CN109119511B - 一种纳米棒阵列异质结结构紫外光探测器的制备方法 - Google Patents
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- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 3
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Abstract
本发明公开了一种纳米棒阵列异质结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,再在其表面生长有序排列的ZnO纳米棒阵列,构成异质结结构,促进光生电子传递。其制备方法简单、反应条件易控、操作费用低。将所制得电极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。该紫外光探测器具有极好的紫外光选择性、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
近年来,随着科技水平的不断提高,光电检测技术测量范围不断变大。该检测技术所能检测到的波长范围已经扩大到了人们不易探测的处于10nm至400nm之间的紫外光区域。检测范围的扩大也相应地使得紫外强度检测仪器的研发与制造得到飞速发展,测量技术也不断改进提高,而其中的紫外探测器是目前国内外光电检测方面的重点研究课题之一。
商业化的紫外光探测器主要基于Si、GaAs等半导体材料,但他们的禁带宽度较窄,紫外光选择性较差。因此,宽禁带的金属氧化物半导体材料(ZnO、SnO2、Ga2O3等)引起了研究者的广泛关注,并且金属氧化物半导体材料易得、结构易控以及具有优异的物理化学性能。
SnO2和ZnO是两种重要的N型宽禁带半导体材料,其中,SnO2的禁带宽度为3.62eV(300K),具有良好的紫外光选择性、较高的电子稳定性及电子传输能力;ZnO的禁带宽度为3.37eV(300K),在紫外光区具有较高的光电导电性,并且化学、热稳定性良好。SnO2和ZnO纳米结构主要包括:纳米棒、纳米线、纳米颗粒等。其中,纳米棒阵列结构可为电子提供定向的传输通道,提高电子的传输速率、减少电子传输过程中的损失。
研究发现,纯SnO2、ZnO纳米棒结构紫外光探测器的响应速率较慢,这是因为尽管SnO2纳米棒的紫外光响应度较高,但其生长速率较慢,反应24h后仅仅200nm左右,影响其对光电子的吸收及传递,导致其光响应时间较长;而水热法制备ZnO纳米棒具有生长速率快的优点,反应4h后长度大于1μm,但光响应度较低。因此,为获得兼具SnO2、ZnO纳米棒阵列结构优点的紫外光探测器,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FTO导电玻璃上旋涂氧化锡晶种层,水热法在其上生长有序排列的SnO2纳米棒阵列,水热法在SnO2纳米棒阵列表面上生长有序排列的ZnO纳米棒阵列,构成异质结结构;SnO2纳米棒阵列的直径为8.93~62.50nm,长度为127.5~553.1nm;ZnO纳米棒阵列的直径为53.55~129.7nm,长度为0.872~3.19μm。
氧化锡晶种层的制备方法如下:将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6~10次后,在400℃条件下高温煅烧30min;
SnO2纳米棒阵列的制备方法如下:向浓度为6~14mM SnCl4·5H2O溶液中加入37~38wt%HCl,二者的体积比为15~20;搅拌5~20min后,加入涂有氧化锡晶种层的FTO导电玻璃,160~200℃反应8~14h;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;
更新SnO2纳米棒阵列生长液的制备方法如下:将干燥的长有SnO2纳米棒阵列的FTO导电玻璃再次放入配制好的SnCl4·5H2O溶液中,后续步骤同上。
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。
ZnO晶种层的制备方法如下:将5.0~10.0mM醋酸锌的乙醇溶液旋涂于FTO导电玻璃上,旋涂速率1500~3000r/min,旋涂时间30s,旋涂4~8次后,在350℃条件下高温煅烧60min;
ZnO纳米棒阵列的制备方法如下:Zn(NO3)2·6H2O和乌洛托品(C6H12N4)按照摩尔比为1:1混合,加入去离子水,控制Zn(NO3)2·6H2O的浓度为15~30mM;搅拌5~30min后,加入涂有ZnO晶种层的FTO导电玻璃,85~100℃反应4~8h;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;
更新ZnO纳米棒阵列生长液的制备方法如下:将干燥的长有ZnO纳米棒阵列的FTO导电玻璃再次放入配制好的Zn(NO3)2·6H2O溶液中,后续步骤同上。
本发明的有益效果:该紫外光探测器具有极好的紫外光选择性、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复合结构断面电镜图(实施例1)。
图2是氧化锡-氧化锌纳米棒阵列复合结构表面电镜图(实施例2)。
图3是氧化锡-氧化锌纳米棒阵列复合结构断面电镜图(实施例2)。
图4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
图5是氧化锡-氧化锌纳米棒阵列复合结构紫外光探测器性能图(实施例2)。
图中:1ZnO纳米棒阵列;2SnO2纳米棒阵列;3FTO导电玻璃;4紫外光。
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15min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。更新3次生长液,即得到所要SnO2纳米棒阵列结构。
