CN108288546B - 镍、钴取代的锌钨杂多配合物/结晶紫有序薄膜的光电转换性能 - Google Patents
镍、钴取代的锌钨杂多配合物/结晶紫有序薄膜的光电转换性能 Download PDFInfo
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/20—Light-sensitive devices
- H01G9/2059—Light-sensitive devices comprising an organic dye as the active light absorbing material, e.g. adsorbed on an electrode or dissolved in solution
- H01G9/2063—Light-sensitive devices comprising an organic dye as the active light absorbing material, e.g. adsorbed on an electrode or dissolved in solution comprising a mixture of two or more dyes
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- Y02E10/542—Dye sensitized solar cells
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Abstract
具有光电转换性能的杂多配合物与有机染料杂化的有序薄膜材料，涉及镍、钴取代的锌钨杂多配合物与结晶紫的有序薄膜的制备方法及光电转换性质的评价。镍、钴取代的锌钨杂多配合物与结晶紫的有序薄膜由[Zn3M2W19O68]12‑(M＝Ni、Co)阴离子和结晶紫阳离子通过静电自组装得到，所制备的4层薄膜在0.1mol/L Na2SO4溶液中，外加偏压为‑0.3V(vs SCE)以及100mW/cm2的白光照射下，产生的光电流密度可分别达到8.19μA/cm2和8.69μA/cm2。所制备的薄膜在太阳能电池工作电极的开发利用方面有潜在的应用前景。
Description
技术领域
本发明涉及一种无机/有机有序薄膜，尤其涉及镍、钴取代的锌钨杂多配合物和结晶紫染料的无机/有机有序薄膜。
背景技术
随着能源危机和环境污染的日益严重，清洁无污染的可再生能源受到人们的广泛关注。太阳能因其储量丰富，可直接开发和利用，且无须开采和运输，使用方便，更加重要的是太阳能具有的清洁无污染的特性使之成为解决能源危机以及保护环境的最佳替代能源之一，越来越受到人们的重视。
1991年，O’Regan和首次报道了基于钌染料的染料敏化太阳能电池(DSSCs)，这一成果为太阳能电池研究开辟了新的领域。与传统的半导体电池相比，DSSCs具有成本更低和质量更轻等优点。DSSCs主要由载有光敏染料的工作电极、对电极和含有氧化还原电对的电解质溶液组成，其中光敏染料对电池的光电转换效率起着重要的作用，所以有关DSSCs的大多数研究致力于开发设计新型高效的光敏染料。
纯有机化合物具有制备相对简单、分子结构设计剪裁容易、成本低、且其光谱吸收易调控等优点；纯无机化合物具有光损伤阈值高、物化性能稳定、光学均匀性好、透光范围适当及易生长大晶体等优点。若将有机化合物和无机化合物进行杂化或复合于一体，可获得兼具无机和有机化合物性质的材料或产生协同作用的材料，由此可以优化材料的性能。近年来，我们将某些杂多配合物与半菁有机衍生物组装成无机-有机杂化的薄膜材料，并研究了薄膜的光电转换性能(参见①Lihua Gao，Jinfeng Zhang，Huili Wang，Xiaoyan Lin，Jianmin Qi，Kezhi Wang.Effects of elemental composition variations of Kegginpolyoxometalates on photocurrent generation of their layer-by-layer self-assembled films with a hemicyanine dye，Electrochimica Acta，2015，166，215-222.