CN106601858A - 一种基于纳米ZnO‑rGO复合材料的光电导型紫外探测器及其制备方法 - Google Patents
一种基于纳米ZnO‑rGO复合材料的光电导型紫外探测器及其制备方法 Download PDFInfo
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 35
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Abstract
本发明公开了一种基于纳米ZnO‑rGO复合材料的光电导型紫外探测器,该紫外探测器依次有低阻Si层、SiO2绝缘层、纳米ZnO‑rGO旋涂层和Al电极。其制备方法如下:先采用溶剂热法制备ZnO纳米颗粒,用APTES对ZnO纳米颗粒进行表面改性,再用水热法制备ZnO‑rGO复合物,然后将复合物溶液旋涂在Si/SiO2的SiO2面上,再在旋凃层表面镀上Al电极获得紫外探测器。相比基于纳米ZnO的紫外探测器,本发明的紫外探测器暗电流低,光电流、响应度、灵敏度都得到较大提升,且该方法制备的器件结构简单、方法简单易行、成本低、适合大面积制备,在军事、民用以及一些特殊领域有重要的应用价值和良好的应用前景。
Description
技术领域
本发明涉及一种紫外探测器的制备方法,尤其涉及一种基于纳米ZnO-rGO复合材料的光电导型紫外波段探测器及其制备方法,属于半导体器件技术领域。
背景技术
紫外探测技术是以紫外光辐射的大气传输与衰减特性和高性能紫外光学传感器为基础的一门新技术。与传统的红外和激光探测技术相比,紫外探测技术在许多方面的特殊优势使得其在很多的场合都有着广泛的应用价值:军事上,用于紫外告警、紫外通信、紫外/红外复合制导、导弹探测和光电对抗等,民用上,利用紫外探测技术探测太阳紫外辐射强度以及检测细胞病变。然而,至今市场上还是以传统光电倍增管和硅基紫外探测器为主。
ZnO作为一种新型的直接带隙半导体材料,室温下禁带宽度为3.37eV,激子束缚能高达60meV,抗辐射能力强,并且可通过Mg掺杂实现禁带宽度在3.37~7.78eV之间调节,以实现对不同波段紫外线的探测。此外,ZnO有着较为丰富的纳米结构且制备过程简便。相对于传统的光电倍增管和硅基紫外探测器,第三代ZnO基宽禁带半导体材料紫外探测器有着体积小、质量轻、稳定、量子率高、噪声低、响应速度快、光谱响应峰值在紫外波段等特点。同时,它对波长大于400nm的可见光和红外光无阻碍透过,可见光抑制比高,不需要外加滤光片,测量精度高,是紫外探测器的主要研究方向。
发明内容
本发明的目的是提供一种制备成本低、工艺简单、易于大面积生产,且灵敏度、响应度较高的基于纳米ZnO-rGO复合材料的光电导型紫外探测器及其制备方法。
本发明的基于纳米ZnO-rGO复合材料的光电导型紫外探测器,自下而上依次有低阻Si层、SiO2绝缘层、纳米ZnO-rGO旋凃层和Al电极。制备方法包括以下步骤:
1)在烧杯中加入粉末状Zn(CH3COO)2·2H2O和NaOH,再加入无水乙醇,使得Zn(CH3COO)2·2H2O的浓度为0.1mol/L,NaOH的浓度为1mol/L,将烧杯封口后置于室温下充分搅拌直至固体完全溶解并且形成乳白色前驱体溶液;
将上述前驱体溶液转移至聚四氟乙烯内胆中,将内胆放入水热釜中,拧紧,置于150℃烘箱中保温2h;
待水热釜冷却至室温后取出并分管离心,离心产物需用无水乙醇洗涤、再离心2次后放置于60℃烘箱内干燥12h,得到纳米ZnO颗粒;
2)将上述纳米ZnO颗粒加入无水乙醇中,超声使其完全分散,然后加入3-氨丙基三乙氧基硅烷(APTES),使得ZnO(mg):APTES(ml)=0.5~1,在60℃下水浴回流处理4h;
