CN107359217A - 一种快速响应紫外光探测器及制备方法 - Google Patents
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Abstract
一种快速响应紫外光探测器及其制备方法,属于半导体光电探测器技术领域。从下到上由石英片衬底、Ag NPs内部修饰的纳米TiO2薄膜有源层基体、在该有源层基体上制备的Au插指电极组成,待测的紫外光从石英片衬底底部入射。首先采用溶胶凝胶技术制备TiO2溶胶,并在石英衬底上依次制备TiO2薄膜、蒸镀Ag NPs、制备TiO2薄膜,得到Ag NPs内部修饰的纳米TiO2薄膜有源层基体材料;接着进行光刻、磁控溅射、剥离金属在薄膜表面形成插指图案的Au电极。本发明制备的快速响应紫外光探测器采用的工艺简单,而且Ag和TiO2资源丰富,易于大规模生产,能够实现对波长250~350nm的紫外光的优良检测。
Description
技术领域
本发明属于半导体光电探测器技术领域,具体涉及一种以石英片为衬底、以AgNPs内部修饰的纳米TiO2薄膜有源层为基体材料、以Au为金属插指电极的快速响应紫外光探测器及其制备方法。
背景技术
宽禁带半导体紫外光探测器由于其小型化、功耗低、成本低、精度高等优点,在现代通信、火焰探测、臭氧检测等方面得到广泛的应用。随着半导体材料和器件在制作技术的更新和发展,现代紫外探测器向着高稳定性、高灵敏度、高速度、高信噪比的方向不断发展。
TiO2作为一种氧化物半导体材料,禁带宽度较大,在紫外波段具有良好的吸收特性,而几乎不吸收可见光。TiO2良好的光电特性和化学稳定性使其在紫外光电器件方面具有明显的优势,但是纯TiO2基紫外探测器的吸收度还有待提高,且其响应恢复时间较长,且暗电流大。
近几年,金属纳米粒子的等离子共振效应在生物传感、纳米光谱、太阳能电池方面得到应用发展。表面等离子体共振是指自由电子在金属和半导体之间的集体振荡。这种效应能够实现对光的聚集和充分利用。相比于纯材料衬底制备的紫外探测器,通过修饰金属纳米粒子产生的等离子体共振效应能够加快器件对光子的收集转换,提高响应度和响应速度。
以Ag NPs内部修饰的纳米TiO2薄膜有源层为基体的快速响应紫外光探测器综合了TiO2作为紫外探测器衬底的优异光电性能和金属纳米粒子等离子体共振速度快等优点,使器件响应时间和恢复时间得到有效改善,显示出在紫外探测器领域的独特优势和发展前景。
发明内容
本发明目的在于提供一种快速响应紫外光探测器及其制备方法。
本发明采用石英片作为衬底,以Ag NPs内部修饰的纳米TiO2薄膜有源层基体材料制备紫外光探测器,可以有效缩短响应时间。同时本发明采用的工艺简单,适与半导体平面工艺兼容、易于集成、适于大批量生产,因而具有重要的应用价值。
本发明的快速响应紫外光探测器从下到上由石英片衬底、Ag NPs内部修饰的纳米TiO2薄膜有源层基体、在该有源层基体上制备的Au插指电极组成,待测的紫外光从石英片衬底底部入射;其中石英片衬底的厚度为0.9~1.1mm,金属插指电极的指间距、指宽度、厚度分别为5~30μm、5~30μm、50~150nm;且Ag NPs内部修饰的纳米TiO2薄膜有源层由如下步骤制备得到:
(一)纳米TiO2溶胶的制备
采用溶胶-凝胶法制备纳米TiO2溶胶:在室温及磁力搅拌条件下,向5~10mL无水乙醇中加入5~10mL钛酸四丁酯,搅拌30~60分钟后,缓慢加入5~10mL冰醋酸后搅拌30~60分钟,得到均匀透明的淡黄色溶液;接着加入5~10mL乙酰丙酮以抑制酯类水解,此时溶液颜色逐渐变深,继续搅拌60~90分钟;最后将8~10mL去离子水逐滴缓慢滴加入上述溶液中,再持续搅拌12~15小时,得到均匀透明的橙黄色溶胶,将其放置陈化6~12小时,得到纳米TiO2溶胶;
