CN117038761A - 一种高性能NdNb2O7紫外探测器及其制备方法 - Google Patents
一种高性能NdNb2O7紫外探测器及其制备方法 Download PDFInfo
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Abstract
本发明公开一种高性能NdNb2O7紫外探测器及其制备方法，包括如下步骤：(a)NdNb2O7纳米片的制备方法。(b)NdNb2O7纳米片薄膜的自组装方法。(c)NdNb2O7纳米片薄膜器件的光电性能。本发明首次公开一种高性能NdNb2O7紫外探测器及其制备方法。这项工作通过固相反应‑液相剥离方法首次制备出NdNb2O7纳米片，通过界面自组装方法获得NdNb2O7纳米片薄膜，并获得高性能NdNb2O7纳米片薄膜紫外探测器，为其在光电探测领域的应用奠定基础。
Description
技术领域
本发明属于紫外光电探测器技术领域，更具体的涉及一种高性能NdNb2O7紫外探测器及其制备方法。
背景技术
层状氧化物钙钛矿由于其独特的层状结构和层间化学反应性，是一种重要的多功能材料，具有丰富的物理和化学性质。在传统的二维材料中，如石墨烯和过渡金属硫族化物，这些主要由s和p轨道的电子决定，它们表现出弱的相互作用。过渡金属氧化物钙钛矿中d轨道的强相互作用电子产生了丰富的奇异相，包括高温超导性、巨磁阻、莫特金属-绝缘体跃迁和多铁性等，为揭示物理学中的新范式和新应用提供了一个良好的平台。目前，通过液相剥离法制备的二维钙钛矿铌酸盐纳米片已引起广泛关注。RbNdNb2O7是一种稳定的双层氧化物钙钛矿，具有Dion-Jacobson相结构。其稳定的性质使NdNb2O7成为广泛应用的有前途的候选者。然而，NdNb2O7纳米片的剥离及其光电性能的研究尚未报道。因此，探索基于二维钙钛矿型NdNb2O7的高性能光电探测器是至关重要的。
发明内容
本发明首次通过固相反应-液相剥离法制备出NdNb2O7纳米片，并通过界面自组装法获得NdNb2O7纳米片薄膜，并实现高性能NdNb2O7纳米片薄膜紫外探测器，为NdNb2O7纳米片在光电子器件领域的应用提供基础。
为达到上述发明创造目的，本发明采用下述技术方案：
根据本发明的第一个方面,本发明提供一种NdNb2O7纳米片的制备方法，包括如下步骤：NdNb2O7纳米片是通过固相反应和液相剥离方法制备的，Rb2CO3、Nd2O3和Nb2O5的混合研磨后煅烧，得RbNdNb2O7粉末；将所得RbNdNb2O7粉末与HNO3水溶液振荡，得到HNdNb2O7产物洗涤并干燥；将HNdNb2O7与四丁基氢氧化铵水溶液中振荡、离心，得到NdNb2O7纳米片。
优选地，按照摩尔比计算，Rb2CO3：Nd2O3：Nb2O5＝1.3:1:2。
优选地，所述煅烧是指在1000℃下空气中煅烧24小时。
优选地，将HNdNb2O7与其等摩尔的四丁基氢氧化铵水溶液中振荡3天。
根据本发明的第二个方面，本发明提供一种气液界面自组装方法制备NdNb2O7纳米片薄膜的方法，包括如下步骤：将上述NdNb2O7纳米片分散在水中，并加入DMF形成混合分散液，然后取混合分散液滴在氯仿表面，自组装形成NdNb2O7纳米片薄膜。优选地，首先将NdNb2O7纳米片分散在水中，并加入少量DMF。然后取部分溶液滴在氯仿表面。随后，NdNb2O7纳米片薄膜开始在水面上形成，并逐渐形成更大的NdNb2O7纳米片薄膜。最后自组装的纳米片薄膜可以直接转移到不同的衬底上，用于器件制造。
根据本发明的第三个方面，本发明提供了一种NdNb2O7紫外光电探测器(简称器件)，将上述NdNb2O7纳米片薄膜转移至衬底上，然后用用硬膜版蒸镀Cr/Au电极来构筑紫外光电探测器。
优选地，所述衬底为Si/SiO2，PET或载玻片；进一步优选为PET。
根据本发明的第四个方面，本发明提供了一种NdNb2O7纳米片的用途，用于制备NdNb2O7紫外光电探测器。
本发明中NdNb2O7纳米片薄膜具有高的可见光透明性，同时该器件具有优异的光电性能，并且在很多弯曲测试仍有良好的光电性能。
透明性能中，NdNb2O7紫外光电探测器具有高的可见光透明性(>80％)。
光电性能中，NdNb2O7紫外光电探测器具有高的光电性能，在3
V电压和260nm光照射下，该器件具有高的光电流为1.4uA,高的响应度为1.2A/W，高的比探测率为7.7*1011Jones。
