CN110845728B - 一种导电高分子/五氧化二铌异质结的制备方法及其应用 - Google Patents

一种导电高分子/五氧化二铌异质结的制备方法及其应用 Download PDF

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CN110845728B
CN110845728B CN201911079915.5A CN201911079915A CN110845728B CN 110845728 B CN110845728 B CN 110845728B CN 201911079915 A CN201911079915 A CN 201911079915A CN 110845728 B CN110845728 B CN 110845728B
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于平平
王群亮
姜岩峰
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Abstract

本发明公开了一种导电高分子/五氧化二铌异质结的制备方法及其应用，属于半导体纳米材料技术领域。本发明以铌箔作为前驱体，水热法制备Nb2O5纳米棒阵列；然后采用原位聚合的方法制备导电高分子/Nb2O5异质结；所述原位聚合是在质子酸溶液体系中进行的，通过质子酸掺杂调控导电高分子的能带，获得更高质量的异质结型光电探测器。

Description

一种导电高分子/五氧化二铌异质结的制备方法及其应用
技术领域
本发明涉及一种导电高分子/五氧化二铌异质结的制备方法及其应用，属于半导体纳米材料技术领域。
背景技术
低维半导体纳米结构的紫外光探测器是纳米材料领域研究的热点和重点，是由于其具有优异的物理和化学性质、光电转化活性高等优势，而且其高比表面积和大大减小的有效导电通道尺寸，通常比传统的薄膜紫外光电探测器具有更高的光灵敏性、选择性和稳定性等优点，对紫外光具有良好的响应性，但存在光电流较小、高暗电流或者较低的响应速度等缺陷。另外，由于表面陷阱态导致在纳米材料表面存在载流子耗尽层，使信号恢复时间较长。
五氧化二铌(Nb2O5)是n型半导体氧化物，禁带宽度为3.0～3.4e V,具有低毒性、导带和价带相差较大、良好的化学稳定性、热稳定性、较高的电子转移率以及高的光催化活性等优点，吸引了很多研究者们的关注，被广泛的应用到诸如气体传感、催化、电致变色等相关领域。基于单根Nb2O5纳米带和中空纳米球形貌结构的探测器已有报道，但是光电性能不理想逊色于ZnO、ZnS和SnO2等，所以Nb2O5作为紫外光探测器仍处于起步阶段，存在光电流小和恢复时间长的问题，急需新型异质结结构提高光电性能。
肖特基势垒(Schottky)、pn结和异质结的光伏效应是解决以上问题的有效途径。目前，报道较多的是无机半导体异质结纳米结构如ZnO/ZnS纳米带、ZnO/ZnSe壳核结构纳米线阵列、GaP/ZnS同轴纳米线和ZnO-Ga2O3核壳结构微米线等，均为n-n型异质结，这是由于无机半导体材料的p型掺杂还相对困难，满足能带匹配的要求构成pn结且紫外光灵敏度高的p型无机半导体较少。有机半导体成为了无机半导体强有力的替代者，其中p型导电高分子(聚苯胺PANI，聚吡咯PPy和聚噻吩PEDOT/P3HT)受到研究者的青睐，主要依赖于其质轻、柔性、易合成、可大面积低成本制备等优点以及类似于金属或半导体的独特电子和光学性能。如PANI/MgZnO、PANI/TiO2的pn结型全固态自驱动日盲紫外探测器以及导电高分子/Se微米管的异质结基自驱动紫外-可见光电探测器，证明可以用于构筑有机/无机半导体异质结，实现自驱动和高性能的紫外光探测器。但是，采用通常直接混合或者中性溶液中制备导电高分子异质结，导致其丧失导电性甚至吸收峰的位置改变影响本质能级结构，进而无法能级匹配来保证异质结质量以及器件性能。
发明内容
为了解决本发明所要解决的技术问题，本发明以铌箔作为前驱体，水热法制备Nb2O5纳米棒阵列，采用原位聚合的方法制备核壳型导电高分子/Nb2O5异质结阵列，通过质子酸掺杂调控导电高分子的能带，获得更高质量的异质结型光电探测器。