(二)衬底的处理
将石英片衬底依次置于丙酮、乙醇和去离子水中分别超声清洗10~15分钟,氮气吹干,最后放入紫外臭氧环境中处理10~15分钟;
(三)Ag NPs内部修饰的TiO2薄膜有源层基体的制备
(1)采用旋涂法将陈化的纳米TiO2溶胶旋涂在处理后的石英片衬底上形成薄膜,旋涂速度为3000~3500转/分钟,100~120℃下烘干10~20分钟;重复此步骤1~4次;然后于450~500℃下烧结2~3小时,自然冷却至室温;
(2)采用蒸镀法在所得TiO2薄膜上蒸镀1.5~4nm的Ag NPs;
(3)在生长有Ag NPs的TiO2薄膜上继续旋涂TiO2溶胶形成薄膜,旋涂速度为3000~3500转/分钟,100~120℃下烘干10~20分钟;重复此步骤1~4次;
(4)最后于450~500℃下烧结2~3小时,自然冷却至室温,从而得到Ag NPs内部修饰的TiO2薄膜有源层基体,该有源层的总厚度为80~120nm。
本发明所述的快速响应紫外光探测器的制备方法,其步骤如下:
(1)在Ag NPs内部修饰的TiO2薄膜有源层基体上采用光刻工艺制备插指电极:在Ag NPs内部修饰的TiO2薄膜有源层衬底上旋涂一层厚度为1~2μm的光刻胶(正胶BP212,转速为2500~3500转/分钟),80~100℃下前烘10-20分钟;采用与插指电极图案互补的掩膜板,对旋涂有光刻胶的衬底进行80~100秒的曝光,经过20~30秒的显影,最后在100~120℃下坚膜15~20分钟,从而在Ag NPs内部修饰的TiO2薄膜有源层衬底上得到所需要的光刻胶插指电极图案;
(2)采用磁控溅射技术制备金属插指电极:将光刻后表面有光刻胶插指电极图案的衬底置于真空室中,抽真空至4.0×10-3~6.0×10-3Pa;接着通Ar气,溅射气压为3~5Pa,溅射功率为50~100W,溅射时间10~15分钟,溅射靶为Au靶;最后将衬底置于丙酮中超声30~50秒,未被曝光的光刻胶及覆盖其上的金属即被剥离,然后用去离子水冲洗后吹干,从而得到一种快速响应紫外光探测器。
附图说明
图1:本发明的器件的结构示意图;
图2:本发明的器件在290nm紫外光照射下的光、暗电流特性曲线;
图3:器件的响应时间曲线。
如图1所示,紫外光从石英片底部照射Ag NPs内部修饰的纳米TiO2薄膜有源层基体上产生光电流;各部件名称为:石英片1、TiO2薄膜2、Ag NPs层3、TiO2薄膜4、金属插指电极5;
如图2所示,可知当Ag NPs在TiO2薄膜内部不同厚度处进行修饰时,在紫外光照及6V偏压下,光暗电流比相差3个数量级,能够用于紫外光的探测;
如图3所示,当Ag NPs在TiO2薄膜内部不同厚度处修饰时,器件的响应时间相比于纯TiO2薄膜基器件的响应时间得到提高,上升时间下降20%~50%左右,下降时间缩短60%~70%左右。
具体实施方式
实施例1:
采用溶胶-凝胶法制备纳米TiO2溶胶:在室温及磁力搅拌的条件下,向100mL无水乙醇中加入10mL钛酸四丁酯,搅拌60分钟后,缓慢加入10mL冰醋酸进行搅拌,在60分钟后,冰醋酸的催化作用使钛酸四丁酯和乙醇完全形成易水解酯,继续搅拌30分钟,得到均匀透明的淡黄色溶液;接着加入10mL乙酰丙酮以抑制酯类水解,此时溶液颜色逐渐变深,继续搅拌90分钟;最后将10mL去离子水缓慢逐滴加入所得溶液中,使搅拌接着持续12小时,得到均匀透明的橙黄色溶胶,将其放置陈化12小时,得到纳米TiO2溶胶。
