CN108074746B - 具有增强光电转换性能的锌钨系列杂多配合物/半菁衍生物有序薄膜 - Google Patents
具有增强光电转换性能的锌钨系列杂多配合物/半菁衍生物有序薄膜 Download PDFInfo
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Abstract
具有增强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，涉及锌钨系列杂多配合物与半菁衍生物的有序薄膜的制备方法及光电转换性质的评价。锌钨系列杂多配合物与半菁衍生物的有序薄膜由[Zn5W19O68]12‑和[Zn3Cu2W19O68]12‑阴离子和H6半菁衍生物阳离子通过静电自组装制备得到，所制备的薄膜在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7.56μA/cm2和4.67μA/cm2，Zn5W19和Zn3Cu2W19杂多配合物对H6的光电转换性能表现出较强的增强作用，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，尤其涉及锌钨系列杂多配合物和一种半菁衍生物无机/有机有序薄膜。
背景技术
目前，人类所使用的绝大多数能源仍然是煤、石油和天然气等化石能源，此类能源不可再生，过度开采造成的能源危机以及使用化石能源所带来的环境污染问题已成为制约经济和社会持续、健康发展的主要因素之一，同时随着世界经济的发展和人口的急剧增加，人类对能源的需求也日益增加。因此，开发和利用清洁的新能源是解决上述问题的有效途径之一。相比于其他能源，太阳能广泛存在于自然界，其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。
染料敏化太阳能电池(DSSC)是一种新型的太阳能电池，主要由载有染料敏化剂的工作电极、电解质和对电极组成。当太阳光照射到工作电极时，染料敏化剂分子吸收光子，电子由基态激发到激发态，处于激发态的染料分子是不稳定的状态，电子会传递给光阳极并注入TiO2的导带中产生阳极光电流或电子传递给电解质中的电子接收体产生阴极光电流。可见，DSSC中染料敏化剂的性能是决定太阳能电池光电转换性能的主要因素。有机染料类光敏剂具有制备相对简单、分子结构设计剪裁容易、成本低、光谱吸收易调控等优点，使其成为染料光敏化剂的一个主要研究方向。具有D-π-A结构的半菁衍生物有机染料具有较强的可见吸收，并且结构易于裁减，作为光敏材料具有良好的光电转换性能。黄春辉等曾报道将半菁有机染料敏化剂通过LB技术制备到导电玻璃上，作为工作电极半菁有机染料敏化剂表现出较好的光电转换性质(A.D.Lang，J.Zhai，C.H.Huang，L.B.Gan，Y.L.Zhao，D.J.Zhou，Z.D.Chen.Relationship between structures and photocurrent generationproperties in a series of hemicyanine congeners，J.Phys.Chem.B 1998，102，1424-1429.)。但是，LB膜的制备需要特殊的仪器设备，并且基片的形状和尺寸受到限制。我们曾开展了将杂多配合物与半菁衍生物组装成具有光电转换活性的薄膜材料的研究工作[参见：(a)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；(b)L.H.Gao＊，Q.L.Sun，K.Z.Wang.Photoelectrochemical properties of a series of electrostaticallyself-assembled films based on sandwich-type polyoxometalates and abichromophore hemicyanine dye，Journal of Colloid and Interface Science，2013，393，92-96；(c)L.H.Gao＊，Q.L.Sun，J.M.Qi，X.Y.Lin，K.Z.Wang.Enhanced photocurrentgeneration from an electrostatically self-assembled film of sandwich-typetetracadmium(II)tungstophosphorate/hemicyanine，Electrochimica Acta，2013，92，236-242；(d)L.H.Gao*，Q.L.Sun，X.y.Lin，J.M.Qi，K.Z.Wang.Photoelectrochemicalproperties of three inorganic/organic hybrid films formed from sandwich-typetetrazinc(II)tungstophosphorate and hemicyanines with varied alkyl chainlengths，Colloids and Surfaces A：Physicochemical and Engineering Aspects，2013，423，162-169.(e)X.Chen，L.H.Gao，Z.B.Zheng，K.Z.Wang*.Photoelectrochemicalproperties of electrostatically self-assembled multilayer films formed bythree bipolar hemicyanines and H4SiW12O40，Mater.Res.Bull.，2013，48(2)，595-602.]，研究结果发现，不同组成和结构的杂多配合物对同一种半菁衍生物光敏剂的光电转换性能的影响有很大差别。例如，含6个CH2烷基链的半菁衍生物(H6)光敏剂与H4SiW12O40形成的(SiW12/H6)1薄膜工作电极产生的最大的光电流密度仅为0.36μA/cm2，(P2W18M4/H6)1(M＝Ni，Cu，Zn，Cd)系列薄膜工作电极的光电流最大可达到2.51～3.68μA/cm2，而(BW11M/H6)1(M＝Co，Ni，Cu)系列薄膜工作电极产生的光电流为3.72～5.07μA/cm2。因此，通过探索改变薄膜工作电极中的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，我们发现锌钨系列杂多配合物能够不同程度的增强半菁衍生物(H6)光敏剂的光电转换性能，目前，该薄膜修饰电极材料未见报道。另外，薄膜工作电极的制备采用了静电自组装方法，基片的形状和大小不受限制，并且不需要特殊的仪器设备，制备方法简单易操作，制备的薄膜工作电极稳定性好，具有实用价值。
发明内容
