CN114086126B - 一种单晶太阳能电池薄膜材料及其制备方法 - Google Patents
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Abstract
本发明公开了一种单晶太阳能电池薄膜材料及其制备方法,涉及新能源材料以及光电应用领域,方法包括如下步骤:S1、以BaS粉末和ZrS2粉末为反应材料进行高温煅烧并压片得到BaZrS3靶材;S2、将步骤S1中合成得到的BaZrS3靶材和清洗好的YSZ衬底放入脉冲激光沉积系统;S3、对YSZ衬底进行真空室温沉积镀膜得到BaZrS3非晶薄膜;S4、对步骤S3获得的产物进行真空高温热处理,得到BaZrS3单晶太阳能电池薄膜材料。本发明探索的制备条件工艺,首次制备了BaZrS3单晶薄膜,为探索该材料光学性质提供了优良的薄膜样品,该材料具有优良的光学吸收,在太阳能电池领域具有较大的应用前景。
Description
技术领域
本发明属于新能源材料以及光电应用领域,具体涉及一种BaZrS3单晶太阳能电池薄膜材料及其制备方法。
背景技术
寻找高效的太阳能电池材料,或者一般的光电子材料,是材料化学和物理学中的一个古老的研究课题。所追求的材料是具有合适光带隙的高质量半导体,目前在开发太阳能电池材料方面取得了重大成功,如硅、砷化镓、碲化镉、铜铟镓硒和卤化铅钙钛矿。不幸的是,这些材料在大规模应用方面仍然存在问题。卤化铅钙钛矿已经显示出优异的光电性能,太阳能电池单结器件的效率超过25%,与硅的单片串联的效率超过29%。但这些化合物的稳定性以及铅所具有的毒性是目前一大挑战,因此,寻找好的太阳能电池材料仍然是最具挑战性和最重要的研究领域之一。
为了解决混合钙钛矿的毒性和稳定性限制,近年来出现了一种新的材料类别无机硫族钙钛矿。2015年,孙等人从理论上筛选出18种用于光伏的ABX3硫族钙钛矿,其中A为Ca/Sr/Ba,B为Ti/Zr/Hf,X为S/Se。几个ABX3硫族钙钛矿被确定具有合适的带隙和光学吸收,可以用于光伏材料。作为典型的硫族钙钛矿,BaZrS3具有1.8eV的直接带隙和强的近边缘吸收。此外,已经证明BaZrS3具有稳定的钙钛矿结构,能够抵抗高压、湿气和热量。然而,由于缺乏高质量的薄膜样品,有关硫族钙钛矿BaZrS3的诸多性质还未被探索,目前,在BaZrS3薄膜制备方面,薄膜样品数极少,且大多数制备的是多晶薄膜,因此,本领域技术人员致力于开发一种在非金属衬底YSZ上外延制备BaZrS3太阳能电池单晶薄膜材料的方法,使得制备的BaZrS3太阳能电池单晶薄膜材料具有优良的光学性能以及较好的稳定性和优异的环境友好性,并且为研究BaZrS3的其他性质提供高质量的薄膜样本。
目前,BaZrS3太阳能电池薄膜材料的制备多采用先制备BaZrO3薄膜,再通CS2或H2S进行硫化,最终得到BaZrS3多晶薄膜,这种制备工艺制备出的BaZrS3薄膜材料是多晶薄膜,导致单晶薄膜才能显现出来的一些性质无法探索。
发明内容
有鉴于现有技术的上述缺陷,本发明所要解决的技术问题是提供一种BaZrS3单晶太阳能电池薄膜材料及其制备方法,使得制备的BaZrS3外延薄膜材料是单晶薄膜,并且具有优良的光学性能以及较好的稳定性和优异的环境友好性,为研究BaZrS3的其他性质提供高质量的薄膜样本。
为实现上述目的,本发明采用如下技术方案:
一种单晶太阳能电池薄膜材料的制备方法,包括如下步骤:
S1、以BaS粉末和ZrS2粉末为反应材料进行高温煅烧并压片得到BaZrS3靶材;
S2、将步骤S1中合成得到的BaZrS3靶材和清洗好的YSZ衬底放入脉冲激光沉积系统;
S3、对YSZ衬底进行真空室温沉积镀膜得到BaZrS3非晶薄膜;
S4、对步骤S3获得的产物进行真空高温热处理,得到BaZrS3单晶太阳能电池薄膜材料。
