CN111501012A - 一种双层WS2/MoS2横向异质结材料、制备方法及应用 - Google Patents
一种双层WS2/MoS2横向异质结材料、制备方法及应用 Download PDFInfo
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Abstract
本发明公开了一种双层WS2/MoS2横向异质结材料、制备方法及应用，将WO3粉、MoO3粉和NaCl固体颗粒混合研磨得到氧化物前驱体混合物，将氧化物前驱体混合物放置在石英管炉膛内800～810℃的温度区间，将衬底放置在氧化物前驱体混合物的正上方，衬底的氧化面朝下，将硫粉放置在石英管炉膛内140～160℃的温度区间，在保护气氛、压强为‑0.1～‑0.05Mpa下反应8～10min，在衬底上沉积双层WS2/MoS2横向异质结材料。本发明采用一步法合成WS2/MoS2横向异质结，无需使用模板，工艺简单且成本低廉。WS2/MoS2横向异质结为双层薄膜结构，且形貌清晰、异质结界面分界明显，薄膜材料的态密度更大，在场效应应用中产生多个导通通道，能够产生相当大的驱动电流，在气敏传感器、太阳能电池、光电探测器等方面具有广阔的应用前景。
Description
技术领域
本发明属于二维材料制备技术领域，具体涉及一种双层WS2/MoS2横向异质结材料、制备方法及应用。
背景技术
过渡金属硫族化合物(TMDs)在工业生产、科学研究等方面有着重要作用。MoS2和WS2是两种二维层状半导体过渡金属硫化物材料，层与层之间通过范德华力结合在一起，其带隙可根据层数的减小由间接带隙转变为直接带隙，且具有良好的柔性特点。横向生长的WS2/MoS2异质结与单一的材料相比，在晶体管的光响应特性、开关响应速度以及气敏特性上都具有显著提高，因此通过对WS2/MoS2横向异质结的生长进行调控，在以上应用上均具有重大意义。
目前，广大科研工作者利用水热法、各种改进CVD法进行WS2/MoS2横向异质结的制备。但这些方法普遍存在制备条件苛刻，制备的异质结薄膜面积小；同时难以对层数进行控制，对其研究主要集中在单层材料上。已有研究证明，与单层TMDs异质结薄膜相比，少数层WS2/MoS2横向异质结薄膜材料的态密度更大，在场效应的应用中产生多个导通通道，能够产生相当大的驱动电流。
为此，发明人经过潜心研究，提出一种制备双层WS2/MoS2横向异质结材料的方法，获得了双层WS2/MoS2横向异质结材料。
发明内容
针对现有技术存在的不足和缺陷，本发明提供了一种双层WS2/MoS2横向异质结材料、制备方法及应用，解决现有的制备方法所需条件较为苛刻且对WS2/MoS2横向异质结生长层数的难以调控的问题。
为了实现上述目的，本发明采用如下技术方案予以实现：
一种双层WS2/MoS2横向异质结材料的制备方法，包括：将WO3粉、MoO3粉和NaCl固体颗粒混合研磨得到氧化物前驱体混合物，将氧化物前驱体混合物放置在石英管炉膛内800～810℃的温度区间，将衬底放置在氧化物前驱体混合物的正上方，衬底的氧化面朝下，将硫粉放置在石英管炉膛内140～160℃的温度区间，在保护气氛、压强为-0.1～-0.05Mpa下反应8～10min，在衬底上沉积双层WS2/MoS2横向异质结材料；
硫粉、WO3粉、MoO3粉和NaCl的质量比为8000：100：100：1。
优选的，以10～15℃/min的升温速度升温至800～810℃。
优选的，所述的保护气氛为氩气，氩气的气体流速为80～100sccm。
优选的，使用双氧水与浓硫酸按体积比1：3配置而成的混合液对衬底进行清洗，然后用惰性气体对清洗好的衬底烘干。
本发明还公开了上述制备方法制备得到的双层WS2/MoS2横向异质结材料。
具体的，该异质结材料为双层WS2/MoS2薄膜，每层WS2/MoS2薄膜以三角形MoS2为核心，WS2沿三角形MoS2的三个边缘外延生长形成整体形状六边形的横向异质结。
本发明还公开了上述双层WS2/MoS2横向异质结材料用于制备光探测器的应用。
与现有技术相比，本发明的有益效果是：
(1)本发明采用NaCl作为辅助剂，NaCl的加入大大降低了金属氧化物前驱体的熔点温度，还可以与MoO3和WO3反应，生成氧氯化物，而这些氧氯化物具有非常强的反应活性，使得反应速率大大提升。
(2)本发明采用真空低压的反应环境，使金属前驱体的质量流即成核密显著提高，有效降低反应难度。
(3)本发明将MoO3和WO3这两种金属氧化物前驱体与颗粒状辅助剂NaCl充分研磨，使其混合均匀，在制备过程中不需要因为蒸发温度的不同对金属氧化物分开放置，因混合均匀距离减小，使得衬底所在区域的反应物浓度大大提高，令反应进行得更加容易和充分。
