CN105734512A - 一种ZnO/Mo/ZnO透明导电薄膜的制备方法 - Google Patents
一种ZnO/Mo/ZnO透明导电薄膜的制备方法 Download PDFInfo
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Abstract
本发明提供了一种ZnO/Mo/ZnO透明导电薄膜的制备方法,室温下先将基片清洗,用氮气枪吹干;然后将ZnO靶材、Mo靶材和基片放入磁控溅射反应室,将反应室抽真空,打开温控电源,将基片加热,向反应室通入氩气和氧气的混合气,开启ZnO靶材一侧的射频电源,溅射ZnO靶材;将反应室重新抽真空,开启Mo靶材一侧的射频电源,溅射Mo靶材;将反应室重新抽真空,再开启ZnO靶材一侧的射频电源,溅射ZnO靶材;然后将样品取出,放到马弗炉中退火,冷却后得到ZnO/Mo/ZnO叠层结构透明导电薄膜。本发明利用ZnO的良好光电性能和Mo的低电阻率,制备成叠层ZnO/Mo/ZnO透明导电薄膜。
Description
技术领域
本发明属于光电薄膜材料领域,具体涉及一种ZnO/Mo/ZnO透明导电薄膜的制备方法。
背景技术
透明导电材料作为多数电子显示器件中不可或缺的组成部分而广泛地应用于各种平板显示、触摸式显示屏、薄膜太阳能电池等很多领域。
20世纪初,透明导电CdO薄膜的出现引起研究者的重视,并从此开启了透明导电氧化物薄膜(TCO)的研究热潮。TCO薄膜导电性能良好、可见光波段透射性高,并且在红外范围内的反射性能良好。并包括In2O3基薄膜、SnO2基薄膜和ZnO基薄膜三大类,其中铟锡氧化物(In2O3:Sn,简称ITO)薄膜是应用最广的TCO薄膜,其光电性能优良、制备简单且易于刻蚀。但ITO薄膜的方阻较大,难以应用于大尺寸平面显示,此外,铟属稀缺金属、有毒,且生产成本大,不能满足平板显示器向大面积和快速显示发展的应用要求。
随着掺杂和制膜工艺的日趋成熟,研究者开始对ZnO薄膜进行掺杂研究。ZnO基薄膜与ITO薄膜相比,价格低廉、无毒、制备温度较低且制膜方法多,往ZnO中掺入B、F、Al之后其薄膜的光电性能及热稳定性都得到提高。其中,ZnO:Al(简称AZO)是最具潜力的一种ZnO基透明导电薄膜,其低电阻率、高可见光透过率使其达到了相关设备器件中的实验要求。但ZnO基薄膜的制膜工艺不易掌控,产品重复性不好,未能满足工业化生产的要求。掺杂条件与工艺还在不断摸索中。
目前国内外有关ZnO的掺杂技术的报道非常多,但有关ZnO/Mo/ZnO叠层透明导电薄膜的制备及研究几乎没有。掺杂工艺的不均匀、不稳定性促使我们寻求制备的新方法,双射频磁控溅射技术在薄膜材料制备上的应用史无前例。
发明内容
针对现有技术中的上述技术问题,本发明提供了一种ZnO/Mo/ZnO透明导电薄膜的制备方法,所述的这种ZnO/Mo/ZnO透明导电薄膜的制备方法要解决现有技术中的ZnO基薄膜的制膜工艺不易掌控、产品重复性不好,未能满足工业化生产的要求的技术问题。
本发明提供了一种ZnO/Mo/ZnO透明导电薄膜的制备方法,包括如下步骤:
1)室温下将基片清洗,然后用氮气枪将其吹干;
2)打开磁控溅射反应室,把纯度为99.999%的ZnO靶材和Mo靶材固定在反应室中,将基片放入磁控溅射反应室,将反应室抽真空到9.9×10-4Pa,打开温控电源,将基片加热到300~400℃,待基片温度均匀后,向反应室通入氩气和氧气的混合气,所述的氩气和氧气的体积比为(3~8):1,开启ZnO靶材一侧的射频电源,将溅射功率调至40~100W,调节压强至2~5Pa,打开挡板,溅射8~16min40s,ZnO厚度为45~65nm;
