CN113224186A - 一种基于石墨烯/氧化锌异质结的柔性自驱动纤维紫外光电探测器 - Google Patents
一种基于石墨烯/氧化锌异质结的柔性自驱动纤维紫外光电探测器 Download PDFInfo
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Abstract
本发明揭示了一种基于石墨烯/氧化锌异质结的柔性自驱动纤维紫外光电探测器，包括第一柔性纤维衬底、p型石墨烯纳米片薄膜层、n型氧化锌纳米线阵列层、导电纤维电极、第二柔性纤维衬底和纤维状透明导电薄膜，第一柔性纤维衬底表面包覆有p型石墨烯纳米片薄膜层，在p型石墨烯纳米片薄膜层表面生长有n型氧化锌纳米线阵列层和纤维状电极，p型石墨烯纳米片薄膜层和n型氧化锌纳米线阵列层组成p‑n纳米异质结活性层，在p‑n纳米异质结活性层上连接导电纤维电极或沉积纤维状透明导电薄膜，得到柔性自驱动纤维紫外光电探测器。该紫外光电探测器采用石墨烯纳米片薄膜和氧化锌纳米线阵列构筑异质结，具有紫外光吸收效率高和柔韧性优异的特点。
Description
技术领域
本发明涉及一种基于石墨烯/氧化锌异质结的柔性自驱动纤维紫外光电探测器，可用于紫外光电探测器技术领域。
背景技术
紫外光探测器可广泛应用于环境污染监测、高温火焰检测、生物剂检测、导弹预警系统和光通信等各个领域，可穿戴紫外光探测器可以为人们提供舒适、方便的光电信息服务，引起了人们的广泛关注。纤维结构紫外光探测器具有柔性、轻质、便携、可编制等优势，是一种极具前景的可穿戴器件结构。此外，从实际应用角度出发，不需额外电源供应的自驱动器件结构，可以降低可穿戴系统电路的复杂性、减少器件重量、提高器件便携性、实现低功耗，是一种极具前景的技术。因此，自驱动纤维紫外光电探测器是一种理想的可穿戴光电探测技术。现有自驱动纤维紫外光电探测器的研究还比较少，且存在响应速度慢、开关比低等问题。
氧化锌材料具有宽的带隙(3.4eV)和大的结合能(60meV)，作为紫外光电探测器活性材料具有紫外光吸收率高、成本低和生物相容性好等优势。基于氧化锌材料的p-n异质结材料可以在异质结界面处产生内建电场，使异质结中的电子和空穴在紫外光辐射高效分离，从而产生光电流，实现器件的自驱动，极具市场应用潜力。
发明内容
本发明的目的就是为了解决现有技术中存在的上述问题，提出一种基于石墨烯/氧化锌异质结的柔性自驱动纤维紫外光电探测器。
本发明的目的将通过以下技术方案得以实现：一种基于石墨烯/氧化锌异质结的柔性自驱动纤维紫外光电探测器，包括第一柔性纤维衬底、p型石墨烯纳米片薄膜层、n型氧化锌纳米线阵列层、导电纤维电极、第二柔性纤维衬底和纤维状透明导电薄膜，所述第一柔性纤维衬底表面包覆有p型石墨烯纳米片薄膜层，在p型石墨烯纳米片薄膜层表面生长有n型氧化锌纳米线阵列层和纤维状电极，其中，p型石墨烯纳米片薄膜层和n型氧化锌纳米线阵列层组成p-n纳米异质结活性层，在p-n纳米异质结活性层上连接导电纤维电极或沉积纤维状透明导电薄膜，得到柔性自驱动纤维紫外光电探测器。
优选地，所述柔性自驱动纤维紫外光电探测器包括平面型和夹层型两种器件结构。
优选地，所述p-n纳米异质结活性层通过在衬底纤维表面逐层沉积p型石墨烯纳米片薄膜层和n型氧化锌纳米线阵列层制得，p型石墨烯纳米片层的厚度为1-5μm，n型氧化锌纳米线阵列层的厚度为0.7-2μm。
优选地，所述平面型器件采用绝缘性柔性纤维衬底，夹层型器件采用导电性纤维衬底；所述绝缘性柔性纤维衬底为棉线、尼龙线、涤纶线、PDMS纤维或PI纤维，导电性纤维衬底为金属丝或采用金属纳米线包覆绝缘性柔性纤维。