本发明的第一个目的是提供一种导电高分子/Nb2O5异质结的制备方法，所述方法是以铌箔作为前驱体，水热法制备Nb2O5纳米棒阵列；然后采用原位聚合的方法制备导电高分子/Nb2O5异质结；所述原位聚合是在质子酸溶液体系中进行的。其中，质子酸作为H+掺杂调控导电高分子的能带，以获得更高质量的异质结型光电探测器。
在本发明一种实施方式中，所述导电高分子为聚苯胺、聚吡咯或者聚噻吩。
在本发明一种实施方式中，所述质子酸为没食子酸、单宁酸、柠檬酸、樟脑磺酸中的一种。
在本发明一种实施方式中，所述质子酸浓度为0.05mol/L-1.5mol/L。
在本发明一种实施方式中，采用水热法制备Nb2O5纳米棒阵列的方法是：将清洗后铌箔放入过氧化氢溶液中，然后加入0.5-2g矿化剂，充分混合，放入水热釜中100-200℃保持10-24h，后自然冷却至室温，在铌箔表面获得Nb2O5纳米棒阵列。
在本发明一种实施方式中，过氧化氢溶液中过氧化氢和去离子水的体积比为(1-2)：1，所述矿化剂为NH4F。
在本发明一种实施方式中，采用原位聚合方法制备导电高分子/Nb2O5异质结是：将导电单体加入质子酸溶液中搅拌5-15min以确保充分分散，加入生长有Nb2O5纳米棒阵列的铌箔，静置1-4h，混合液温度保持在-4～0℃；加入过硫酸铵(APS)加入质子酸溶液中，反应20～30h，反应完成后的样品多次用去离子水清洗后真空烘箱80℃干燥12h，所以在铌箔上得到聚苯胺/Nb2O5的异质结阵列。
在本发明一种实施方式中，所述单体为苯胺、吡咯或者噻吩；所述单体与过硫酸铵的摩尔比为(0.25-4):1。
本发明的第二个目的是提供一种上述制备方法制备得到的导电高分子/五氧化二铌纳米棒异质结。
本发明的第三个目的是提供一种上述导电高分子/五氧化二铌纳米棒异质结在光电探测器中的应用。
本发明的有益效果：
纳米棒异质结生长过程中采用通常直接混合或者中性溶液中制备导电高分子异质结，导致其丧失导电性甚至吸收峰的位置改变影响本质能级结构，进而无法能级匹配来保证异质结质量以及器件性能。本发明原位聚合有机/无极异质结纳米结构，改变导电高分子单体和调整质子酸参数，能够实现高内建电场的异质结的制备。
附图说明
图1为实例1制备的Nb2O5纳米棒阵列的扫描电镜图片；左边为低倍SEM图，右边为高倍SEM图。
图2为实例1制备的聚苯胺/Nb2O5纳米棒异质结阵列的扫描电镜图片。
具体实施方式
以下对本发明的优选实施例进行说明，应当理解实施例是为了更好地解释本发明，不用于限制本发明。
光电性能测试方法：通过磁控溅射方法将Ti/Au镀膜于聚苯胺/Nb2O5异质结的掩膜版，作为上层电极，掩膜版的叉指长10mm宽390mm，得到两Ti/Au电极间距离2mm左右。器件的电流-电压(I-V)和电流-时间(I-t)特性测试采用双探针法。
实施例1：制备PANI/Nb2O5异质结纳米棒
采用水热法生长高质量的Nb2O5纳米棒阵列，具体参数条件是：依次采用丙酮、乙醇和去离子水清洗的铌箔，其规格为2×2cm，厚度0.25mm，放入过氧化氢和去离子水比例为1：0.5的混合液中，然后加入0.5的NH4F作为矿化剂，充分混合，放入水热釜中100-200℃保持12h，后自然冷却至室温，在铌箔表面获得Nb2O5纳米棒阵列，如图1所示。
采用原位聚合生长纳米厚度的聚苯胺壳层，具体生长条件是：适量苯胺单体(AN)加入质子酸溶液中搅拌10min以确保充分分散，生长有Nb2O5纳米棒阵列的铌箔加入以上溶液充分静置2h，混合液温度保持在0℃。适量的过硫酸铵(APS)加入0.5M没食子酸溶液中，搅拌5min。AN:APS的摩尔比为2:1。聚合反应温度在0℃，反应时间为24h，反应完成后的样品多次用去离子水清洗后真空烘箱80℃干燥12h，所以在铌箔上得到PANI/Nb2O5的异质结阵列。如图2所示，PANI均匀的包裹着Nb2O5纳米棒，形成核壳结构。制作异质结器件，波长320nm的激光照射电压为0V时光电流达到60pA，上升时间15s和恢复时间9s。
实施例2：制备PPy/Nb2O5异质结纳米棒
采用水热法生长高质量的Nb2O5纳米棒阵列，具体参数条件是：依次采用丙酮、乙醇和去离子水清洗的铌箔，其规格为2×2cm，厚度0.25mm，放入过氧化氢和去离子水比例为1:0.5的混合液中，然后加入0.5g的NH4F作为矿化剂，充分混合，放入水热釜中100-200℃保持12h，后自然冷却至室温，在铌箔表面获得Nb2O5纳米棒阵列，如图1所示。
