CN107046084A - 一种基于柔性聚合物衬底的ZnO紫外探测器的制备方法 - Google Patents
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Abstract
本发明公开了一种基于柔性聚合物衬底的ZnO紫外探测器的制备方法，属于紫外探测器的技术领域。首先，在柔性聚合物衬底表面生长一层ZnO籽晶层；其次，将长有籽晶层的衬底放入装有配制溶液的反应釜生长ZnO纳米阵列；最后在长有ZnO纳米阵列的柔性衬底两边制备导电电极，制成一个金属‑半导体‑金属MSM型的ZnO紫外探测器。本发明方法制备的ZnO紫外探测器是基于聚酯纤维等柔性聚合物衬底，因此具有良好的柔韧性和弯曲性，在未来便携式、可穿戴式微/纳紫外传感器中有着广阔的应用前景。
Description
技术领域
本发明属于紫外探测器的技术领域，具体涉及一类基于柔性聚合物衬底的ZnO紫外探测器的制备方法。
背景技术
紫外探测技术是继红外和激光探测技术之后发展起来的又一军民两用的光电探测技术，在国防、科研、工业、生活等许多领域都有着广泛的应用。ZnO作为宽禁带半导体材料的代表，带隙宽度约为3.37eV，所对应的光波长正好位于紫外光区；并且，ZnO在室温下的紫外受激辐射具有较高光学增益、高能量转换效率以及高光响应等特性，是理想的紫外探测材料。与其他半导体材料紫外探测器相比，ZnO紫外探测器具有灵敏度高、光谱响应分布好、性能稳定、体积小、对环境要求低等优势而备受科研工作者关注。近年来研究者把目光放到一维ZnO纳米材料上，由于一维ZnO纳米材料具有高的比表面积和高的内部光电导增益等优势，用其构建的紫外探测器展示出较好的光电响应性能，因而拥有巨大的发展潜力。目前，大多数紫外探测器都建立在ITO或FTO等硬质衬底上，例如：中国专利申请201310259647.1公开的一种MSM型半导体紫外光电探测器，他们利用水热法在ITO或FTO导电玻璃上生长纳米线阵列，并制备出相应的ZnO紫外探测器。但因为整个器件生长在硬衬底上，不仅影响了器件的集成化和大规模化生长，而且限制了器件在可穿戴、便携式等领域的使用范围。
发明内容
本发明的目的在于提供了一种基于柔性聚合物衬底ZnO紫外探测器的制备方法。基于柔性聚合物衬底的ZnO紫外探测器能够到达普遍的探测水平，同时其区别于其他探测器最大的优势就是，所构建的基于柔性聚合物衬底ZnO纳米阵列的紫外探测器具有很好的柔韧性，使其具有非常广阔的实际应用前景。
本发明提供的制备技术方案如下：
一种基于柔性聚合物衬底的ZnO紫外探测器的制备方法，步骤如下：
步骤1：以柔性聚合物为基底，依次用丙酮、乙醇、去离子水进行超声清洗，并用氮气吹干，备用；
步骤2：在步骤1处理过的柔性聚合物衬底表面，生长一层厚度为20-30nm的ZnO籽晶层；
步骤3：按照等摩尔比，配制乙酸锌(Zn(CH3COO)2·2H2O)和六次甲基四胺(C6H12N4)的浓度为30mM-50mM的混合溶液，搅拌均匀至溶解；
步骤4：将步骤2长有ZnO籽晶层的样品置于步骤3的混合溶液中，在90-100℃温度条件下，时间为3-5h，生长直径为100-200nm、长度为3-5μm的ZnO纳米阵列；
步骤5：在ZnO纳米阵列的两侧分别制备导电电极，并引线和封装，即得到ZnO纳米紫外探测器。
所述的柔性聚合物衬底包括但不限于涤纶(聚酯纤维)，丙纶，晴纶，尼龙，锦纶等人造纤维，以及粘胶纤维、人造丝、人造棉等合成纤维类的柔性聚合物材料。
所述的导电电极可以为金、银、铜、铂等金属，制备导电电极采用导电银浆直接涂抹的方法，还可采用蒸空镀膜机、磁控溅射、电子束蒸发等方法。
所述的ZnO籽晶层的生长方法可以选择磁控溅射法、旋涂法溶液生长等多种方法。
本发明的有益效果：在柔性聚合物衬底上进行ZnO纳米阵列的生长及制备的ZnO紫外探测器的工艺简单，成本低廉、适宜大规模生产；所制备的紫外探测器具有良好的响应和探测性能；此外，由于采用聚酯纤维等柔性聚合物作为衬底，因此可以将探测器嵌入人体中进行紫外光探测使用。
附图说明
图1为本发明提供的基于聚酯纤维柔性衬底的ZnO紫外探测器的结构示意图。
图2为在聚酯纤维衬底上生长ZnO纳米阵列的扫描电子显微镜图片。
图3为ZnO紫外探测器的I-V特性曲线图。
图4为ZnO紫外探测器在365nm紫外光照下的光响应特性曲线图。
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：
(1)称取一定量的乙酸锌和六次甲基四胺粉末，其摩尔比例为1:1。然后采用去离子水，将等摩尔的乙酸锌和六次甲基四胺充分混合，配制体积为50mL的混合溶液。均匀搅拌15min，使得反应物充分溶解，溶液的浓度为30mM。
(2)选取聚酯面料为器件的基底(面积为1cm×1cm)，将其放入干净的烧杯内，用丙酮、乙醇分别超声清洗10min，并用去离子水反复冲洗，最后将清洗完的衬底放在烘箱内(80℃)烘干1小时，备用。
(3)采用真空射频磁控溅射在清洗干净的聚醋纤维衬底上生长一层致密、连续的，厚度为20-30nm的ZnO籽晶层。生长条件：氩气压强为3.5Pa，射频功率为180W，衬底温度为室温。
(4)将长有ZnO籽晶层的聚酯面料衬底垂直放入装有配制溶液的反应釜当中。将反应釜严格密封，并放入烘箱内生长。生长温度为95℃，生长时间为3小时。反应结束后，从烘箱中取出反应釜并降至室温后将样品取出，用去离子水反复冲洗、烘干。
