CN114744060B - 一种电网电晕监测器及其制备方法 - Google Patents
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Abstract
本发明公开了一种电网电晕监测器及其制备方法，包括FTO衬底，所述FTO衬底的至少一侧具有氟掺杂氧化锡层，所述氟掺杂氧化锡层上生长有GaOOH纳米柱阵列，所述GaOOH纳米柱阵列经退火后形成α/β‑Ga2O3相结纳米柱阵列，所述α/β‑Ga2O3相结纳米柱阵列上设置有Ti3C2/Ag纳米线复合层，所述Ti3C2/Ag纳米线复合层上设置有Ag电极，所述Ti3C2/Ag纳米线复合层上的Ti3C2层与所述α/β‑Ga2O3相结纳米柱阵列之间形成Ti3C2/α/β‑Ga2O3纳米柱阵列范德瓦尔斯异质结，具有三维空间异质结界面结构和日盲特性，具有优异的化学和热稳定性，耐压强，工作温度和功耗低，重复性良好，是一个具有超高响应度的自供电电网电晕监测器，可定向识别波长位于日盲波段的200‑280nm的紫外光。
Description
技术领域
本发明涉及紫外光电探测器技术领域，具体涉及到一种电网电晕监测器及其制备方法。
背景技术
电弧是一种气体放电现象，电流通过某些绝缘介质(例如空气)所产生的瞬间火花，这些现象长时间出现会损害高压设备，引发电力系统瘫痪，对电力系统造成严重的危害。此外，电弧放电也会严重地影响人身安全。因此，如何准确、及时、有效地检测电弧放电的位置及强弱对保证电力系统可靠运行、减少设备损坏和确保人身安全具有重要的意义。
电弧放电的监测通常有人工目视检查、远红外望远镜、超声波电晕检测和日盲紫外检测技术等，由于太阳光中含有很强的红外线，用红外线望远镜观察误检率较高，而超声波电晕检测装置探测距离较近，在使用中的人为影响因素较多，检测误差较大。日盲紫外检测技术是近几年来新兴的一种电弧检测方式，可以检测电弧放电发出的200-280nm波段深紫外光谱，而不受太阳光中300～360nm波段的紫外线干扰，检测精度高。本发明的电网电晕监测器，具有三维空间异质结界面结构和日盲特性，具有优异的化学和热稳定性，耐压强，工作温度和功耗低，重复性良好，是一个具有超高响应度的自供电电网电晕监测器。
发明内容
为了克服上述现有技术中的缺陷，本发明提供了一种电网电晕监测器及其制备方法，基于Ti3C2/α/β-Ga2O3纳米柱阵列范德瓦尔斯异质结，灵敏度高、稳定性好、响应时间短、高响应度、具有日盲特性。
技术方案
一种电网电晕监测器，包括FTO衬底，所述FTO衬底的至少一侧具有氟掺杂氧化锡层，所述氟掺杂氧化锡层上生长有GaOOH纳米柱阵列，所述GaOOH纳米柱阵列经退火后形成α/β-Ga2O3相结纳米柱阵列，所述α/β-Ga2O3相结纳米柱阵列上设置有Ti3C2/Ag纳米线复合层，所述Ti3C2/Ag纳米线复合层上设置有Ag电极，所述Ti3C2/Ag纳米线复合层上的Ti3C2层与所述α/β-Ga2O3相结纳米柱阵列之间形成Ti3C2/α/β-Ga2O3纳米柱阵列范德瓦尔斯异质结，所述氟掺杂氧化锡层与所述Ag电极形成通路。
进一步的，所述Ti3C2/α/β-Ga2O3纳米柱阵列范德瓦尔斯异质结由二维层状材料Ti3C2薄膜和n型α/β-Ga2O3相结纳米柱阵列构成。
进一步的，所述二维层状材料Ti3C2薄膜的厚度为200-300nm，所述n型α/β-Ga2O3相结纳米柱阵列由若干α/β-Ga2O3纳米柱构成，所述n型α/β-Ga2O3纳米柱的直径为50-200nm、长度为1.0～1.5μm。