采用原位聚合生长纳米厚度的聚吡咯壳层，具体生长条件是：适量吡咯单体(Py)加入质子酸溶液中搅拌10min以确保充分分散，生长有Nb2O5纳米棒阵列的铌箔加入以上溶液充分静置2h，混合液温度保持在0℃。适量的过硫酸铵(APS)加入0.5M没食子酸溶液中，搅拌5min。Py:APS的摩尔比为2:1。聚合反应温度在0℃，反应时间为24h，反应完成后的样品多次用去离子水清洗后真空烘箱80℃干燥12h，所以在铌箔上得到PPy/Nb2O5的异质结阵列。制作异质结器件，波长320nm的激光照射电压为0V时光电流达到55pA，上升时间20s和恢复时间14s。
实施例3：制备PEDOT/Nb2O5异质结纳米棒
采用水热法生长高质量的Nb2O5纳米棒阵列，具体参数条件是：依次采用丙酮、乙醇和去离子水清洗的铌箔，其规格为2×2cm，厚度0.25mm，放入过氧化氢和去离子水比例为1:0.5的混合液中，然后加入0.5g的NH4F作为矿化剂，充分混合，放入水热釜中100-200℃保持12h，后自然冷却至室温，在铌箔表面获得Nb2O5纳米棒阵列，如图1所示。
采用原位聚合生长纳米厚度的聚噻吩壳层，具体生长条件是：适量噻吩单体(EDOT)加入质子酸溶液中搅拌10min以确保充分分散，生长有Nb2O5纳米棒阵列的铌箔加入以上溶液充分静置2h，混合液温度保持在0℃。适量的过硫酸铵(APS)加入0.5M没食子酸溶液中，搅拌5min。EDOT:APS的摩尔比为2:1。聚合反应温度在0℃，反应时间为24h，反应完成后的样品多次用去离子水清洗后真空烘箱80℃干燥12h，所以在铌箔上得到聚噻吩/Nb2O5的异质结阵列。制作异质结器件，波长320nm的激光照射电压为0V时光电流达到50pA，上升时间23s和恢复时间16s。
实施例4：不同种类质子酸对PANI/Nb2O5异质结性能的影响
参考实施例1的制备方法制备PANI/Nb2O5的异质结，区别仅在于：质子酸种类不同，将没食子酸替换成单宁酸、柠檬酸、樟脑磺酸、盐酸、对甲基苯磺酸。
表1不同种类质子酸对PANI/Nb2O5异质结性能的影响
Figure GDA0002748633480000041
从表1中可以看出质子酸种类不同对PANI/Nb2O5异质结器件的光电性能影响不同，没食子酸掺杂异质结获得的暗电流最小，光电流与暗电流之比数值最大达到12，恢复时间最短，而其他种类质子酸的掺杂在提高光电流的同时也增大了暗电流，导致光暗电流比值较小，恢复时间也略延长。证明不同种类质子酸的掺杂对异质结光电性能影响差异很大，需要合理选择，此处没食子酸的性能最优。
实施例5：不同浓度质子酸对导电高分子/Nb2O5异质结性能的影响
参考实施例1的制备方法制备PANI/Nb2O5的异质结，区别仅在于：没食子酸浓度不同，将质子酸浓度调整成0.05-1.5M。
表2不同浓度质子酸对导电高分子/Nb2O5异质结性能的影响
Figure GDA0002748633480000051
从表2中可以看出不同浓度的没食子酸对PANI/Nb2O5异质结的光电性能影响不同，质子酸浓度在0.5-0.8mol/L时光电流能达60pA，恢复时间最短，仅需9s。因此质子酸的浓度不能太低或者太高都不利于高电导率聚苯胺生长，也不利于提高异质结的光电性能。
实施例6：不同单体和氧化剂用量比对导电高分子/Nb2O5异质结性能的影响
参考实施例1的制备方法制备PANI/Nb2O5的异质结，区别仅在于：单体和氧化剂用量比不同，将单体和氧化剂摩尔比调整成1:4、1:2、2:1和4:1。
表3单体和氧化剂摩尔比对导电高分子/Nb2O5异质结性能的影响
Figure GDA0002748633480000052
从表3中可以看出在单体与氧化剂用量比为1:1～2:1范围内，导电性能较好，单体与氧化剂用量比较高和较低是都不利于聚苯胺的生长，影响聚苯胺电导率以及能带结构，从而影响异质结的光暗电流比值，单体/APS比值为2:1时达到最高值，恢复时间也最短。
对比例1：
参考实施例1的制备方法制备PANI/Nb2O5的异质结，区别仅在于：将质子酸替换成去离子水，由于苯胺不聚合，无法得到PANI/Nb2O5的异质结。
虽然本发明已以较佳实施例公开如上，但其并非用以限定本发明，任何熟悉此技术的人，在不脱离本发明的精神和范围内，都可做各种的改动与修饰，因此本发明的保护范围应该以权利要求书所界定的为准。