优选地，所述平面型器件通过在异质结纤维活性层外表面平行排布两根导电纤维电极构筑；所述夹层型器件通过在异质结纤维活性层内外表面分别排布一根导电纤维和一层纤维状透明导电薄膜层作为内部电极和外部电极构筑。
优选地，所述平面型器件中的两根导电纤维电极通过缠绕打结方式构筑于异质结纤维活性层外表面；所述夹层型器件的内部电极为导电纤维衬底，外部电极通过在异质结纤维活性层外表面沉积一层纤维状透明导电薄膜层构筑。
本发明采用以上技术方案与现有技术相比，具有以下技术效果：该自驱动紫外光电探测器采用石墨烯纳米片薄膜和氧化锌纳米线阵列构筑异质结，具有活性异质结界面比表面积大、紫外光吸收效率高和柔韧性优异的特点。该自驱动紫外光电探测器具有快速的紫外光探测响应速度，响应时间小于90ms。该自驱动紫外光电探测器具有良好的机械稳定性，在弯折6000次后器件性能没有明显衰减。该器件组装工艺简单、产品成本低，易于大规模推广应用。
附图说明
图1为本发明的平面型自驱动纤维紫外光电探测器的结果示意图。
图2为本发明的夹层型自驱动纤维紫外光电探测器的结果示意图。
图3为本发明的石墨烯/氧化锌异质结活性层的SEM图。
图4为本发明的柔性自驱动纤维紫外光电探测器的紫外光探测性能。
图中标号：1为第一柔性纤维衬底，2为p型石墨烯纳米片薄膜层，3为n型氧化锌纳米线阵列层，4为导电纤维电极，5为第二柔性纤维衬底，6为纤维状透明导电薄膜。
具体实施方式
本发明的目的、优点和特点，将通过下面优选实施例的非限制性说明进行图示和解释。这些实施例仅是应用本发明技术方案的典型范例，凡采取等同替换或者等效变换而形成的技术方案，均落在本发明要求保护的范围之内。
本发明揭示了一种基于石墨烯/氧化锌异质结的柔性自驱动纤维紫外光电探测器，如图1和图2所示，该柔性自驱动纤维紫外光电探测器包括第一柔性纤维衬底1、p型石墨烯纳米片薄膜层2、n型氧化锌纳米线阵列层3、导电纤维电极4、第二柔性纤维衬底5和纤维状透明导电薄膜6。所述第一柔性纤维衬底为绝缘性纤维衬底。
所述第一柔性纤维衬底表面包覆有p型石墨烯纳米片薄膜层，在p型石墨烯纳米片薄膜层表面生长有n型氧化锌纳米线阵列层和纤维状电极，其中，p型石墨烯纳米片薄膜层和n型氧化锌纳米线阵列层组成p-n纳米异质结活性层，在p-n纳米异质结活性层上连接导电纤维电极或沉积纤维状透明导电薄膜，得到柔性自驱动纤维紫外光电探测器。所述p-n纳米异质结活性层通过在衬底纤维表面逐层沉积p型石墨烯纳米片薄膜层和n型氧化锌纳米线阵列层制得，p型石墨烯纳米片层的厚度为1-5μm，n型氧化锌纳米线阵列层的厚度为0.7-2μm。
在本发明中，采用p型石墨烯纳米片薄膜层和n型氧化锌纳米线阵列层组成纤维状p-n纳米异质结活性层。利用氧化石墨烯纳米片在纤维束中的毛细组装作用，实现氧化石墨烯纳米片薄膜层在柔性纤维表面的均匀、紧密包覆。将氧化石墨烯纳米片薄膜层进行氢碘酸还原制得还原石墨烯纳米片薄膜层，其厚度为1-5μm。进一步，在还原石墨烯纳米片薄膜层上生长氧化锌纳米线阵列层，厚度为0.7-2μm，获得纤维状p-n纳米异质结结构。
所述柔性自驱动纤维紫外光电探测器包括平面型和夹层型两种器件结构，在夹层型自驱动纤维紫外光光电探测器中，采用导电纤维同时作为纤维衬底和内部电极。所述平面型器件采用绝缘性柔性纤维衬底，夹层型器件采用导电性纤维衬底；所述绝缘性柔性纤维衬底为棉线、尼龙线、涤纶线、PDMS纤维或PI纤维，导电性纤维衬底为金属丝或采用金属纳米线包覆绝缘性柔性纤维。采用的金属纳米线包括金纳米线、银纳米线和铜纳米线；采用的金属丝包括金丝、银丝、铜丝、镍丝和不锈钢丝。