氧化锡纳米棒直径为44.64nm,长度为357.14nm。
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3mL HCl(wt%=37~38%),磁力搅拌15min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5.0mM醋酸锌的乙醇溶液旋涂于FTO导电玻璃上,旋涂速率2000r/min,旋涂时间30s,旋涂6次后,在350℃条件下高温煅烧60min。将处理好的样品置于含有0.37g Zn(NO3)2·6H2O和0.17g乌洛托品(C6H12N4)的50mL水溶液中;磁力搅拌15min后,加入涂有ZnO晶种层的FTO导电玻璃,95℃反应4h;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。重复上述条件更新ZnO生长液1次,得到所要的SnO2-ZnO纳米棒阵列结构。
氧化锌纳米棒直径为116.07nm,长度为3.134μm。
氧化锡-氧化锌纳米棒阵列复合结构紫外光光探测器的光电流达0.23mA,暗电流为3.57μA,上升时间和恢复时间分别为0.2s和5.6s,紫外光选择性达64.43。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 (4)
1.一种纳米棒阵列异质结结构紫外光探测器的制备方法,其特征在于,步骤如下:
在FTO导电玻璃上旋涂氧化锡晶种层,水热法在其上生长有序排列的SnO2纳米棒阵列,水热法在SnO2纳米棒阵列表面上生长有序排列的ZnO纳米棒阵列,构成异质结结构;SnO2纳米棒阵列的直径为8.93~62.50nm,长度为127.5~553.1nm;ZnO纳米棒阵列的直径为53.55~129.7nm,长度为0.872~3.19μm。
2.根据权利要求1所述的制备方法,其特征在于,
氧化锡晶种层的制备方法如下:将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6~10次后,在400℃条件下高温煅烧30min;
SnO2纳米棒阵列的制备方法如下:向浓度为6~14mM SnCl4·5H2O溶液中加入37~38wt%HCl,二者的体积比为15~20;搅拌5~20min后,加入涂有氧化锡晶种层的FTO导电玻璃,160~200℃反应8~14h;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;
更新SnO2纳米棒阵列生长液的制备方法如下:将干燥的长有SnO2纳米棒阵列的FTO导电玻璃再次放入配制好的SnCl4·5H2O溶液中,后续步骤同上。
3.根据权利要求2所述的制备方法,其特征在于,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。
4.根据权利要求1~3任一所述的制备方法,其特征在于,
ZnO晶种层的制备方法如下:将5.0~10.0mM醋酸锌的乙醇溶液旋涂于FTO导电玻璃上,旋涂速率1500~3000r/min,旋涂时间30s,旋涂4~8次后,在350℃条件下高温煅烧60min;
ZnO纳米棒阵列的制备方法如下:Zn(NO3)2·6H2O和乌洛托品(C6H12N4)按照摩尔比为1:1混合,加入去离子水,控制Zn(NO3)2·6H2O的浓度为15~30mM;搅拌5~30min后,加入涂有ZnO晶种层的FTO导电玻璃,85~100℃反应4~8h;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;
更新ZnO纳米棒阵列生长液的制备方法如下:将干燥的长有ZnO纳米棒阵列的FTO导电玻璃再次放入配制好的Zn(NO3)2·6H2O溶液中,后续步骤同上。
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CN101323975B (zh) * | 2008-07-14 | 2011-01-12 | 中国科学院理化技术研究所 | 制备SnO2-ZnO异质纳米枝杈结构的方法 |
KR20130023608A (ko) * | 2011-08-29 | 2013-03-08 | 한국과학기술연구원 | 벌크 헤테로 접합 무기 박막 태양전지 및 이의 제조 방법 |
KR101498157B1 (ko) * | 2013-05-24 | 2015-03-09 | 인하대학교 산학협력단 | 산화아연-산화주석의 나노섬유-나노와이어 줄기-가지 이종구조물, 이의 제조방법 및 이를 포함하는 가스센서 |
LU92836B1 (fr) * | 2015-09-24 | 2017-04-03 | Luxembourg Inst Science & Tech List | Membranes de filtration biocompatibles et poreuses comprenant des photocatalyseurs |
CN105603713B (zh) * | 2015-11-13 | 2017-12-08 | 大连民族大学 | 一种同轴异质结构的SnO2/ZnO纳米复合纤维材料的制备方法和应用 |
CN105948105B (zh) * | 2016-05-06 | 2017-10-31 | 西北大学 | 一种SnO2/ZnO纳米复合材料及其制备方法 |
CN106053556B (zh) * | 2016-05-13 | 2018-05-22 | 吉林大学 | 一种基于ZnO/SnO2异质结构复合材料的乙醇气体传感器及其制备方法 |
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