(4)本发明采用一步法合成WS2/MoS2横向异质结，合成方法简单，无需使用任何模板，工艺简单且成本低廉。
(5)本发明合成的WS2/MoS2横向异质结为双层薄膜结构，且形貌清晰、异质结界面分界明显，这种异质结薄膜材料的态密度更大，在场效应的应用中产生多个导通通道，能够产生相当大的驱动电流，在气敏传感器、太阳能电池、光电探测器等方面具有广阔的应用前景。
附图说明
图1是实施例1合成的WS2/MoS2横向异质结的光学图片，图中1、2、3分别表示测试点。
图2是实施例1合成的WS2/MoS2横向异质结的拉曼图谱
图3是实施例1合成的WS2/MoS2横向异质结整体的拉曼Mapping
图4是实施例1合成的WS2/MoS2横向异质结外围WS2的E1 2g的拉曼Mapping。
图5是实施例1合成的WS2/MoS2横向异质结核心MoS2的E1 2g的拉曼Mapping。
图6是实施例2合成的WS2/MoS2横向异质结的光学图片，图中1、2、3分别表示测试点。
图7是实施例2合成的WS2/MoS2横向异质结的拉曼图谱。
图8是实施例2合成的WS2/MoS2横向异质结整体的拉曼Mapping。
图9是实施例2合成的WS2/MoS2横向异质结外围WS2的E1 2g的拉曼Mapping。
图10是实施例2合成的WS2/MoS2横向异质结核心MoS2的E1 2g的拉曼Mapping。
图11是本发明合成的双层WS2/MoS2横向异质结的AFM图谱。
图12是对比例1合成的MoS2的光学图片。
图13是对比例1合成的MoS2的拉曼图谱。
图14是对比例3合成的WS2的光学图片。
图15是对比例3合成的WS2的拉曼图谱。
图16是对比例4合成的MoS2的光学图片。
图17是对比例4合成的MoS2的拉曼图谱。
以下结合说明书附图和具体实施方式对本发明做具体说明。
具体实施方式
本发明公开的一种双层WS2/MoS2横向异质结材料的制备方法，具体包括以下步骤：
步骤1，使用双氧水与浓硫酸按体积比1：3配置而成的混合液对衬底进行超声清洗，再使用去离子水和无水乙醇对衬底进行超声清洗，然后用惰性气体对清洗好的衬底烘干；
步骤2，将WO3粉、MoO3粉和NaCl固体颗粒按照质量比为100：100：1混合研磨得到氧化物前驱体混合物，将硫粉、氧化物前驱体混合物和衬底放置在石英管内各自温度区间，其中，硫粉、WO3粉、MoO3粉和NaCl的质量比为8000：100：100：1。氧化物前驱体混合物所处温度为800～810℃，硫粉所处温度为140～160℃，氧化物前驱体混合物平铺在衬底的氧化面的正下方；在保护气氛、压强为-0.1～-0.05Mpa下反应8～10min，最后在衬底上沉积双层WS2/MoS2横向异质结材料。
其中，石英管内以10～15℃/min的升温速度升温至800～810℃。保护气体优选氩气，氩气的气体流速为80～100sccm。
通过上述制备方法可得到双层WS2/MoS2横向异质结材料，结合实施例1中的图3可以看出，该异质结材料为双层WS2/MoS2薄膜；综合图1至图5可以说明，每层WS2/MoS2薄膜以三角形MoS2为核心，WS2沿三角形MoS2的三个边缘外延生长形成整体形状六边形的横向异质结。
以下给出本发明的具体实施例，需要说明的是本发明并不局限于以下具体实施例中，凡在本申请技术方案基础上做的等同变换均落入本发明的保护范围。
实施例1
步骤1，将30％双氧水按照体积比1：3的比例缓慢地倒入浓硫酸中，在加入的过程中使用玻璃棒不断搅拌散热，将冷却至室温后的该混合液对衬底进行超声清洗10min，本实施例中衬底为SiO2/Si，衬底总厚度为500μm，氧化层SiO2厚度为300nm。再使用去离子水和无水乙醇对衬底分别超声清洗10min，然后在氩气气氛下烘干清洗好的衬底。
步骤2，分别称取0.1g纯度为99.5％W03粉末和0.1g纯度为99.5％的MoO3，将WO3和MoO3粉末在研钵内进行研磨使其充分混合，再称取0.003g混合物待用。称取15μg纯度为99.8％的NaCl颗粒，与0.003g混合物继续进行研磨，将三者的混合物一起放置在石英舟上，将步骤1的衬底氧化层面朝下覆盖在平铺均匀的混合物正上方，将该石英舟放置在石英管炉膛的加热中心，此温区的温度设置为800℃；
称取0.12g纯度为99.98％的硫粉放置在石英舟上，将该石英舟放置在石英管炉膛的低温区，此温区的温度设置为140～160℃；S粉：WO3粉：MoO3粉：NaCl＝8000：100：100：1。
使用氩气将石英管内环境清洗五分钟，用真空泵将石英管内环境抽至-0.1Mp的低压，将升温速率设置为10℃/min，气体流速设置为100sccm，生长时间设置为8min，生长结束后冷却降温至室温，最后在衬底上沉积双层WS2/MoS2横向异质结材料。