所述平面型器件通过在异质结纤维活性层外表面平行排布两根导电纤维电极构筑；所述夹层型器件通过在异质结纤维活性层内外表面分别排布一根导电纤维和一层纤维状透明导电薄膜层作为内部电极和外部电极构筑。所述平面型器件中的两根导电纤维电极通过缠绕打结方式构筑于异质结纤维活性层外表面；所述夹层型器件的内部电极为导电纤维衬底，外部电极通过在异质结纤维活性层外表面沉积一一层纤维状透明导电薄膜层构筑。
夹层型器件中的内部导电纤维电极可采用金属纳米线包覆绝缘性柔性纤维或直接使用金属丝。采用的金属纳米线包括金纳米线、银纳米线和铜纳米线；采用的金属丝包括金丝、银丝、铜丝、镍丝和不锈钢丝。金属纳米线包覆绝缘性柔性纤维制得的导电纤维采用毛细组装涂覆方式制备，其线电阻为2-5Ω/cm。纤维状透明导电薄膜层可以为金纳米线/银纳米线/碳纳米管网格薄膜，采用浸渍涂覆方式制备，其线电阻为4-10Ω/cm。
本发明中，该柔性自驱动纤维紫外光电探测器的制备方法分别如下：
S1：衬底纤维处理：将衬底纤维依次在乙醇、丙酮、异丙醇和去离子水中超声清洗，真空烘干得到清洗后的衬底纤维。
其中平面型器件采用绝缘性柔性纤维衬底；夹层型器件采用导电性纤维衬底。
S2：在所示S1步骤后得到的衬底纤维上沉积石墨烯纳米片薄膜层：将处理后的衬底纤维捆绑成束放入氧化石墨烯纳米片的乙醇分散液。在毛细作用下，氧化石墨烯纳米片分散液将进入纤维束之间的区域。浸渍一段时间后，取出烘干，氧化石墨烯纳米片层覆盖于纤维表面。重复数次上述毛细过程，以使氧化石墨烯纳米片层在纤维表面均匀涂覆，形成氧化石墨烯纳米片薄膜。将氧化石墨烯纳米片薄膜进行氢碘酸蒸汽还原处理制得p型还原石墨烯纳米片薄膜层。
S3：石墨烯/氧化锌p-n异质结纤维的制备：在制备好的石墨烯纤维上浸渍于氧化锌晶种溶液中24h，取出后150℃下退火1h，获得氧化锌晶种层涂覆的石墨烯纤维。然后，将石墨烯纤维放入氧化锌生长液中，80-95℃水热加热1-4h；取出纤维，用大量去离子水冲洗；100℃下真空干燥2h，制得石墨烯/氧化锌p-n异质结纤维。
S4：电极的组装：对于平面型和夹层型器件分别采用平行排布电极和内外排布电极两种方式进行电极的组装。
在所述S4步骤中，其中，平面型器件采用两根平行导电纤维电极结构，电极通过缠绕打结方式平行排布于石墨烯/氧化锌p-n异质结纤维表面；夹层型器件的内部和外部电极结构，内部电极为导电纤维衬底，外部电极通过在石墨烯/氧化锌p-n异质结纤维外表面沉积层纤维状透明导电薄膜层构筑。
实施例1
如附图1所示，平面型自驱动纤维紫外光电探测器的制备过程如下：
(1)衬底纤维预处理：将棉线纤维依次在乙醇、丙酮、异丙醇和去离子水中超声清洗，真空烘干，其中平面型器件采用绝缘性柔性纤维衬底。
(2)在衬底纤维上沉积石墨烯纳米片薄膜层：取一定长度预处理后的纱线，捆绑成束后放入质量浓度为1mg/ml的氧化石墨烯纳米片的乙醇分散。在毛细作用下，氧化石墨烯纳米片分散液将进入纤维束之间的区域，浸渍10min后，取出放入100℃真空干燥箱中烘干30min。重复数次上述毛细组装过程3次，获得均匀涂覆于棉线纤维表面的氧化石墨烯纳米片薄膜层。将制备好的纱线悬挂在装有2ml氢碘酸和5ml冰醋酸的烧杯中，将烧杯密封，放入40℃油浴锅中进行氧化石墨烯蒸汽还原处理，反应时间为24h；定时间后将纱线取出，并用大量去离子水冲洗，放入100℃真空干燥箱中烘干24h，获得还原石墨烯纱线纤维。