采用旋涂法将陈化的纳米TiO2溶胶旋涂在处理后的石英片衬底上形成薄膜,旋涂速度为3000转/分钟;120℃下烘干10分钟,旋涂次数为1次,接着放入马弗炉中在450℃下烧结2.1小时,自然冷却至室温,得到的TiO2膜厚为20nm;采用蒸镀法在40A、的条件下进行蒸镀1.5nm厚的Ag NPs;接着重复如上所述的TiO2溶胶旋涂烘干步骤,旋涂4层TiO2溶胶凝胶进行450℃,2.1小时烧结,并自然冷却至室温,得到TiO2薄膜有源层基体,所得有源层膜厚为93nm。
在制备好的Ag NPs内部修饰的纳米TiO2薄膜有源层基体上采用标准光刻工艺制备插指电极:在衬底上旋涂一层光刻胶(正胶BP212,转速为3500转/分钟),100℃下前烘10分钟;在光刻机上采用在与金属插指电极图形互补的掩模板对涂有光刻胶的衬底进行93秒的曝光,经过20秒的显影(显影液由上述正型光刻胶显影液与去离子水按体积比2:1配成),并用去离子水进行冲洗,氮气枪吹干;最后在120℃下坚膜15分钟,最后在Ag NPs内部修饰的纳米TiO2薄膜有源层基体上得到所需要的光刻胶插指电极图案。
采用磁控溅射技术制备金属电极,将光刻后表面有光刻胶插指电极图案的石英片衬底置于真空室中,抽真空至50×10-3Pa;接着通Ar气,溅射气压为5Pa,溅射功率80W,溅射时间10分钟,溅射靶材为Au靶;得到Au薄膜的厚度为100nm;最后将所得石英衬底置于丙酮中超声30秒,未被曝光的光刻胶及覆盖其上的金属即被剥离,将器件用去离子水冲洗后用氮气枪吹干,从而得到一种快速响应紫外探测器,其结构如图1所示。
如图2曲线(1)所示,对本发明所制作的器件的光电性能进行了测试。器件的光暗电流比在6V偏压下能够达到3个数量级,说明该器件对紫外光具有良好的探测能力。
图3(b)为本例制得的快速响应紫外探测器响应时间特性图。器件的上升时间813.6ms,下降时间1.625s。相比于用溶胶-凝胶法制备的纯TiO2基紫外探测器的响应时间(如图3(a)所示,上升时间1.134s,下降时间4.509s),器件的响应时间下降了28.3%,恢复时间下降了64.0%,说明采用Ag NPs修饰后TiO2基紫外探测器的响应时间得到了提高。
实施例2:
采用溶胶-凝胶法制备纳米TiO2溶胶:在室温及磁力搅拌的条件下,向100mL无水乙醇中加入10mL钛酸四丁酯,搅拌60分钟后,缓慢加入10mL冰醋酸进行搅拌,在60分钟后,冰醋酸的催化作用使钛酸四丁酯和乙醇完全形成易水解酯,继续搅拌30分钟,得到均匀透明的淡黄色溶液;接着加入10mL乙酰丙酮以抑制酯类水解,此时溶液颜色逐渐变深,继续搅拌90分钟;最后将10mL去离子水缓慢逐滴加入所得溶液中,使搅拌接着持续12小时,得到均匀透明的橙黄色溶胶,将其放置陈化12小时,得到纳米TiO2溶胶。
采用旋涂法将陈化的纳米TiO2溶胶旋涂在处理后的石英片衬底上形成薄膜,旋涂速度为3000转/分钟;120℃下烘干10分钟,重复上述旋涂烘干步骤,使得旋涂次数为2,接着放入马弗炉中在450℃下烧结2.1小时,自然冷却至室温,得到的TiO2膜厚为35nm;采用蒸镀法在40A、的条件下蒸镀1.5nm厚的Ag NPs;接着用如上所述的方法继续旋涂3层TiO2溶胶凝胶进行450℃,2.1小时烧结,并自然冷却至室温,得到有源层薄膜衬底,所得有源层膜厚为105nm。
在制备好的Ag NPs内部修饰的纳米TiO2薄膜有源层基体上采用标准光刻工艺制备插指电极:在衬底上旋涂一层光刻胶(正胶BP212,转速为3500转/分钟),100℃下前烘10分钟;在光刻机上采用在与金属插指电极图形互补的掩模板对涂有光刻胶的衬底进行93秒的曝光,经过20秒的显影(显影液由上述正型光刻胶显影液与去离子水按体积比2:1配成),并用去离子水进行冲洗,氮气枪吹干;最后在120℃下坚膜15分钟,最后在Ag NPs内部修饰的纳米TiO2薄膜有源层基体上得到所需要的光刻胶插指电极图案。
