CN111916531B - 一种用于光电探测的复合材料制备方法 - Google Patents

一种用于光电探测的复合材料制备方法 Download PDF

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CN111916531B
CN111916531B CN202010835436.8A CN202010835436A CN111916531B CN 111916531 B CN111916531 B CN 111916531B CN 202010835436 A CN202010835436 A CN 202010835436A CN 111916531 B CN111916531 B CN 111916531B
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秦鹏超
付永启
冯双龙
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Abstract

本发明公开了一种用于光电探测的复合材料制备方法，属于材料制备技术领域。本发明在石墨烯薄膜上引入了氧化锌量子点，用于制造促进晶核生长的缺陷，有助于硫化铅薄膜的沉积。同时氧化锌作为宽禁带半导体材料具有优异的透光性与电学性，形成的异质结可以有效提高光电探测的增益与响应度。

Description

一种用于光电探测的复合材料制备方法
技术领域
本发明属于新材料制备技术领域，特别是涉及一种氧化锌/石墨烯/硫化铅复合材料及其制备方法。
背景技术
光电探测器在包括军事、民用、天文、医药等众多领域有广泛应用，对于光电探测器进行深入研究的重要意义首先在于其作为现代战争广泛使用的核心技术在军事方面的重要应用，如夜间探测、光电侦察、导航和搜索功能、导弹制导和跟踪等多种功能。尤其是新一代光电探测器的发展使武器具有更长作用距离和多目标探测能力。
石墨烯具有优异的光学、电学、热学和力学的性能，并迅速成为材料、物理、电子领域的研究热点，石墨烯表现出的优异特性为零带隙、超高载流子迁移率、高透光率、宽吸收光谱和室温下的量子霍尔效应，其中高光电响应具有非常重要的研究价值。
硫化铅红外探测器是一种非制冷红外探测器，现有技术中，可以利用电化学沉积将石墨烯与硫化铅吸光层相结合，形成复合结构，石墨烯的电子移动能够填补硫化铅的光生空穴，实现光生载流子的分离，提高光电探测的响应度与增益或光电响应度与增益，但目前在石墨烯薄膜上使用电化学沉积法沉积硫化铅薄膜很难实现均匀、致密的特点。
发明内容
针对背景技术中存在的问题，本发明在石墨烯薄膜与硫化铅薄膜之间，引入了氧化锌量子点，用于制造促进晶核生长的缺陷，有助于硫化铅的沉积。氧化锌作为宽禁带半导体材料具有优异的透光性与电学性，形成的异质结可以有效提高光电探测的增益与响应度。
本发明采用的技术方案如下：
一种用于光电探测的复合材料的制备方法，其特征在于，包括以下步骤:
S1.将硝酸锌溶解于超纯水中，得到浓度为0.04-0.07mol/l的硝酸锌溶液。
S2.在硝酸锌溶液中加入能够使硝酸锌完全反应的氨水，并磁力搅拌进行反应，得到氢氧化锌混合溶液。
S3.将石墨烯薄膜利用湿法技术转移到硅片基底上，然后置于氢氧化锌混合溶液中，水浴沉积，分离，得到前置样品。
S4.将前置样品预加热0.5h-3h，加热温度为90℃—150℃；然后采用化学气相沉积法，在保护气体氛围下，对前置样品加热，其中加热时间为1-5min，微波功率为700W，得到氧化锌/石墨烯样品。
S5.采用电化学沉积法，将氧化锌/石墨烯样品置于前驱体混合溶液中，在氧化锌/石墨烯样品上沉积硫化铅薄膜；所述前驱体混合溶液为乙酸铅、乙二胺四乙酸二钠、硫化钠的混合溶液。
S6.沉积完成后，获得硫化铅/氧化锌/石墨烯的复合材料。
进一步地，步骤S4中所述保护气体为氩气。
进一步地，步骤S5中，所述的前驱体混合溶液的制备方法为：依次倒入乙酸铅混合溶液、乙二胺四乙酸二钠溶液、硫化钠溶液；其中：乙酸铅溶液浓度为20mmol/l，乙二胺四乙酸二钠溶液浓度为10mmol/l，硫化钠溶液浓度为0.15mmol/l，乙酸铅溶液：乙二胺四乙酸二钠溶液：硫化钠溶液的体积比为2：2：1。
进一步地，步骤S5中，电化学沉积法选择恒电位沉积，其中沉积电位的选择由线性循环伏安分析来确定，沉积电位选择范围为-0.75v～-0.95v，沉积时间范围为10min-60min。
本发明将不同性质的材料进行优化合成为新的材料。利用氢氧化锌在空气中的高温脱水反应，然后在微波等离子体的反应室进行辉光放电，通入氩气，在微波的激励下，分子离化，产生等离子体，使得氧化锌薄膜烧结的同时被破坏，不再连续，形成量子点缺陷，有助于改善石墨烯的疏水性，促进硫化铅的电化学沉积，最终形成异质结。
本发明通过在等离子体反应的区域加热得到氧化锌量子点，制备方法简单有效，利用微波等离子体刻蚀薄膜，既可以保证氢氧化锌完全转化为氧化锌，同时完成了对氧化锌薄膜的破坏。然后采用电化学沉积法，在氧化锌量子点表面沉积硫化铅薄膜，氧化锌量子点既有促进硫化铅沉积的作用，又可以形成异质结。本发明制备的氧化锌/石墨烯/硫化铅的三明治结构可以使自由电子的行动能力加快，自由电子的迁移率可以大大增加，能够有效提高光电响应。
附图说明
图1为在硅片基底上做出氧化锌/石墨烯/硫化铅复合材料的示意图；
图2为实施例1制备得到的复合材料图；
图3为实施例2制备得到的复合材料图；
图4为实施例3制备得到的复合材料图；
图中：硅片基底(1)、石墨烯(2)、硫化铅(3)、氧化锌(4)。
具体实施方式
下面结合实施例对本发明作进一步说明，但不应该理解为本发明上述主题范围仅限于下述实施例。在不脱离本发明上述技术思想的情况下，根据本领域普通技术知识和惯用手段，做出各种替换和变更，均应包括在本发明的保护范围内。
实施例1：
本实施例中，氧化锌/石墨烯/硫化铅复合材料的制备方法，包括以下步骤:
S1.将17g六水合硝酸锌(Zn(NO3)2.6H2O)溶解于100ml超纯水中，得到硝酸锌溶液。
S2.在硝酸锌溶液中加入5ml氨水(浓度为13.33mol/l)，并磁力搅拌进行反应，转速为65rpm，温度为85℃，得到氢氧化锌混合溶液。
S3.将石墨烯薄膜利用湿法技术转移到硅片基底上，然后置于氢氧化锌混合溶液中，水浴沉积1min，分离，得到前置样品。
S4.将前置样品放置于加热板上预加热3h，加热温度为120℃。
S5.然后再放置于微波等离子体化学气相沉积装置中，采用化学气相沉积法，在氩气氛围下，对前置样品加热。其中氩气的流速为120sccm，加热时间为3min，微波功率为700W，得到氧化锌/石墨烯样品。
S6.采用电化学沉积法，将氧化锌/石墨烯样品固定在电化学反应工作站的工作电极上，对比电极为铂片，参比电极为氯化钾电极，然后将三相电极的反应端置于前驱体混合溶液中，还原反应电压为-0.75v，沉积时间为30min，在氧化锌/石墨烯样品上沉积硫化铅薄膜。所述前驱体混合溶液为乙酸铅、乙二胺四乙酸二钠、硫化钠的混合溶液，调节混合溶液,PH值为9.0；乙酸铅溶液浓度为20mmol/l，乙二胺四乙酸二钠溶液浓度为10mmol/l，硫化钠溶液浓度为0.15mmol/l，乙酸铅溶液：乙二胺四乙酸二钠溶液：硫化钠溶液的体积比为2：2：1。
S7.沉积完成后，获得如图2所示的硫化铅/氧化锌/石墨烯的复合材料。
实施例2：
本实施例与实施例1的不同点在于：步骤S6中，还原反应电压为-0.85v，获得的硫化铅/氧化锌/石墨烯的复合材料如图3所示。
实施例3：
本实施例与实施例1的不同点在于：步骤S6中，还原反应电压为-0.95v，获得的硫化铅/氧化锌/石墨烯的复合材料如图4所示的。
参考附图2-4，随着沉积电位往负方向移动，沉积的硫化铅薄膜致密性较好，颗粒变大，其中实施例1中得到的复合材料均匀度最好。