将液体分管离心,并用无水乙醇洗涤、再离心2次后置于60℃的烘箱内干燥12h,得到表面改性后的纳米ZnO颗粒;
3)将表面改性后的纳米ZnO颗粒加入去离子水中,超声使其完全分散后,加入2mg/ml GO水溶液形成混合液,使得GO的质量分数为5%~10%,室温下充分搅拌2h后使GO与ZnO混合均匀;
将上述混合液转移至聚四氟乙烯内胆中,将内胆放入水热釜中,拧紧,置于180℃烘箱中保温12h;
待水热反应完成后装置自然冷却至室温,将产物离心并且先后用去离子水和无水乙醇交替洗涤4次后置于60℃烘箱中干燥12h,得到纳米ZnO-rGO复合材料,并配制浓度为25mg/ml的ZnO-rGO/无水乙醇混合液。
4)在洁净、低阻Si片(1)的SiO2绝缘层(2)上旋涂步骤3)的ZnO-rGO/无水乙醇混合液,转速为1000~3000r/min,旋涂30s,旋涂次数为1~2次,得到纳米ZnO-rGO旋凃层(3);
5)在上述的旋凃层(3)上蒸镀厚度为70~100nm的Al电极(4),获得基于纳米ZnO-rGO复合材料的光电导型紫外探测器。
本发明的基于纳米ZnO-rGO复合材料的光电导型紫外探测器的工作原理是:在一定偏压下,无光照时,纳米ZnO-rGO复合材料导电性较差,暗电流较小;当紫外光照射时,ZnO中产生光子电子和空穴,由于ZnO纳米材料存在表面态和缺陷,易形成陷阱中心捕获光生载流子,而还原氧化石墨烯是良好的受电子体,其特殊的能带结构和优良的导电性能为电子转移和快速传输提供了很好的通道,两者复合使得光生电子和空穴实现快速分离,形成的电流被外电路收集,从而完成对紫外线的探测过程。
本发明的有益效果在于:
1)采用水热法制备纳米氧化锌和还原氧化石墨烯的复合材料,简单易行且重复性好;
2)利用还原氧化石墨烯快速导电子的能力加快ZnO中载流子分离,使得紫外探测器具有较大的光电流,从而有利于获得较高的灵敏度和响应度;
3)本发明的紫外探测器结构简单,其制备方法简便、成本低且适合于大面积制备,在军事、民用以及一些特殊领域有重要的应用价值。
附图说明
图1是基于纳米ZnO-rGO复合材料的光电导型紫外探测器的结构示意图。
图中:1为低阻Si层、2为SiO2绝缘层、3为纳米ZnO-rGO旋凃层、4为Al电极。
具体实施方式
以下结合附图及具体实施例对本发明做进一步阐述。
参照图1,本发明的基于纳米ZnO-rGO复合材料的光电导型紫外探测器,自下而上依次有低阻Si层1、SiO2绝缘层2、纳米ZnO-rGO旋涂层3和Al电极4。
实施例1
1)在250ml烧杯中加入4.36g的粉末状Zn(CH3COO)2·2H2O和8g的片状NaOH,再加入200ml无水乙醇,使得Zn(CH3COO)2·2H2O的浓度为0.1mol/L,NaOH的浓度为1mol/L,将烧杯封口后置于室温下充分搅拌直至固体完全溶解并且形成乳白色前驱体溶液;
将上述前驱体溶液转移至聚四氟乙烯内胆中,将内胆放入水热釜中,将拧紧的水热釜置于150℃烘箱中保温2h;
待水热釜冷却至室温后取出并分管离心,离心产物需用无水乙醇洗涤、再离心2次后放置于60℃烘箱内干燥12h,得到纳米ZnO颗粒。
2)在500ml锥形瓶中加入0.5g纳米ZnO颗粒和200ml无水乙醇,超声30min使其完全分散,然后加入0.5ml 3-氨丙基三乙氧基硅烷(APTES),在60℃下水浴回流处理4h;
将液体分管离心,并用无水乙醇洗涤、再离心2次后置于60℃的烘箱内干燥12h,得到表面改性后的纳米ZnO颗粒。
3)在100ml烧杯中放入0.2g表面改性后的纳米ZnO颗粒和10ml去离子水,超声30min使其完全分散后,加入2mg/ml GO水溶液形成GO的质量分数为10%的混合液,室温下充分搅拌2h后使GO与ZnO能够混合均匀;
