CN105349966A - 一种绒面复合结构ZnO-TCO薄膜的制备方法及应用 - Google Patents
一种绒面复合结构ZnO-TCO薄膜的制备方法及应用 Download PDFInfo
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- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
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Abstract
一种绒面复合结构ZnO-TCO薄膜的制备方法及应用,所述绒面结构ZnO-TCO薄膜的结构特征为微米级绒面玻璃/MOCVD-ZnO:B纳米薄膜,制备步骤是:1)先用去离子水和稀盐酸(HCl)溶液对玻璃表面进行清洗,然后采用蒙砂粉进行蒙砂刻蚀;抛光次数为1-12次,形成微米级尺寸绒面玻璃,特征尺寸~5至25μm;2)以二乙基锌(DEZn)和水(H2O)为原料,氢稀释浓度为1.0%的硼烷B2H6作为掺杂气体,利用MOCVD技术在上述粗糙微米玻璃上生长纳米尺寸(~300-800nm)高电导ZnO:B透明导电薄膜,薄膜厚度为1000-3000nm。本发明的优点是:成本低廉,可实现微纳米尺寸复合结构的ZnO薄膜,提高光散射能力,用于pin型Si基叠层薄膜太阳电池,可实现较高光电转化效率。
Description
技术领域
本发明涉及太阳电池透明导电氧化物薄膜,特别是一种绒面结构ZnO-TCO薄膜的制备方法及其应用。
背景技术
氢化非晶硅(a-Si:H)的光学带宽为1.7eV左右,其吸收系数在短波方向较高,而氢化微晶硅(μc-Si:H)的光学带宽约为1.1eV,其吸收系数在长波方向较高,并能吸收到近红外长波区域,吸收波长可扩展至1100nm,这就使太阳光谱能得到更好利用。此外,相比于非晶硅薄膜材料,微晶硅薄膜材料结构有序性程度高,因此,微晶硅薄膜电池具有很好的器件稳定性,无明显衰退现象。由此可见,微晶硅薄膜太阳电池可较好地利用太阳光谱的近红外光区域,而新型非晶硅/微晶硅(a-Si:H/μc-Si:H)叠层薄膜太阳电池将扩展太阳光谱应用范围,整体提高电池稳定性和效率,参见:J.Meier,S.Dubail,R.Platz,etc.Sol.EnergyMater.Sol.Cells49(1997)35;ArvindShah,J.Meier,E.Vallat-Sauvain,etc,ThinSolidFilms403-404(2002)179。绒面结构(texturedstructure)透明导电氧化物-TCO薄膜的应用可以增强光散射作用,改善陷光效果,它对提高Si基薄膜太阳电池的效率和稳定性(SW效应)起到决定性的影响,参见:A.V.Shah,H.Schade,M.Vanecek,etc,ProgressinPhotovoltaics,12(2004)113。绒面结构主要与薄膜的晶粒尺寸,晶粒形状和粗糙度等因素有关。
MOCVD(metalorganicchemicalvapordeposition-MOCVD,即金属有机物化学气相沉积)技术可直接生长出绒面结构的ZnO薄膜,参见:X.L.Chen,X.H.Geng,J.M.Xue,etc.J.Cryst.Growth,296(2006)43;W.W.Wenas,A.Yamada,K.Takahashi,etc,J.Appl.Phys.70(1991)7119;S.U.Kroll,C.Bucher,etc,Sol.EnergyMater.Sol.Cells86(2005)385;S.L.Feitknecht,R.Schluchter,etc,Sol.EnergyMater.Sol.Cells90(2006)2960。