CN108682716A - 一种高性能半导体氧化物复合结构紫外光探测器的制备方法 - Google Patents
一种高性能半导体氧化物复合结构紫外光探测器的制备方法 Download PDFInfo
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Abstract
本发明公开了一种高性能半导体氧化物复合结构紫外光探测器的制备方法，属于半导体光电探测技术领域。本发明首先水热合成了有序排列的SnO2纳米棒阵列，再在其表面担载具有大量分枝结构的TiO2纳米颗粒，构成多级分枝结构，其制备方法简单、操作费用低。之后，将所制得电极板材料导电面面对面贴合，构成结构简单的三明治结构的紫外光探测器。该探测器不仅具有极好的紫外光选择性、较高的探测灵敏度，而且具有优异的紫外光响应度和光响应速率，解决了紫外光探测器高响应度和高响应速率难以兼得的问题，是一种高性能的紫外光探测器。
Description
技术领域
本发明属于半导体光电探测技术领域，具体涉及一种金属氧化物半导体纳米复合材料电极制备的方法。
背景技术
光探测器是一种能够把光辐射能量转换成便于测量的物理量的器件，其原理是光电效应——在高于一个特定频率的电磁波照射下，某些物质内部的电子会被光子激发出来生成电流，即光生电。其中，紫外光探测器在军事、医疗、科学研究等各个领域中均有广泛应用，如环境监测、紫外通信、紫外预警及生物化学分析等。然而，商业化的紫外光探测器仍具有紫外光选择性差、响应时间长、响应度低等缺点，这不仅有碍于紫外光监测，还会产生大量能源消耗。因此，亟需制备高性能的紫外光探测器。
已经商业化的紫外光探测器半导体材料禁带宽度较窄，紫外光选择性较差，需配有可见、红外光过滤器，器件复杂且成本较高。而禁带宽度大于3eV的宽带隙材料，具有本征的对可见光不响应的特点，具有优异的紫外光选择性。以宽禁带材料为吸收介质研制的探测器将对紫外光子产生直接响应，可简化光通道，大幅降低成本，并在热导、热稳定性、抗腐蚀方面有很大的优势。氧化锡半导体材料在常温下禁带宽度为3.6eV，不仅具有较大的禁带宽度，而且具有较高的电子稳定性及电子传输能力，引起了研究者的广泛关注。研究发现，氧化锡纳米材料具有极高的紫外光响应度，但响应速率较低，需对其进行进一步的改进。
发明内容
基于现有技术中存在的问题，本发明的目的在于制备一种兼具高光响应度和高光响应速率的紫外光探测器的方法。
本发明的技术方案：
一种高性能半导体氧化物复合结构紫外光探测器的制备方法，步骤如下：
在掺杂F的氧化锡(FTO)导电玻璃上旋涂一层氧化锡晶种，水热法在其上生长有序排列的氧化锡纳米棒阵列，沉积法在氧化锡纳米棒阵列表面上担载多分枝结构的氧化钛纳米颗粒。
所述的晶种层的制备方法如下：将1.0～5.0mM醋酸亚锡的乙醇溶液旋涂于FTO导电玻璃上，旋涂速率2000～3000r/min，旋涂时间30s，旋涂4～10次后，在400℃条件下高温煅烧30～60min；
所述的氧化锡纳米棒阵列的制备方法如下：向浓度为6.0-14.0mM
SnCl4·5H2O溶液中加入37～38wt％HCl，其中，SnCl4·5H2O溶液中使用的溶剂为体积比为1:1的去离子水和无水乙醇，SnCl4·5H2O溶液与37～38wt％HCl的体积比不大于2:3～7；磁力搅拌10min后，加入涂有晶种层的FTO导电玻璃，140～200℃反应6～14h；反应结束冷却至室温，去离子水和无水乙醇交替冲洗3次后60℃干燥，400℃条件下高温煅烧30min。
所述的氧化锡纳米棒阵列直径为8～70nm，长度为120～200nm。
所述的多分枝结构的氧化钛纳米颗粒的制备方法如下：将长有氧化锡纳米棒阵列的FTO导电玻璃置于0.1～0.4M TiCl4的水溶液中，室温条件下反应24～72h。
所述的氧化钛纳米颗粒具有大量分枝结构，其直径分布在200-450nm之间。
本发明的有益效果：该紫外光探测器对可见光及红外光几乎无吸收能力，具有极好的紫外光选择性和较高的探测灵敏度，且兼具优异的紫外光响应度和光响应速率。
附图说明
图1是氧化锡纳米棒阵列表面电镜图(实施例1)。
图2是氧化锡纳米棒阵列-氧化钛纳米颗粒复合结构表面电镜图(实施例2)。