②Lihua Gao，Jingping Su，Jianing Zhang，Kezhi Wang.Enhancement of photocurrentgeneration from a series of hybrid nanocomposite self-assembled films oftransition element-substituted tungstoborates/hemicyanine，Journal ofMaterials Science，2015，50，8064-8072.③Wei Yang，Lihua Gao，Kezhi Wang，Photoelectric properties of polyoxometalate-based thin films-Recent advancesand future perspective，Polyhedron，2014，82，80-87.④高丽华，王克志，粟京平，具有光电化学活性的半菁衍生物和多金属氧酸盐自组装薄膜，中国发明专利，ZL201210029119.2.)，研究结果表明：杂化薄膜材料的光电流产生性质主要来源于有机阳离子染料，但是杂多配合物的组成和结构对有机染料的光电流产生性质有不同的影响。因此，通过探索改变薄膜中的有机阳离子染料和杂多配合物的组成和结构，可以获得具有增强光电转换性能的薄膜材料。经过大量的实验探索，我们通过简单易操作的静电自组装方法制备的结晶紫与镍、钴取代的锌钨杂多配合物的多层薄膜表现出较好的光电转换性质，并且制备的薄膜工作电极稳定性好。目前，该薄膜修饰电极材料未见报道。
发明内容
本发明的目的是制备一种具有良好光电转换性能的杂多配合物/结晶紫有序薄膜。
本发明的技术方案如下：将清洁的导电玻璃基片在氨水和过氧化氢的混合溶液中进行羟基化后，浸入到3-氨基丙基-三乙氧基硅烷的乙醇溶液中进行硅烷化，将经过硅烷化的基片浸入pH＝3的硫酸溶液中进行质子化。然后，将质子化的基片浸入到杂多配合物溶液(pH＝3)中一定时间，此时基片表面经过静电作用吸附一层杂多阴离子，取出、充分洗去物理吸附的杂多阴离子后，再将该基片浸入到结晶紫溶液中一定时间，取出、充分洗涤，吹干后制得含有一层杂多阴离子和一层结晶紫阳离子的薄膜；重复将基片依次浸入到杂多配合物和结晶紫溶液中，即可制得厚度不同的(杂多配合物/结晶紫)n(n＝1，2，3，……)有序薄膜。
本发明采用的结晶紫染料简写为JJZ，其结构式如下：
本发明采用的杂多配合物为Na12[Zn3M2W19O68](M＝Ni，简写为ZnNiW；M＝Co，简写为ZnCoW)。
本发明制备的杂多配合物/结晶紫有序薄膜是首次制备的。这种薄膜是通过杂多配合物阴离子与半菁衍生物阳离子的静电作用在导电玻璃基片上有序地组装形成的，该薄膜稳定，并且在光照下，薄膜材料具有良好的光电转化性能。
附图说明
图1是(ZnNiW/JJZ)n薄膜的紫外可见吸收光谱。
图2是(ZnCoW/JJZ)n薄膜的紫外可见吸收光谱。
图3是(ZnNiW/JJZ)n(n＝1～5)薄膜在-0.3V、100mW/cm2白光照射下的光电流响应。
图4是(ZnCoW/JJZ)n(n＝1～5)薄膜在-0.3V、100mW/cm2白光照射下的光电流响应。
具体实施方式
实施例1：(ZnNiW/JJZ)n多层有序薄膜的制备和表征
(ZnNiW/JJZ)n多层无机/有机有序薄膜的制备通过如下几步完成。
基片羟基化：导电玻璃基片浸入到1∶1∶5的氨水(25％)、过氧化氢(30％)和水的混合溶液，加热到70℃，浸泡20min，取出后用蒸馏水洗净，空气吹干。
基片硅烷化：羟基化的导电玻璃基片浸入到体积比为5％的3-氨基丙基-三乙氧基硅烷的乙醇溶液中8h，取出后用乙醇洗净，空气吹干。
基片质子化：将硅烷化的基片浸入pH＝3的硫酸溶液中30min，取出后用蒸馏水洗净，空气吹干。
将质子化的导电玻璃基片浸入1.0×10-3mol/L的ZnNiW水溶液(pH＝3)中1h，取出后用蒸馏水充分清洗，空气吹干。然后再浸入到1.0×10-3mol/L的结晶紫水溶液中1h，取出后用蒸馏水充分清洗，空气吹干。至此制备了含有一层ZnNiW阴离子和一层结晶紫阳离子的薄膜。根据需要，重复将基片浸入到ZnNiW水溶液和结晶紫水溶液中，可制得所需层数的(ZnNiW/JJZ)n多层无机/有机有序薄膜。