进一步的，所述FTO衬底的厚度为2.2mm。
进一步的，所述Ti3C2/Ag纳米线复合层包括所述Ti3C2层及位于所述Ti3C2层上的Ag纳米线。
进一步的，所述氟掺杂氧化锡层的接线处和所述Ag电极的接线处位于所述FTO衬底1的同一侧。
进一步的，一种电网电晕监测器定向探测波长为200-280nm的日盲紫外光。
一种电网电晕监测器的制备方法，包括以下步骤：
步骤一、将FTO衬底依次浸泡到丙酮、乙醇、去离子水中各超声10分钟，取出后再用去离子水冲洗，用干燥的氮气吹干；
步骤二、取浓度为10-15g/L的Ga(NO3)3溶液置于反应釜内胆中，然后将步骤一中用干燥的氮气吹干后的所述FTO衬底斜靠在反应釜内胆中，并浸没于Ga(NO3)3溶液中，其中氟掺杂氧化锡层朝向所斜靠的反应釜内胆一侧；
步骤三、将步骤二中的所述反应釜转移至烘箱中，在150℃下反应12h，随后取出FTO衬底，用去离子水和无水乙醇交替清洗次，烘干后在高温炉中400-500℃先退火3.0-4.0小时，得到α-Ga2O3纳米柱阵列，然后将高温炉快速升温至700-800℃，并继续退火10-20分钟，获得α/β-Ga2O3相结纳米柱阵列；
步骤四、在步骤三中得到的所述α/β-Ga2O3相结纳米柱阵列上分别旋涂覆盖一层Ti3C2和银纳米线溶液，并在90℃下真空干燥箱中烘干，制作Ti3C2/Ag纳米线复合层；
步骤五、在步骤四中所得的所述Ti3C2/Ag纳米线复合层上方沉积一滴银胶作为上电极，即Ag电极，刮去FTO衬底边缘表面部分，露出氟掺杂氧化锡层表面，作为下电极。
进一步的，步骤三中的所述将高温炉快速升温至700-800℃的快速升温时间为5-10分钟。
进一步的，步骤四中的所述银纳米线溶液的浓度为0.5-1.0mol/L，所述Ti3C2的浓度为25mg/L。
有益效果
本发明与现有技术相比，具有以下有益效果：
1、性能稳定，反应灵敏，高响应度，具有日盲光电特性，所采用的α/β-Ga2O3相结纳米柱阵列均匀、有序，纳米柱尺寸可控；
2、α/β-Ga2O3相结纳米柱的直径为50-100nm，光电性能更佳，Ga2O3相结的成分比例可控，β-Ga2O3的厚度控制在10-30nm范围内，Ti3C2/Ag纳米线复合电极增强器件导电性和透光率，易获得加工，导电性良好，连接了电极下方的纳米柱阵列，提高了电网电晕监测器整体的性能；
3、Ti3C2层的厚度为200～300nm可控，使得探测器光电性能更佳；
4、具有三维空间多异质结界面结构，日盲特性稳定，具有优异的化学和热稳定性，高响应度，成本低，重复性良好，可以检测日盲波段的200-280nm的紫外光，可应用于便捷式可穿戴紫外线检测设备；
5、通过水热法在FTO衬底上生长氧化镓相结纳米柱阵列，覆盖一层Ti3C2/银纳米线复合透明导电电极，制作成多异质结结构的柔性日盲紫外探测器，该探测器的制备工艺可控性强，易操作，器件与衬底的结合力强，便于大面积制备、重复性好，成本低，在紫外线检测等领域具有很大的应用前景；
6、通过水热法在氟掺杂氧化锡层上方定向生长一层GaOOH纳米柱阵列，并退火生成α/β-Ga2O3相结纳米柱阵列。生长方向、尺寸、结构可控，后在α/β-Ga2O3相结纳米柱阵列上方旋涂一层Ti3C2/Ag纳米线复合电极，最后在其上方滴涂一圆形银胶作为上电极，氟掺杂氧化锡层衬底作为下电极，制备基于Ti3C2/α/β-Ga2O3纳米柱阵列范德瓦尔斯异质结的电网电晕监测器。