图3是本发明的高性能半导体氧化物复合结构紫外光探测器示意图。
具体实施方式
以下结合附图和技术方案，进一步说明本发明的具体实施方式。
实施例1
配置13mM的SnCl4·5H2O溶液(去离子水：无水乙醇＝1:1)60mL，加入3mL HCl(wt％＝37～38％)，磁力搅拌10min后，加入涂有晶种层的FTO导电玻璃，180℃反应12h。反应结束冷却至室温，去离子水和无水乙醇交替冲洗3次后60℃干燥，400℃条件下高温煅烧30min，即得到所要SnO2纳米棒阵列结构。
氧化锡纳米棒直径为30nm，长度为200nm。
实施例2
配置13mM的SnCl4·5H2O溶液(去离子水：无水乙醇＝1:1)60mL，加入4mL HCl(wt％＝37～38％)，磁力搅拌10min后，加入涂有晶种层的FTO导电玻璃，180℃反应12h。反应结束冷却至室温，去离子水和无水乙醇交替冲洗3次后60℃干燥，400℃条件下高温煅烧30min。将所得产物置于30mL、0.2M TiCl4水溶液中，室温条件下反应36h后，去离子水和无水乙醇交替冲洗3次后室温干燥。
所得氧化钛纳米颗粒直径约为450nm，具有大量的分枝结构，有利于光电子的生成。
氧化锡纳米棒阵列-氧化钛纳米颗粒复合结构紫外光光探测器的光响应度达21.61AW-1，响应时间小于1s，紫外光选择性达113。复合结构光探测器的光电流随紫外光光强的增加而增大，在较低的光强度183nW下，仍具有较好的光响应度，即具有较高的探测灵敏度。并且，该光探测器对可见光及红外光几乎无吸收能力，具有极好的紫外光选择性。
Claims (10)
1.一种高性能半导体氧化物复合结构紫外光探测器的制备方法，其特征在于，步骤如下：
在掺杂F的氧化锡导电玻璃FTO上旋涂氧化锡晶种层，水热法在其上生长有序排列的氧化锡纳米棒阵列，沉积法在氧化锡纳米棒阵列表面上担载多分枝结构的氧化钛纳米颗粒。
2.根据权利要求1所述的制备方法，其特征在于，所述的氧化锡晶种层的制备方法如下：将1.0～5.0mM醋酸亚锡的乙醇溶液旋涂于FTO导电玻璃上，旋涂速率2000～3000r/min，旋涂时间30s，旋涂4～10次后，在400℃条件下高温煅烧30～60min。
3.根据权利要求1或2所述的制备方法，其特征在于，所述的氧化锡纳米棒阵列的制备方法如下：向浓度为6.0-14.0mM SnCl4·5H2O溶液中加入37～38wt％HCl，其中，SnCl4·5H2O溶液中使用的溶剂为体积比为1:1的去离子水和无水乙醇，SnCl4·5H2O溶液与37～38wt％HCl的体积比不大于2:3～7；磁力搅拌10min后，加入涂有晶种层的FTO导电玻璃，140～200℃反应6～14h；反应结束冷却至室温，去离子水和无水乙醇交替冲洗3次后60℃干燥，400℃条件下高温煅烧30min。
4.根据权利要求1或2所述的制备方法，其特征在于，所述的氧化锡纳米棒阵列直径为8～70nm，长度为120～200nm。
5.根据权利要求3所述的制备方法，其特征在于，所述的氧化锡纳米棒阵列直径为8～70nm，长度为120～200nm。
6.根据权利要求1、2或5所述的制备方法，其特征在于，所述的多分枝结构的氧化钛纳米颗粒的制备方法如下：将长有氧化锡纳米棒阵列的FTO导电玻璃置于0.1～0.4M TiCl4的水溶液中，室温条件下反应24～72h。
7.根据权利要求3所述的制备方法，其特征在于，所述的多分枝结构的氧化钛纳米颗粒的制备方法如下：将长有氧化锡纳米棒阵列的FTO导电玻璃置于0.1～0.4M TiCl4的水溶液中，室温条件下反应24～72h。
8.根据权利要求4所述的制备方法，其特征在于，所述的多分枝结构的氧化钛纳米颗粒的制备方法如下：将长有氧化锡纳米棒阵列的FTO导电玻璃置于0.1～0.4M TiCl4的水溶液中，室温条件下反应24～72h。
9.根据权利要求1、2、5、7或8所述的制备方法，其特征在于，所述的氧化钛纳米颗粒具有大量分枝结构，其直径分布在200-450nm之间。
10.根据权利要求6所述的制备方法，其特征在于，所述的氧化钛纳米颗粒具有大量分枝结构，其直径分布在200-450nm之间。
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