CN113540271A - 一种日盲型紫外光电探测器及其制备方法 - Google Patents
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Abstract
本发明提供了一种日盲型紫外光电探测器及其制备方法，该日盲型紫外光电探测器，包括：导电基底，其上开设有沟道；Ga2O3纳米柱阵列，其位于所述沟道上；聚甲基丙烯酸甲酯层，其覆盖Ga2O3纳米柱阵列。本发明的日盲型紫外光电探测器，Ga2O3具有高的热稳定性和化学稳定性，其禁带宽度约为4.9eV，只对日盲区的深紫外光敏感，相比传统使用AlGaN、MgZnO等材料，Ga2O3不需要任何掺杂来调节带隙，避免了合金相的成分波动和相分离；而使用的聚甲基丙烯酸甲酯层，使得日盲型紫外光电探测器具有较低的暗电流，在低光强下仍具有较高的开关比。
Description
技术领域
本发明涉及光电探测器技术领域，尤其涉及一种日盲型紫外光电探测器及其制备方法。
背景技术
由于臭氧层的吸收，波长在200nm-280nm的紫外光不能到达地球，该波段的光被称为日盲紫外光。因此，基于日盲紫外的探测器具有高信噪比、低误报率、可全方位全天候工作等优点，可被广泛应用于军事和民生，如导弹跟踪，安全通信，臭氧空洞监测，化学/生物分析和电晕检测等。目前，在制备日盲型紫外光电探测器时常用的日盲探测材料如：AlGaN、MgZnO等，但申请人发现采用这些材料需要通过掺杂来调节带隙；而且这些材料采用高组分合金，带来相分离和难以外延成膜的缺点。
基于现有的日盲型紫外光电探测器存在的缺陷，有必要对此进行改进。
发明内容
有鉴于此，本发明提出了一种日盲型紫外光电探测器及其制备方法，以解决或部分解决现有技术中存在的技术问题。
第一方面，本发明提供了一种日盲型紫外光电探测器，包括：
导电基底，其上开设有沟道；
Ga2O3纳米柱阵列，其位于所述沟道上；
聚甲基丙烯酸甲酯层，其覆盖所述Ga2O3纳米柱阵列。
优选的是，所述的日盲型紫外光电探测器，其特征在于，所述导电基底为FTO导电玻璃。
第二方面，本发明还提供了一种所述的日盲型紫外光电探测器的制备方法，包括以下步骤：
提供导电基底；
配制含镓前驱体溶液；
配制聚甲基丙烯酸甲酯溶液；
将导电基底位于沟道之外的部分进行遮挡，然后将导电基底置于含镓前驱体溶液中，进行水热反应，即在导电基底的沟道上制备得到Ga2O3纳米柱阵列；
将聚甲基丙烯酸甲酯溶液涂覆在导电基底的沟道上并覆盖Ga2O3纳米柱阵列，干燥后即形成聚甲基丙烯酸甲酯层。
优选的是，所述的日盲型紫外光电探测器的制备方法，配制含镓前驱体溶液具体为：将镓盐加入至水中，混合均匀即得含镓前驱体溶液。
优选的是，所述的日盲型紫外光电探测器的制备方法，配制聚甲基丙烯酸甲酯溶液具体为：将聚甲基丙烯酸甲酯溶于至氯苯中即得聚甲基丙烯酸甲酯溶液。
优选的是，所述的日盲型紫外光电探测器的制备方法，将导电基底置于含镓前驱体溶液中进行水热反应之前还包括：将导电基底置于紫外臭氧仪下照射40～50min。
优选的是，所述的日盲型紫外光电探测器的制备方法，将聚甲基丙烯酸甲酯溶液涂覆在导电基底的沟道上之前还包括：将导电基底于500～600℃下退火1～3h。
优选的是，所述的日盲型紫外光电探测器的制备方法，所述聚甲基丙烯酸甲酯溶液的浓度为4～20mg/ml，所述水热反应的温度为130～170℃、反应时间为1～3h。
优选的是，所述的日盲型紫外光电探测器的制备方法，将聚甲基丙烯酸甲酯溶液涂覆在导电基底的沟道上并覆盖Ga2O3纳米柱阵列，干燥后即形成聚甲基丙烯酸甲酯层具体为：将80～120μl的聚甲基丙烯酸甲酯溶液滴在沟道上并覆盖Ga2O3纳米柱阵列，然后于2000～4000r/min的转速下，旋涂20～40s，再于80～120℃下干燥20～40min，即得聚甲基丙烯酸甲酯层。