3)将反应室重新抽真空至9.9×10-4Pa,开启Mo靶材一侧的射频电源,将溅射功率调至75~100W,向反应室通入氩气,调节压强至0.4~0.6Pa,打开挡板,溅射10~40s,Mo层厚度在5~15nm;
4)将反应室重新抽真空至9.9×10-4Pa,再开启ZnO靶材一侧的射频电源,将溅射功率调至40~100W,向反应室通入氩气和氧气的混合气,所述的氩气和氧气的体积比为(3~8):1,调节压强至2~5Pa,打开挡板,溅射8~16min40s,ZnO厚度为45~65nm;
5)待反应室温度降至常温,将样品取出,放到马弗炉中在150~400℃退火1h,冷却至常温,得到ZnO/Mo/ZnO叠层结构透明导电薄膜。
进一步的,室温下将基片依次用无水乙醇、丙酮、去离子水超声清洗。
进一步的,所述的基片是载玻片。
本发明利用双射频磁控溅射技术,利用ZnO的良好光电性能和Mo的低电阻率,制备成叠层ZnO/Mo/ZnO透明导电薄膜,Mo的加入提高了膜系的载流子浓度,提高了薄膜的导电性能,Mo离子与Zn离子离子半径接近,在Mo/ZnO晶界处晶格畸变小,可减少界面对光子的散射,保证光学透过率在80%以上。本发明利用双射频磁控溅射系统制备出膜厚均匀,导电性能优异,光学透过率良好的ZnO/Mo/ZnO透明导电薄膜,其电阻率低至9.3×10-5Ω·cm,400~800nm平均透过率达到80%以上。且此方法镀膜均匀,薄膜质量较高。
本发明和已有技术相比,其技术进步是显著的。本发明工艺简单,双射频磁控溅射,易于控制条件,且制备的薄膜均匀性好,薄膜性能优异,可用于制造平板显示器、太阳能电池、发光二极管、手机等光电显示器件的电极材料。
附图说明
图1为本发明方法制备的ZnO/Mo/ZnO叠层透明导电薄膜示意图,其中1为基片,2为ZnO薄膜层,3为中间Mo薄膜层。
图2为实例1不同退火温度下的ZnO/Mo/ZnO透明导电薄膜在400~800nm之间的透过率曲线。
图3为实例1制备的ZnO/Mo/ZnO透明导电薄膜的SEM图像。
具体实施方式
下面对本发明实施例作详细说明。本实施例以本发明技术方案为前提下进行实施,给出了详细的实施方案和操作过程。但本发明的保护范围不限于下述实施例。
实施例1
室温下将基片依次用无水乙醇、丙酮、去离子水超声清洗20min。之后用高纯度的氮气枪将其吹干。打开反应室把纯度为99.999%ZnO靶材和Mo靶材固定(ZnO在左侧),将样品放入磁控溅射反应室,将反应室抽真空到9.0×10-4Pa。打开温控电源,将基片加热到300℃。待基片温度均匀后,向反应室通入高纯度的氩气氧气(氩氧比例为3:1),开启左侧射频电源,将溅射功率调至40W,调节压强至2Pa,打开挡板,溅射16min40s,ZnO厚度约50nm。
将反应室重新抽真空至9.0×10-4Pa,开启右侧射频电源,将溅射功率调至75W,向反应室通入氩气,调节压强至0.5Pa,打开挡板,溅射26s,Mo厚度约10nm。
将反应室重新抽真空至9.0×10-4Pa,再开启左侧射频电源,将溅射功率调至40W,向反应室通入氩气氧气(氩气氧气比例为3:1),调节压强至2Pa,打开挡板,溅射16min40s,ZnO厚度约50nm。