附图说明
图1是本发明中一种电网电晕监测器的结构示意图；
图2是α/β-Ga2O3相结纳米柱阵列的XRD图谱；
图3是α/β-Ga2O3相结纳米柱阵列的SEM表面；
图4是α/β-Ga2O3相结纳米柱阵列的SEM截面；
图5是电网电晕监测器在254nm紫外光照下的I-t图。
附图标记
FTO衬底1、氟掺杂氧化锡层2、GaOOH纳米柱阵列3、α/β-Ga2O3相结纳米柱阵列4、Ti3C2/Ag纳米线复合层5、Ag电极6。
具体实施方式
为更好地说明阐述本发明内容，下面结合附图和实施实例进行展开说明：
有图1-图5所示，本发明公开了一种电网电晕监测器，包括FTO衬底1，所述FTO衬底1的至少一侧具有氟掺杂氧化锡层2，所述氟掺杂氧化锡层2上生长有GaOOH纳米柱阵列3，所述GaOOH纳米柱阵列3经退火后形成α/β-Ga2O3相结纳米柱阵列4，所述α/β-Ga2O3相结纳米柱阵列4上设置有Ti3C2/Ag纳米线复合层5，所述Ti3C2/Ag纳米线复合层5上设置有Ag电极6，所述Ti3C2/Ag纳米线复合层5上的Ti3C2层与所述α/β-Ga2O3相结纳米柱阵列4之间形成Ti3C2/α/β-Ga2O3纳米柱阵列范德瓦尔斯异质结，所述氟掺杂氧化锡层2与所述Ag电极6形成通路。
进一步的，所述Ti3C2/α/β-Ga2O3纳米柱阵列范德瓦尔斯异质结由二维层状材料Ti3C2薄膜和n型α/β-Ga2O3相结纳米柱阵列构成。
进一步的，所述二维层状材料Ti3C2薄膜的厚度为200-300nm，所述n型α/β-Ga2O3相结纳米柱阵列由若干α/β-Ga2O3纳米柱构成，所述n型α/β-Ga2O3纳米柱的直径为50-200nm、长度为1.0～1.5μm。
进一步的，所述FTO衬底1的厚度为2.2mm。
进一步的，所述Ti3C2/Ag纳米线复合层5包括所述Ti3C2层及位于所述Ti3C2层上的Ag纳米线。
进一步的，所述氟掺杂氧化锡层2的接线处和所述Ag电极6的接线处位于所述FTO衬底1的同一侧。
进一步的，一种电网电晕监测器定向探测波长为200-280nm的日盲紫外光。
一种电网电晕监测器的制备方法，包括以下步骤：
步骤一、将FTO衬底1依次浸泡到丙酮、乙醇、去离子水中各超声10分钟，取出后再用去离子水冲洗，用干燥的氮气吹干；
步骤二、取浓度为10-15g/L的Ga(NO3)3溶液置于反应釜内胆中，然后将步骤一中用干燥的氮气吹干后的所述FTO衬底1斜靠在反应釜内胆中，并浸没于Ga(NO3)3溶液中，其中氟掺杂氧化锡层2朝向所斜靠的反应釜内胆一侧；
步骤三、将步骤二中的所述反应釜转移至烘箱中，在150℃下反应12h，随后取出FTO衬底1，用去离子水和无水乙醇交替清洗次，烘干后在高温炉中400-500℃先退火3.0-4.0小时，得到α-Ga2O3纳米柱阵列，然后将高温炉快速升温至700-800℃，并继续退火10-20分钟，获得α/β-Ga2O3相结纳米柱阵列4；
步骤四、在步骤三中得到的所述α/β-Ga2O3相结纳米柱阵列4上分别旋涂覆盖一层Ti3C2和银纳米线溶液，并在90℃下真空干燥箱中烘干，制作Ti3C2/Ag纳米线复合层5；
步骤五、在步骤四中所得的所述Ti3C2/Ag纳米线复合层5上方沉积一滴银胶作为上电极，即Ag电极6，刮去FTO衬底1边缘表面部分，露出氟掺杂氧化锡层2表面，作为下电极。