本发明的目的是制备一种具有增强光电转换性能的杂多配合物/半菁衍生物有序薄膜。
本发明的技术方案如下：首先，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，然后浸入到3-氨基丙基-三乙氧基硅烷的乙醇溶液中进行硅烷化，此时基片表面带有一层NH2基团；将经过硅烷化的基片浸入pH＝2的硫酸溶液中进行质子化使基片表面带有一层NH2 +基团。然后，将质子化的基片浸入到杂多配合物的酸性溶液一定时间，此时基片表面带有一层杂多阴离子，再将该基片浸入到半菁衍生物溶液中一定时间，此后重复将基片依次浸入到杂多配合物和半菁衍生物溶液中，即可制得厚度不同的(杂多配合物/半菁衍生物)n(n＝1，2，3，……)有序薄膜。
本发明采用的半菁衍生物为溴化(E)-1，1′-(1，6-己基)双(4-(4-(甲氨基)苯乙烯基)吡啶)，简写为H6，其结构式如下：
本发明采用的杂多配合物为Na12[Zn5W19O68]·46H2O(简写为Zn5W19)和Na12[Zn3Cu2W19O68]·48H2O(简写为Zn3Cu2W19)。
本发明制备的杂多配合物/半菁衍生物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而有序地组装在导电玻璃基片上，由于杂多配合物阴离子Zn5W19和Zn3Cu2W19的影响，有效地抑制了半菁衍生物中光生电子和空穴的复合，增强了半菁衍生物的光电转化性能。
附图说明
图1是(Zn5W19/H6)n薄膜的紫外可见吸收光谱。
图2是(Zn3Cu2W19/H6)n薄膜的紫外可见吸收光谱。
图3是(Zn5W19/H6)1薄膜在不同偏压、100mW/cm2白光照射下的光电流响应。
图4是(Zn3Cu2W19/H6)1薄膜在不同偏压、100mW/cm2白光照射下的光电流响应。
具体实施方式
实施例1：(Zn5W19/H6)n多层无机/有机有序薄膜的制备和表征
(Zn5W19/H6)n多层无机/有机有序薄膜的制备通过如下几步完成。
(1)配制体积比为1∶1∶5的氨水(25％)、过氧化氢(30％)和水的混合溶液，加热到70℃；然后将导电玻璃基片浸入到上述混合液中20min，取出后用蒸馏水洗净，空气吹干。
(2)将经过第(1)步处理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8小时，取出后用乙醇洗净，空气吹干。再将此基片浸入pH＝2的硫酸溶液中30min，取出后用蒸馏水洗净，空气吹干。
(3)将经过第(2)步处理的导电玻璃基片浸入1.0×10-3M的Zn5W19水溶液中1小时，取出后用蒸馏水洗净，空气吹干。
(4)将经过第(3)步处理的导电玻璃基片浸入1.0×10-3M的H6水溶液中1小时，取出后用蒸馏水洗净，空气吹干。至此制备了含有一层Zn5W19阴离子和一层H6阳离子的薄膜。
(5)根据需要，重复循环第(3)步和第(4)步，可制得所需层数的(Zn5W19/H6)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(Zn5W19/H6)n薄膜的紫外可见吸收光谱进行监控薄膜的组装。实施例1制备的(Zn5W19/H6)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268nm和488nm处Zn5W19和H6的特征吸收峰的吸光度随着层数的增加而线性的增大，说明每层薄膜Zn5W19和H6都均匀沉积在基片上。
实施例2：(Zn3Cu2W19/H6)n多层无机/有机有序薄膜的制备和表征
(Zn3Cu2W19/H6)n薄膜的制备步骤与测试步骤参照实施例1。其中第(3)步中基片浸入的溶液采用1.0×10-3M的Zn3Cu2W19水溶液。
实施例2制备的(Zn3Cu2W19/H6)n薄膜的紫外可见吸收光谱如图2所示。所制备的薄膜在270nm和470nm处Zn3Cu2W19和H6的特征吸收峰的吸光度随着层数的增加而线性的增大，说明每层薄膜Zn3Cu2W19和H6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(Zn5W19/H6)n或(Zn3Cu2W19/H6)n薄膜作为工作电极(其有效光照面积为0.28cm2)，铂丝为对电极，饱和甘汞电极为参比电极，在室温下、0.1M 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(Zn5W19/H6)1薄膜在不同偏压、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(Zn3Cu2W19/H6)1薄膜在不同偏压、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(Zn5W19/H6)1薄膜和(Zn3Cu2W19/H6)1薄膜上时，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。(Zn5W19/H6)1和(Zn3Cu2W19/H6)1薄膜产生的光电流密度随着负偏压的增加逐渐增大，在偏压为-0.3V时光电流密度分别达到7.56μA/cm2和4.67μA/cm2，表明此类薄膜具有良好光电转换性能。Zn5W19和Zn3Cu2W19杂多配合物对H6的光电转换性能表现出较强的增强作用，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 (2)
1.一种杂多配合物和半菁衍生物的有序薄膜材料，其特征在于：该薄膜材料由杂多配合物[Zn5W19O68]12-阴离子与半菁衍生物(E)-1，1′-(1，6-己基)双(4-(4-(甲氨基)苯乙烯基)吡啶)阳离子组成，该薄膜为(Zn5W19/H6)n薄膜，该薄膜具有增强的光电转换性质，用于太阳能电池工作电极。
2.一种杂多配合物和半菁衍生物的有序薄膜材料，其特征在于：该薄膜材料由杂多配合物[Zn3Cu2W19O68]12-阴离子与半菁衍生物(E)-1，1′-(1，6-己基)双(4-(4-(甲氨基)苯乙烯基)吡啶)阳离子组成，该薄膜为(Zn3Cu2W19/H6)n薄膜，该薄膜具有增强的光电转换性质，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 |
| CN104900410A (zh) * | 2014-12-18 | 2015-09-09 | 北京工商大学 | 磷钨钛杂多配合物与半菁染料杂化的光电转换薄膜及其传感性质 |
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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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