CN103730523B - 一种石墨烯基碲镉汞复合薄膜材料及其制备方法 - Google Patents
一种石墨烯基碲镉汞复合薄膜材料及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种石墨烯基碲镉汞复合薄膜材料及其制备方法，包括衬底层，衬底层上有单层或多层石墨烯层，石墨烯层上面沉积有碲镉汞薄膜层，Hg1-xCdxTe，0.2≤x≤0.3。采用化学气相沉积（CVD）方法在铜箔上制备单层石墨烯薄膜，采用湿法转移石墨烯层至所需衬底层上，利用激光分子束外延生长（LMBE）方法在石墨烯层上沉积制备碲镉汞薄膜。本发明材料衬底选择多样化且衬底的改变不会引起碲镉汞膜层性质的改变；具有良高的透明性、更好的电学性能和更低的噪声影响；石墨烯层数可控，可更好地控制调节，其透光性、导电性、噪声、响应。
Description
技术领域
本发明涉及一种石墨烯基碲镉汞复合薄膜材料及其制备方法，属于红外探测材料技术领域。
背景技术
碲镉汞（Hg1-xCdxTe，MCT）材料是直接带隙半导体材料，具有高量子效率、可高温工作、响应波长可随组分连续变化可调、可探测中波、长波和超长波红外辐射的特点，一直是三代红外焦平面（FPA）探测器件的主要使用材料，被广泛的应用于卫星遥感、气象及环境监测，医学成像以及夜视***等方面。
早期的碲镉汞材料以制备单晶为主，由于在生长中存在着组分不均匀、晶格完整性差、不能大面积生长、重复率低等问题，自20世纪80年代之后，各国的研究小组逐渐将研究重点放到了碲镉汞外延薄膜的研究上。随着各种外延技术的发展，碲镉汞薄膜材料的质量也取得了较大的进展。衬底材料则多采用结晶性较高、质量好的硬质单晶块体材料，材料选择主要集中在以CdZnTe、CdTe为主的同质衬底材料和以GaAs、Al2O3、Si为主的异质衬底材料上，也有很多已用于工业化生产中。但是随着社会的不断进步和技术的不断创新，我们对碲镉汞红外探测器件也有了更高的发展要求：大面阵FPA、降低成本、大尺寸（10.16cm以上）晶片成为目前研制的主导，同时还要求仪器小型化、轻型化。而目前常用的各种硬质单晶衬底材料无法同时满足这些要求，极大地限制了碲镉汞FPA器件的发展，衬底的选择单一、品质要求高、稳定性差等问题已成为碲镉汞薄膜质量、性质、性能进一步改善的关键问题。
发明内容
本发明的目的是克服上述不足而提供一种石墨烯基碲镉汞复合薄膜材料及其制备方法，具有良高的透明性、更好的电学性能和更低的噪声影响。
为实现上述目的，本发明采取以下技术方案：
一种石墨烯基碲镉汞复合薄膜材料，包括衬底层，衬底层上有单层或多层石墨烯层，石墨烯层上面沉积有碲镉汞薄膜层，Hg1-xCdxTe,，0.2≤x≤0.3。
所述的衬底层为CdZnTe、CdTe、GaAs、Al2O3、Si、石英、非晶玻璃等常见硬质耐高温（高于100℃）衬底材料。
采用化学气相沉积（CVD）方法在铜箔上制备单层石墨烯薄膜，采用湿法转移石墨烯层至所需衬底层上，利用激光分子束外延生长（LMBE）方法在石墨烯层上沉积制备碲镉汞薄膜。
一种石墨烯基碲镉汞复合薄膜材料的制备方法，包括步骤如下：
（1）石墨烯层的制备：将铜箔清洗烘干后放入真空化学气相沉积***中，将***密闭抽至10Pa以下，开始升温，随温度升高在小于300℃时首先通入H2，继续升温至1050℃，保持恒温，后通入CH4，保持恒温40-50分钟，之后先后关闭CH4、H2，并迅速冷却得到单层石墨烯；
（2）石墨烯层的转移：将沉积有石墨烯的铜箔剪切成小正方形，在附有石墨烯的方形铜箔上均匀旋涂PMMA，加热烘烤，然后放入腐蚀性溶液中室温浸泡，将铜完全腐蚀，得到石墨烯/PMMA结构材料，将石墨烯+PMMA膜迁移至所需衬底材料上，待自然干燥，加热烘烤，将烘干的PMMA+石墨烯+衬底置于丙酮溶液中，去除PMMA，然后利用乙醇清洗并自然干燥，得到单层石墨烯/衬底结构材料；重复所述转移操作可得多层石墨烯/衬底结构材料；