将上述混合液转移至聚四氟乙烯内胆中,将内胆放入水热釜中,将拧紧的水热釜置于180℃烘箱中保温12h;
待水热反应完成后装置自然冷却至室温,将产物离心并且先后用去离子水和无水乙醇交替洗涤4次后置于60℃烘箱中干燥12h,得到纳米ZnO-rGO复合材料,并配制浓度为25mg/ml的ZnO-rGO/无水乙醇混合液。
4)在洁净、低阻Si片(1)的SiO2绝缘层(2)上旋涂步骤3)的ZnO-rGO/无水乙醇混合液,转速为1000r/min,旋涂30s,旋涂次数为2次,得到纳米ZnO-rGO旋凃层(3);
5)在上述的旋凃层(3)上蒸镀厚度为70nm的Al电极(4),获得基于纳米ZnO-rGO复合材料的光电导型紫外探测器。
本例制得的基于纳米ZnO-rGO复合材料的光电导型紫外探测器的灵敏度为:S=(Iphoto-Idark)/Idark=532。
实施例2
1)在250ml烧杯中加入4.36g的粉末状Zn(CH3COO)2·2H2O和8g的片状NaOH,再加入200ml无水乙醇,使得Zn(CH3COO)2·2H2O的浓度为0.1mol/L,NaOH的浓度为1mol/L,将烧杯封口后置于室温下充分搅拌直至固体完全溶解并且形成乳白色前驱体溶液;
将上述前驱体溶液转移至聚四氟乙烯内胆中,将内胆放入水热釜中,将拧紧的水热釜置于150℃烘箱中保温2h;
待水热釜冷却至室温后取出并分管离心,离心产物需用无水乙醇洗涤、再离心2次后放置于60℃烘箱内干燥12h,得到纳米ZnO颗粒。
2)在500ml锥形瓶中加入0.5g纳米ZnO颗粒和200ml无水乙醇,超声30min使其完全分散,然后加入0.5ml 3-氨丙基三乙氧基硅烷(APTES),在60℃下水浴回流处理4h;
将液体分管离心,并用无水乙醇洗涤、再离心2次后置于60℃的烘箱内干燥12h,得到表面改性后的纳米ZnO颗粒。
3)在100ml烧杯中放入0.2g表面改性后的纳米ZnO颗粒和10ml去离子水,超声30min使其完全分散后,加入2mg/ml GO水溶液形成GO的质量分数为5%的混合液,室温下充分搅拌2h后使GO与ZnO能够混合均匀;
将上述混合液转移至聚四氟乙烯内胆中,将内胆放入水热釜中,将拧紧的水热釜置于180℃烘箱中保温12h;
待水热反应完成后装置自然冷却至室温,将产物离心并且先后用去离子水和无水乙醇交替洗涤4次后置于60℃烘箱中干燥12h,得到纳米ZnO-rGO复合材料,并配制浓度为25mg/ml的ZnO-rGO/无水乙醇混合液。
4)在洁净、低阻Si片(1)的SiO2绝缘层(2)上旋涂步骤3)的ZnO-rGO/无水乙醇混合液,转速为1000r/min,旋涂30s,旋涂次数为1次,得到纳米ZnO-rGO旋凃层(3);
5)在上述的旋凃层(3)上蒸镀厚度为70nm的Al电极(4),获得基于纳米ZnO-rGO复合材料的光电导型紫外探测器。
本例制得的基于纳米ZnO-rGO复合材料的光电导型紫外探测器的灵敏度为:S=(Iphoto-Idark)/Idark=475。
实施例3
1)在250ml烧杯中加入4.36g的粉末状Zn(CH3COO)2·2H2O和8g的片状NaOH,再加入200ml无水乙醇,使得Zn(CH3COO)2·2H2O的浓度为0.1mol/L,NaOH的浓度为1mol/L,将烧杯封口后置于室温下充分搅拌直至固体完全溶解并且形成乳白色前驱体溶液;
将上述前驱体溶液转移至聚四氟乙烯内胆中,将内胆放入水热釜中,将拧紧的水热釜置于150℃烘箱中保温2h;
待水热釜冷却至室温后取出并分管离心,离心产物需用无水乙醇洗涤、再离心2次后放置于60℃烘箱内干燥12h,得到纳米ZnO颗粒。
2)在500ml锥形瓶中加入0.5g纳米ZnO颗粒和200ml无水乙醇,超声30min使其完全分散,然后加入1ml 3-氨丙基三乙氧基硅烷(APTES),在60℃下水浴回流处理4h;