柔性性能中，NdNb2O7紫外光电探测器在进行200次弯曲测试后，仍然具有优异的光电性能，具有较高的光电流为0.12uA,较大的开关比为100。
本发明首次提出一种高性能NdNb2O7紫外探测器，大大拓展NdNb2O7纳米片在光电子器件中的应用。
本发明具有突出优点：
1，本发明首次提出高性能柔性透明NdNb2O7紫外探测器，制备简单、成本低廉、具有可产业化前景。
2，NdNb2O7纳米片是通过固相反应和液相剥离方法制备的。
3，NdNb2O7纳米片薄膜是通过气液界面自组装方法实现的。
4，NdNb2O7纳米片薄膜紫外探测器具有优异的紫外探测性能，在3V和260nm光照射下具有高的光电流(1.4uA)，高响应度(1.2AW-1)和高比探测率(7.7*1011)。
5，NdNb2O7纳米片薄膜器件经过多次弯曲测试也能保持优异的性能，表现出令人满意的光电流(0.12uA)和大的开/关比(100)。
附图说明
图1为实施例NdNb2O7纳米片制备过程的示意图，其中a为纳米片的制备过程示意图；b,c,d分别为材料制备过程中的扫描电子显微镜图。
图2为NdNb2O7纳米片的表征图，a,b,c分别为纳米片的Nd、Nb、O元素的mapping图，d,e,f分别为纳米片的Nd、Nb、O元素的X射线光电子谱图。
图3为NdNb2O7纳米片薄膜的自组装过程示意图，a,b,c为纳米片自组装过程示意图，d,e分别为纳米片薄膜的透射电子显微镜图和扫描电子显微镜图。
图4为NdNb2O7纳米片薄膜器件的光电性能，a为该纳米片薄膜的透明度图，b为该器件的柔性弯曲展示图，c,d为该器件弯曲测试的I-V和I-t图，e,f为该薄膜器件的响应度和探测率。
具体实施方式
NdNb2O7纳米片薄膜紫外探测器的光电性能是通过半导体测量系统(Keithley4200)、探针台和光源组合系统进行测试的。所有测量均在室温下的大气环境中进行。
实施例1
(1)NdNb2O7纳米片的制备。首先，将Rb2CO3、Nd2O3和Nb2O5(摩尔比为1.3:1:2)的混合物彻底研磨。将混合物在1000℃下空气中煅烧24小时后，重复一次研磨和煅烧。其次，将所得RbNdNb2O7粉末与5MHNO3水溶液缓慢振荡5天，每天更新HNO3水溶液，得到HNdNb2O7产物洗涤并干燥。最后，将HNdNb2O7产物与其等摩尔四丁基氢氧化铵水溶液中进行振荡3天，然后对溶液进行离心，得到NdNb2O7纳米片。
图1为NdNb2O7纳米片的制备过程示意图和形貌表征，图1中a为纳米片的制备过程示意图，分别对应于固相烧结,质子化，液相剥离步骤。图1中b为固相烧结的RbNdNb2O7粉末的扫描电镜图，可以看出获得大尺寸的块状颗粒。图1中c为质子化的HNdNb2O7粉体的扫描电镜图，可以看出其具有明显的层状结构和层间缝隙。图1中d图为液相剥离的NdNb2O7纳米片的扫描电镜图，可以看出成功的剥离出NdNb2O7纳米片。
图2为NdNb2O7纳米片的表征图。a,b,c分别为纳米片的透射电镜Mapping图对应Nd、Nb、O元素的分布图，可以看出三种元素均匀地分布于纳米片中。d,e,f分别为纳米片的X射线光电子谱图，可以看出NdNb2O7纳米片对应的Nd3d，Nb3d，O1s态。
(2)NdNb2O7纳米片薄膜的界面自组装方法，首先将NdNb2O7纳米片分散在水中，并加入少量DMF。然后取部分溶液滴在氯仿表面。随后，薄膜开始在水面上形成，并逐渐形成更大的薄膜。最后自组装的纳米片薄膜可以直接转移到不同的衬底上(Si/SiO2，PET，载玻片)，用于器件制造。
图3为纳米片的自组装过程示意图和纳米片薄膜表征图。图3中a,b,c为NdNb2O7纳米片自组装过程示意图。将适量的DMF滴入纳米片的水溶液中。DMF可与水和氯仿混溶，降低了它们之间的界面能，增加纳米片的流动性。将氯仿加入玻璃容器中，然后将纳米片溶液小心地加入氯仿表面(图3中a)。随着氯仿的蒸发，纳米片悬浮液迁移到水-空气界面(图3中b)。纳米片的流动性导致纳米片并排排列，组装成平整的宏观薄膜。如图3中c所示，小的NdNb2O7颗粒选择性地从纳米片中分离并粘附在容器壁上。大的NdNb2O7颗粒保留在氯仿-水界面，对组装结构没有贡献。表面配体(四丁基离子)仍然分散在水溶液中。因此通过界面自组装方法获得的平坦性和均匀性良好的纳米片薄膜。d-e分别为纳米片薄膜的原子力显微镜图和扫描电镜图，可以看出纳米片薄膜具有良好的平整度。
(3)NdNb2O7纳米片薄膜器件的光电性能。
纳米片通过界面自组装方法获得纳米片薄膜，然后转移到PET衬底，然后用硬膜版蒸镀Cr/Au电极来构筑器件。