（3）碲镉汞薄膜层的制备：选择Hg1-xCdxTe,，0.2≤x≤0.3材料制成体靶，采用激光分子束外延（LMBE）设备，将高能量脉冲激光聚焦在靶材表面，以步骤（2）得到的石墨烯/衬底结构材料为基片，激光沉积得碲镉汞薄膜。
步骤（1）所述的H2流量50sccm，CH4流量50sccm。
步骤（2）所述的加热烘烤均为在100-300℃的加热板上烘烤5-50min。
步骤（2）所述的腐蚀性溶液为1-2mol/L的FeCl3溶液。
步骤（3）所述激光沉积：激光波长为248nm，能量为100-150mJ，激光频率：2-10Hz，沉积温度100℃，沉积时背景压强范围10-2-101Pa，沉积时间10-120分钟。
本发明利用具有良好的力学强度、透光性、柔韧性、红外透光性以及优异的电学性能和化学稳定性的石墨烯作为载体采用激光分子束外延法（LMBE）制备生长高质量的石墨烯基碲镉汞复合薄膜。
与目前的碲镉汞薄膜材料相比，本发明具有以下优点：
（1）衬底选择更加多样化，衬底的改变不会引起碲镉汞膜层性质的改变且可保持碲镉汞的结晶性；
（2）将具有良高的透明性、更好的电学性能和更低的噪声影响；
（3）石墨烯层数可控，因此可更好地控制调节，其透光性、导电性、噪声、响应；
（4）制备过程简单，且具有成本低、面积大、更易加工、性质稳定等特点。
附图说明
图1单层石墨烯基碲镉汞复合薄膜材料结构示意图；
图2多层石墨烯基碲镉汞复合薄膜材料结构示意图；
图3制备石墨烯基碲镉汞复合薄膜材料的方法流程图；
图4为本发明实施例1制备的（a）非晶玻璃衬底石墨烯基碲镉汞复合薄膜材料与（b）非晶玻璃衬底碲镉汞薄膜材料的X射线衍射光谱，图中标注“●”为碲镉汞材料衍射峰，其他衍射信号为衬底及石墨烯层对应衍射峰；
其中，1.碲镉汞薄膜层，2.单层石墨烯，3.衬底。
具体实施方式
以下结合附图对本发明的优选实施例进行说明，应当理解，此处所描述的优选实施例仅限于说明解释本发明，并不用于限定本发明。所述材料如无特别说明均能从公开商业途径而得。
实施例1
（1）石墨烯的制备
将铜箔放入采用高温管式炉和复合分子泵组成的真空化学气相沉积（CVD）***中，将***密闭抽至10Pa以下，开始升温。升温至300℃时通入H2（流量50sccm），继续升温至1050℃，恒温20分钟后通入CH4（流量50sccm），通气50分钟后关闭通入CH4，保持恒温15分钟后，关闭H2，之后迅速冷却得到单层石墨烯。
（2）利用湿法转移技术将单层石墨烯转移到非晶玻璃衬底上
具体操作为：将沉积有石墨烯的铜箔剪切成15mm*15mm正方形，并将其中一面均匀旋涂PMMA，之后将其置于130℃的加热板上烘烤30min，然后放入1mol/l的FeCl3溶液中室温浸泡，直到石墨烯+PMMA膜从铜基底上脱落，并将铜腐蚀完全。将石墨烯+PMMA膜迁移到去离子水溶液中漂洗30min后迁移到非晶玻璃衬底上，待自然干燥，置于130℃的加热板上烘烤30min。将烘干的PMMA+石墨烯+透明衬底置于丙酮溶液中，直到PMMA去除干净，然后利用乙醇清洗并自然干燥。
（3）碲镉汞薄膜的制备
采用激光分子束外延（LMBE）设备，248nm、150mJ、5Hz准分子高能量脉冲激光作为溅射光源，选择Hg0.8Cd0.2Te材料制成体靶，在步骤（1）中制备的石墨烯/非晶玻璃衬底结构材料上沉积生长碲镉汞薄膜。沉积温度100℃。沉积时背景压强5Pa，沉积时间120分钟。
经X射线衍射测试测定：利用上述方法在非晶玻璃衬底上生长的单层石墨烯基碲镉汞薄膜为多晶结构，同时的结晶质量明显好于直接以非晶玻璃为衬底的碲镉汞薄膜（附图4）。同时经扫描电镜-能量色散X射线能谱（SEM-EDAX）分析，所得碲镉汞薄膜配比，Hg1-xCdxTe中x=0.21。
实施例2
（1）将铜箔放入采用高温管式炉和复合分子泵组成的真空化学气相沉积（CVD）***中，将***密闭抽至10Pa以下，开始升温。升温至300℃时通入H2（流量50sccm），继续升温至1050℃，恒温20分钟后通入CH4（流量50sccm），通气50分钟后关闭通入CH4，保持恒温15分钟后，关闭H2，之后迅速冷却得到单层石墨烯。
