FTO透明导电薄膜表面处理及其复合膜的研究
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摘要
透明导电氧化物(TCO)薄膜具有良好的导电性、优异的透明度等光电特性,已在光伏电池组件、平面显示器、触控面板、发光二极管(LEDs)、气敏传感器等不同领域获得了广泛应用。值得注意的是,TCO薄膜的透明度和导电性往往是矛盾和相互抑制的。而在应用于许多光电器件尤其是太阳能电池时,良好的综合光电性能是迫切需要的。为了满足高透明度和低方阻的应用需求,人们对TCO薄膜的研究除了集中于制备方法上外,还包括对制备好的TCO膜进行后续处理(如表面微纳米结构复合、热退火、激光退火)和双层/多层复合优化。
在TCO薄膜中,掺氟二氧化锡(FTO)薄膜成本相对较低(不含昂贵的铟元素),且热稳定性和化学稳定性好,近些年也得到了广泛的研究和应用。但是与掺锡氧化铟(ITO)薄膜相比,FTO薄膜的导电性略差,且相关工艺及后续处理研究不够深入,性能优化途径方面还有拓展空间,这些都需要材料学界的研究者进一步研究辨识和探讨。基于此,本文以FTO透明导电膜为对象,开展了表面金属微纳米粒子复合、热退火处理、表面激光处理、双层复合优化与后续处理等方面的研究,获得了一些有意义的结果。
1、采用直流磁控溅射法和管式炉内热退火处理的方法在FTO膜表面复合Ag粒子结构,对比了不同基片材料表面Ag粒子形成的条件,重点讨论了退火温度、退火时间和原始Ag膜厚度对FTO膜表面Ag粒子的形成和形貌以及薄膜光电性能的影响。结果表明,与单晶硅和载玻片基片相比,FTO膜表面开始形成Ag粒子所需的退火温度更低,退火时间更短。实验中选用原始Ag膜厚度为200nm、退火温度为500℃左右、退火时间为20～30min时可在FTO膜表面获得形态相对良好的Ag粒子,此时在薄膜透射率曲线上出现对应于Ag粒子表面等离子体共振吸收的透射峰。
2、采用管式炉中热退火的方法对FTO薄膜进行了退火处理,研究了不同的气氛条件、退火温度和退火时间等对薄膜结构、表面形貌及光电性能的影响,深入分析了造成这些影响的机理,并通过计算性能指数对各薄膜样品的综合光电性能进行了评价。结果表明,在氮气、空气和氧气中退火时,薄膜结晶性均得到一定的改善,但在氮气中退火后薄膜的综合光电性能最好。在氮气中退火时,退火时间对FTO膜透光率和方块电阻的影响不如退火温度的影响显著,且500℃下退火20min后FTO膜的综合光电性能最好,性能指数为5.56×10-3Ω-1。
3、采用波长为532nm的纳秒脉冲激光对FTO膜表面进行辐照处理,研究了激光能量密度和扫描速度对薄膜表面形貌、透光率和导电性的影响。结果表明,激光能量密度和扫描速度适中可使FTO膜表面获得较好的退火效果,在激光作用区域内的晶粒通过再结晶过程长大,使得其透光率提高,而方块电阻却减小。实验中获得的最佳激光参数为能量密度F=1.02J/cm2和扫描速度v=10mm/s,此时FTO膜在380～780nm波段的平均透光率由原来的75.4%提高到了82.7%,方块电阻由原来的10.20Ω/口降低到了8.83Ω/口。
4、采用直流磁控溅射法在FTO膜上镀制掺铝氧化锌(AZO)膜制备出AZO/FTO双层复合膜,研究了AZO膜层厚度对AZO/FTO双层复合膜结构和微观形貌以及光电性能的影响,初步探讨了其影响机理。结果显示,随着AZO膜层厚度的增大,AZO/FTO膜的表面粗糙度逐渐降低,方块电阻先减小后变化趋于平缓,透光率则先增大后减小。实验中,AZO膜层厚度为495nm的AZO/FTO双层复合膜具有最佳的光电性能,性能指数达到1.43×10Ω-1。
5、对优化制备的AZO/FTO双层复合膜进行后续热退火处理和激光表面辐照处理,进一步实现了薄膜性能优化,研究了不同参数下AZO/FTO膜形貌和光电性能的变化。结果显示,热退火可提高薄膜的致密度和平整度,薄膜的透光率随着退火温度升高或退火时间延长而小幅度提高,而方块电阻在温度达到300℃前已有较大程度的下降,其后温度的升高及500℃下退火时间的延长对AZO/FTO膜的方块电阻的影响并不显著；激光辐照处理也可对AZO/FTO膜起到一定退火作用,采用1.02J/cm2的能量密度和10mm/s的扫描速度处理时可达到最佳效果。
Transparent conductive oxide (TCO) films have multiple properties including an excellent optical transparency and a good electrical conductivity, which enable TCO films to have been widely used in various applications, such as photovoltaic modules, flat panel displays, touch panels, light-emitting diodes (LEDs) and gas sensors. It must be noted that the optical transparency and the electrical conductivity of TCO films are contradictory and restrain each other. However, as for applications of them in photoelectric devices especially in solar cells, a good photoelectric performance is absolutely required. In order to meet the application requirements of high transparency and low sheet resistance, many researches about TCO films have been focused on preparation methods of them, even the post-treatment processes (such as micro/nano structure combination on surface, thermal annealing and laser annealing) and double-layer/multilayer composite optimization.