采用磁控溅射技术制备金属电极,将光刻后表面有光刻胶插指电极图案的石英片衬底置于真空室中,抽真空至50×10-3Pa;接着通Ar气,溅射气压为5Pa,溅射功率80W,溅射时间10分钟,溅射靶材为Au靶;得到Au薄膜的厚度为100nm;最后将所得石英衬底置于丙酮中超声30秒,未被曝光的光刻胶及覆盖其上的金属即被剥离,将器件用去离子水冲洗后用氮气枪吹干,从而得到一种快速响应紫外探测器紫外光探测器,其结构如图1所示。
如图2曲线(2)所示,对本发明所制作的器件的光电性能进行了测试。器件的光暗电流比在6V偏压下能够超过3个数量级,说明该器件对紫外光具有优良的探测能力。
图3(c)为本例制得的快速响应紫外探测器响应时间特性图。器件的上升时间663.6ms,下降时间1.321s。相比于用溶胶-凝胶法制备的纯TiO2基紫外探测器的响应时间(如图3(a)所示,上升时间1.134s,下降时间4.509s),器件的响应时间下降了41.5%,恢复时间下降了70.7%,说明采用Ag NPs在TiO2薄膜内部进行修饰后TiO2基紫外探测器的响应时间得到了有效的提高。
实施例3:
采用溶胶-凝胶法制备纳米TiO2溶胶:在室温及磁力搅拌的条件下,向100mL无水乙醇中加入10mL钛酸四丁酯,搅拌60分钟后,缓慢加入10mL冰醋酸进行搅拌,在60分钟后,冰醋酸的催化作用使钛酸四丁酯和乙醇完全形成易水解酯,继续搅拌30分钟,得到均匀透明的淡黄色溶液;接着加入10mL乙酰丙酮以抑制酯类水解,此时溶液颜色逐渐变深,继续搅拌90分钟;最后将10mL去离子水缓慢逐滴加入所得溶液中,使搅拌接着持续12小时,得到均匀透明的橙黄色溶胶,将其放置陈化12小时,得到纳米TiO2溶胶。
采用旋涂法将陈化的纳米TiO2溶胶旋涂在处理后的石英片衬底上形成薄膜,旋涂速度为3000转/分钟;120℃下烘干10分钟,重复上述旋涂烘干步骤,使得旋涂次数为4次,接着放入马弗炉中在450℃下烧结2.1小时,自然冷却至室温,得到的TiO2膜厚为50nm;采用蒸镀法在40A、的条件下蒸镀1.5nm厚的Ag NPs;接着用如上所述的方法继续旋涂1层TiO2溶胶凝胶进行450℃,2.1小时烧结,并自然冷却至室温,得到有源层薄膜衬底,所得有源层膜厚为112nm。
在制备好的Ag NPs内部修饰的纳米TiO2薄膜有源层基体上采用标准光刻工艺制备插指电极:在衬底上旋涂一层光刻胶(正胶BP212,转速为3500转/分钟),100℃下前烘10分钟;在光刻机上采用在与金属插指电极图形互补的掩模板对涂有光刻胶的衬底进行93秒的曝光,经过20秒的显影(显影液由上述正型光刻胶显影液与去离子水按体积比2:1配成),并用去离子水进行冲洗,氮气枪吹干;最后在120℃下坚膜15分钟,最后在Ag NPs内部修饰的纳米TiO2薄膜有源层基体上得到所需要的光刻胶插指电极图案。
采用磁控溅射技术制备金属电极,将光刻后表面有光刻胶插指电极图案的石英片衬底置于真空室中,抽真空至50×10-3Pa;接着通Ar气,溅射气压为5Pa,溅射功率80W,溅射时间10分钟,溅射靶材为Au靶;得到Au薄膜的厚度为100nm;最后将所得石英衬底置于丙酮中超声30秒,未被曝光的光刻胶及覆盖其上的金属即被剥离,将器件用去离子水冲洗后用氮气枪吹干,从而得到一种快速响应紫外探测器紫外光探测器,其结构如图1所示。
如图2曲线(3)所示,对本发明所制作的器件的光电性能进行了测试。器件的光暗电流比在6V偏压下能够达到3个数量级,说明该器件对紫外光具有良好的探测能力。