Claims (10)

1.一种导电高分子/五氧化二铌异质结的制备方法，其特征在于，所述方法是以铌箔作为前驱体，水热法制备Nb2O5纳米棒阵列；然后采用原位聚合的方法制备导电高分子/Nb2O5异质结；所述原位聚合是在质子酸溶液体系中进行的；所述质子酸为没食子酸，质子酸浓度为0.5 mol/L-0.8 mol/L。
2.根据权利要求1所述的制备方法，其特征在于，所述导电高分子为聚苯胺、聚吡咯或者聚噻吩。
3.根据权利要求1或2所述的制备方法，其特征在于，采用水热法制备Nb2O5纳米棒阵列具体是：将清洗后的铌箔放入过氧化氢溶液中，然后加入矿化剂，充分混合，放入水热釜中100-200℃保持10-24h，后冷却至室温，在铌箔表面获得Nb2O5纳米棒阵列。
4.根据权利要求3所述的制备方法，其特征在于，过氧化氢溶液中过氧化氢和去离子水的体积比为（1-2）：1，所述矿化剂为NH4F。
5.根据权利要求1、2或4任一所述的制备方法，其特征在于，采用原位聚合方法制备导电高分子/Nb2O5异质结是：将导电单体加入质子酸溶液中分散均匀，加入生长有Nb2O5纳米棒阵列的铌箔，静置1-4 h，混合液温度保持在-4~0℃；加入过硫酸铵到质子酸溶液中，配制成含过硫酸铵的质子酸溶液；再将含过硫酸铵的质子酸溶液加入到上述混合液中反应20~30 h，反应完成后清洗、干燥得到导电高分子/Nb2O5的异质结。
6.根据权利要求3所述的制备方法，其特征在于，采用原位聚合方法制备导电高分子/Nb2O5异质结是：将导电单体加入质子酸溶液中分散均匀，加入生长有Nb2O5纳米棒阵列的铌箔，静置1-4 h，混合液温度保持在-4~0℃；加入过硫酸铵到质子酸溶液中，配制成含过硫酸铵的质子酸溶液；再将含过硫酸铵的质子酸溶液加入到上述混合液中反应20~30 h，反应完成后清洗、干燥得到导电高分子/Nb2O5的异质结。
7.根据权利要求5所述的制备方法，其特征在于，所述导电单体与过硫酸铵的摩尔比为（0.25-4）:1。
8.根据权利要求6所述的制备方法，其特征在于，所述导电单体与过硫酸铵的摩尔比为（0.25-4）:1。
9.权利要求1~8任一所述的制备方法制备得到的导电高分子/ Nb2O5异质结。
10.权利要求9所述的导电高分子/ Nb2O5异质结在光电探测器中的应用。
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