Among the TCO films, the fluorine-doped tin oxide (FTO) film has virtues of relatively low cost (containing no expensive indium element), good thermal stability and high chemical stability, so it has been studied and applied abroad in recent years. But compared with tin-doped indium oxide (ITO) film, FTO film has disadvantages of slightly low conductivity, insufficient research in related processes (including post-treatment processes) and expanded methods for performance optimization, which are all need to be further identified and studied by researchers in the filed of materials science. Based on these, some studies about FTO films, such as metal particles combination, thermal annealing, laser treatment, double-layer composite optimization and post treatment, are carried out. Also some significative results are obtained.
1. Silver (Ag) particles are prepared on FTO film substrates by direct current magnetron sputtering and thermal annealing treatment. The conductions for formation of Ag particles on different substrates are comparatively studied. The effects of annealing temperature, annealing time and thickness of initial Ag film on formation and morphology of Ag particles, as well as photoelectric properties of FTO films, are mainly discussed. The results indicate that lower annealing temperature and shorter annealing time are needed to form Ag particles on a FTO film substrate compared with a silicon substrate or a glass substrate. Some good-shaped Ag particles are formed on FTO film substrates when Ag films are annealed at500℃for20-30min with an initial Ag-film thickness of200nm in this experiment. The transmission spectra of the films show resonance peaks of Ag particles surface plasmon.
2. Some FTO films are thermal annealed in tubular furnace. The effects of annealing atmosphere, annealing temperature and time on structure, surface morphology and photoelectric properties of the FTO films are studied, and the mechanisms of these effects are deeply analyzed. Also the integrated photoelectric properties of all the FTO films are appraised by calculating figure of merit. The results indicate that the crystallinity of the FTO films are improved when annealed in nitrogen, air or oxygen, and the integrated photoelectric properties of the FTO films annealed in nitrogen are best. When annealing in nitrogen, the effects of annealing time on transmittance and sheet resistance of the FTO films are not as dramatical as those of annealing temperature, and the best integrated photoelectric property with a figure of merit of5.56×10-3Ω-1is achieved by annealing at500℃for20min.
3. The surfaces of FTO films are irradiated by a nanosecond pulsed laser with a wavelength of532nm. The effects of laser fluence and scan speed on morphologies and photoelectric properties of the films were discussed. The results indicate that the film irradiated by laser with moderate laser fluence and scan speed achieved better laser annealing effects. The crystalline grains in laser irradiate zone grow up through a recrystallization process, which results in improvement of transmittance and decrease of sheet resistance. The laser fluence of1.02J/cm2and the scan speed of10mm/s are the optimal laser parameters in this experiment, with the average optical transmittance of the film in the waveband of380-780nm increased from75.4%to82.7%and the sheet resistance of the film decreased from10.20Ω/□to8.83Ω/□.
4. By depositing aluminum-doped zinc oxide (AZO) films on FTO films using direct current magnetron sputtering, some AZO/FTO composite films are prepared. The effects of AZO-layer thickness on structure, micro-morphology and photoelectric property of the AZO/FTO films are investigated, and the mechanisms of these effects are preliminary discussed. The results show that the surface roughnesses of AZO/FTO films gradually reduce when the AZO-layer thickness increases, with the sheet resistances of the films decrease firstly and then change gently, as well as the transmittances of them increase firstly and then decrease. It is found in this experiment that the AZO/FTO film with an AZO-layer thickness of495nm has the best photoelectric property with a figure of merit of1.43x10-2Ω-1.
