CN104576775B - 一种具有高绒度的fzo透明导电薄膜的制备方法 - Google Patents
一种具有高绒度的fzo透明导电薄膜的制备方法 Download PDFInfo
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Abstract
本发明公开的一种具有高绒度的FZO透明导电薄膜的制备方法，包括如下步骤：1）采用磁控溅射法制备氟掺氧化锌薄膜；2）将步骤1）的FZO薄膜浸入体积浓度为0.01~1.0%的腐蚀性溶液中刻蚀，取出后清洗并干燥；3）将经步骤2）处理的FZO薄膜再放入磁控溅射设备生长室中，进行等离子刻蚀10‑30min，获得具有高绒度的FZO薄膜。本发明采用磁控溅射法结合湿化学刻蚀、等离子刻蚀的方法制备FZO透明导电薄膜，所获得的薄膜具有较高的绒度，且电学性能明显提高，有利于其在太阳能电池中的应用，此外，本发明的制备方法工艺简单，重复性好，适用于大面积生长。
Description
技术领域
本发明涉及一种FZO透明导电薄膜的制备方法，尤其涉及一种具有高绒度的FZO透明导电薄膜的制备方法。
背景技术
目前，一般用SnO2:F（FTO）透明导电薄膜作为多晶或者非晶Si太阳能电池器件的前电极，通常会通过一定的腐蚀处理使FTO层具备一定的绒面效果，以此来增强光在电池器件中的散射，从而提高光的利用率。但是对于该种太阳能电池器件，目前仍存在一个重大的缺陷，即：在高氢稀释的等离子体作用下，氧化锡易被原子氢还原，大大降低透明导电膜的透过率，从而会显著降低电池器件的性能。
为了解决这一问题，新的透明导电膜开始被研究，以代替FTO在电池器件中的应用。目前较为理想的半导体材料是氧化锌，氧化锌不仅在氢气等离子体条件下很稳定，而且其透光率和电学性能都非常优异。基于上述两方面的优势，ZnO基薄膜完全能够与FTO相媲美，甚至更佳。本征氧化锌的主要问题是电导率不够高。为了解决这一问题，人们采用掺杂的方法来增加其电导率。常用的掺杂元素是Al、Ga、In、B、F等。
理论研究表明，F是ZnO的一种良好的n型掺杂剂，FO的施主能级距导带底仅为0.08eV，比Al(0.12eV)更小。由ZnO的能带结构可知，价带最高能级主要是由O2p轨道组成，当F以替位形式占据O格点时主要是对价带产生微扰，对导带电子的散射作用小，有利于提高电子迁移率。另外,不像ZnO的金属阳离子掺杂，F是非电学活性的，其扩散到a-Si:H薄膜中不会恶化太阳能电池的性能，表明掺F的ZnO（FZO）透明导电薄膜更适合于在a-Si:H薄膜太阳能电池中应用。对于金属掺杂的 ZnO 薄膜来说，其等离子体频率相对较低（因为载流子浓度高）所以对于波长通常在 1000nm 的光波，都会出现明显的吸收，导致透过率下降，使得其在太阳电池中的应用前景受到影响。而 ZnO:F 对应的等离子波长为 2μm，因此用ZnO:F 材料制备的透明导电薄膜在2000nm 处仍有较高的透过率。
为了提高ZnO基太阳能器件的性能，必须通过刻蚀方法增强ZnO表面的粗糙度。一般常用的腐蚀剂包括HF、HCl、HNO3、NaOH、NH4Cl等，但是这样得到FZO薄膜虽然绒度增加，但是电学性能会出现较大幅度的下降，因此有必要采用新的方法来提高ZnO基薄膜的绒面效果，使其在提高散射能力的同时仍具有较高的电学性能。
发明内容
本发明的目的是提供一种电学性能良好且工艺简单的具有高绒度的FZO透明导电薄膜的制备方法。
本发明的具有高绒度的FZO透明导电薄膜的制备方法，包括如下步骤：1）制备氟掺氧化锌薄膜：将洁净的衬底放入磁控溅射设备生长室内，以Zn1-xFxO陶瓷靶为靶材，0<x≤0.3，抽真空至真空度至少为5×10-6Torr，加热衬底至25～500℃，向生长室中通入Ar，并调节生长气压至1~20mTorr，溅射功率为50～200W，生长15~60min，获得FZO薄膜；
2）湿化学刻蚀：将步骤1）的FZO薄膜浸入体积浓度为0.01 ~ 1.0 %的腐蚀性溶液中保持1~60s，取出后清洗并干燥；
3）等离子刻蚀：将经步骤2）处理的FZO薄膜放入磁控溅射设备生长室中，抽真空至真空度至少为5×10-6Torr，加热衬底至20～200℃，向生长室内按流量比为100:5-30通入Ar和H2，调节工作气压至10~50Pa，溅射功率为20-100W，进行等离子刻蚀10-30min，获得具有高绒度的FZO薄膜。
上述技术方案中，所述的衬底为玻璃、硅片、PC（聚碳酸酯）、PET（聚对苯二甲酸乙二酯）、PI（聚酰亚胺）或PMMA（聚甲基丙烯酸甲酯）。
步骤2）中所述的腐蚀剂溶液为HCl溶液、HF溶液、NaOH溶液、HNO3溶液或NH4Cl溶液。
本发明的有益效果是：本发明采用磁控溅射法结合湿化学刻蚀、等离子刻蚀的方法制备FZO透明导电薄膜，所获得的薄膜具有较高的绒度，绒度可高达50-60%，能够对可见光进行有效的散射，此外，本发明采用的Ar/H2等离子处理，一方面等离子体轰击薄膜表面进一步增大薄膜绒度，另一方面H掺入其中变成替代氧位的HO，形成浅施主能级，使得薄膜的导电性能明显提高，有利于其在太阳能电池中的应用，本发明的制备方法工艺简单，重复性好，适用于大面积生长。