进一步的，步骤三中的所述将高温炉快速升温至700-800℃的快速升温时间为5-10分钟。
进一步的，步骤四中的所述银纳米线溶液的浓度为0.5-1.0mol/L，所述Ti3C2的浓度为25mg/L。
具体地，实施例1
(1)将FTO衬底1依次浸泡到丙酮、乙醇、去离子水中各超声10分钟，取出后再用去离子水冲洗，用干燥的氮气吹干；(2)取30mL浓度为5g/L的Ga(NO3)3溶液置于反应釜内胆中，然后将步骤(1)所得的FTO衬底1斜靠在反应釜内胆中，并浸没于Ga(NO3)3溶液中，其中氟掺杂氧化锡层2朝下(即朝向所斜靠的反应釜内胆一侧)；(3)将反应釜转移至烘箱中，在150℃下反应12h，随后取出，用去离子水和无水乙醇交替清洗3次，烘干后在高温炉中400℃先退火1.0小时，得到α-Ga2O3纳米柱阵列，然后将高温炉快速升温至750℃，并继续退火10分钟，获得α/β-Ga2O3相结纳米柱阵列4；(4)在步骤(3)得到的α/β-Ga2O3相结纳米柱阵列4上分别滴涂覆盖一层Ti3C2和银纳米线溶液，并在80℃下真空干燥箱中烘干，制作Ti3C2/Ag纳米线复合透明导电电极，即Ti3C2/Ag纳米线复合层5；(5)在步骤(4)所得的Ti3C2/Ag纳米线复合层5上方沉积一滴银胶作为上电极，即Ag电极6，刮去样品边缘表面部分，露出氟掺杂氧化锡层2表面，作为下电极；
在本实施例中，步骤(3)中的高温炉由400℃快速升温至750℃的快速升温时间为10分钟，在其它实施例中，快速升温时间只要控制在5-10分钟内即可，例如在5分钟、6分钟、7分钟、8分钟或9分钟等，通过控制快速升温时间以控制α-Ga2O3相转化为β-Ga2O3相的相变；
步骤(4)中的银纳米线溶液的浓度为0.5mol/L，Ti3C2溶液的浓度为25mg/L，先滴涂Ti3C2溶液于α/β-Ga2O3相结纳米柱阵列4上，形成干膜后再滴涂银纳米线溶液；
步骤(3)采用水热法制备α/β-Ga2O3相结纳米柱阵列4，在FTO衬底1生长GaOOH纳米柱阵列3，并进一步退火，将GaOOH纳米柱阵列3在不同的退火温度下分步转化为α/β-Ga2O3相结纳米柱阵列4；
将步骤(3)中退火前和退火后所得样品分别进行XRD分析，从图2中可以看出，(021)、(002)、(070)衍射峰为GaOOH相的特征峰，表明水热法生成的产物为GaOOH，(110)、(300)衍射峰为α-Ga2O3相的特征峰，表明400℃退火后得到的是α-Ga2O3，(002)、(111)、(401)衍射峰均为β-Ga2O3相的特征峰(图2)，没有发现其它杂质的特征峰，表明在750℃退火后得到的是β-Ga2O3材料，因此，在合适的退火时间下，可以获得α/β-Ga2O3相结材料，随着退火时间的增加，α-Ga2O3相将完全转变为β-Ga2O3相，将步骤(3)中所得样品在扫描电镜中观察，发现纳米柱生长均匀，图(3)为α/β-Ga2O3异质结纳米柱阵列端面的扫描电镜图，显示α/β-Ga2O3异质结纳米柱的直径为100-200nm，图(4)异质结纳米柱阵列的侧面扫描图，可以看出α/β-Ga2O3异质结纳米柱高度为1.2-1.5μm，Ti3C2的厚度为100nm；