待反应室温度降至常温,将样品取出,放到马弗炉中在150~400℃退火1h。冷却至常温,得到厚度约110nm的ZnO/Mo/ZnO叠层结构透明导电薄膜。
对实施例1在不同退火温度下可见光范围内的透过率和表面形貌进行表征,由图2可见,在250℃下退火1h得到的ZnO/Mo/ZnO透明导电薄膜在400-800nm波段的光学透过率约为82%。由图3可见,ZnO/Mo/ZnO薄膜表面形貌均匀,结晶程度好,界面散射和吸收少,有利于提高光学透过率。
实施例2
室温下将基片依次用无水乙醇、丙酮、去离子水超声清洗20min。之后用高纯度的氮气枪将其吹干。打开反应室把纯度为99.999%ZnO靶材和Mo靶材固定(ZnO在左侧),将样品放入磁控溅射反应室,将反应室抽真空到9.0×10-4Pa。打开温控电源,将基片加热到350℃。待基片温度均匀后,向反应室通入高纯度的氩气氧气(氩氧比例为4:1),开启左侧射频电源,将溅射功率调至60W,调节压强至2Pa,打开挡板,溅射12min,ZnO厚度约45nm。
将反应室重新抽真空至9.0×10-4Pa,开启右侧射频电源,将溅射功率调至85W,向反应室通入氩气,调节压强至0.5Pa,打开挡板,溅射10s,Mo厚度约5nm。
将反应室重新抽真空至9.0×10-4Pa,再开启左侧射频电源,将溅射功率调至60W,向反应室通入氩气氧气(氩气氧气比例为4:1),调节压强至2Pa,打开挡板,溅射12min,ZnO厚度约45nm。
待反应室温度降至常温,将样品取出,放到马弗炉中在250℃退火1h。冷却至常温,得到厚度约95nm的ZnO/Mo/ZnO叠层结构透明导电薄膜。
实施例3
室温下将基片依次用无水乙醇、丙酮、去离子水超声清洗20min。之后用高纯度的氮气枪将其吹干。打开反应室把纯度为99.999%ZnO靶材和Mo靶材固定(ZnO在左侧),将样品放入磁控溅射反应室,将反应室抽真空到9.0×10-4Pa。打开温控电源,将基片加热到300℃。待基片温度均匀后,向反应室通入高纯度的氩气氧气(氩氧比例为6:1),开启左侧射频电源,将溅射功率调至80W,调节压强至2Pa,打开挡板,溅射10min,ZnO厚度约65nm。
将反应室重新抽真空至9.0×10-4Pa,开启右侧射频电源,将溅射功率调至75W,向反应室通入氩气,调节压强至0.5Pa,打开挡板,溅射20s,Mo厚度约8nm。
将反应室重新抽真空至9.0×10-4Pa,再开启左侧射频电源,将溅射功率调至80W,向反应室通入氩气氧气(氩气氧气比例为6:1),调节压强至2Pa,打开挡板,溅射10min,ZnO厚度约65nm。
待反应室温度降至常温,将样品取出,放到马弗炉中在250℃退火1h。冷却至常温,得到厚度约138nm的ZnO/Mo/ZnO叠层结构透明导电薄膜。
实施例4
室温下将基片依次用无水乙醇、丙酮、去离子水超声清洗20min。之后用高纯度的氮气枪将其吹干。打开反应室把纯度为99.999%ZnO靶材和Mo靶材固定(ZnO在左侧),将样品放入磁控溅射反应室,将反应室抽真空到9.0×10-4Pa。打开温控电源,将基片加热到400℃。待基片温度均匀后,向反应室通入高纯度的氩气氧气(氩氧比例为8:1),开启左侧射频电源,将溅射功率调至80W,调节压强至2Pa,打开挡板,溅射8min,ZnO厚度约55nm。
将反应室重新抽真空至9.0×10-4Pa,开启右侧射频电源,将溅射功率调至100W,向反应室通入氩气,调节压强至0.5Pa,打开挡板,溅射16s,Mo厚度约12nm。