附图说明
图1为实施例1中步骤2所获得的FZO薄膜的扫描图。
图2 为实施例1中步骤3所获得的FZO薄膜的扫描图。
图3为实施例1中步骤2的FZO薄膜与步骤3所获得的FZO薄膜的烟雾度对比图。
图4为实施例1中步骤2的FZO薄膜与步骤3所获得的FZO薄膜分别作为非晶硅太阳能电池前电极时的电池量子效率对比图。
具体实施方式
下面结合附图及具体实施例对本发明做进一步阐述。
实施例1
1) 将洁净的玻璃片放入磁控溅射设备生长室内，以Zn1-xFxO陶瓷靶为靶材，x=0.03，抽真空至真空度至少为5×10-6Torr，加热衬底至300℃，向生长室中通入Ar，并调节生长气压至8mTorr，溅射功率为100W，生长60min，获得厚度为700nm左右的FZO薄膜；
2) 将FZO薄膜放入体积浓度为0.5%的HCl溶液中静置15s，取出后清洗并干燥；获得的FZO薄膜的SEM图如图1所示；
3) 将步骤2)中得到的FZO薄膜重新放入磁控溅射设备的腔体，打开真空系统，抽真空至真空度下降至5×10-6Torr，加热衬底至200℃，向腔体中按流量比100:10通入Ar和H2，调节腔体内气压到20Pa，开启衬底电源，设置溅射功率为80W，进行等离子刻蚀20min，获得具有高绒度的FZO薄膜，其SEM图如图2所示；
表1为步骤2所得的FZO薄膜及步骤3所得的FZO薄膜的电学性能的对比，可知经两种刻蚀方法结合处理的FZO薄膜具有更好的电学性能。
表1
通过图1和图2的对比可以看出，经湿化学刻蚀及等离子刻蚀的FZO薄膜明显比仅经湿化学刻蚀的FZO薄膜表面更为粗糙，图3为步骤2所得的FZO薄膜及步骤3所得的FZO薄膜的烟雾度对比图，图4为其分别作为非晶硅太阳能电池前电极时的量子效率对比图，可以看出对于人们普遍利用的低于600nm的光来说，经两种刻蚀方法结合处理的FZO薄膜，其烟雾度更高，表明其光学散射能力更强，且将其作为太阳能电池前电极时，电池的量子效率更高。
实施例2
1) 将洁净的硅片放入磁控溅射设备生长室内，以Zn1-xFxO陶瓷靶为靶材，x=0.3，抽真空至真空度至少为5×10-6Torr，加热衬底至500℃，向生长室中通入Ar，并调节生长气压至20mTorr，溅射功率为50W，生长15min，获得FZO薄膜；
2) 将FZO薄膜放入体积浓度为1%的NH4Cl溶液中静置1s，取出后清洗并干燥；
3) 将步骤2)中得到的FZO薄膜重新放入磁控溅射设备的腔体，打开真空系统，抽真空至真空度下降至5×10-6Torr，加热衬底至200℃，向腔体中按流量比100:5通入Ar和H2，调节腔体内气压到10Pa，开启衬底电源，设置溅射功率为100W，进行等离子刻蚀30min，获得具有高绒度的FZO薄膜。
实施例3
1) 将洁净的PC放入磁控溅射设备生长室内，以Zn1-xFxO陶瓷靶为靶材，x=0.3，抽真空至真空度至少为5×10-6Torr，加热衬底至25℃，向生长室中通入Ar，并调节生长气压至1mTorr，溅射功率为200W，生长60min，获得FZO薄膜；
2) 将FZO薄膜放入体积浓度为0.01%的HNO3溶液中静置60s，取出后清洗并干燥；
3) 将步骤2)中得到的FZO薄膜重新放入磁控溅射设备的腔体，打开真空系统，抽真空至真空度下降至5×10-6Torr，加热衬底至20℃，向腔体中按流量比100:30通入Ar和H2，调节腔体内气压到50Pa，开启衬底电源，设置溅射功率为20W，进行等离子刻蚀10min，获得具有高绒度的FZO薄膜。
Claims (3)
1.一种具有高绒度的FZO透明导电薄膜的制备方法，其特征在于包括如下步骤：
1）制备氟掺氧化锌薄膜：将洁净的衬底放入磁控溅射设备生长室内，以Zn1-xFxO陶瓷靶为靶材，0<x≤0.3，抽真空至真空度至少为5×10-6Torr，加热衬底至25～500℃，向生长室中通入Ar，并调节生长气压至1~20mTorr，溅射功率为50～200W，生长15~60min，获得FZO薄膜；
2）湿化学刻蚀：将步骤1）的FZO薄膜浸入体积浓度为0.01 ~ 1.0 %的腐蚀性溶液中保持1~60s，取出后清洗并干燥；
3）等离子刻蚀：将经步骤2）处理的FZO薄膜放入磁控溅射设备生长室中，抽真空至真空度至少为5×10-6Torr，加热衬底至20～200℃，向生长室内按流量比为100:5-30通入Ar和H2，调节工作气压至10~50Pa，溅射功率为20-100W，进行等离子刻蚀10-30min，获得具有高绒度的FZO薄膜。
2.根据权利要求1的具有高绒度的FZO透明导电薄膜的制备方法，其特征在于所述的衬底为玻璃、硅片、PC、PET、PI或PMMA。
3.根据权利要求1的具有高绒度的FZO透明导电薄膜的制备方法，其特征在于步骤2）中所述的腐蚀剂溶液为HCl溶液、HF溶液、NaOH溶液、HNO3溶液或NH4Cl溶液。
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