进一步地,步骤S1中BaS粉末和ZrS2粉末化学计量比为1:1,将两者在手套箱内进行称量混合研磨20min,并用压靶机压片,压力为20Mpa,压片时间20min,压片磨具的直径为12.5mm,将压完片的靶材转移至石英管中,利用真空封管机进行封管,最后将真空封好的靶材转移至管式炉中进行高温热处理,待炉内温度降至室温,取出石英管并取出其中的靶材。
进一步地,真空封管机中的真空度为10-4Pa。
进一步地,将真空封好的靶材转移至管式炉中进行高温热处理的条件如下:从室温加热至900-1000℃,加热速率7℃/min,保温15h。
进一步地,步骤S2中合成好的BaZrS3靶材需用砂纸进行表面打磨,并用导电碳胶粘到靶托上;YSZ基片分别用丙酮、酒精、去离子水进行超声波清洗,清洗时间为5min、5min、10min;将清洗好的YSZ基片用氮气吹干,并用导电银浆粘到基片托上;将放有靶材的靶托和放有YSZ的基片托放入脉冲激光沉积系统的溅射室中,靶材和YSZ基底的间距控制在5-6cm。
进一步地,步骤S3中脉冲激光沉积系统的真空度为10-5Pa,温度为室温,激光光束的频率为8Hz,发射能量为200mJ,沉积脉冲数为8000。
进一步地,步骤S4中对获得的产物利用真空封管机进行封管,最后将真空封好的靶材转移至管式炉中进行高温热处理,待炉内温度降至室温,取出石英管并取出其中的靶材,得到BaZrS3单晶太阳能电池薄膜材料。
进一步地,真空封管机中的真空度为10-4Pa。
进一步地,将真空封好的靶材转移至管式炉中进行高温热处理的条件如下:从室温加热至900-1100℃,加热速率7℃/min,保温10h。
与现有技术相比,本发明具有如下的有益效果:
(1)本发明探索的制备条件工艺,首次制备了BaZrS3单晶外延薄膜,为探索该材料光学性质提供了优良的薄膜样品。
(2)本发明所制备的材料具有优良的光学吸收以及较低的光学带隙,在太阳能电池领域具有较大的应用前景。
(3)本发明提供的外延制备方法比较新颖,为薄膜制备领域提供新的思路。
附图说明
图1是本发明的单晶太阳能电池薄膜材料的制备工艺流程图;
图2是本发明实施例1制备的BaZrS3薄膜的校准YSZ(002)取向测得的XRD图;
图3是本发明实施例1制备的BaZrS3薄膜的校准YSZ(202)取向测得的XRD图;
图4是本发明实施例1制备的BaZrS3薄膜的校准BaZrS3(112)测得的Phi扫描图;
图5是本发明实施例制备的BaZrS3薄膜的光学吸收图谱;
图6是本发明实施例制备的BaZrS3薄膜的PL图谱。
具体实施方式
在本发明的实施例中,如图1所示,所述单晶太阳能电池薄膜材料的制备方法,包括如下步骤:
S1、BaS粉末和ZrS2,粉末化学计量比为1:1,将两者在手套箱内进行称量、混合研磨20min,并用压靶机压片,压力为20MPa,压片时间20min,压片磨具的直径为12.5mm,将压完片的靶材转移至石英管中,利用真空封管机进行封管,真空度为10-4Pa,最后将真空封好的靶材转移至管式炉中进行高温热处理,从室温加热至900-1000℃,加热速率7℃/min,保温15h,待炉内温度降至室温,取出石英管并取出其中的靶材;
S2、合成好的BaZrS3靶材需用砂纸进行表面打磨,并用导电碳胶粘到靶托上;YSZ基片分别用丙酮、酒精、去离子水进行超声波清洗,清洗时间为5min、5min、10min;将清洗好的YSZ基片用氮气吹干,并用导电银浆粘到基片托上;将放有靶材的靶托和放有YSZ的基片托放入脉冲激光沉积系统的溅射室中,靶材和YSZ基底的间距控制在5-6cm;
S3、脉冲激光沉积系统的真空度为10-5Pa,温度为室温,激光光束的频率为8Hz,发射能量为200mJ,沉积脉冲数为8000;