优选的是，所述的日盲型紫外光电探测器的制备方法，所述镓盐为硝酸镓，所述硝酸镓与水的质量体积比为(0.2～0.6)g:(20～40)mL。
本发明的一种日盲型紫外光电探测器及方法相对于现有技术具有以下有益效果：
(1)本发明的日盲型紫外光电探测器，Ga2O3纳米柱阵列位于沟道上，聚甲基丙烯酸甲酯层位于沟道上并覆盖Ga2O3纳米柱阵列，Ga2O3具有高的热稳定性和化学稳定性，其禁带宽度约为4.9eV，只对日盲区的深紫外光敏感，相比传统使用AlGaN、MgZnO等材料，Ga2O3不需要任何掺杂来调节带隙，避免了合金相的成分波动和相分离；而使用的聚甲基丙烯酸甲酯层，使得日盲型紫外光电探测器具有较低的暗电流，在低光强下仍具有较高的开关比；
(2)本发明的日盲型紫外光电探测器的制备方法，工艺简单、成本低、环境友好，为氧化镓纳米柱阵列光电紫外探测器的大规模生产创造了良好的前提条件；且使用FTO导电玻璃作为导电基底，不需要额外制作电极，大大简化了实验步骤和实验成本。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例或现有技术描述中所需要使用的附图作简单的介绍。显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。
图1为本发明的日盲型紫外光电探测器的结构示意图；
图2为本发明的导电基底的结构示意图；
图3为实施例1中制备得到的日盲型紫外光电探测器的Ga2O3纳米柱在沟道表面的低倍SEM图；
图4为图3中方框处的放大图；
图5为实施例1中制备得到的日盲型紫外光电探测器的Ga2O3纳米柱的截面示意图；
图6～7为实施例1中制备得到的日盲型紫外光电探测器的Ga2O3纳米柱的EDS能谱图；
图8为实施例1和对比例2中制备得到的日盲型紫外光电探测器的Ga2O3纳米柱的XRD图；
图9为对比例1中制备得到的日盲型紫外光电探测器的I-T特性曲线图；
图10为实施例1中制备得到的日盲型紫外光电探测器的I-T特性曲线图；
图11为实施例2中制备得到的日盲型紫外光电探测器的I-T特性曲线图。
具体实施方式
下面将结合本发明实施方式，对本发明实施方式中的技术方案进行清楚、完整的描述，显然，所描述的实施方式仅仅是本发明一部分实施方式，而不是全部的实施方式。基于本发明中的实施方式，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施方式，都属于本发明保护的范围。
本申请实施例提供了一种日盲型紫外光电探测器，如图1～2所示，包括：
导电基底1，其上开设有沟道11；
Ga2O3纳米柱阵列2，其位于沟道11上；
聚甲基丙烯酸甲酯层3，其覆盖Ga2O3纳米柱阵列2。
需要说明的是，本申请的日盲型紫外光电探测器，包括导电基底1、Ga2O3纳米柱阵列2和聚甲基丙烯酸甲酯层3，其中，导电基底1上开设有沟道11，这里的沟道类似凹槽，Ga2O3纳米柱阵列2位于沟道上，聚甲基丙烯酸甲酯层3位于沟道11上并覆盖Ga2O3纳米柱阵列2，Ga2O3纳米柱阵列2为电子传输层。Ga2O3具有高的热稳定性和化学稳定性，其禁带宽度约为4.9eV，只对日盲区的深紫外光敏感，相比传统使用AlGaN、MgZnO等材料，Ga2O3不需要任何掺杂来调节带隙，避免了合金相的成分波动和相分离。而使用的聚甲基丙烯酸甲酯层3，使得日盲型紫外光电探测器具有较低的暗电流，在低光强下仍具有较高的开关比。