对步骤(5)中所得的基于Ti3C2/α/β-Ga2O3纳米柱阵列范德瓦尔斯异质结的电网电晕监测器进行光电性能测试，图5给出了基于Ti3C2/Ga2O3不同结构纳米柱阵列的电网电晕监测器在光强为1mW/cm2的254nm光照下通过不断开关光源测得的I-T曲线图，重复测试4个I-T循环，均表现出很好的重复性，其中Ti3C2/α-Ga2O3纳米柱阵列对应的最大光电流为1.5nA，Ti3C2/β-Ga2O3纳米柱阵列对应的最大光电流为1800nA，而Ti3C2/α/β-Ga2O3相结纳米柱阵列对应的最大光电流明显优于前两者，为2800nA，这是由于Ga2O3相异质结在界面处能形成第二类型的能带排列，即某相的导带与价带位置均比另一相要高，对于光电器件来说，能使光照下产生的电子空穴对在界面处发生分离，电子流向能量低的一侧，而空穴则转移至能量高的一侧，实现光生载流子快速、有效地分离，提高光电器件的性能，而Ti3C2/β-Ga2O3和Ti3C2/α-Ga2O3只有单一的肖特基结构，相比Ti3C2/α/β-Ga2O3多异质结，分离电子空穴对的效率要相对低一些。
实施例2
步骤(1)、(4)和(5)均与实施例1相同；
步骤(2)中的Ga(NO3)3溶液的浓度为10g/L；
步骤(3)：在150℃下反应12h，水热生长羟基氧化镓，随后将GaOOH转移到高温炉中退火，先400℃退火1.5小时，得到α-Ga2O3纳米柱阵列，然后将高温炉快速升温至700℃，并继续退火20分钟，获得α/β-Ga2O3相结纳米柱阵列4；所得α/β-Ga2O3相结纳米柱阵列4的晶体结构、化学成分以及基于Ti3C2/α/β-Ga2O3纳米柱阵列范德瓦尔斯异质结的电网电晕监测器的光电特性均与实例1类似。
实施例3
步骤(1)、(4)和(5)均与实施例1相同；
步骤(2)中的Ga(NO3)3溶液的浓度为10g/L；
步骤(3)：在150℃下反应12h，水热生长羟基氧化镓，随后将GaOOH转移到高温炉中退火，先500℃退火2.0小时，得到α-Ga2O3纳米柱阵列，然后将高温炉快速升温至800℃，并继续退火10分钟，获得α/β-Ga2O3相结纳米柱阵列4，所得α/β-Ga2O3相结纳米柱阵列4的晶体结构、化学成分以及基于Ti3C2/α/β-Ga2O3纳米柱阵列范德瓦尔斯异质结的电网电晕监测器的光电特性均与实例1类似。
实施例4
步骤(1)、(4)和(5)均与实施例1相同；
步骤(2)中的Ga(NO3)3溶液的浓度为10g/L；
步骤(3)：在150℃下反应12h，水热生长羟基氧化镓，随后将GaOOH转移到高温炉中退火，在500℃退火2.0小时，得到α-Ga2O3纳米柱阵列，所得α-Ga2O3纳米柱阵列的晶体结构、化学成分与实施例1中第一次退火后所得的样品类似，基于Ti3C2/α-Ga2O3纳米柱阵列范德瓦尔斯异质结的电网电晕监测器的光电性能明显低于基于Ti3C2/α/β-Ga2O3纳米柱阵列范德瓦尔斯异质结的电网电晕监测器的光电性能(图4)。
实施例5
步骤(1)、(4)和(5)均与实施例1相同；
步骤(2)中的Ga(NO3)3溶液的浓度为10g/L；
步骤(3)：在150℃下反应12h，水热生长羟基氧化镓，随后将GaOOH转移到高温炉中退火，在800℃退火2.0小时，得到β-Ga2O3纳米柱阵列，所得β-Ga2O3纳米柱阵列的晶体结构、化学成分与实施例1中第二次退火后所得的样品类似，基于Ti3C2/β-Ga2O3纳米柱阵列纳米柱阵列柔性日盲紫外探测器的光电性能略低于Ti3C2/α/β-Ga2O3的光电性能(图4)。
实施例6