5. The optimally prepared AZO/FTO films are post-treated by both thermal annealing and laser irradiation to further improve their properties. The variations in surface morphologies and photoelectric properties of the films treated with different parameters are studies. The results show that the compactnesses and planenesses of the films treated by thermal annealing are enhanced, and the transmittances of them keep on slightly improving with increases in annealing temperature or annealing time. While the sheet resistances of them decrease greatly before the annealing temperature is up to300℃, and then are almost not affected with the increases in annealing temperature or annealing time at500℃. Laser irradiation can also achieve a certain annealing effects on AZO/FTO films, and the optimal effect is obtained by treating them with a laser fluence of1.02J/cm2and a scan speed of10mm/s.
在TCO薄膜中,掺氟二氧化锡(FTO)薄膜成本相对较低(不含昂贵的铟元素),且热稳定性和化学稳定性好,近些年也得到了广泛的研究和应用。但是与掺锡氧化铟(ITO)薄膜相比,FTO薄膜的导电性略差,且相关工艺及后续处理研究不够深入,性能优化途径方面还有拓展空间,这些都需要材料学界的研究者进一步研究辨识和探讨。基于此,本文以FTO透明导电膜为对象,开展了表面金属微纳米粒子复合、热退火处理、表面激光处理、双层复合优化与后续处理等方面的研究,获得了一些有意义的结果。
1、采用直流磁控溅射法和管式炉内热退火处理的方法在FTO膜表面复合Ag粒子结构,对比了不同基片材料表面Ag粒子形成的条件,重点讨论了退火温度、退火时间和原始Ag膜厚度对FTO膜表面Ag粒子的形成和形貌以及薄膜光电性能的影响。结果表明,与单晶硅和载玻片基片相比,FTO膜表面开始形成Ag粒子所需的退火温度更低,退火时间更短。实验中选用原始Ag膜厚度为200nm、退火温度为500℃左右、退火时间为20～30min时可在FTO膜表面获得形态相对良好的Ag粒子,此时在薄膜透射率曲线上出现对应于Ag粒子表面等离子体共振吸收的透射峰。
2、采用管式炉中热退火的方法对FTO薄膜进行了退火处理,研究了不同的气氛条件、退火温度和退火时间等对薄膜结构、表面形貌及光电性能的影响,深入分析了造成这些影响的机理,并通过计算性能指数对各薄膜样品的综合光电性能进行了评价。结果表明,在氮气、空气和氧气中退火时,薄膜结晶性均得到一定的改善,但在氮气中退火后薄膜的综合光电性能最好。在氮气中退火时,退火时间对FTO膜透光率和方块电阻的影响不如退火温度的影响显著,且500℃下退火20min后FTO膜的综合光电性能最好,性能指数为5.56×10-3Ω-1。
3、采用波长为532nm的纳秒脉冲激光对FTO膜表面进行辐照处理,研究了激光能量密度和扫描速度对薄膜表面形貌、透光率和导电性的影响。结果表明,激光能量密度和扫描速度适中可使FTO膜表面获得较好的退火效果,在激光作用区域内的晶粒通过再结晶过程长大,使得其透光率提高,而方块电阻却减小。实验中获得的最佳激光参数为能量密度F=1.02J/cm2和扫描速度v=10mm/s,此时FTO膜在380～780nm波段的平均透光率由原来的75.4%提高到了82.7%,方块电阻由原来的10.20Ω/口降低到了8.83Ω/口。
4、采用直流磁控溅射法在FTO膜上镀制掺铝氧化锌(AZO)膜制备出AZO/FTO双层复合膜,研究了AZO膜层厚度对AZO/FTO双层复合膜结构和微观形貌以及光电性能的影响,初步探讨了其影响机理。结果显示,随着AZO膜层厚度的增大,AZO/FTO膜的表面粗糙度逐渐降低,方块电阻先减小后变化趋于平缓,透光率则先增大后减小。实验中,AZO膜层厚度为495nm的AZO/FTO双层复合膜具有最佳的光电性能,性能指数达到1.43×10Ω-1。
5、对优化制备的AZO/FTO双层复合膜进行后续热退火处理和激光表面辐照处理,进一步实现了薄膜性能优化,研究了不同参数下AZO/FTO膜形貌和光电性能的变化。结果显示,热退火可提高薄膜的致密度和平整度,薄膜的透光率随着退火温度升高或退火时间延长而小幅度提高,而方块电阻在温度达到300℃前已有较大程度的下降,其后温度的升高及500℃下退火时间的延长对AZO/FTO膜的方块电阻的影响并不显著；激光辐照处理也可对AZO/FTO膜起到一定退火作用,采用1.02J/cm2的能量密度和10mm/s的扫描速度处理时可达到最佳效果。
Transparent conductive oxide (TCO) films have multiple properties including an excellent optical transparency and a good electrical conductivity, which enable TCO films to have been widely used in various applications, such as photovoltaic modules, flat panel displays, touch panels, light-emitting diodes (LEDs) and gas sensors. It must be noted that the optical transparency and the electrical conductivity of TCO films are contradictory and restrain each other. However, as for applications of them in photoelectric devices especially in solar cells, a good photoelectric performance is absolutely required. In order to meet the application requirements of high transparency and low sheet resistance, many researches about TCO films have been focused on preparation methods of them, even the post-treatment processes (such as micro/nano structure combination on surface, thermal annealing and laser annealing) and double-layer/multilayer composite optimization.