在一些实施例中，导电基底1为FTO导电玻璃，显然实际中导电基底1还可以采用ITO导电玻璃。FTO导电玻璃本身导电，因而在FTO导电玻璃的沟道两侧自然形成电极，而且目前大多数器件都需要额外制作电极，不仅增加了实验步骤还大大增加了实验成本，本发明采用FTO导电玻璃，大大简化了实验步骤和实验成本。
基于同一发明构思，本申请实施例还提供了一种上述的日盲型紫外光电探测器的制备方法，包括以下步骤：
S1、提供导电基底；
S2、配制含镓前驱体溶液；
S3、配制聚甲基丙烯酸甲酯溶液；
S4、将导电基底位于沟道之外的部分进行遮挡，然后将导电基底置于含镓前驱体溶液中，进行水热反应，即在导电基底的沟道上制备得到Ga2O3纳米柱阵列；
S5、将聚甲基丙烯酸甲酯溶液涂覆在导电基底的沟道上并覆盖Ga2O3纳米柱阵列，干燥后即形成聚甲基丙烯酸甲酯层。
需要说明的是，本申请实施例中日盲型紫外光电探测器的制备方法，将导电基底位于沟道之外的部分进行遮挡，具体的，可在导电基底位于沟道之外的地方贴上耐高温胶带，这样在后续的水热反应过程中，只有沟道上生长Ga2O3纳米柱阵列，而在导电基底上位于沟道以外的地方则不生长Ga2O3纳米柱阵列。本申请的日盲型紫外光电探测器，未旋凃聚甲基丙烯酸甲酯(PMMA)溶液，则探测器的主要连接关系为FTO电极-氧化镓纳米柱-FTO电极；旋凃了聚甲基丙烯酸甲酯溶液，则探测器的主要连接关系为FTO电极-PMMA-氧化镓纳米柱-PMMA-FTO电极。
在一些实施例中，将导电基底置于含镓前驱体溶液中，进行水热反应之前还包括将导电基底分别使用丙酮、无水乙醇、去离子水超声处理20min，以清除导电基底上的杂质。
在一些实施例中，水热反应在反应釜中进行，具体的，将前驱体置于反应釜中之前，还将反应釜分别使用丙酮、无水乙醇、去离子水超声处理，每个超声处理过程均20～30min，以清除反应釜内的杂质。
在一些实施例中，配制含镓前驱体溶液具体为：将镓盐加入至水中，混合均匀即得含镓前驱体溶液。
在一些实施例中，配制聚甲基丙烯酸甲酯溶液具体为：将聚甲基丙烯酸甲酯溶于至氯苯中即得聚甲基丙烯酸甲酯溶液。
在一些实施例中，将导电基底置于含镓前驱体溶液中进行水热反应之前还包括：将导电基底置于紫外臭氧仪下照射40～50min。使用紫外臭氧仪照射的目的是，改善导电基底表面的功函数，使其羟基化，有助于水热反应时提升接触面之间的亲水性，并能防止表面出现裂纹与分布不均。
在一些实施例中，由于水热反应完成后会在导电基底的正面和背面都会留下残留的前驱体溶液以及杂质，所以需要反复冲洗正反两面，如果纳米柱阵列已经生长出来，此时无法用去离子水冲刷掉表面一层肉眼可见的白色纳米柱，将其冲洗干净后再次使用恒温干燥台在空气中用80℃干燥10min。
在一些实施例中，将聚甲基丙烯酸甲酯溶液涂覆在导电基底的沟道上之前还包括：将导电基底于500～600℃下退火1～3h。具体的，将生长有Ga2O3纳米柱阵列的导电基底在室温下以3～8℃/min升温至500～600℃并保温1～3h，然后以3～8℃/min降温至室温，即完成退火。
具体的，在一些实施例中，退火时，将生长有Ga2O3纳米柱阵列放入培养皿或者陶瓷舟，然后用锡纸封闭包装，再将培养皿或者陶瓷舟放入高温退火炉中进行退火；锡纸封闭包装，其目的是为了防止灰尘进入，显然退火前同样对培养皿或者陶瓷舟使用分别使用丙酮、无水乙醇、去离子水超声处理20min。
在一些实施例中，聚甲基丙烯酸甲酯溶液的浓度为4～20mg/ml，水热反应的温度为130～170℃、反应时间为1～3h。
在一些实施例中，将聚甲基丙烯酸甲酯溶液涂覆在导电基底的沟道上并覆盖Ga2O3纳米柱阵列，干燥后即形成聚甲基丙烯酸甲酯层具体为：将80～120μl的聚甲基丙烯酸甲酯溶液滴在沟道上并覆盖Ga2O3纳米柱阵列，然后于2000～5000r/min的转速下，旋涂20～40s，再于80～120℃下干燥20～40min，即得聚甲基丙烯酸甲酯层。
