CN104388894A - 脉冲激光沉积制备低带隙铁电光伏薄膜的方法 - Google Patents
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Abstract
本发明提供一种脉冲激光沉积制备低带隙铁电光伏薄膜的方法，具体步骤为：以Pt/Ti/SiO2/Si(100)作为衬底，依次用丙酮、无水乙醇、去离子水经超声波清洗器清洗10分钟，超声波工作频率40kHz，然后用氮气吹干后立即装入真空腔内，设定衬底温度为600～800℃、真空室氧压为0～5Pa、激光脉冲能量为100～500mJ、脉冲激光频率为1～20Hz，烧蚀陶瓷靶材得到低带隙薄膜产物。本发明为物理气相沉积法，其所选用的原料较少、经济、无污染，制备工艺简单、操作方便，易于生产，为开发基于铁电半导体的太阳能电池开辟了一种全新的途径。
Description
技术领域
本发明涉及一种脉冲激光沉积制备低带隙铁电光伏薄膜的方法。该方法采用脉冲激光沉积，一种物理气相沉积法，制备得到结晶性良好并且可吸收大部分可见光的低带隙铁电光伏薄膜，属于光伏材料与技术领域。
背景技术
作为铁电材料特征之一的自发极化在太阳能电池应用中具有巨大潜力，因为由光吸收产生的正电荷和负电荷(光生载流子)能在自发极化形成的内建电场作用下有效分离，这使得它们更容易被高效收集。但是，大多数已知的铁电材料都有比较宽的禁带，即它们只吸收构成太阳光谱一小部分的高能光子，例如目前被广泛研究的BiFeO3体系铁电光伏薄膜，最低带隙约为2.7eV，波长大于460nm的可见光都不能被其有效吸收。2013年，Ilya Grinberg等人采用常规的固态反应合成方法，利用廉价和无毒性的元素制成了单相氧化物固溶体[KNbO3]1-x[BaNi1/2Nb1/2O3-δ]x(Nature,503,509-512,DOI:10.1038/nature12622)，这类氧化物既具有铁电性质，还表现出了变化范围在1.1～3.8eV的直接带隙。在x＝0.1下，[KNbO3]1-x[BaNi1/2Nb1/2O3-δ]x的光电流密度比经典的铁电体(Pb,La)(Zr,Ti)O3材料大～50倍，光吸收能力比目前的铁电体材料高3至6倍。
到目前为止，尚未见文献报道制备(KNbO3)0.9(BaNi0.5Nb0.5O3)0.1(以下简称为KBNNO)铁电光伏薄膜材料的方法，本发明创新性地利用脉冲激光沉积(PLD)法制备(KNbO3)0.9(BaNi0.5Nb0.5O3)0.1(KBNNO)铁电光伏薄膜材料。通过控制脉冲激光能量、脉冲频率、沉积时间、沉积温度、沉积氧压等参数，在Pt/Ti/SiO2/Si(100)衬底上得到了结晶性良好的(KNbO3)0.9(BaNi0.5Nb0.5O3)0.1(KBNNO)薄膜，并且通过调节沉积氧压对禁带宽度进行调控，得到低带隙的铁电薄膜，它可吸收绝大部分可见光，为提高太阳能电池的光电转换效率提供了可能。
发明内容
本发明提供脉冲激光沉积制备低带隙铁电光伏薄膜的方法，它是一种物理气相沉积法，即：脉冲激光沉积法。一方面其弥补了目前(KNbO3)0.9(BaNi0.5Nb0.5O3)0.1(KBNNO)铁电光伏薄膜制备手段上的缺失，另一方面，相比于陶瓷块材，薄膜材料在太阳能电池器件中具有更为直接的用途。
本发明提供脉冲激光沉积制备低带隙铁电光伏薄膜的方法，包括以下步骤：
(1)将(KNbO3)0.9(BaNi0.5Nb0.5O3)0.1(KBNNO)陶瓷靶材和清洗后的衬底分别固定在靶台和样品台上装入真空室，调整样品台与靶台间距；
(2)调节样品台加热器功率，升温并稳定在生长低带隙薄膜所需的温度值；
(3)通过调节氧气进气角阀和旁抽阀，使真空室中的氧气压强稳定在生长低带隙薄膜所需的氧压值；
(4)根据设计的实验方案设定激光器的工作模式为恒能模式，并选择所需的激光脉冲能量、激光脉冲频率等参数；
(5)先启动样品台和靶台的自转，再开激光器高压，激光预溅射靶材3分钟，然后旋开样品台的挡板，开始沉积薄膜，一定时间后停止沉积并关闭激光器，关闭氧气进气角阀后让样品自然冷却至室温后再取出真空室。