Among the TCO films, the fluorine-doped tin oxide (FTO) film has virtues of relatively low cost (containing no expensive indium element), good thermal stability and high chemical stability, so it has been studied and applied abroad in recent years. But compared with tin-doped indium oxide (ITO) film, FTO film has disadvantages of slightly low conductivity, insufficient research in related processes (including post-treatment processes) and expanded methods for performance optimization, which are all need to be further identified and studied by researchers in the filed of materials science. Based on these, some studies about FTO films, such as metal particles combination, thermal annealing, laser treatment, double-layer composite optimization and post treatment, are carried out. Also some significative results are obtained.
1. Silver (Ag) particles are prepared on FTO film substrates by direct current magnetron sputtering and thermal annealing treatment. The conductions for formation of Ag particles on different substrates are comparatively studied. The effects of annealing temperature, annealing time and thickness of initial Ag film on formation and morphology of Ag particles, as well as photoelectric properties of FTO films, are mainly discussed. The results indicate that lower annealing temperature and shorter annealing time are needed to form Ag particles on a FTO film substrate compared with a silicon substrate or a glass substrate. Some good-shaped Ag particles are formed on FTO film substrates when Ag films are annealed at500℃for20-30min with an initial Ag-film thickness of200nm in this experiment. The transmission spectra of the films show resonance peaks of Ag particles surface plasmon.
2. Some FTO films are thermal annealed in tubular furnace. The effects of annealing atmosphere, annealing temperature and time on structure, surface morphology and photoelectric properties of the FTO films are studied, and the mechanisms of these effects are deeply analyzed. Also the integrated photoelectric properties of all the FTO films are appraised by calculating figure of merit. The results indicate that the crystallinity of the FTO films are improved when annealed in nitrogen, air or oxygen, and the integrated photoelectric properties of the FTO films annealed in nitrogen are best. When annealing in nitrogen, the effects of annealing time on transmittance and sheet resistance of the FTO films are not as dramatical as those of annealing temperature, and the best integrated photoelectric property with a figure of merit of5.56×10-3Ω-1is achieved by annealing at500℃for20min.
3. The surfaces of FTO films are irradiated by a nanosecond pulsed laser with a wavelength of532nm. The effects of laser fluence and scan speed on morphologies and photoelectric properties of the films were discussed. The results indicate that the film irradiated by laser with moderate laser fluence and scan speed achieved better laser annealing effects. The crystalline grains in laser irradiate zone grow up through a recrystallization process, which results in improvement of transmittance and decrease of sheet resistance. The laser fluence of1.02J/cm2and the scan speed of10mm/s are the optimal laser parameters in this experiment, with the average optical transmittance of the film in the waveband of380-780nm increased from75.4%to82.7%and the sheet resistance of the film decreased from10.20Ω/□to8.83Ω/□.
4. By depositing aluminum-doped zinc oxide (AZO) films on FTO films using direct current magnetron sputtering, some AZO/FTO composite films are prepared. The effects of AZO-layer thickness on structure, micro-morphology and photoelectric property of the AZO/FTO films are investigated, and the mechanisms of these effects are preliminary discussed. The results show that the surface roughnesses of AZO/FTO films gradually reduce when the AZO-layer thickness increases, with the sheet resistances of the films decrease firstly and then change gently, as well as the transmittances of them increase firstly and then decrease. It is found in this experiment that the AZO/FTO film with an AZO-layer thickness of495nm has the best photoelectric property with a figure of merit of1.43x10-2Ω-1.
5. The optimally prepared AZO/FTO films are post-treated by both thermal annealing and laser irradiation to further improve their properties. The variations in surface morphologies and photoelectric properties of the films treated with different parameters are studies. The results show that the compactnesses and planenesses of the films treated by thermal annealing are enhanced, and the transmittances of them keep on slightly improving with increases in annealing temperature or annealing time. While the sheet resistances of them decrease greatly before the annealing temperature is up to300℃, and then are almost not affected with the increases in annealing temperature or annealing time at500℃. Laser irradiation can also achieve a certain annealing effects on AZO/FTO films, and the optimal effect is obtained by treating them with a laser fluence of1.02J/cm2and a scan speed of10mm/s.
引文
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