薄膜生长过程为无粒子轰击的热分解过程,沉积温度低(~423K);可以实现高速度、大面积且均匀的ZnO薄膜生长,符合产业化发展要求。典型的MOCVD-ZnO薄膜的表面形貌,晶粒呈现“类金字塔”状,XRD衍射谱中对应(110)峰择优取向,特征晶粒尺寸~300-500nm,平均粗糙度σrms=40-80nm,电阻率ρ~1.5-3×10-3Ωcm。
国际上研究了绒面结构ZnO薄膜衬底并应用于薄膜电池。意大利ENEA研究组的M.L.Addonizio等人采用Ar等离子体对薄膜表面进行了不同刻蚀时间的处理,随着处理时间的增长,薄膜表面的金字塔装结构逐渐减小,最终变为弹坑状结构,虽然薄膜表面粗糙度和Haze值都有所下降,但表面较为圆滑,改善了TCO层与a-Si电池p层的接触特性,电池的Voc、Jsc都有所提高[AddonizioML,AntonaiaA.,ThinSolidFilms,2009,518(4):1026-1031.]。2013年,荷兰H.R.Tan等人采用HF和H2O2混合溶液对玻璃表面进行湿法腐蚀,获得了横向尺寸~20μm的弹坑状形貌。沉积AZO薄膜后,以其作为前电极制备纳米晶硅(nc-Si:H)电池的Jsc为12.0mA/cm2,效率为13.3%[TanHR,PsomadakiE,IsabellaO,etal..AppliedPhysicsLetters,2013,103:173905(1)-173905(5).]。2013年,新加坡S.Venkataraj等人采用Al诱导法对玻璃表面进行了刻蚀处理,具体方法为:首先,采用蒸发法在玻璃表面沉积Al薄膜,Al会和SiO2发生反应生成Si和Al2O3,再通过HNO3/HF混合溶液对其进行腐蚀,腐蚀后得到了横向尺寸~5μm的弹坑状结构,制备的AZO/glass在800nm处的Haze值~58%[VenkatarajS,WangJ,VayalakkaraP,etal.IEEEJournalofPhotovoltaics,3(2):605-612.]
综述所述,开发具有适合太阳电池应用的绒面ZnO-TCO薄膜成为当前科研工作中的重点和未来发展方向。
发明内容
本发明的目的是提供一种宽光谱高绒度绒面结构TCO薄膜,从而提高Si薄膜电池在光电性能,获得一种宽光谱高绒度绒面结构ZnO-TCO薄膜及其应用方法,采用湿法刻蚀技术获得粗糙表面的微米结构玻璃衬底,而后采用MOCVD技术制备纳米结构ZnO:B薄膜。
本发明的技术方案:
一种绒面微纳结构ZnO-TCO薄膜的制备方法,所述绒面结构ZnO-TCO薄膜的结构特征为微米结构玻璃/MOCVD-ZnO纳米结构,制备步骤如下:
1)先用去离子水和稀盐酸溶液对玻璃表面进行清洗,然后采用蒙砂粉进行蒙砂刻蚀,刻蚀时间为1分35秒,处理完之后,为去除蒙砂过程中生成的附着物,需要用主要成分为HF/H2SO4的抛光液对其进行抛光处理;抛光次数为1-12次,每次抛光时间为5分钟;获得的微米级玻璃衬底,其弹坑状尺寸为~5-20μm;
2)以纯度为99.995%二乙基锌和水为原料,氢稀释浓度为1.0%的硼烷B2H6作为掺杂气体,利用MOCVD技术在上述粗糙微米玻璃上生长纳米尺寸(300-800nm)高电导ZnO:B透明导电薄膜,薄膜厚度1000-3000nm,利用MOCVD技术的工艺参数:衬底温度为135-165℃,B2H6掺杂气体流量为二乙基锌流量的1.0%,反应压力为1.0Torr,生长速率为20-100nm/min。