S4、取出步骤S3所得的产物,将其在10-4Pa真空度下进行封管,并放入管式炉中以5-8℃/min的速率升温至900-1100℃,保温时间5-10h,得到BaZrS3单晶太阳能电池薄膜材料。
下面通过3个实施例具体介绍本发明的实施过程。
实施例1
如图1所示,一种单晶太阳能电池薄膜材料的制备方法,包括如下步骤:
S1、称取5gBaS粉末和ZrS2,粉末化学计量比为1:1,将两者在手套箱内进行称量、混合研磨20min,并用压靶机压片,压力为20MPa,压片时间20min,压片磨具的直径为12.5mm,将压完片的靶材转移至石英管中,利用真空封管机进行封管,真空度为10-4Pa,最后将真空封好的靶材转移至管式炉中进行高温热处理,从室温加热至1000℃,加热速率7C/min,保温15h,待炉内温度降至室温,取出石英管并取出其中的靶材;
S2、合成好的BaZrS3靶材需用砂纸进行表面打磨,并用导电碳胶粘到靶托上;YSZ基片分别用丙酮、酒精、去离子水进行超声波清洗,清洗时间为5min、5min、10min;将清洗好的YSZ基片用氮气吹干,并用导电银浆粘到基片托上;将放有靶材的靶托和放有YSZ的基片托放入脉冲激光沉积系统的溅射室中,靶材和YSZ基底的间距控制在5cm;
S3、脉冲激光沉积系统的真空度为10-5Pa,温度为室温,激光光束的频率为8Hz,发射能量为200mJ,沉积脉冲数为8000;
S4、取出步骤S3所得的产物,将其在10-4Pa真空度下进行封管,并放入管式炉中以8℃/min的速率升温至1000℃,保温时间10h,得到BaZrS3单晶太阳能电池薄膜材料。
实施例2
如图1所示,一种单晶太阳能电池薄膜材料的制备方法,包括如下步骤:
S1、称取4.5gBaS粉末和ZrS2,粉末化学计量比为1:1,将两者在手套箱内进行称量、混合研磨20min,并用压靶机压片,压力为20MPa,压片时间20min,压片磨具的直径为12.5mm,将压完片的靶材转移至石英管中,利用真空封管机进行封管,真空度为10-4Pa,最后将真空封好的靶材转移至管式炉中进行高温热处理,从室温加热至900℃,加热速率7C/min,保温15h,待炉内温度降至室温,取出石英管并取出其中的靶材;
S2、合成好的BaZrS3靶材需用砂纸进行表面打磨,并用导电碳胶粘到靶托上;YSZ基片分别用丙酮、酒精、去离子水进行超声波清洗,清洗时间为5min、5min、10min;将清洗好的YSZ基片用氮气吹干,并用导电银浆粘到基片托上;将放有靶材的靶托和放有YSZ的基片托放入脉冲激光沉积系统的溅射室中,靶材和YSZ基底的间距控制在5cm;
S3、脉冲激光沉积系统的真空度为10-5Pa,温度为室温,激光光束的频率为8Hz,发射能量为200mJ,沉积脉冲数为8000;
S4、取出步骤S3所得的产物,将其在10-4Pa真空度下进行封管,并放入管式炉中以6℃/min的速率升温至900℃,保温时间10h,得到单晶太阳能电池薄膜材料。
实施例3
如图1所示,一种单晶太阳能电池薄膜材料的制备方法,包括如下步骤:
S1、称取4gBaS粉末和ZrS2,粉末化学计量比为1:1,将两者在手套箱内进行称量、混合研磨20min,并用压靶机压片,压力为20MPa,压片时间20min,压片磨具的直径为12.5mm,将压完片的靶材转移至石英管中,利用真空封管机进行封管,真空度为10-4Pa,最后将真空封好的靶材转移至管式炉中进行高温热处理,从室温加热至1000℃,加热速率7C/min,保温15h,待炉内温度降至室温,取出石英管并取出其中的靶材;
S2、合成好的BaZrS3靶材需用砂纸进行表面打磨,并用导电碳胶粘到靶托上;YSZ基片分别用丙酮、酒精、去离子水进行超声波清洗,清洗时间为5min、5min、10min;将清洗好的YSZ基片用氮气吹干,并用导电银浆粘到基片托上;将放有靶材的靶托和放有YSZ的基片托放入脉冲激光沉积系统的溅射室中,靶材和YSZ基底的间距控制在5cm;