将反应室重新抽真空至9.0×10-4Pa,再开启左侧射频电源,将溅射功率调至80W,向反应室通入氩气氧气(氩气氧气比例为8:1),调节压强至2Pa,打开挡板,溅射8min,ZnO厚度约55nm。
待反应室温度降至常温,将样品取出,放到马弗炉中在250℃退火1h。冷却至常温,得到厚度约122nm的ZnO/Mo/ZnO叠层结构透明导电薄膜。
实施例5
室温下将基片依次用无水乙醇、丙酮、去离子水超声清洗20min。之后用高纯度的氮气枪将其吹干。打开反应室把纯度为99.999%ZnO靶材和Mo靶材固定(ZnO在左侧),将样品放入磁控溅射反应室,将反应室抽真空到9.0×10-4Pa。打开温控电源,将基片加热到400℃。待基片温度均匀后,向反应室通入高纯度的氩气氧气(氩氧比例为3:1),开启左侧射频电源,将溅射功率调至100W,调节压强至2Pa,打开挡板,溅射8min,ZnO厚度约60nm。
将反应室重新抽真空至9.0×10-4Pa,开启右侧射频电源,将溅射功率调至75W,向反应室通入氩气,调节压强至0.5Pa,打开挡板,溅射40s,Mo厚度约15nm。
将反应室重新抽真空至9.0×10-4Pa,再开启左侧射频电源,将溅射功率调至100W,向反应室通入氩气氧气(氩气氧气比例为3:1),调节压强至2Pa,打开挡板,溅射8min,ZnO厚度约60nm。
待反应室温度降至常温,将样品取出,放到马弗炉中在250℃退火1h。冷却至常温,得到厚度约135nm的ZnO/Mo/ZnO叠层结构透明导电薄膜。
Claims (3)
1.一种ZnO/Mo/ZnO透明导电薄膜的制备方法,其特征在于包括如下步骤:
1)室温下将基片清洗,然后用氮气枪将其吹干;
2)打开磁控溅射反应室,把纯度为99.999%的ZnO靶材和Mo靶材固定在反应室中,将基片放入磁控溅射反应室,将反应室抽真空到9.9×10-4Pa,打开温控电源,将基片加热到300~400℃,待基片温度均匀后,向反应室通入氩气和氧气的混合气,所述的氩气和氧气的体积比为(3~8):1,开启ZnO靶材一侧的射频电源,将溅射功率调至40~100W,调节压强至2~5Pa,打开挡板,溅射8~16min40s,ZnO厚度为45~65nm;
3)将反应室重新抽真空至9.9×10-4Pa,开启Mo靶材一侧的射频电源,将溅射功率调至75~100W,向反应室通入氩气,调节压强至0.4~0.6Pa,打开挡板,溅射10~40s,Mo层厚度在5~15nm;
4)将反应室重新抽真空至9.9×10-4Pa,再开启ZnO靶材一侧的射频电源,将溅射功率调至40~100W,向反应室通入氩气和氧气的混合气,所述的氩气和氧气的体积比为(3~8):1,调节压强至2~5Pa,打开挡板,溅射8~16min40s,ZnO厚度为45~65nm;
5)待反应室温度降至常温,将样品取出,放到马弗炉中在150~400℃退火1h,冷却至常温,得到ZnO/Mo/ZnO叠层结构透明导电薄膜。
2.根据权利要求1所述的一种ZnO/Mo/ZnO透明导电薄膜的制备方法,其特征在于:室温下将基片依次用无水乙醇、丙酮、去离子水超声清洗。
3.根据权利要求1所述的一种ZnO/Mo/ZnO透明导电薄膜的制备方法,其特征在于:所述的基片是载玻片。
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