如图4中a所示，NdNb2O7薄膜在350nm附近表现出透射率的明显降低，随后从350nm逐渐降低到300nm。由于其宽带隙，它在可见光范围(400-760nm)内保持80％的平均透射率。拍摄的照片清楚地展示了NdNb2O7纳米片的透明度。NdNb2O7薄膜器件的柔性展示如图4中b所示。NdNb2O7纳米片薄膜器件可以大角度弯曲，并测试了相应的光电性能。NdNb2O7薄膜器件在经历重复弯曲循环后，在黑暗和300nm光照下的I-V特性如图4中c所示。在弯曲测试之前，该器件在300nm光照射下在3V下表现出12nA的暗电流和2.3uA的光电流。图4中d示出了在300nm光照下特定弯曲角度下NdNb2O7薄膜器件的I-t曲线。即使在多次弯曲循环之后，该器件也表现出快速且可重复的光响应，没有任何明显的延迟。在打开和关闭入射光时，光电流迅速增加到1.2μA、0.56μA和0.12μA，然后分别迅速衰减到6.8nA、3.9nA和1.1nA。相应的开关比估计为176、143和109。图4中e展示了NdNb2O7薄膜器件的高响应度，在3V时在260nm处达到1.2AW-1。图4中f突出了NdNb2O7膜器件的高检测率，达到7.7*1011Jones。考虑到简单的制造工艺以及器件的灵活性和透明度，即使在反复弯曲测试后，NdNb2O7薄膜器件也能保持令人满意的性能。
综上所述，本发明首次提出高性能NdNb2O7纳米片薄膜紫外探测器，并提供一种剥离和自组装方法，将为NdNb2O7纳米片在光电子器件领域的应用奠定基础。
Claims (10)
1.一种NdNb2O7纳米片的制备方法，包括如下步骤：NdNb2O7纳米片是通过固相反应和液相剥离方法制备的，Rb2CO3、Nd2O3和Nb2O5的混合研磨后煅烧，得RbNdNb2O7粉末；将所得RbNdNb2O7粉末与HNO3水溶液振荡，得到HNdNb2O7产物洗涤并干燥；将HNdNb2O7与四丁基氢氧化铵水溶液中振荡、离心，得到NdNb2O7纳米片。
2.根据权利要求1所述的方法，其特征在于：按照摩尔比计算，Rb2CO3：Nd2O3：Nb2O5＝1.3:1:2；
和/或，所述煅烧是指在1000℃下空气中煅烧24小时；
和/或，将HNdNb2O7与其等摩尔的四丁基氢氧化铵水溶液中振荡3天。
3.一种气液界面自组装方法制备NdNb2O7纳米片薄膜的方法，包括如下步骤：将权利要求1或2所述方法制备出的NdNb2O7纳米片分散在水中，并加入DMF形成混合分散液，然后取混合分散液滴在氯仿表面，自组装形成NdNb2O7纳米片薄膜。
4.一种NdNb2O7紫外光电探测器，将权利要求3所述方法制备出的NdNb2O7纳米片薄膜转移至衬底上，然后用硬膜版蒸镀Cr/Au电极来构筑紫外光电探测器。
5.根据权利要求4所述的NdNb2O7紫外光电探测器，所述衬底为Si/SiO2，PET或载玻片；进一步优选为PET。
6.一种NdNb2O7纳米片的用途，用于制备NdNb2O7紫外光电探测器。
7.根据权利要求6所述的用途，用于制备高性能柔性透明紫外探测器。
8.一种NdNb2O7紫外光电探测器的制备方法，包括如下步骤：
NdNb2O7纳米片的制备：NdNb2O7纳米片是通过固相反应和液相剥离方法制备的，Rb2CO3、Nd2O3和Nb2O5的混合研磨后煅烧，得RbNdNb2O7粉末；将所得RbNdNb2O7粉末与HNO3水溶液振荡，得到HNdNb2O7产物洗涤并干燥；将HNdNb2O7与四丁基氢氧化铵水溶液中振荡、离心，得到NdNb2O7纳米片；
NdNb2O7纳米片薄膜的制备：将NdNb2O7纳米片分散在水中，并加入DMF形成混合分散液，然后取混合分散液滴在氯仿表面，自组装形成NdNb2O7纳米片薄膜；
NdNb2O7纳米片薄膜转移至PET衬底上，然后用硬膜版蒸镀Cr/Au电极来构筑紫外光电探测器。
9.根据权利要求8所述的方法，所述NdNb2O7纳米片薄膜紫外探测器具有优异的光电性能，在3V和260nm光照射下，光电流为1.4uA，响应度为1.2A/W，比探测率为7.7*1011Jones。
10.根据权利要求8所述的高性能NdNb2O7紫外探测器，其特征在于：NdNb2O7纳米片薄膜紫外探测器具有优异的柔性光电性能，在200次弯曲测试后，NdNb2O7紫外探测器的光电流为0.12uA，开关比为100。
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