（2）利用湿法转移技术转移多层石墨烯到非晶玻璃衬底上
具体操作为：将沉积有石墨烯的铜箔剪切成多个15mm*15mm的正方形，并其中一面均匀旋涂PMMA，之后将其置于130℃的加热板上烘烤30min，然后放入1mol/l的FeCl3溶液中室温浸泡，直到石墨烯+PMMA膜从铜基底上脱落，并将铜腐蚀完全。将迁移到去离子水溶液中漂洗30min后，选取其中一片迁移到非晶玻璃衬底上，待自然干燥，置于130℃的加热板上烘烤30min。将烘干的PMMA+单层石墨烯+透明衬底置于丙酮溶液中，直到PMMA去除干净，然后利用乙醇清洗并自然干燥，得到“单层石墨烯+玻璃衬底”。之后再从去离子水溶液中再选取一片石墨烯+PMMA膜，再次迁移到上述得到的“单层石墨烯+玻璃衬底”上，之后重复上述步骤去除PMMA膜，烘干，得到“两层石墨烯+玻璃衬底”结构材料。
（3）采用激光分子束外延（LMBE）设备，248nm、120mJ、8Hz准分子高能量脉冲激光作为溅射光源，选择Hg0.8Cd0.2Te材料制成体靶，在步骤（1）中制备的石墨烯/非晶玻璃衬底结构材料上沉积生长碲镉汞薄膜。沉积温度100℃。沉积时背景压强5Pa，沉积时间100分钟。
Claims (7)
1.一种石墨烯基碲镉汞复合薄膜材料，其特征是，包括衬底层，衬底层上有单层或多层石墨烯层，石墨烯层上面沉积有碲镉汞薄膜层，碲镉汞薄膜层的化学式为Hg1-xCdxTe，0.2≤x≤0.3，所述复合薄膜材料采用化学气相沉积方法在铜箔上制备单层石墨烯薄膜，采用湿法转移石墨烯层至所需衬底层上，利用激光分子束外延生长方法在石墨烯层上沉积制备碲镉汞薄膜。
2.根据权利要求1所述的一种石墨烯基碲镉汞复合薄膜材料，其特征是，所述的衬底层为CdZnTe、CdTe、GaAs、Al2O3、Si、石英或非晶玻璃。
3.一种石墨烯基碲镉汞复合薄膜材料的制备方法，其特征是，包括步骤如下：
（1）石墨烯层的制备：将铜箔清洗烘干后放入真空化学气相沉积***中，将***密闭抽至10Pa以下，开始升温，随温度升高在300℃时首先通入H2，继续升温至1050℃，保持恒温，后通入CH4，保持恒温40-50分钟，之后先后关闭CH4、H2，并迅速冷却得到单层石墨烯；
（2）石墨烯层的转移：将沉积有石墨烯的铜箔剪切成小正方形，在附有石墨烯的方形铜箔上均匀旋涂PMMA，加热烘烤，然后放入腐蚀性溶液中室温浸泡，将铜完全腐蚀，得到石墨烯/PMMA结构材料，将石墨烯+PMMA膜迁移至所需衬底材料上，待自然干燥，加热烘烤，将烘干的PMMA+石墨烯+衬底置于丙酮溶液中，去除PMMA，然后利用乙醇清洗并自然干燥，得到单层石墨烯/衬底结构材料；重复所述转移操作可得多层石墨烯/衬底结构材料；
（3）碲镉汞薄膜层的制备：选择Hg1-xCdxTe，0.2≤x≤0.3材料制成体靶，采用激光分子束外延（LMBE）设备，将高能量脉冲激光聚焦在靶材表面，以步骤（2）得到的石墨烯/衬底结构材料为基片，激光溅射沉积得碲镉汞薄膜。
4.根据权利要求3所述的一种石墨烯基碲镉汞复合薄膜材料的制备方法，其特征是，步骤（1）所述的H2流量50sccm，CH4流量50sccm。
5.根据权利要求3所述的一种石墨烯基碲镉汞复合薄膜材料的制备方法，其特征是，步骤（2）所述的腐蚀性溶液为1-2mol/L的FeCl3溶液的。
6.根据权利要求3所述的一种石墨烯基碲镉汞复合薄膜材料的制备方法，其特征是，步骤（2）所述的加热烘烤均为在100-300℃的加热板上烘烤5-50min。
7.根据权利要求3所述的一种石墨烯基碲镉汞复合薄膜材料的制备方法，其特征是，步骤（3）所述激光沉积：激光波长为：248nm，能量：100-150mJ，激光频率：2-10Hz，沉积温度100-150℃，沉积时背景压强范围10-2-101Pa，沉积时间10-120分钟。
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