进一步的,步骤1)中所述的抛光次数为3次。
一种所制备的绒面结构ZnO-TCO薄膜的应用,用于pin型Si基薄膜太阳电池。
本发明的优点及效果:湿法刻蚀技术可获得不同弹坑状微米结构玻璃衬底,而MOCVD技术可调节获得纳米尺寸ZnO:B薄膜,获得的玻璃衬底/ZnO薄膜具有微纳米复合结构,提高光散射特性,实现较高光电转化效率。
本发明的基本思想是结合MOCVD技术生长纳米结构ZnO晶粒尺寸和微米级粗糙绒面结构玻璃的优点,实现新型复合微米纳米结构ZnO:B薄膜,并将其应用于Si基薄膜太阳电池。首先,利用蒙砂刻蚀技术实现微米级玻璃衬底,其弹坑状尺寸为5-25μm;其次,MOCVD技术在粗糙的微米尺寸玻璃衬底上制备纳米级尺寸ZnO:B透明导电薄膜,金字塔状晶粒尺寸300-800nm。新型复合绒面结构ZnO:B应用于Si基薄膜太阳电池。
采用蒙砂刻蚀法对平面玻璃(超白玻璃)表面进行湿法腐蚀处理,从而获得微米级尺寸弹坑状结构,其横向尺寸范围为~8至25μm。当抛光次数(x)为1时,玻璃的表面粗糙度(RMSroughness)达到409.0nm,在400nm-1100nm的波长范围内绒度(Haze)值~80%。复合结构玻璃/ZnO:B薄膜方块电阻可达到~20欧姆。
附图说明
图1是蒙砂刻蚀获得的微米级尺寸玻璃扫描电镜(SEM)图像。
图2是该玻璃/MOCVD-ZnO薄膜扫描电镜(SEM)图像。
图3是该玻璃/MOCVD-ZnO薄膜应用于pin型Si基叠层薄膜太阳电池的电流-电压(J-V)曲线。
具体实施方式
实施例1:
一种绒面复合结构ZnO-TCO薄膜的制备方法,所述绒面结构ZnO-TCO薄膜的结构特征为微米级结构玻璃/纳米级尺寸MOCVD-ZnO:B薄膜,制备步骤如下:
1)为得到干净的玻璃表面,先用去离子水和稀盐酸(HCl)溶液对玻璃表面进行清洗,然后采用蒙砂粉进行蒙砂刻蚀,刻蚀时间为1分35秒,处理完之后,为去除蒙砂过程中生成的附着物,需要用主要成分为HF/H2SO4的抛光液(其成分为HF和H2SO4的水溶液,HF和H2SO4比例1-10,溶液浓度5-30%)对其进行抛光处理;抛光次数为3,每次抛光时间为5分钟;获得的微米级玻璃衬底,其弹坑状尺寸为~8-10μm;
图1是蒙砂刻蚀获得的微米级尺寸玻璃扫描电镜(SEM)图像,图中表明,玻璃呈现微米级尺寸的弹坑状形貌。
2)以纯度为99.995%二乙基锌(DEZn)和水(H2O)为原料,氢稀释浓度为1.0%的硼烷B2H6作为掺杂气体,利用MOCVD技术在上述粗糙微米玻璃上生长纳米尺寸(300-800nm)高电导ZnO:B透明导电薄膜,薄膜厚度2140nm,利用MOCVD技术的工艺参数:衬底温度为135-165℃,B2H6掺杂气体流量为二乙基锌流量的1.0%,反应压力为1.0Torr,生长速率为20-100nm/min。
图2是该玻璃/MOCVD-ZnO薄膜扫描电镜(SEM)图像,图中表明:薄膜表面呈现复合结构的微纳米相结合的ZnO薄膜。
将该玻璃/MOCVD-ZnO薄膜应用于pin型硅基薄膜太阳电池,为非晶硅a-Si:H太阳电池。与以传统平面玻璃/ZnO:B绒面结构薄膜作为前电极太阳电池相比,电池效率从6.88%提高至7.22%,如图3所示。
实施例2:
一种绒面结构ZnO-TCO薄膜的制备方法,所述绒面结构ZnO-TCO薄膜的结构特征为微米级结构玻璃/纳米级尺寸MOCVD-ZnO:B薄膜,制备步骤如下:
1)为得到干净的玻璃表面,先用去离子水和稀盐酸(HCl)溶液对玻璃表面进行清洗,然后采用蒙砂粉进行蒙砂刻蚀,刻蚀时间为1分35秒,处理完之后,为去除蒙砂过程中生成的附着物,需要用主要成分为HF/H2SO4的抛光液(其成分为HF和H2SO4的水溶液,HF和H2SO4比例1-10,溶液浓度5-30%)对其进行抛光处理;抛光次数为1,每次抛光时间为5分钟;获得的微米级玻璃衬底,其弹坑状尺寸为~5μm;
2)以纯度为99.995%二乙基锌(DEZn)和水(H2O)为原料,氢稀释浓度为1.0%的硼烷B2H6作为掺杂气体,利用MOCVD技术在上述粗糙微米玻璃上生长纳米尺寸高电导ZnO:B透明导电薄膜,薄膜厚度1500nm,利用MOCVD技术的工艺参数:衬底温度为135-165℃,B2H6掺杂气体流量为二乙基锌流量的1.0%,反应压力为1.0Torr,生长速率为20-100nm/min。
将该玻璃/MOCVD-ZnO薄膜应用于pin型硅基薄膜太阳电池,与实施例1相同。
实施例3:
一种绒面结构ZnO-TCO薄膜的制备方法,所述绒面结构ZnO-TCO薄膜的结构特征为微米级结构玻璃/纳米级尺寸MOCVD-ZnO:B薄膜,制备步骤如下:
1)为得到干净的玻璃表面,先用去离子水和稀盐酸(HCl)溶液对玻璃表面进行清洗,然后采用蒙砂粉进行蒙砂刻蚀,刻蚀时间为1分35秒,处理完之后,为去除蒙砂过程中生成的附着物,需要用主要成分为HF/H2SO4的抛光液(其成分为HF和H2SO4的水溶液,HF和H2SO4比例1-10,溶液浓度5-30%)对其进行抛光处理;抛光次数为12,每次抛光时间为5分钟;获得的微米级玻璃衬底,其弹坑状尺寸为~20μm;
2)以纯度为99.995%二乙基锌(DEZn)和水(H2O)为原料,氢稀释浓度为1.0%的硼烷B2H6作为掺杂气体,利用MOCVD技术在上述粗糙微米玻璃上生长纳米尺寸高电导ZnO:B透明导电薄膜,薄膜厚度1200nm,利用MOCVD技术的工艺参数:衬底温度为135-165℃,B2H6掺杂气体流量为二乙基锌流量的1.0%,反应压力为1.0Torr,生长速率为20-100nm/min。
将该玻璃/MOCVD-ZnO薄膜应用于pin型硅基薄膜太阳电池,与实施例1相同。
Claims (3)
1.一种绒面复合结构ZnO-TCO薄膜的制备方法,所述绒面结构ZnO-TCO薄膜的结构特征为微米结构玻璃/MOCVD-ZnO纳米结构,制备步骤如下:
1)先用去离子水和稀盐酸溶液对玻璃表面进行清洗,然后采用蒙砂粉进行蒙砂刻蚀,刻蚀时间为1分35秒,处理完之后,为去除蒙砂过程中生成的附着物,需要用主要成分为HF/H2SO4的抛光液对其进行抛光处理;抛光次数为1-12次,每次抛光时间为5分钟;获得的微米级玻璃衬底,其弹坑状尺寸为~5-20μm;
2)以纯度为99.995%二乙基锌和水为原料,氢稀释浓度为1.0%的硼烷B2H6作为掺杂气体,利用MOCVD技术在上述粗糙微米玻璃上生长纳米尺寸(300-800nm)高电导ZnO:B透明导电薄膜,薄膜厚度1000-3000nm,利用MOCVD技术的工艺参数:衬底温度为135-165℃,B2H6掺杂气体流量为二乙基锌流量的1.0%,反应压力为1.0Torr,生长速率为20-100nm/min。
2.根据权利要求1所述的绒面复合结构ZnO-TCO薄膜的制备方法,其特征在于:步骤1)中所述的抛光次数为3次。
3.一种权利要求1所制备的绒面结构ZnO-TCO薄膜的应用,其特征在于:用于pin型Si基叠层薄膜太阳电池。
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