CN112647042A - 一种用热板制备二维WS2/PbI2垂直异质结的制备方法 - Google Patents
一种用热板制备二维WS2/PbI2垂直异质结的制备方法 Download PDFInfo
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Abstract
本专利公开了一种用热板制备二维WS2/PbI2垂直异质结的制备方法，其技术方案要点是:使用热板作为热源，直接蒸发碘化铅，制备方法简单，对环境的要求降低，对样品的损伤小，对仪器的要求低，基本每个实验室都能满足，成本低，样品结晶质量高，并且扩展了二维层状材料体系，范德瓦尔斯异质结构更加多样化。
Description
技术领域
本专利涉及材料的气相合成法制备领域，具体涉及一种用热板制备二维WS2/PbI2垂直异质结的制备方法。
背景技术
石墨烯的发现引起了人们对二维层状材料的广泛关注，其中包含石墨烯、六方氮化硼(hBN)和过渡金属双卤代烃(TMDs)等。由于这些层状材料层内以共价键结合，层间以弱的范德华力作用，可以很容易地分离或合成为单原子层或少原子层，并且可以灵活的组合成不同的异质结构。
除了石墨烯和六方氮化硼，对于于二维层状材料的研究主要集中在硫族化合物，比如过渡金属双卤代烃(TMDs)、IIIA-VIA族(GaS2、 GaSe2)、IVA-VIA族(SnS2、SnSe2)等材料，这些硫系材料通常表现出层数依赖的电子和光学性质。
除了硫族化合物，IVA-VIIA族金属卤化物最近也引起了一些关注。PbI2 是一种层状半导体，在可见范围内有2.5eV左右的带隙。与TMDs类似，PbI2具有六方晶系，铅原子层夹在两层碘原子之间，层间以较强的共价键结合，层间以弱的范德华力结合。更重要的是，PbI2为p 型半导体，而MoS2和WS2这样的大多数显示n型行为。PbI2与不同的TMDs结合可以形成丰富多样的p-n结，成为现代电子设备的基本构件。
最成熟的晶体生长方法是基于蒸汽和溶液处理技术，物理蒸汽输运(PVT)通常产生与基片紧密接触的高质量单晶；然而，它相对比较复杂和成本高，因为它必须包括一个高真空或惰性载气环境。此外，它的原料利用率，即初始的粉末与生长在基底单晶的比例，比较低。由此，基于溶液的处理技术更受人们的青睐，但是一些材料对溶剂的溶解度不高，并且形成的晶体可能含有溶剂分子，这限制了溶液法的应用，尽管在过去的几十年里发展了大量的改良生长方法，但由于生产效率低、通用性差，特别对溶解度差、稳定性差的材料，具有一定的阻碍。目前，合成PbI2的方法主要有原子层沉积(ALD)，液相剥离法，溶液法，物理气相沉积法(PVD)，但是这些方法的应用成本高，生产效率低，可控性差，开发一种有效而简单的方法来生长晶体材料是很重要的。本发明使用热板法生长PbI2，制备简单，操作方便，成本低，不需要昂贵的实验设备，基本每个实验室都可以配备，并且结晶度高。
发明内容
针对现有研究内容的不足，本专利的目的在于提供一种利用用热板制备二维WS2/PbI2垂直异质结的方法，以PbI2为源，热板提供热源，利用载玻片形成微间距，可控的制备WS2/PbI2异质结。
为了实现以上目的，本专利采用以下实验方案：
这种用热板制备二维WS2/PbI2垂直异质结的制备方法，包括如下步骤：
(1)通过热蒸发和具有镂空图案的掩膜版在300nm SiO2/Si基底上蒸镀12nm WO3源，得到具有图案的12nm WO3源的SiO2/Si 基底；
(2)用化学气相沉积的方法，将带有图案的SiO2/Si基底放置在管式炉温区中心，通入300sccm氩气，10-20min后，调整氩气流量为12sccm，将炉温升温至1000℃，通入20sccm硫化氢气体，反应 90-100s，打开炉盖降温并且停止通入硫化氢气体，得到WS2三角片；
(3)将上述CVD制备的WS2三角片作为基底制备异质结。将加热台温度设置为330℃，在加热台上放置载玻片形成微间距，待温度达到330℃时放置PbI2粉末和WS2三角片于载玻片上，产生温度差，WS2基底片和PbI2之间设有间距，产生类真空环境，反应1-2min，得到二维WS2/PbI2垂直异质结。
进一步的，炉温以25℃/分钟升温至1000℃。
本发明的有益效果：
使用热板作为热源，直接蒸发碘化铅，制备方法简单，对环境的要求降低，对样品的损伤小，对仪器的要求低，基本每个实验室都能满足，成本低，样品结晶质量高，并且扩展了二维层状材料体系，范德瓦尔斯异质结构更加多样化。
附图说明
图1为本发明的制备流程图；
图2为通过热板生长的二维WS2/PbI2垂直异质结光学图；
图3为本发明的异质结的拉曼光谱图；
图4为本发明的异质结的荧光光谱图；
图5为本发明的异质结的AFM图。