图3(d)为本例制得的快速响应紫外探测器响应时间特性图。器件的上升时间534.6ms,下降时间1.232s。相比于用溶胶-凝胶法制备的纯TiO2基紫外探测器的响应时间(如图3(a)所示,上升时间1.134s,下降时间4.509s),器件的响应时间下降了52.9%,恢复时间下降了72.7%,说明采用Ag NPs修饰后TiO2基紫外探测器的响应时间得到了有效的提高,并且当Ag NPs越远离石英衬底,靠近叉指电极一侧时,器件的响应时间越快。
Claims (6)
1.一种快速响应紫外光探测器,其特征在于:从下到上由石英片衬底、Ag NPs内部修饰的纳米TiO2薄膜有源层基体、在该有源层基体上制备的Au插指电极组成,待测的紫外光从石英片衬底底部入射;并且Ag NPs内部修饰的纳米TiO2薄膜有源层由如下步骤制备得到,
(1)采用旋涂法将陈化的纳米TiO2溶胶旋涂在处理后的石英片衬底上形成薄膜,旋涂速度为3000~3500转/分钟,100~120℃下烘干10~20分钟;重复此步骤1~4次;然后于450~500℃下烧结2~3小时,自然冷却至室温;
(2)采用蒸镀法在所得TiO2薄膜上蒸镀1.5~4nm的Ag NPs;
(3)在生长有Ag NPs的TiO2薄膜上继续旋涂TiO2溶胶形成薄膜,旋涂速度为3000~3500转/分钟,100~120℃下烘干10~20分钟;重复此步骤1~4次;
(4)最后于450~500℃下烧结2~3小时,自然冷却至室温,从而得到Ag NPs内部修饰的TiO2薄膜有源层基体,该有源层的总厚度为80~120nm。
2.如权利要求1所述的一种快速响应紫外光探测器,其特征在于:石英片衬底的厚度为0.9~1.1mm,金属插指电极的指间距、指宽度、厚度分别为5~30μm、5~30μm、50~150nm。
3.如权利要求1所述的一种快速响应紫外光探测器,其特征在于:是在室温及磁力搅拌条件下,向5~10mL无水乙醇中加入5~10mL钛酸四丁酯,搅拌30~60分钟后,缓慢加入5~10mL冰醋酸后搅拌30~60分钟,得到均匀透明的淡黄色溶液;接着加入5~10mL乙酰丙酮以抑制酯类水解,此时溶液颜色逐渐变深,继续搅拌60~90分钟;最后将8~10mL去离子水逐滴缓慢滴加入上述溶液中,再持续搅拌12~15小时,得到均匀透明的橙黄色溶胶,将其放置陈化6~12小时,得到纳米TiO2溶胶。
4.如权利要求1所述的一种快速响应紫外光探测器,其特征在于:处理后的石英片衬底是将石英片衬底依次置于丙酮、乙醇和去离子水中分别超声清洗10~15分钟,氮气吹干,最后放入紫外臭氧环境中处理10~15分钟。
5.权利要求1~4任何一项所述的一种快速响应紫外光探测器的制备方法,其步骤如下:
(1)在Ag NPs内部修饰的TiO2薄膜有源层基体上采用光刻工艺制备插指电极:在Ag NPs内部修饰的TiO2薄膜有源层衬底上旋涂一层厚度为1~2μm的光刻胶,80~100℃下前烘10-20分钟;采用与插指电极图案互补的掩膜板,对旋涂有光刻胶的衬底进行80~100秒的曝光,经过20~30秒的显影,最后在100~120℃下坚膜15~20分钟,从而在Ag NPs内部修饰的TiO2薄膜有源层衬底上得到所需要的光刻胶插指电极图案;
(2)采用磁控溅射技术制备金属插指电极:将光刻后表面有光刻胶插指电极图案的衬底置于真空室中,抽真空至4.0×10-3~6.0×10-3Pa;接着通Ar气,溅射气压为3~5Pa,溅射功率为50~100W,溅射时间10~15分钟,溅射靶为Au靶;最后将衬底置于丙酮中超声30~50秒,未被曝光的光刻胶及覆盖其上的金属即被剥离,然后用去离子水冲洗后吹干,从而得到快速响应紫外光探测器。
6.如权利要求5所述的一种快速响应紫外光探测器的制备方法,其特征在于:光刻胶为正胶BP212。
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