(5)在样品两侧涂抹导电银浆，距离约为4mm，并引线和封装，得到柔性的ZnO紫外探测器。
上述实施例1仅是示例性，其中样品基底的选择、生长过程中各个参数的设定仅作为举例，不是对本发明的方法的限定。例如：用于作为基底的聚酯纤维面料，还可以选择尼龙，锦纶等其他面料。样品两端的导电电极还可以为金、铝、铜、铂等金属等等。
对实例1所述方法制备的ZnO紫外探测器，用扫描电镜(SEM)进行测量分析，确定聚酯纤维衬底上生长的ZnO纳米结构的形貌、物质结构等，并测试了样品的伏安特性以及紫外光的光电相应特性。以下结合附图进行说明。
图1所示为基于聚酯纤维衬底的ZnO紫外探测器的制备流程。首先，在清洗干净的聚酯纤维柔性衬底上沉积一层ZnO籽晶层，然后采用低温水溶液发在上面生长一维ZnO纳米阵列，最后再样品两端制备导电电极。可见，该方法操作简单，成本低廉、适宜大规模生产。
图2为本发明提供的基于在聚酯纤维衬底上生长ZnO纳米阵列的扫描电子显微镜图片。从图中可以看到，生长的ZnO纳米阵列均匀致密地覆盖酯纤维表面，具有良好的取向性。
图3所示为暗室和紫外光照射下，ZnO紫外探测器的电流-电压特性曲线从图中可以看到，I-V特性曲线均呈中心对称性，当探测器受到紫外光照时，光电流明细变大。
图4以及ZnO紫外探测器在365nm紫外光照下的光响应特性曲线图，从图中可以看到，ZnO紫外探测性能具有良好的重复性和稳定性。
Claims (5)
1.一种基于柔性聚合物衬底的ZnO紫外探测器的制备方法，其特征在于步骤如下：
步骤1：以柔性聚合物为基底，依次用丙酮、乙醇、去离子水进行超声清洗，并用氮气吹干，备用；
步骤2：在步骤1处理过的柔性聚合物衬底表面，生长一层厚度为20‐30nm的ZnO籽晶层；
步骤3：按照等摩尔比，配制乙酸锌和六次甲基四胺的浓度为30mM‐50mM的混合溶液，搅拌均匀至溶解；
步骤4：将步骤2长有ZnO籽晶层的样品置于步骤3的混合溶液中，在90‐100℃温度条件下，时间为3‐5h，生长直径为100‐200nm、长度为3‐5μm的ZnO纳米阵列；
步骤5：在ZnO纳米阵列的两侧分别制备导电电极，并引线和封装，即得到ZnO纳米紫外探测器。
2.根据权利要求1所述的制备方法，其特征在于，所述的柔性聚合物衬底为涤纶、丙纶、晴纶、尼龙、锦纶、粘胶纤维、人造丝或人造棉。
3.根据权利要求1或2所述的制备方法，其特征在于，所述的导电电极的材质为金、银、铜或铂，制备导电电极采用导电银浆直接涂抹的方法、蒸空镀膜机、磁控溅射或电子束蒸发法。
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ZnO籽晶层的生长方法为磁控溅射法或旋涂法。
5.根据权利要求3所述的制备方法，其特征在于，所述的ZnO籽晶层的生长方法为磁控溅射法或旋涂法。
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Cited By (6)
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|---|---|---|---|---|
| CN109768164A (zh) * | 2018-12-18 | 2019-05-17 | 杭州电子科技大学 | 一种柔性光探测器的制备方法 |
| CN111000566A (zh) * | 2019-12-13 | 2020-04-14 | 江南大学 | 具有光热效应和抗菌功能的可穿戴柔性传感器 |
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| CN111668336A (zh) * | 2020-05-29 | 2020-09-15 | 中国科学院长春光学精密机械与物理研究所 | 一种360度超大广角紫外探测器 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109768164A (zh) * | 2018-12-18 | 2019-05-17 | 杭州电子科技大学 | 一种柔性光探测器的制备方法 |
| CN111000566A (zh) * | 2019-12-13 | 2020-04-14 | 江南大学 | 具有光热效应和抗菌功能的可穿戴柔性传感器 |
| CN111244201A (zh) * | 2020-01-15 | 2020-06-05 | 中国科学院长春光学精密机械与物理研究所 | 一种柔性自支撑ZnO紫外探测器及其制备方法 |
| CN111668336A (zh) * | 2020-05-29 | 2020-09-15 | 中国科学院长春光学精密机械与物理研究所 | 一种360度超大广角紫外探测器 |
| CN113937182A (zh) * | 2020-07-13 | 2022-01-14 | 中国科学院理化技术研究所 | 一种具有柔性基底的尺寸可控的氧化锌基光电器件及其制备方法 |
| CN116040573A (zh) * | 2023-04-03 | 2023-05-02 | 三序光学科技(苏州)有限公司 | 一种二维纳米空腔阵列结构及其制备方法和应用 |
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