本实施例所得的双层WS2/MoS2横向异质结材料光学照片如图1所示，拉曼图谱如图2所示，整体的拉曼Mapping如图3所示，WS2的E1 2gMapping如图4所示，MoS2的E1 2gMapping如图5所示。结合图1、图3、图4以及图5可以说明所得产物是以MoS2三角形为核心，WS2沿其边缘继续外延生长而成的六边形横向异质结。图2说明了横向异质结各个位置的拉曼峰位，WS2和MoS2的交界部位体现了异质结的拉曼峰。图3的拉曼峰位差及图11的AFM均可证明，所合成的WS2/MoS2横向异质结为双层。
本实施例得到的双层异质结薄膜材料可用于制备光探测器，由于该双层异质结薄膜材料的态密度大，在场效应的应用中产生多个导通通道，促进光电探测器中电子的流通，能够产生相当大的驱动电流。该双层异质结薄膜材料还可应用于制备气敏传感器、太阳能电池等方面。
实施例2
本实施例与实施例1的区别在于：所述的步骤2中称取称取20μg纯度为99.8％的NaCl颗粒，与0.004g混合物继续进行研磨，将三者的混合物一起放置在石英舟上，将步骤1的衬底氧化层面朝下覆盖在平铺均匀的混合物正上方，将该石英舟放置在石英管炉膛的加热中心，此温区的温度设置为810℃。
本实施例所得WS2/MoS2横向异质结的光学照片如图6所示，拉曼图谱如图7所示，整体的拉曼Mapping如图8所示，WS2的E1 2gMapping如图9所示，MoS2的E1 2gMapping如图10所示。结合图6、图8、图9以及图10可以说明所得产物是以MoS2三角形为核心，WS2沿其边缘继续外延生长而成的六边形横向异质结。图7说明了横向异质结各个位置的拉曼峰位，WS2和MoS2的交界部位体现了异质结的拉曼峰。图8的拉曼峰位差及图11的AFM均可证明，所合成的WS2/MoS2横向异质结为双层。
对比例1
本对比例与实施例1的区别在于：石英管内压强为0Mp。
本对比例所得产物形貌如图12所示，是大面积单独的MoS2，其拉曼图谱如图13所示，样品中未发现WS2/MoS2横向异质结的存在。
对比例2
本对比例与实施例1的区别在于：步骤2中，将衬底氧化面朝上放置，WO3粉、MoO3粉和NaCl颗粒三者的混合物平铺在衬底氧化面上。
本对比例所得产物未发现WS2/MoS2横向异质结的存在。
对比例3
本对比例与实施例1的区别在于：所述的氧化物前驱体混合物所处的石英管炉膛加热中心的温度为850℃。
本对比例所得的产物形貌如图14所示，是多层WS2叠层生长的形式，只是单独WS2三角形和六边形的随意堆叠。其拉曼图谱如图15所示，样品中并未发现WS2/MoS2横向异质结的存在。
对比例4
本对比例与实施例1的区别在于：所述的氧化物前驱体混合物所处的石英管炉膛加热中心的温度为750℃。
本对比例所得产物形貌如图16所示，是块状MoS2叠层生长的形式，其拉曼图谱如图17所示，样品中并未发现WS2/MoS2横向异质结的存在。
Claims (7)
1.一种双层WS2/MoS2横向异质结材料的制备方法，其特征在于，包括：将WO3粉、MoO3粉和NaCl固体颗粒混合研磨得到氧化物前驱体混合物，将氧化物前驱体混合物放置在石英管炉膛内800～810℃的温度区间，将衬底放置在氧化物前驱体混合物的正上方，衬底的氧化面朝下，将硫粉放置在石英管炉膛内140～160℃的温度区间，在保护气氛、压强为-0.1～-0.05Mpa下反应8～10min，在衬底上沉积双层WS2/MoS2横向异质结材料；
所述的硫粉、WO3粉、MoO3粉和NaCl的质量比为8000：100：100：1。
2.如权利要求1所述的双层WS2/MoS2横向异质结材料的制备方法，其特征在于，以10～15℃/min的升温速度升温至800～810℃。
3.如权利要求1所述的双层WS2/MoS2横向异质结材料的制备方法，其特征在于，所述的保护气氛为氩气，氩气的气体流速为80～100sccm。
4.如权利要求1所述的双层WS2/MoS2横向异质结材料的制备方法，其特征在于，使用双氧水与浓硫酸按体积比1：3配置而成的混合液对衬底进行清洗，然后用惰性气体对清洗好的衬底烘干。
5.权利要求1至4任一项所述的制备方法制备得到的双层WS2/MoS2横向异质结材料。
6.如权利要求5所述的双层WS2/MoS2横向异质结材料，其特征在于，该异质结材料为双层WS2/MoS2薄膜，每层WS2/MoS2薄膜以三角形MoS2为核心，WS2沿三角形MoS2的三个边缘外延生长形成整体形状六边形的横向异质结。
7.权利要求5或6所述的双层WS2/MoS2横向异质结材料用于制备光探测器的应用。
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