将液体分管离心,并用无水乙醇洗涤、再离心2次后置于60℃的烘箱内干燥12h,得到表面改性后的纳米ZnO颗粒。
3)在100ml烧杯中放入0.2g表面改性后的纳米ZnO颗粒和10ml去离子水,超声30min使其完全分散后,加入2mg/ml GO水溶液形成GO的质量分数为10%的混合液,室温下充分搅拌2h后使GO与ZnO能够混合均匀;
将上述混合液转移至聚四氟乙烯内胆中,将内胆放入水热釜中,将拧紧的水热釜置于180℃烘箱中保温12h;
待水热反应完成后装置自然冷却至室温,将产物离心并且先后用去离子水和无水乙醇交替洗涤4次后置于60℃烘箱中干燥12h,得到纳米ZnO-rGO复合材料,并配制浓度为25mg/ml的ZnO-rGO/无水乙醇混合液。
4)在洁净、低阻Si片(1)的SiO2绝缘层(2)上旋涂步骤3)的ZnO-rGO/无水乙醇混合液,转速为2000r/min,旋涂30s,旋涂次数为2次,得到纳米ZnO-rGO旋凃层(3);
5)在上述的旋凃层(3)上蒸镀厚度为100nm的Al电极(4),获得基于纳米ZnO-rGO复合材料的光电导型紫外探测器。
本例制得的基于纳米ZnO-rGO复合材料的光电导型紫外探测器的灵敏度为:S=(Iphoto-Idark)/Idark=557。
Claims (2)
1.一种基于纳米ZnO-rGO复合材料的光电导型紫外探测器,其特征在于,该探测器自下而上依次有低阻Si层(1)、SiO2绝缘层(2)、纳米ZnO-rGO旋凃层(3)和Al电极(4)。
2.如权利要求1所述的基于纳米ZnO-rGO复合材料的光电导型紫外探测器的制备方法,其特征在于,该探测器的制备方法包括以下步骤:
1)在烧杯中加入粉末状Zn(CH3COO)2·2H2O和NaOH,再加入无水乙醇,使得Zn(CH3COO)2·2H2O的浓度为0.1mol/L,NaOH的浓度为1mol/L,将烧杯封口后置于室温下充分搅拌直至固体完全溶解并且形成乳白色前驱体溶液;
将上述前驱体溶液转移至聚四氟乙烯内胆中,将内胆放入水热釜中,拧紧,置于150℃烘箱中保温2h;
待水热釜冷却至室温后取出并分管离心,离心产物需用无水乙醇洗涤、再离心2次后放置于60℃烘箱内干燥12h,得到纳米ZnO颗粒;
2)将上述纳米ZnO颗粒加入无水乙醇中,超声使其完全分散,然后加入3-氨丙基三乙氧基硅烷(APTES),使得ZnO(mg):APTES(ml)=0.5~1,在60℃下水浴回流处理4h;
将液体分管离心,并用无水乙醇洗涤、再离心2次后置于60℃的烘箱内干燥12h,得到表面改性后的纳米ZnO颗粒;
3)将表面改性后的纳米ZnO颗粒加入去离子水中,超声使其完全分散后,加入2mg/mlGO水溶液形成混合液,使得GO的质量分数为5%~10%,室温下充分搅拌2h后使GO与ZnO混合均匀;
将上述混合液转移至聚四氟乙烯内胆中,将内胆放入水热釜中,拧紧,置于180℃烘箱中保温12h;
待水热反应完成后装置自然冷却至室温,将产物离心并且先后用去离子水和无水乙醇交替洗涤4次后置于60℃烘箱中干燥12h,得到纳米ZnO-rGO复合材料,并配制浓度为25mg/ml的ZnO-rGO/无水乙醇混合液。
4)在洁净、低阻Si片(1)的SiO2绝缘层(2)上旋涂步骤3)的ZnO-rGO/无水乙醇混合液,转速为1000~3000r/min,旋涂30s,旋涂次数为1~2次,得到纳米ZnO-rGO旋凃层(3);
5)在上述的旋凃层(3)上蒸镀厚度为70~100nm的Al电极(4),获得基于纳米ZnO-rGO复合材料的光电导型紫外探测器。
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