在一些实施例中，镓盐为硝酸镓，硝酸镓与水的质量体积比为(0.2～0.6)g:(20～40)mL。
具体的，在一些实施例中，配制含镓前驱体溶液具体为：将0.3g的硝酸镓溶于30mL去离子中，然后使用搅拌10min使其均匀，用pH测试仪测其溶液显示为酸性，pH值约为2.1。
以下进一步以具体实施例的说明本申请的日盲型紫外光电探测器的制备方法。
实施例1
本申请实施例提供了一种日盲型紫外光电探测器的制备方法，包括以下步骤：
S1、提供一自带沟道的FTO导电玻璃，其中，FTO导电玻璃的长宽高分别为20mm、20mm、2mm；将FTO导电玻璃分别置于丙酮、无水乙醇、去离子水中超声清洗20min，备用；
S2、将0.3g的硝酸镓加入至30ml去离子水中搅拌均匀后得到含镓前驱体溶液；
S3、将40mg的聚甲基丙烯酸甲酯溶于2ml的氯苯，混合均匀得到聚甲基丙烯酸甲酯溶液；
S4、将FTO导电玻璃位于沟道以外的地方贴上耐高温胶带进行遮挡，然后使用紫外臭氧仪(PSD-UV4)对FTO导电玻璃照射45min，然后将FTO导电玻璃置于含镓前驱体溶液中，于150℃下反应2h；
S5、去除耐高温胶带，然后将生长有Ga2O3纳米柱阵列的FTO导电玻璃使用清水清洗，再于80℃下干燥10min；
S6、将生长有Ga2O3纳米柱阵列的FTO导电玻璃置于退火炉中，由室温以5℃/min升温至550℃并保温2h，然后以5℃/min降温至室温，完成退火；
S7、将聚甲基丙烯酸甲酯溶液滴在沟道上并覆盖Ga2O3纳米柱阵列，4000r/min的转速下，旋涂30s，再于100℃下干燥30min，即得聚甲基丙烯酸甲酯层。
实施例2
本申请实施例提供了一种日盲型紫外光电探测器的制备方法，同实施例1，不同在于，步骤S7中为：将聚甲基丙烯酸甲酯溶液滴在沟道上并覆盖Ga2O3纳米柱阵列，5000r/min的转速下，旋涂30s，再于100℃下干燥30min，即得聚甲基丙烯酸甲酯层。
对比例1
本对比例提供了一种日盲型紫外光电探测器的制备方法，同实施例1，不同在于，不使用步骤S7中聚甲基丙烯酸甲酯溶液旋涂，其余工艺均与实施例1相同。
对比例2
本对比例提供了一种日盲型紫外光电探测器的制备方法，同实施例1，不同在于，不经过S6中的退火步骤，其余工艺均与实施例1相同。
性能测试
图3为本发明实施例1中制备得到的日盲型紫外光电探测器Ga2O3纳米柱在沟道表面的低倍SEM图；图4为图3中方框处的放大图；图5为本发明实施例1中制备得到的日盲型紫外光电探测器Ga2O3纳米柱的截面示意图。图6～7为本发明实施例1中制备得到的日盲型紫外光电探测器的Ga2O3纳米柱阵列的EDS图。其中，图6中的电子图像就是EDS扫描的区域。
从图3中可以看出，Ga2O3纳米柱阵列生长在沟道上了；图4中可以看出Ga2O3纳米柱阵列横截面为菱形，对角线的平均尺寸在400nm(长对角线)和200nm(短对角线)左右；图5中可以看出Ga2O3纳米柱阵列长度为1.02μm。
从图6～7中可以计算出氧元素的重量百分比为25.61％，Ga元素的重量百分比为74.39％，由此说明Ga原子与O原子的原子比为2:3，说明生长出来的物质为Ga2O3。
图8为实施例1和对比例2中制备得到的日盲型紫外光电探测器的Ga2O3纳米柱的XRD图。对照XRD标准卡(JCPDS PDF#06-0503)可知，在33.8°、36.0°、55.1°、64.8°位置处的三个衍射峰分别对应于α-Ga2O3的(104)、(110)、(116)、(300)晶面。本申请实施例1中制备得到的日盲型紫外光电探测器的Ga2O3纳米柱在退火前为GaOOH，经过退火，才变为Ga2O3。
