄色的样品。
所述的金膜厚度为100±20nm。
所述的硅基片与ZnS粉末之间的距离为15-17cm。
所述的白色样品距离CdS粉末17-19cm。
所述的ZnS粉末与CdS粉末的质量比为：6.5-7.5:1。
本发明的有益效果：利用Au纳米颗粒作为催化剂，采取两步化学气相法，通过调控ZnS、CdS的质量比、沉积温度等工艺参数，实现了ZnS纳米带/CdS纳米柱异质结的合成。本发明具有实验方案简易、成本较低、实验可重复性强等优势和特点，从而为该类型功能材料的实际应用研究和开发提供了实验基础。
本发明以ZnS、CdS粉末为原料，以氩气为载流气体，以Au纳米颗粒为催化剂，利用化学气相沉积法成功地合成出了高选择性的ZnS纳米带/CdS纳米柱异质结，为该类型异质节复合物的物性研究和开发奠定了坚实的实验基础。
附图说明
图1是所合成样品的场发射扫描电子显微镜照片，图1a和1b所示，通过仔细的扫描电镜可以观察出所合成的样品为双层结构，其底层为带状结构，上层为针状阵列结构；
图2为所合成样品X射线衍射图，结果分析结果除催化剂和基片为，所合成的样品为ZnS和CdS的混合相，结合所有所得实验结果，样品的表征结果表明所合成的样品为高选择性的ZnS纳米带/CdS纳米柱异质结。
具体实施方式
以下是本发明的实例(实例中所用试剂均为化学纯)，该实验过程的主要步骤分三步：
实施例1
第一步：利用离子溅射仪在硅片（100晶向、0.9cm*0.9cm）上镀厚度约为100nm的Au膜，并以此镀膜硅片作为催化剂。第二步：将盛有0.7gZnS粉末的陶瓷舟推入石英管内至管式炉热电偶位置处，然后将上述基片推入石英管至距此陶瓷舟下风口15cm处。之后通入氩气30分钟以排出石英管内存在的氧气，在氩气的保护下将反应温度由室温升至900℃并在该温度下反应2小时，待整个装置冷却至室温，可观察到在基片上沉积有一定量的白色样品。第三步：将盛有0.1gCdS粉末的陶瓷舟放置在热电偶位置处，将第二步已制备好的白色样品放置距离盛有CdS粉末的陶瓷舟下风口17cm位置处。之后通入氩气30分钟以排出石英管内存在的氧气，在氩气的保护下快速升温至800℃，并在此温度下反应1小时。反应完成后待整个装置冷却至室温后，可在镀金硅片上得到一层淡黄色样品。
表1：所设计实验的可重复性统计
| 编号 | 反应温度（℃） | 距离（cm） | ZnS/CdS | 氩气（sccm） | 压强（MPa） | 样品选择性 |
| 1 | 900/800 | 15/17 | 7:1 | 30 | 0.1 | 95% |
| 2 | 900/800 | 15/17 | 7:1 | 30 | 0.1 | 94% |
| 3 | 900/800 | 15/17 | 7:1 | 30 | 0.1 | 96% |
实施例2
第一步：利用离子溅射仪在硅片（100晶向、0.9 cm*0.9 cm）上镀厚度约为120 nm的Au膜，并以此镀膜硅片作为催化剂。第二步：将盛有0.75g ZnS粉末的陶瓷舟推入石英管内至管式炉热电偶位置处，然后将上述基片推入石英管至距此陶瓷舟下风口16 cm处。之后通入氩气30分钟以排出石英管内存在的氧气，在氩气的保护下将反应温度由室温升至920℃并在该温度下反应2.5小时，待整个装置冷却至室温，可观察到在基片上沉积有一定量的白色样品。第三步：将盛有0.1gCdS粉末的陶瓷舟放置在热电偶位置处，将第二步已制备好的白色样品放置距离盛有CdS粉末的陶瓷舟下风口18cm位置处。之后通入氩气30分钟以排出石英管内存在的氧气，在氩气的保护下快速升温至820℃，并在此温度下反应1.2小时。反应完成后待整个装置冷却至室温后，可在镀金硅片上得到一层淡黄色样品。
实施例3
第一步：利用离子溅射仪在硅片（100晶向、0.9 cm*0.9 cm）上镀厚度约为80nm的Au膜，并以此镀膜硅片作为催化剂。第二步：将盛有0.65g ZnS粉末的陶瓷舟推入石英管内至管式炉热电偶位置处，然后将上述基片推入石英管至距此陶瓷舟下风口17cm处。之后通入氩气30分钟以排出石英管内存在的氧气，在氩气的保护下将反应温度由室温升至880℃并在该温度下反应1.5小时，待整个装置冷却至室温，可观察到在基片上沉积有一定量的白色样品。第三步：将盛有0.1g CdS粉末的陶瓷舟放置在热电偶位置处，将第二步已制备好的白色样品放置距离盛有CdS粉末的陶瓷舟下风口19cm位置处。之后通入氩气30分钟以排出石英管内存在的氧气，在氩气的保护下快速升温至780℃，并在此温度下反应0.8小时。反应完成后待整个装置冷却至室温后，可在镀金硅片上得到一层淡黄色样品。
Claims (5)
1.一种ZnS纳米带/CdS纳米柱异质结的合成方法，其特征在于：包含以下步骤：首先，利用离子溅射仪在硅基片上沉积金膜，ZnS粉末放置在陶瓷舟里，并将陶瓷舟放置在管式炉的热电偶位置处，然后，将上述的硅基片放置在ZnS粉末的下风向，通入氩气，在氩气的保护下将反应温度升至900±20℃，并在此温度反应2±0.5h，反应结束后硅片上有白色样品生成，最后，打开装置将CdS粉末放置在热电偶位置处，将上述制备的白色样品放置在距离CdS粉末下风口处，在氩气的保护下将反应温度升至800±20℃，并在氩气的保护下在此温度反应1±0.3h，待反应完成并降到室温，在硅基片上得到淡黄色的样品。
2.根据权利要求1所述的一种ZnS纳米带/CdS纳米柱异质结的合成方法，其特征在于：金膜厚度为100±20nm。
3.根据权利要求1所述的一种ZnS纳米带/CdS纳米柱异质结的合成方法，其特征在于：硅基片与ZnS粉末之间的距离为15-17cm。
4.根据权利要求1所述的一种ZnS纳米带/CdS纳米柱异质结的合成方法，其特征在于：白色样品距离CdS粉末17-19cm。
5.根据权利要求1所述的一种ZnS纳米带/CdS纳米柱异质结的合成方法，其特征在于：ZnS粉末与CdS粉末的质量比为：6.5-7.5:1。
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| CN112663144A (zh) * | 2020-12-10 | 2021-04-16 | 华中科技大学 | 二维In2S3/SnS异质结晶体材料的制备方法 |
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| CN102263036A (zh) * | 2011-07-01 | 2011-11-30 | 新疆大学 | 一种制备CdS/ZnS纳米线异质结的方法 |
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| CN102263036A (zh) * | 2011-07-01 | 2011-11-30 | 新疆大学 | 一种制备CdS/ZnS纳米线异质结的方法 |
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| Title |
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| 刘洪超: "半导体纳米材料的制备与性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
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| CN112663144A (zh) * | 2020-12-10 | 2021-04-16 | 华中科技大学 | 二维In2S3/SnS异质结晶体材料的制备方法 |
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