一种电网电晕监测器，包括Ag上电极，氟掺杂氧化锡层下电极，位于所述Ag上电极和所述氟掺杂氧化锡层下电极之间的α/β-Ga2O3相结纳米柱阵列和Ti3C2/Ag纳米线复合电极，其中玻璃片作为氟掺杂氧化锡层下电极的衬底；所述α/β-Ga2O3相结纳米柱阵列包括若干间隔设置的α/β-Ga2O3相结纳米柱；所述Ti3C2/Ag纳米线复合电极位于所述α/β-Ga2O3相结纳米柱背离所述氟掺杂氧化锡层下电极一端，所述Ag上电极部分覆盖所述Ti3C2/Ag纳米线复合电极。
其中，所述α/β-Ga2O3纳米相结包括α-Ga2O3内核和包覆于α-Ga2O3内核侧壁和顶部的β-Ga2O3纳米相；所述氟掺杂氧化锡层下电极直接与所述α-Ga2O3内核的底部和所述β-Ga2O3纳米相的底部接触。
其中，所述氟掺杂氧化锡层的厚度为200～300nm，所述α/β-Ga2O3相结纳米柱的直径为50-100nm，长度为1μm～1.5μm，所述β-Ga2O3纳米相的厚度为10-30nm；所述玻璃片的厚度为2.2mm，所述β-Ga2O3纳米相的厚度是指β-Ga2O3纳米相平行于所述玻璃片平面方向的所述β-Ga2O3纳米相的尺寸。
其中，所述Ti3C2/Ag纳米线复合电极由Ti3C2片和Ag纳米线复合而成，形成透明导电电极，并串联所述α/β-Ga2O3相结纳米柱阵列。
最后应说明的是：以上实施例仅用以说明本发明的技术方案，而非对其限制；尽管参照前述实施例对本发明技术方案进行了详细的说明，本领域的技术人员应当理解，其依然可以对前述实施例所记载的技术方案进行修改，或者对其中部分技术特征进行同等替换；而这些修改或者替换，并不使相应技术方案的本质脱离本发明各实施例技术方案的精神与范围。
Claims (3)
1.一种电网电晕监测器的制备方法，其特征在于，包括以下步骤：
步骤一、将FTO衬底（1）依次浸泡到丙酮、乙醇、去离子水中各超声10分钟，取出后再用去离子水冲洗，用干燥的氮气吹干；
步骤二、取浓度为10-15 g/L的Ga(NO3)3溶液置于反应釜内胆中，然后将步骤一中用干燥的氮气吹干后的所述FTO衬底（1）斜靠在反应釜内胆中，并浸没于Ga(NO3)3溶液中，其中氟掺杂氧化锡层（2）朝向所斜靠的反应釜内胆一侧；
步骤三、将步骤二中的所述反应釜转移至烘箱中，在150 °C下反应12 h，随后取出FTO衬底（1），用去离子水和无水乙醇交替清洗次，烘干后在高温炉中400-500 °C先退火3.0-4.0小时，得到α-Ga2O3纳米柱阵列，然后将高温炉快速升温至700-800 °C，并继续退火10-20分钟，获得α/β-Ga2O3相结纳米柱阵列（4）；
步骤四、在步骤三中得到的所述α/β-Ga2O3相结纳米柱阵列（4）上分别旋涂覆盖一层Ti3C2和银纳米线溶液，并在90°C下真空干燥箱中烘干，制作Ti3C2/Ag纳米线复合层（5）；
步骤五、在步骤四中所得的所述Ti3C2/Ag纳米线复合层（5）上方沉积一滴银胶作为上电极，即Ag电极（6），刮去FTO衬底（1）边缘表面部分，露出氟掺杂氧化锡层（2）表面，作为下电极。
2.根据权利要求1所述的一种电网电晕监测器的制备方法，其特征在于，步骤三中的所述将高温炉快速升温至700-800 °C的快速升温时间为5-10分钟。
3.根据权利要求1所述的一种电网电晕监测器的制备方法，其特征在于，步骤四中的所述银纳米线溶液的浓度为0.5-1.0 mol/L，所述Ti3C2的浓度为25mg/L。
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