测试实施例1～2以及对比例1中制备得到的日盲型紫外光电探测器在未加254nm的紫外光和外加50μW/cm2的光强254nm的紫外光、1V的偏压下的I-T特性曲线，结果如图9～11所示。
具体测试方法为：将实施例1以及对比例1中制备得到的日盲型紫外光电探测器分别放置在探针台上，用探针分别连接沟道两边的电极，然后添加1V的偏压，以50μW/cm2的光强254nm的紫外光对沟道进行照射，1min为一个光照周期，即30s暗30s亮。
从图9中可以看出，对比例1中制备得到的日盲型紫外光电探测器的光电流/暗电流(开关比)约为400；从图10中可以看出，实施例1中制备得到的日盲型紫外光电探测器的开关比约为1700，可以明显看出旋凃PMMA的样品的开关比大大增加了。进一步的从图9～10还可以看出，实施例1中经过旋凃PMMA制备得到的日盲型紫外光电探测器的暗电流明显降低了，从10-7A下降到了10-8A。从图11中可以看出，实施例2中制备得到的日盲型紫外光电探测器的开关比约6000。
上所述仅为本发明的较佳实施方式而已，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (10)
1.一种日盲型紫外光电探测器，其特征在于，包括：
导电基底，其上开设有沟道；
Ga2O3纳米柱阵列，其位于所述沟道上；
聚甲基丙烯酸甲酯层，其覆盖所述Ga2O3纳米柱阵列。
2.如权利要求1所述的日盲型紫外光电探测器，其特征在于，所述导电基底为FTO导电玻璃。
3.一种如权利要求1～2任一所述的日盲型紫外光电探测器的制备方法，其特征在于，包括以下步骤：
提供导电基底；
配制含镓前驱体溶液；
配制聚甲基丙烯酸甲酯溶液；
将导电基底位于沟道之外的部分进行遮挡，然后将导电基底置于含镓前驱体溶液中，进行水热反应，即在导电基底的沟道上制备得到Ga2O3纳米柱阵列；
将聚甲基丙烯酸甲酯溶液涂覆在导电基底的沟道上并覆盖Ga2O3纳米柱阵列，干燥后即形成聚甲基丙烯酸甲酯层。
4.如权利要求3所述的日盲型紫外光电探测器的制备方法，其特征在于，配制含镓前驱体溶液具体为：将镓盐加入至水中，混合均匀即得含镓前驱体溶液。
5.如权利要求3所述的日盲型紫外光电探测器的制备方法，其特征在于，配制聚甲基丙烯酸甲酯溶液具体为：将聚甲基丙烯酸甲酯溶于至氯苯中即得聚甲基丙烯酸甲酯溶液。
6.如权利要求3所述的日盲型紫外光电探测器的制备方法，其特征在于，将导电基底置于含镓前驱体溶液中进行水热反应之前还包括：将导电基底置于紫外臭氧仪下照射40～50min。
7.如权利要求3所述的日盲型紫外光电探测器的制备方法，其特征在于，将聚甲基丙烯酸甲酯溶液涂覆在导电基底的沟道上之前还包括：将导电基底于500～600℃下退火1～3h。
8.如权利要求5所述的日盲型紫外光电探测器的制备方法，其特征在于，所述聚甲基丙烯酸甲酯溶液的浓度为4～20mg/ml，所述水热反应的温度为130～170℃、反应时间为1～3h。
9.如权利要求3所述的日盲型紫外光电探测器的制备方法，其特征在于，将聚甲基丙烯酸甲酯溶液涂覆在导电基底的沟道上并覆盖Ga2O3纳米柱阵列，干燥后即形成聚甲基丙烯酸甲酯层具体为：将80～120μl的聚甲基丙烯酸甲酯溶液滴在沟道上并覆盖Ga2O3纳米柱阵列，然后于2000～4000r/min的转速下，旋涂20～40s，再于80～120℃下干燥20～40min，即得聚甲基丙烯酸甲酯层。
10.如权利要求4所述的日盲型紫外光电探测器的制备方法，其特征在于，所述镓盐为硝酸镓，所述硝酸镓与水的质量体积比为(0.2～0.6)g:(20～40)mL。
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