ZnO-TiO_2核壳结构的性能研究及其染料敏化太阳能电池应用
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摘要
染料敏化太阳能电池是一种新型的第三代太阳能电池,目前其光电转换效率已经达到12.3%。光生载流子的复合问题制约着转换效率的进一步提高。作为负载染料和传递光生电子的光阳极在染料敏化太阳能电池中扮演者重要的作用。近年来,利用ZnO和TiO2独特的物理化学性质,对光阳极结构设计提供了新的思路。本论文提出利用ZnO表面缺陷作为TiO2的形核中心,使其外延生长得到具有枝状TiO2结构的核壳复合结构光阳极,基于缺陷生长的壳层材料,可以在消除缺陷的同时,有利于电子通过TiO2传递到ZnO。通过元素掺杂进一步调整ZnO/TiO2的能带体系,减小界面转移阻抗并钝化表面缺陷,促进光生载流子的注入与传输。具体研究内容为：
(1)通过溶胶凝胶法和磁控溅射法制备ZnO晶种层薄膜,作为减少ZnO纳米阵列晶格失配的基底,比较两种方法制备的薄膜微观形貌和结构的差异。优化溅射沉积的相关工艺参数,考察溅射功率、气体分压比和靶间距对ZnO晶种层晶粒的影响。通过正交实验法研究Al元素掺杂的ZnO纳米阵列的制备工艺,考察Al元素掺杂对ZnO晶种层薄膜导电性的影响。
(2)通过化学水浴沉积工艺,在晶种层上合成ZnO和Al元素掺杂ZnO纳米阵列。改变生长液中的Zn源浓度、温度、时间和Al元素掺杂量,得到不同形貌的ZnO/Al:ZnO纳米阵列。探索制备垂直于底面有序生长ZnO纳米阵列和Al元素掺杂ZnO纳米阵列的最佳工艺参数,同时研究纳米阵列的形成机理。通过改进的连续水浴沉积工艺,优化纳米阵列的生长条件,促进ZnO纳米阵列的形核与生长。
(3)通过磁控溅射工艺,在ZnO纳米棒阵列的表面沉积具有枝状分级结构的连续TiO2壳层,研究气体分压比、热处理温度和其他工艺因素对微观形貌和结构的影响。探索ZnO-TiO2核壳结构的形成机理。
(4)基于上述各种纳米结构的光阳极,组装染料敏化太阳能电池。研究不同结构器件的光电转换效率,开路电压,短路电流和填充因子等相关性能参数。通过电化学阻抗技术研究核壳界面处的光生载流子传输性能。讨论核壳结构对抑制光生载流子复合的作用机理。
通过对ZnO-TiO2核壳结构的研究得到如下结果：
(1)溶胶凝胶法制备的ZnO晶种层随着热处理温度的增加,晶粒的结晶取向性显著增强。条纹状弯曲畴晶的形成与高度取向的纳米晶表面能降低有关。磁控溅射法制备的ZnO晶种层,晶粒尺寸受到靶间距、溅射功率、氧氩比的影响。通过优化溅射工艺确定最佳参数为靶间距50mm、溅射功率100W、氧氩比1：3。当退火热处理温度为400℃时,晶种层内应力最小。通过正交实验法确定A1元素掺杂ZnO晶种层的最佳参数为溅射温度200℃,溅射功率40W,氧流量20%,退火温度400℃。此条件下制备的Al：ZnO晶种层电学性能最好,少量A1元素掺杂可以提高光致发光强度。
(2)ZnO纳米棒阵列受化学水浴沉积工艺中基底和生长液浓度等因素的影响。ZnO纳米棒对应纤锌矿结构,具有择优取向。热处理温度和时间的增加,促进了纳米棒垂直于基底均匀生长。生长液浓度增加,纳米棒直径增大,间隙减小。连续CBD法能够稳定生长液反应过程中的溶质浓度,有利于其定向有序生长。基于连续CBD法的DSSC组件转换效率达到0.31%。A1元素掺杂ZnO纳米阵列,当掺杂量为2%时具有最好的电学性能和发光性能。生长液浓度为O.01mol/L时制备的5%掺杂A1元素ZnO纳米阵列的DSSC组件效率达到0.42%。
(3)直流反应磁控溅射制备的ZnO-TiO2核壳结构,当氧氩比为1：1时,纳米棒表面由一层粗糙晶粒组成的Ti02所包覆。当氧氩比为1：3时,Ti02在ZnO纳米棒的侧表面形核生长,受到气-固生长模式的影响最终形成枝状生长的金红石Ti02结构。基于ZnO-TiO2核壳结构光阳极的染料敏化电池,能够有效地促进载流子传输和抑制表面复合,效率达到0.94%。基于不同染料吸附量的光阳极结构DSSC组件,经过包覆的光阳极能够作为阻挡层钝化表面缺陷,抑制复合的发生,从而提高开路电压和填充因子,其光电转换效率相对于纯ZnO纳米阵列提高了132%。电化学阻抗谱证明包覆Ti02的纳米阵列能够有效地促进电子注入与传输,同时抑制电子的反向传输,防止复合现象的发生,最终提高DSSC组件的光电转换效率
Dye sensitized solar cells is a noval third generation solar cells. Its current maxium conversion efficiency has achieved12.3%. The recombinations of photo induced electron restrict the improvement of conversion efficiency. Photoanode plays a key role in DSSC as dye loader and electron transfer and transmission. Recently, research group use unique physics and chemical properties of ZnO and TiO2, developed new route for photoanode design. This paper introduced take advantage of surface defects of ZnO as nucleation centre, and epitaxial growth branched structure TiO2core-shell photoanode. The shell could growth from defects, and good for electron transfer from TiO2to ZnO. Element doping could adjust the energy band of ZnO/TiO2prompt electron transfer and transmission, passivating interface defects. The research content as follow:
(1) Prepare ZnO seed layer with sol-gel method and magnetron sputtering, as substrate to overcome lattice mismatch. Compare the microstructure of different methods. Optimize magnetron sputtering parameter, about deposition power, O2/Ar ratio and spacing adjustment of ZnO seed layer. Investigate the properties of Al doping ZnO seed layer with orthogonal experimental design.
(2) Prepare ZnO and Al:ZnO nano array on seed layer by chemical bath deposition. Adjust Zinc concentration of solution, temperature, duration and Al doping content. Explore the optimized parameter and nano array growth mechanism. With continuous chemical bath deposition method, optimize the nano array, prompt the nucleation and growth of ZnO nanorod.
(3) Branched continuous TiO2shell structure were obtain from magnetron sputtering. Investigate O2/Ar ratio, heat treatment temperature, and microstructure. Discuss the shell formation mechanism.
(4) Prepare DSSC module with different photoanode. Study the conversion efficiency, open circuit voltage, short circuit current, and fill factor. Investigate interface transfer and transmission of photo induced electron with electrochemical impediance spectrum. Discuss the mechanism of core-shell structure for inhibition recombination.
The results have achieved from experiment and analysis as follow:
(1) The ZnO seed layer prepared by sol-gel mothod has strong crystal orientation with increasement of heat treatment temperature. The formation of stipe grain has strong correlation with the decrease of surface energy of nanocrystalline. The optimized parameter of ZnO seed layer prepared by magnetron sputtering is spacing50mm, sputtering power100W, O2/Ar ratio1:3. The internal stress of seed layer reached minimum when temperature is400℃. The optimized parameter of Al:ZnO seed layer is200℃,40W, oxygen flux20%, and treatment temperature is400℃. Under these condition, Al:ZnO layer has best conductivity and photoluminescence.
(2) Preferred orientation ZnO nano array with wurtzite structure was affect by substrate and concentration. The increasement of temperature and duration could prompt growth of ZnO nanorod perpendicular substrate. The diameter of nanorod increased with concentration elevated. Continuous chemical bath deposition could maintain concentration in solution, to the benefit of directional growth of nanorod. The conversion efficiency of DSSC modules based c-CBD method reached0.31%. Doping conten2%of Al:ZnO have optimized electrical properties and photoluminescence. When concentration is0.01mol/L, the module of5%Al doping ZnO nanoarray has reached0.42%.