在美国瓦里安公司生产的CARY-50型紫外-可见分光光度计上测定每层(ZnNiW/JJZ)薄膜的紫外可见吸收光谱对薄膜的组装进行监控。实施例1制备的(ZnNiW/JJZ)n薄膜的紫外可见吸收光谱如图1所示。可见所制备的薄膜在紫外区203、246nm处的吸收是由ZnNiW和结晶紫共同吸收产生的，可见区566～604nm区域表现出结晶紫特征吸收峰，这些特征吸收峰的吸光度随着层数的增加而线性增加，表明每层薄膜ZnNiW和结晶紫都均匀沉积在基片上。
实施例2：(ZnCoW/JJZ)n多层有序薄膜的制备和表征
(ZnCoW/JJZ)n薄膜的制备步骤与测试步骤参照实施例1。其中1.0×10-3mol/L的ZnNiW水溶液替换为1.0×10-3mol/L的ZnCoW水溶液。
实施例2制备的(ZnCoW/JJZ)n薄膜的紫外可见吸收光谱如图2所示。所制备的薄膜在203、250以及566～610nm区域的特征吸收峰的吸光度随着层数的增加而线性增加，表明每层薄膜ZnCoW和结晶紫都均匀沉积在基片上。
实施例3：薄膜的光电流测试
薄膜的光电流测试实验的具体过程为：在导电玻璃基片上沉积的(ZnNiW/JJZ)n或(ZnCoW/JJZ)n薄膜作为工作电极，铂丝为对电极，饱和甘汞电极为参比电极，在室温下、0.1mol/L Na2SO4的水溶液中进行测试。光源为北京畅拓科技有限公司组装的500W超高压球形氙灯高亮度光源系统，测试时模拟太阳光100mW/cm2(730nm＞λ＞325nm)，入射光强度利用北京师范大学光学仪器厂生产的标准硅电池校正后的辐照计测定。
实施例1制备的不同层数(ZnNiW/JJZ)n薄膜在-0.3V、光强100mW/cm2的白光照射下产生的光电流响应如图3所示。实施例2制备的不同层数(ZnCoW/JJZ)n薄膜在-0.3V、光强100mW/cm2的白光照射下产生的光电流响应如图4所示。可见，当白光照射到(ZnNiW/JJZ)n薄膜和(ZnCoW/JJZ)n薄膜时，均能够快速地产生稳定的光电流，在多次的光照、无光照循环下，光电流的产生是快速的和可重复的。(ZnNiW/JJZ)n和(ZnCoW/JJZ)n薄膜产生的光电流密度随着层数从1层到4层逐渐增大，在偏压为-0.3V时光电流密度可分别达到8.19μA/cm2和8.69μA/cm2，表明此类薄膜具有良好光电转换性能。ZnNiW和ZnCoW杂多配合物对结晶紫的光电性能增强起到了协同的作用，所制备的薄膜对太阳能电池工作电极的开发利用有潜在的应用前景。
Claims (1)
1.一种杂多配合物和结晶紫的有序薄膜材料，其特征在于：该薄膜材料由杂多配合物[Zn3Ni2W19O68]12-或[Zn3Co2W19O68]12-阴离子分别与结晶紫阳离子组成，该薄膜为多层薄膜，该薄膜具有增强的光电转换性质，可用于太阳能电池工作电极。
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| CN102637827A (zh) * | 2012-02-10 | 2012-08-15 | 北京工商大学 | 具有光电化学活性的半菁衍生物和多金属氧酸盐自组装薄膜 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102637827A (zh) * | 2012-02-10 | 2012-08-15 | 北京工商大学 | 具有光电化学活性的半菁衍生物和多金属氧酸盐自组装薄膜 |
Non-Patent Citations (3)
| Title |
|---|
| "Enhancement of photocurrent generation from a series of hybrid nanocomposite self-assembled films of transition element-substituted tungstoborates/hemicyanine";Lihua Gao等;《J Mater Sci》;20150829;第50卷;第8064-8072页 * |
| "杂多配合物与碱性品红染料薄膜的制备及其光电转换性质";张佳凝等;《中国化学会第六届全国多酸化学学术研讨会论文集》;20150930;第83页 * |
| "钨锌多元杂多化合物的合成、表征和催化活性";陈玉慧;《化工时刊》;20121130;第26卷(第11期);第7页左栏第1段、第8页右栏第1段、第9页左栏第2段、第9页右栏3.2.1节 * |
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