Claims (4)

1.一种用于光电探测的复合材料的制备方法，其特征在于，包括以下步骤:
S1.将硝酸锌溶解于超纯水中，得到浓度为0.04-0.07mol/l的硝酸锌溶液；
S2.在硝酸锌溶液中加入能够使硝酸锌完全反应的氨水，并磁力搅拌进行反应，得到氢氧化锌混合溶液；
S3.将石墨烯薄膜利用湿法技术转移到硅片基底上，然后置于氢氧化锌混合溶液中，水浴沉积，分离，得到前置样品；
S4.将前置样品预加热0.5h-3h，加热温度为90℃—150℃；然后采用化学气相沉积法，在保护气体氛围下，对前置样品加热，其中加热时间为1-5min，微波功率为700W，得到氧化锌/石墨烯样品；
S5.采用电化学沉积法，将氧化锌/石墨烯样品置于前驱体混合溶液中，在氧化锌/石墨烯样品上沉积硫化铅薄膜；所述前驱体混合溶液为乙酸铅、乙二胺四乙酸二钠、硫化钠的混合溶液；
S6.沉积完成后，获得硫化铅/氧化锌/石墨烯的复合材料。
2.如权利要求1所述的一种用于光电探测的复合材料的制备方法，其特征在于，步骤S5中所述的前驱体混合溶液的制备方法为：在乙酸铅混合溶液中依次倒入乙二胺四乙酸二钠溶液、硫化钠溶液，其中：乙酸铅溶液浓度为20mmol/l，乙二胺四乙酸二钠溶液浓度为10mmol/l，硫化钠溶液浓度为0.15mmol/l；乙酸铅溶液：乙二胺四乙酸二钠溶液：硫化钠溶液的体积比为2：2：1。
3.如权利要求1或2所述的一种用于光电探测的复合材料的制备方法，其特征在于，步骤S5中电化学沉积法选择恒电位沉积，其中沉积电位的选择由线性循环伏安分析来确定，沉积电位选择范围为-0.75v～-0.95v，沉积时间范围为10min-60min。
4.如权利要求3所述的一种用于光电探测的复合材料的制备方法，其特征在于，步骤S4中所述保护气体为氩气。
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