(3)p-n异质结的制备：将还原石墨烯纱线纤维放入氧化锌晶种溶液中彻夜浸泡24h，氧化锌晶种溶液为0.055g二水乙酸锌和50ml乙醇混和而成的溶液，将浸泡后的还原石墨烯纱线放入干净的石英舟中用铝箔密封，150℃下退火1h，获得氧化锌晶种层涂覆的石墨烯纤维；然后，将得到的石墨烯纤维放入氧化锌生长液中，80-95℃水热加热1-4h，取出纤维，用大量去离子水冲洗；100℃下真空干燥2h，制得石墨烯/氧化锌p-n异质结/纱线纤维，如图3所示。氧化锌生长液为1.4g六次甲基四胺、2.98g六水合硝酸锌、0.2mol聚乙烯亚胺溶于100ml去离子水，
(4)电极的组装：将两根铜丝导电纤维通过缠绕打结方式平行排布于石墨烯/氧化锌p-n异质结纱线纤维表面，即制得平面型自驱动纤维紫外光电探测器。
在以上制备过程中，衬底纤维可采用尼龙线、涤纶线、PDMS纤维、PI纤维。导电纤维可采用金丝、银丝、铜丝、镍丝和不锈钢丝，在实际操作过程中，试验人员可根据实际需要选取。
导电纤维还可采用金属纳米线包覆纱线纤维制得的导电纤维，其制备方法如下：将纱线(棉线、尼龙线、涤纶线)浸入金属纳米线(金纳米线、银纳米线和铜纳米线)的乙醇分散液中，放置10min后取出，真空干燥，重复上述步骤3-5次，制得金属纳米线包覆纱线的导电纤维。
实施例2
如附图2所示，夹层型自驱动纤维紫外光电探测器的制备过程如下：
(1)衬底纤维预处理：将铜丝纤维依次在乙醇、丙酮、异丙醇和去离子水中超声清洗，真空烘干。
(2)在衬底纤维上沉积石墨烯纳米片薄膜层：取一定长度的铜丝纤维，捆绑成束后放入质量浓度为1mg/ml的氧化石墨烯纳米片的乙醇分散。在毛细作用下，氧化石墨烯纳米片分散液将进入纤维束之间的区域，浸渍10min后，取出放入100℃真空干燥箱中烘干30min，重复数次上述毛细组装过程3次，获得均匀涂覆于棉线纤维表面的氧化石墨烯纳米片薄膜层。将制备好的纱线悬挂在装有2ml氢碘酸和5ml冰醋酸的烧杯中，将烧杯密封，放入40℃油浴锅中进行氧化石墨烯蒸汽还原处理，反应时间为24h。将纱线取出，并用大量去离子水冲洗，放入100℃真空干燥箱中烘干24h，获得还原石墨烯纱线纤维。
(3)p-n异质结的制备：将还原石墨烯纱线放入氧化锌晶种溶液(0.055g二水乙酸锌和50ml乙醇混和而成的溶液)中浸泡24h。将浸泡后的还原石墨烯纱线放入干净的石英舟中用铝箔密封，150℃下退火1h，获得氧化锌晶种层涂覆的石墨烯纤维，然后，将石墨烯纤维放入氧化锌生长液(1.4g六次甲基四胺、2.98g六水合硝酸锌和0.2mol聚乙烯亚胺溶于100ml去离子水)中，80-95℃水热加热1-4h。取出纤维，用大量去离子水冲洗；100℃下真空干燥2h，制得石墨烯/氧化锌p-n异质结/铜丝纤维。
(4)电极的组装：器件的内部电极为铜丝纤维，外部电极通过在石墨烯/氧化锌p-n异质结外表面采用毛细组装方式制备的纤维状银纳米线透明导电薄膜，即制得夹层型自驱动纤维紫外光电探测器。
其中，纤维状银纳米线透明导电薄膜的制备方式如下：将石墨烯/氧化锌p-n异质结/铜丝纤维浸入银纳米线的乙醇分散液中，放置10min后取出，真空干燥，重复上述步骤3-5次，制得纤维状银纳米线透明导电薄膜。
上述制备过程中，衬底导电纤维可采用金丝、银丝、镍丝和不锈钢丝。衬底导电纤维还可采用金属纳米线包覆绝缘性柔性纤维制得的导电纤维，具体制备方式如实施例1。纤维状透明导电薄膜中的导电材料还可使用金纳米线和碳纳米管。
由于石墨烯纳米片和氧化锌纳米线构成的纤维状p-n异质结构具有大的比表面积和高的紫外光吸收率，在紫外光辐射下光生电子空穴对可快速分离，从而在零偏压下产生光电流，实现自驱动紫外光电探测功能。该自驱动紫外光电探测器响应时间小于90ms，如附图4所示，在弯折6000次后器件性能没有明显衰减，具有制作工艺简单、工作稳定性好、响应速度快、高柔性等优点。