S3、脉冲激光沉积系统的真空度为10-5Pa,温度为室温,激光光束的频率为8Hz,发射能量为200mJ,沉积脉冲数为8000;
S4、取出步骤S3所得的产物,将其在10-4Pa真空度下进行封管,并放入管式炉中以5℃/min的速率升温至1100℃,保温时间10h,得到单晶太阳能电池薄膜材料。
图2是本发明实施例1制备的BaZrS3薄膜的校准YSZ(002)取向测得的XRD图,图3是本发明实施例1制备的BaZrS3薄膜的校准YSZ(202)取向测得的XRD图,图2与图3显示BaZrS3的薄膜峰与标准Pnma图对应良好,可以看出在YSZ上已经形成质量良好的BaZrS3薄膜,图4是本发明实施例1制备的BaZrS3薄膜的校准BaZrS3(112)测得的Phi扫描图,发现在0-360度范围内出现4个峰,显示薄膜具有四重对称性,形成了良好的单晶薄膜BaZrS3。
图5是本发明实施例1制备的BaZrS3薄膜的光学吸收图谱,图谱显示出制备的BaZrS3薄膜的光学带隙在1.8eV左右;图6是本发明本发明实施例1制备的BaZrS3薄膜的PL图谱,从PL图谱可以看出,在约1.8eV的中可以观察到一个宽的PL峰。吸收和PL图谱结果表明,本发明实施例1制备的BaZrS3薄膜是一个理想的低带隙光伏材料,光学带隙在1.8eV左右,在光电应用方面具有理想的光学特性。
以上详细描述了本发明的较佳具体实施例。应当理解,本领域的普通技术无需创造性劳动就可以根据本发明的构思做出诸多修改和变化。因此,凡本技术领域中技术人员依本发明的构思在现有技术的基础上通过逻辑分析、推理或者有限的实验可以得到的技术方案,皆应在由权利要求书所确定的保护范围内。
Claims (6)
1.一种单晶太阳能电池薄膜材料的制备方法,其特征在于,包括如下步骤:
S1、以BaS粉末和ZrS2粉末按化学计量比为1:1为反应材料,将真空封好的靶材转移至管式炉中进行高温热处理,从室温加热至900-1000℃,加热速率7℃/min,保温15h,待炉内温度降至室温,得到BaZrS3靶材;
S2、将步骤S1中合成得到的BaZrS3靶材和清洗好的YSZ衬底放入脉冲激光沉积系统;
S3、对YSZ衬底进行真空室温沉积镀膜得到BaZrS3非晶薄膜;
S4、取出步骤S3所得的产物,将其在真空度下进行封管,并放入管式炉中以5-8℃/min的速率升温至900-1100℃,保温时间5-10h,得到BaZrS3单晶太阳能电池薄膜材料。
2.权利要求1所述的单晶太阳能电池薄膜材料的制备方法,其特征在于,步骤S1中的真空度为10-4Pa。
3.根据权利要求1所述的单晶太阳能电池薄膜材料的制备方法,其特征在于,步骤S2中合成好的BaZrS3靶材需用砂纸进行表面打磨,并用导电碳胶粘到靶托上;YSZ基片分别用丙酮、酒精、去离子水进行超声波清洗,清洗时间为5min、5min、10min;将清洗好的YSZ基片用氮气吹干,并用导电银浆粘到基片托上;将放有靶材的靶托和放有YSZ的基片托放入脉冲激光沉积系统的溅射室中,靶材和YSZ基底的间距控制在5-6cm。
4.根据权利要求1所述的单晶太阳能电池薄膜材料的制备方法,其特征在于,步骤S3中脉冲激光沉积系统的真空度为10-5Pa,温度为室温,激光光束的频率为8Hz,发射能量为200mJ,沉积脉冲数为8000。
5.权利要求1所述的单晶太阳能电池薄膜材料的制备方法,其特征在于,步骤S4中的的真空度为10-4Pa。
6.一种根据权利要求1-5任一项所述方法制备的单晶太阳能电池薄膜材料。
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