具体实施方式：
以下将结合附图对本专利作进一步的描述，需要说明的是，本实施例以本技术方案为前提，给出了详细的实施方式和具体的操作过程，但本专利的保护范围并不限于本实施例。
实施例1
这种用热板制备二维WS2/PbI2垂直异质结的制备方法，包括如下步骤：
(1)通过热蒸发和具有镂空图案的掩膜版在300nm SiO2/Si基底上蒸镀12nm WO3源，得到具有图案的12nm WO3源的SiO2/Si 基底；
(2)用化学气相沉积的方法，将带有图案的SiO2/Si基底放置在管式炉温区中心，通入300sccm氩气，10min后，调整氩气流量为 12sccm，炉温以25℃/分钟升温至1000℃，通入20sccm硫化氢气体，反应90s，打开炉盖降温并且停止通入硫化氢气体，得到WS2 三角片；
(3)将上述CVD制备的WS2三角片作为基底制备异质结。将加热台温度设置为330℃，在加热台上放置载玻片形成微间距，待温度达到330℃时放置PbI2粉末和WS2三角片于载玻片上，产生温度差，WS2基底片和PbI2之间设有间距，产生类真空环境，反应1-2min，得到二维WS2/PbI2垂直异质结。
实施例2
这种用热板制备二维WS2/PbI2垂直异质结的制备方法包括如下步骤：
(1)通过热蒸发和具有镂空图案的掩膜版在300nm SiO2/Si基底上蒸镀12nm WO3源，得到具有图案的12nm WO3源的SiO2/Si 基底；
(2)用化学气相沉积的方法，将带有图案的SiO2/Si基底放置在管式炉温区中心，通入300sccm氩气，15min后，调整氩气流量为 12sccm，将炉温升温至1000℃，通入20sccm硫化氢气体，反应95s，打开炉盖降温并且停止通入硫化氢气体，得到WS2三角片；
(3)将上述CVD制备的WS2三角片作为基底制备异质结。将加热台温度设置为330℃，在加热台上放置载玻片形成微间距，待温度达到330℃时放置PbI2粉末和WS2三角片于载玻片上，产生温度差，WS2基底片和PbI2之间设有间距，产生类真空环境，反应1-2min，得到二维WS2/PbI2垂直异质结。
实施例3
这种用热板制备二维WS2/PbI2垂直异质结的制备方法，包括如下步骤：
(1)通过热蒸发和具有镂空图案的掩膜版在300nm SiO2/Si基底上蒸镀12nm WO3源，得到具有图案的12nm WO3源的SiO2/Si 基底；
(2)用化学气相沉积的方法，将带有图案的SiO2/Si基底放置在管式炉温区中心，通入300sccm氩气，20min后，调整氩气流量为 12sccm，将炉温升温至1000℃，通入20sccm硫化氢气体，反应100s，打开炉盖降温并且停止通入硫化氢气体，得到WS2三角片；
(3)将上述CVD制备的WS2三角片作为基底制备异质结。将加热台温度设置为330℃，在加热台上放置载玻片形成微间距，待温度达到330℃时放置PbI2粉末和WS2三角片于载玻片上，产生温度差，WS2基底片和PbI2之间设有间距，产生类真空环境，反应1-2min，得到二维WS2/PbI2垂直异质结。
以上所述仅是本发明的优选实施方式，本发明的保护范围并不仅局限于上述实施例，凡属于本发明思路下的技术方案均属于本发明的保护范围。应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理前提下的若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。
Claims (2)
1.一种用热板制备二维WS2/PbI2垂直异质结的制备方法，其特征在于，包括如下步骤：
(1)通过热蒸发和具有镂空图案的掩膜版在300nm SiO2/Si基底上蒸镀12nm WO3源，得到具有图案的12nm WO3源的SiO2/Si基底；
(2)用化学气相沉积的方法，将带有图案的SiO2/Si基底放置在管式炉温区中心，通入300sccm氩气，10-20min后，调整氩气流量为12sccm，将炉温升温至1000℃，通入20sccm硫化氢气体，反应90-100s，打开炉盖降温并且停止通入硫化氢气体，得到WS2三角片；
(3)将上述CVD制备的WS2三角片作为基底制备异质结。将加热台温度设置为330℃，在加热台上放置载玻片形成微间距，待温度达到330℃时放置PbI2粉末和WS2三角片于载玻片上，产生温度差，WS2基底片和PbI2之间设有间距，产生类真空环境，反应1-2min，得到二维WS2/PbI2垂直异质结。
2.根据权利要求1所述的一种用热板制备二维WS2/PbI2垂直异质结的制备方法，其特征在于：炉温以25℃/分钟升温至1000℃。
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