本发明尚有多种实施方式，凡采用等同变换或者等效变换而形成的所有技术方案，均落在本发明的保护范围之内。
Claims (6)
1.一种基于石墨烯/氧化锌异质结的柔性自驱动纤维紫外光电探测器，其特征在于：包括第一柔性纤维衬底（1）、p型石墨烯纳米片薄膜层（2）、n型氧化锌纳米线阵列层（3）、导电纤维电极（4）、第二柔性纤维衬底（5）和纤维状透明导电薄膜（6），所述第一柔性纤维衬底表面包覆有p型石墨烯纳米片薄膜层，在p型石墨烯纳米片薄膜层表面生长有n型氧化锌纳米线阵列层和纤维状电极，其中，p型石墨烯纳米片薄膜层和n型氧化锌纳米线阵列层组成p-n纳米异质结活性层，在p-n纳米异质结活性层上连接导电纤维电极或沉积纤维状透明导电薄膜，得到柔性自驱动纤维紫外光电探测器。
2.根据权利要求1所述的一种基于石墨烯/氧化锌异质结的柔性自驱动纤维紫外光电探测器，其特征在于：所述柔性自驱动纤维紫外光电探测器包括平面型和夹层型两种器件结构。
3.根据权利要求1所述的一种基于石墨烯/氧化锌异质结的柔性自驱动纤维紫外光电探测器，其特征在于：所述p-n纳米异质结活性层通过在衬底纤维表面逐层沉积p型石墨烯纳米片薄膜层和n型氧化锌纳米线阵列层制得，p型石墨烯纳米片层的厚度为1-5 μm，n型氧化锌纳米线阵列层的厚度为0.7-2 μm。
4.根据权利要求2所述的一种基于石墨烯/氧化锌异质结的柔性自驱动纤维紫外光电探测器，其特征在于：所述平面型器件采用绝缘性柔性纤维衬底，夹层型器件采用导电性纤维衬底；所述绝缘性柔性纤维衬底为棉线、尼龙线、涤纶线、PDMS纤维或PI纤维，导电性纤维衬底为金属丝或采用金属纳米线包覆绝缘性柔性纤维。
5.根据权利要求2所述的一种基于石墨烯/氧化锌异质结的柔性自驱动纤维紫外光电探测器，其特征在于：所述平面型器件通过在异质结纤维活性层外表面平行排布两根导电纤维电极构筑；所述夹层型器件通过在异质结纤维活性层内外表面分别排布一根导电纤维和一层纤维状透明导电薄膜层作为内部电极和外部电极构筑。
6.根据权利要求2所述的一种基于石墨烯/氧化锌异质结的柔性自驱动纤维紫外光电探测器，其特征在于：所述平面型器件中的两根导电纤维电极通过缠绕打结方式构筑于异质结纤维活性层外表面；所述夹层型器件的内部电极为导电纤维衬底，外部电极通过在异质结纤维活性层外表面沉积一层纤维状透明导电薄膜层构筑。
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| CN104894640A (zh) * | 2015-05-14 | 2015-09-09 | 天津理工大学 | 一种石墨烯衬底上ZnO分级纳米阵列及其制备方法及应用 |
| CN107799623A (zh) * | 2017-09-27 | 2018-03-13 | 南京理工大学 | 一种基于氧化锌纳米棒阵列/银纳米线/石墨烯多层结构的紫外光探测器织物及制备方法 |
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| CN104894640A (zh) * | 2015-05-14 | 2015-09-09 | 天津理工大学 | 一种石墨烯衬底上ZnO分级纳米阵列及其制备方法及应用 |
| CN107799623A (zh) * | 2017-09-27 | 2018-03-13 | 南京理工大学 | 一种基于氧化锌纳米棒阵列/银纳米线/石墨烯多层结构的紫外光探测器织物及制备方法 |
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