CN110552037B - 一种基于电化学沉积制备氧化锌纳米墙的方法 - Google Patents
一种基于电化学沉积制备氧化锌纳米墙的方法 Download PDFInfo
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 119
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- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000000758 substrate Substances 0.000 claims abstract description 21
- 238000000137 annealing Methods 0.000 claims abstract description 18
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- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims abstract description 3
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- 238000001069 Raman spectroscopy Methods 0.000 description 1
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开一种基于电化学沉积制备氧化锌纳米墙的方法，即采用传统的电化学沉积方法在导电衬底上生长出二维纳米结构的氧化锌纳米墙。该电化学沉积利用一种简单的电化学沉积装置，主要包括直流稳压电源、阳极、电解槽、绝缘挡板和加热装置等部分；将带有氧化锌籽晶层的导电衬底作为阴极、碳棒作为阳极，浸入盛有硝酸锌(Zn(NO3)2·6H2O)水溶液的电解槽中，利用加热装置加热到设定温度后通上直流电压在阴极产生金属锌离子还原反应而生长出氧化锌纳米墙，随后进行退火处理。本发明制备的氧化锌纳米墙具有形貌可控、尺寸均匀和结晶度高等优点，为二维纳米结构氧化锌纳米墙的广泛应用奠定坚实基础。
Description
技术领域
本发明属于半导体纳米材料制备领域，具体涉及到一种电化学沉积制备氧化锌纳米墙的方法。
背景技术
氧化锌(ZnO)是一种Ⅱ-Ⅵ族宽禁带半导体材料，具有优异的光学、电学、机械性能、化学稳定性和热稳定性。氧化锌在室温下的禁带宽度为3.37eV、激子束缚能为60 meV，具有很强的近紫外发射和光学透明电导性；低维的氧化锌纳米材料，如纳米棒、纳米线、纳米带、纳米墙和纳米管，其独特纳米结构产生量子效应的增强，使其表现出独特的光学、电学和声学性能。尤其是二维结构的氧化锌纳米墙是一种空间网络蜂窝状材料，蜂窝由氧化锌片层交织而成，具有高的比表面积、好的电子连续性和高的电子迁移率，是制备传感器、锂离子电池、场致电子发射器和催化剂载体的理想材料。
常见氧化锌纳米墙的制备方法很多，主要有金属有机化学气相沉积法、热蒸发法和低温水热法等。韩国的S.W.Kim等人采用金属有机化学气相沉积法，在硅衬底上制备的氧化锌纳米墙，在室温下有较高氢掺入性能；中国台湾T.P.Chen等人采用热蒸发法在玻璃衬底上制备氧化锌纳米墙，对甲烷气体具有较高灵敏度；西安交通大学张雯等人采用水热法在 ITO玻璃衬底上制备的氧化锌纳米墙，在383nm处有较强烈的紫外激发峰。金属有机化学气相沉积法成本较高，部分反应物易燃易爆或有毒性；热蒸发法工艺简单，但反应速率较低、成膜质量较差；水热法成本低不需要任何的模板或表面活性剂，但是不能精确控制反应容器内的实际温度。电化学沉积法不仅操作方便、对环境友好，而且容易在衬底上大面积均匀沉积薄膜，目前关于电化学沉积法制备氧化锌纳米墙报道文献很少。本专利利用电化学沉积法，在导电衬底上制备出尺寸均匀的氧化锌纳米墙，且可通过调节硝酸锌水溶液浓度、沉积电压及沉积时间，实现对氧化锌纳米墙形貌的有效调控。
发明内容
本发明目的是提供一种基于电化学沉积制备氧化锌纳米墙的方法。
针对上述目的，本发明采用的技术方案是：首先通过磁控溅射在导电衬底上射频沉积氧化锌籽晶层，并在大气中退火处理；其次，采用电化学沉积法，将带有氧化锌籽晶层的导电衬底为阴极、碳棒为阳极，浸入配置好的硝酸锌水溶液中，利用加热装置恒温加热，通过直流稳压电源在电极两端加上直流电压，产生金属锌离子还原反应而生长出氧化锌纳米墙；最后，沉积结束取出样品，在大气中进行退火处理，即可得到氧化锌纳米墙薄膜。