(3) ZnO-TiO2core-shell structure prepared by magnetron sputtering with different O2/Ar ratio varied from1:1to1:3. The formation of shell was affected by gas-solid growth pattern, and finally achieved TiO2shell with rutile structure. Core-shell strucre could effectively prompt electron transmission and inhibite recombination. The conversion efficiency reached0.94%. Core-shell structure with different dye load content has132%efficiency compared with ZnO nano array. Chemical impediance spectrum reveals TiO2shell could effectively accelerate electron transter and transmission, inhibite reverse transmission and recombination.
(1)通过溶胶凝胶法和磁控溅射法制备ZnO晶种层薄膜,作为减少ZnO纳米阵列晶格失配的基底,比较两种方法制备的薄膜微观形貌和结构的差异。优化溅射沉积的相关工艺参数,考察溅射功率、气体分压比和靶间距对ZnO晶种层晶粒的影响。通过正交实验法研究Al元素掺杂的ZnO纳米阵列的制备工艺,考察Al元素掺杂对ZnO晶种层薄膜导电性的影响。
(2)通过化学水浴沉积工艺,在晶种层上合成ZnO和Al元素掺杂ZnO纳米阵列。改变生长液中的Zn源浓度、温度、时间和Al元素掺杂量,得到不同形貌的ZnO/Al:ZnO纳米阵列。探索制备垂直于底面有序生长ZnO纳米阵列和Al元素掺杂ZnO纳米阵列的最佳工艺参数,同时研究纳米阵列的形成机理。通过改进的连续水浴沉积工艺,优化纳米阵列的生长条件,促进ZnO纳米阵列的形核与生长。
(3)通过磁控溅射工艺,在ZnO纳米棒阵列的表面沉积具有枝状分级结构的连续TiO2壳层,研究气体分压比、热处理温度和其他工艺因素对微观形貌和结构的影响。探索ZnO-TiO2核壳结构的形成机理。
(4)基于上述各种纳米结构的光阳极,组装染料敏化太阳能电池。研究不同结构器件的光电转换效率,开路电压,短路电流和填充因子等相关性能参数。通过电化学阻抗技术研究核壳界面处的光生载流子传输性能。讨论核壳结构对抑制光生载流子复合的作用机理。
通过对ZnO-TiO2核壳结构的研究得到如下结果：
(1)溶胶凝胶法制备的ZnO晶种层随着热处理温度的增加,晶粒的结晶取向性显著增强。条纹状弯曲畴晶的形成与高度取向的纳米晶表面能降低有关。磁控溅射法制备的ZnO晶种层,晶粒尺寸受到靶间距、溅射功率、氧氩比的影响。通过优化溅射工艺确定最佳参数为靶间距50mm、溅射功率100W、氧氩比1：3。当退火热处理温度为400℃时,晶种层内应力最小。通过正交实验法确定A1元素掺杂ZnO晶种层的最佳参数为溅射温度200℃,溅射功率40W,氧流量20%,退火温度400℃。此条件下制备的Al：ZnO晶种层电学性能最好,少量A1元素掺杂可以提高光致发光强度。
(2)ZnO纳米棒阵列受化学水浴沉积工艺中基底和生长液浓度等因素的影响。ZnO纳米棒对应纤锌矿结构,具有择优取向。热处理温度和时间的增加,促进了纳米棒垂直于基底均匀生长。生长液浓度增加,纳米棒直径增大,间隙减小。连续CBD法能够稳定生长液反应过程中的溶质浓度,有利于其定向有序生长。基于连续CBD法的DSSC组件转换效率达到0.31%。A1元素掺杂ZnO纳米阵列,当掺杂量为2%时具有最好的电学性能和发光性能。生长液浓度为O.01mol/L时制备的5%掺杂A1元素ZnO纳米阵列的DSSC组件效率达到0.42%。
(3)直流反应磁控溅射制备的ZnO-TiO2核壳结构,当氧氩比为1：1时,纳米棒表面由一层粗糙晶粒组成的Ti02所包覆。当氧氩比为1：3时,Ti02在ZnO纳米棒的侧表面形核生长,受到气-固生长模式的影响最终形成枝状生长的金红石Ti02结构。基于ZnO-TiO2核壳结构光阳极的染料敏化电池,能够有效地促进载流子传输和抑制表面复合,效率达到0.94%。基于不同染料吸附量的光阳极结构DSSC组件,经过包覆的光阳极能够作为阻挡层钝化表面缺陷,抑制复合的发生,从而提高开路电压和填充因子,其光电转换效率相对于纯ZnO纳米阵列提高了132%。电化学阻抗谱证明包覆Ti02的纳米阵列能够有效地促进电子注入与传输,同时抑制电子的反向传输,防止复合现象的发生,最终提高DSSC组件的光电转换效率
Dye sensitized solar cells is a noval third generation solar cells. Its current maxium conversion efficiency has achieved12.3%. The recombinations of photo induced electron restrict the improvement of conversion efficiency. Photoanode plays a key role in DSSC as dye loader and electron transfer and transmission. Recently, research group use unique physics and chemical properties of ZnO and TiO2, developed new route for photoanode design. This paper introduced take advantage of surface defects of ZnO as nucleation centre, and epitaxial growth branched structure TiO2core-shell photoanode. The shell could growth from defects, and good for electron transfer from TiO2to ZnO. Element doping could adjust the energy band of ZnO/TiO2prompt electron transfer and transmission, passivating interface defects. The research content as follow:
(1) Prepare ZnO seed layer with sol-gel method and magnetron sputtering, as substrate to overcome lattice mismatch. Compare the microstructure of different methods. Optimize magnetron sputtering parameter, about deposition power, O2/Ar ratio and spacing adjustment of ZnO seed layer. Investigate the properties of Al doping ZnO seed layer with orthogonal experimental design.
(2) Prepare ZnO and Al:ZnO nano array on seed layer by chemical bath deposition. Adjust Zinc concentration of solution, temperature, duration and Al doping content. Explore the optimized parameter and nano array growth mechanism. With continuous chemical bath deposition method, optimize the nano array, prompt the nucleation and growth of ZnO nanorod.
(3) Branched continuous TiO2shell structure were obtain from magnetron sputtering. Investigate O2/Ar ratio, heat treatment temperature, and microstructure. Discuss the shell formation mechanism.
(4) Prepare DSSC module with different photoanode. Study the conversion efficiency, open circuit voltage, short circuit current, and fill factor. Investigate interface transfer and transmission of photo induced electron with electrochemical impediance spectrum. Discuss the mechanism of core-shell structure for inhibition recombination.
The results have achieved from experiment and analysis as follow:
(1) The ZnO seed layer prepared by sol-gel mothod has strong crystal orientation with increasement of heat treatment temperature. The formation of stipe grain has strong correlation with the decrease of surface energy of nanocrystalline. The optimized parameter of ZnO seed layer prepared by magnetron sputtering is spacing50mm, sputtering power100W, O2/Ar ratio1:3. The internal stress of seed layer reached minimum when temperature is400℃. The optimized parameter of Al:ZnO seed layer is200℃,40W, oxygen flux20%, and treatment temperature is400℃. Under these condition, Al:ZnO layer has best conductivity and photoluminescence.
(2) Preferred orientation ZnO nano array with wurtzite structure was affect by substrate and concentration. The increasement of temperature and duration could prompt growth of ZnO nanorod perpendicular substrate. The diameter of nanorod increased with concentration elevated. Continuous chemical bath deposition could maintain concentration in solution, to the benefit of directional growth of nanorod. The conversion efficiency of DSSC modules based c-CBD method reached0.31%. Doping conten2%of Al:ZnO have optimized electrical properties and photoluminescence. When concentration is0.01mol/L, the module of5%Al doping ZnO nanoarray has reached0.42%.
(3) ZnO-TiO2core-shell structure prepared by magnetron sputtering with different O2/Ar ratio varied from1:1to1:3. The formation of shell was affected by gas-solid growth pattern, and finally achieved TiO2shell with rutile structure. Core-shell strucre could effectively prompt electron transmission and inhibite recombination. The conversion efficiency reached0.94%. Core-shell structure with different dye load content has132%efficiency compared with ZnO nano array. Chemical impediance spectrum reveals TiO2shell could effectively accelerate electron transter and transmission, inhibite reverse transmission and recombination.
引文
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