上述导电衬底的选择，可使用ITO玻璃、金电极、铜电极和铝电极。
上述氧化锌籽晶层退火处理，在大气条件下温度为300～500℃，时间为2～4h。
上述制备方法中磁控溅射氧化锌籽晶层，溅射功率为50～150W，溅射气压为0.5～5Pa，溅射时间为5～30min。
上述制备方法中沉积氧化锌纳米墙，硝酸锌水溶液配制浓度为0.01～0.5mol/L，直流电压为0.5～5V，沉积时间为3～8h，恒温加热温度为45～85℃。
上述制备方法中对生长的氧化锌纳米墙进行退火处理，在大气条件下400～750℃退火处理2～6h。
本发明的优点如下：
1、本发明采用传统的电化学沉积生长氧化锌纳米墙，在温度为45～85℃条件下即可进行，具有成本低廉、重复性高、无污染和操作简单等优点。
2、本发明利用电化学沉积法生长氧化锌纳米墙，通过调节硝酸锌水溶液浓度、沉积生长电压和时间，可实现对二维结构氧化锌纳米墙形貌的有效调控。
3、本发明所制备的氧化锌纳米墙，尺寸均匀、可大面积化，在传感器、电容器电极和场致电子发射器等领域有广泛的应用前景。
附图说明
图1是本发明中氧化锌纳米墙薄膜的扫描电子显微镜照片。
图2是本发明中氧化锌纳米墙薄膜的X射线衍射图。
图3是本发明中氧化锌纳米墙薄膜的Raman光谱图。
具体实施方式
下面结合附图和实施案例对本发明进一步详细说明，但本发明的保护范围不仅限于这些实施案例。
实施案例1
(1)通过磁控溅射、退火处理在导电衬底上制备氧化锌籽晶层。其中，磁控溅射功率为70W、溅射气压为1.0pa、溅射时间为20min；在大气中350℃退火处理2h。
(2)将带氧化锌籽晶层的ITO衬底作为阴极、碳棒作为阳极，浸入浓度为0.05mol/L的硝酸锌水溶液中，利用电化学沉积法生长氧化锌纳米墙。其中，沉积反应电压为1.8V、沉积时间为5h，恒温加热温度为60℃。
(3)电化学沉积结束后，在大气条件400℃退火处理3h，，得到样品S1。
实施案例2
(1)通过磁控溅射、退火处理在导电衬底上制备氧化锌籽晶层。其中，溅射功率为100W、溅射气压为1.0pa、溅射时间为10min；在大气中350℃退火处理2h。
(2)将沉积氧化锌籽晶层的ITO衬底作为阴极、碳棒作为阳极，浸入浓度为0.1mol/L 的硝酸锌水溶液中，利用电化学沉积法生长氧化锌纳米墙。其中，沉积反应电压为1.2V、沉积时间为4h，恒温加热温度为75℃。
(3)电化学沉积结束后，在大气条件下500℃退火处理3h，得到样品S2。
采用扫描电子显微镜、X射线衍射仪和拉曼光谱仪分别对实施案例S1、S2制备的样品进行表征分析。从图1可看出，本发明制备的氧化锌纳米墙是一种空间网络蜂窝状结构，蜂窝尺寸均匀，蜂窝片层厚度在40-60nm范围内，垂直于衬底生长。从图2可看出，在衍射角2θ为31.7°、34.4°、36.2°、47.5°和62.8°附近均出现了衍射峰，分别对应氧化锌的(100)、(002)、(101)、(102)和(103)的衍射峰，说明氧化锌为纤锌矿结构，且沿着(002)晶面择优取向生长。从图3可看出，氧化锌纳米墙在438cm-1处出现E2(H) 模的散射峰，在574cm-1处出现A1(LO)模的散射峰，进一步证实了氧化锌纳米墙为纤锌矿结构。
Claims (4)
1.一种基于电化学沉积制备氧化锌纳米墙的方法，其特征在于：首先通过磁控溅射在导电衬底上射频沉积氧化锌籽晶层，并进行退火处理，退火处理温度为300～500℃，退火时间为2～4h；其次，以带氧化锌籽晶的导电衬底为阴极、碳棒为阳极，浸入盛有硝酸锌水溶液的电解槽中，硝酸锌水溶液配制浓度为0.01～0.5mol/L，并搅拌均匀，利用加热装置恒温加热，通上直流电压在阴极产生金属锌离子还原反应而生长出氧化锌纳米墙；最后，待反应结束对样品进行退火处理，退火处理设置温度为400～750℃，退火时间为2～6h，即可得到氧化锌纳米墙，氧化锌纳米墙生长过程外加设置直流电压为0.5～5V，沉积时间为3～8h，恒温加热温度为45～85℃。
2.根据权利要求1所述的一种基于电化学沉积制备氧化锌纳米墙的方法，其特征在于：射频磁控溅射沉积氧化锌籽晶层的功率为50～150W，溅射气压为0.5～5Pa，溅射时间为5～30min；籽晶退火处理温度为300～500℃，退火时间为2～4h。
3.根据权利要求1所述的一种基于电化学沉积制备氧化锌纳米墙的方法，其特征在于：硝酸锌水溶液浓度为0.01～0.5mol/L，并搅拌均匀。
4.根据权利要求1所述的一种基于电化学沉积制备氧化锌纳米墙的方法，其特征在于：所述的导电衬底指的是氧化铟锡ITO玻璃、金电极、铜电极或铝电极。
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