本发明的步骤(1)中选用的衬底为Pt/Ti/SiO2/Si(100)基片，依次用丙酮、无水乙醇、去离子水经超声波清洗器清洗10分钟，超声波清洗器工作频率40kHz，然后用氮气吹干后立即装入真空腔内，并调节样品台与靶台间距为30～60mm。
本发明的步骤(2)中衬底温度为600～800℃。
本发明的步骤(3)中真空室的氧压为0～5Pa。
本发明的步骤(4)中激光脉冲能量为100～500mJ，激光脉冲频率为1～20Hz。
本发明的有益效果为：
1、本发明方法为物理气相沉积法，其所选用的原料较少、经济、无污染，制备工艺简单、操作方便，易于生产。
2、本发明利用物理气相沉积法，即脉冲激光沉积法，制备得到低带隙(KNbO3)0.9(BaNi0.5Nb0.5O3)0.1(KBNNO)铁电光伏薄膜。
3、确定适宜低带隙薄膜制备的各工艺参数，得到带隙约为1.5eV的低带隙(KNbO3)0.9(BaNi0.5Nb0.5O3)0.1(KBNNO)铁电光伏薄膜材料。该材料带隙是现有铁电光伏薄膜材料报道中的最低值之一，它可吸收绝大部分可见光，而目前被广泛研究的BiFeO3体系铁电光伏薄膜，最低带隙约为2.7eV，波长大于460nm的可见光都不能被其有效吸收。本发明方法为开发基于铁电体半导体的太阳能电池提供了一种全新的光吸收材料的制备手段。
附图说明
图1为本发明方法所制备的低带隙(KNbO3)0.9(BaNi0.5Nb0.5O3)0.1铁电光伏薄膜的X射线衍射(XRD)测试图谱；
图2为本发明方法所制备的低带隙(KNbO3)0.9(BaNi0.5Nb0.5O3)0.1铁电光伏薄膜的吸收系数平方(α2)与入射光子能量(hν)关系曲线。
具体实施方式
实施例1
采用Pt/Ti/SiO2/Si(100)作为衬底，依次用丙酮、无水乙醇、去离子水经超声波清洗器清洗10分钟，超声波清洗器工作频率40kHz，然后用氮气吹干后立即装入真空腔内。设定靶台与样品台间距为30mm、衬底温度为600℃、真空室氧压为0Pa、激光脉冲能量为100mJ、脉冲激光频率为1Hz、样品台和靶台自转速度分别为10r/min和5r/min、沉积时间为10分钟条件下，制备得到低带隙(KNbO3)0.9(BaNi0.5Nb0.5O3)0.1(KBNNO)铁电光伏薄膜。
实施例2
采用Pt/Ti/SiO2/Si(100)作为衬底，依次用丙酮、无水乙醇、去离子水经超声波清洗器清洗10分钟，超声波清洗器工作频率40kHz，然后用氮气吹干并立即装入真空腔内。设定靶台与样品台间距为30mm、衬底温度为700℃、真空室氧压为0.01Pa、激光脉冲能量为100mJ、脉冲激光频率为5Hz、样品台和靶台自转速度分别为10r/min和5r/min、沉积20分钟，制备得到低带隙(KNbO3)0.9(BaNi0.5Nb0.5O3)0.1(KBNNO)铁电光伏薄膜。
实施例3
采用Pt/Ti/SiO2/Si(100)作为衬底，依次用丙酮、无水乙醇、去离子水经超声波清洗器清洗10分钟，超声波清洗器工作频率40kHz，然后用氮气吹干并立即装入真空腔内。设定靶台与样品台间距为55mm、衬底温度为700℃、真空室氧压为0Pa、激光脉冲能量为300mJ、脉冲激光频率为5Hz、样品台和靶台自转速度分别为10r/min和5r/min、沉积时间为20分钟条件下，制备得到(KNbO3)0.9(BaNi0.5Nb0.5O3)0.1(KBNNO)铁电光伏薄膜。图2示出该薄膜吸收系数与入射光子能量关系曲线，从中可得知此KBNNO薄膜的禁带宽度(带隙)约为1.4eV，而目前被广泛研究的BiFeO3体系铁电光伏薄膜的最低带隙约为2.7eV，由此可知，本发明的KBNNO薄膜具有较窄的禁带宽度。
实施例4
采用Pt/Ti/SiO2/Si(100)作为衬底，依次用丙酮、无水乙醇、去离子水经超声波清洗器清洗10分钟，超声波清洗器工作频率40kHz，然后用氮气吹干并立即装入真空腔内。设定靶台与样品台间距为55mm、衬底温度为700℃、真空室氧压为0.1Pa、激光脉冲能量为300mJ、脉冲激光频率为5Hz、样品台和靶台自转速度分别为10r/min和5r/min、沉积时间为20分钟条件下，制备得到低带隙(KNbO3)0.9(BaNi0.5Nb0.5O3)0.1(KBNNO)铁电光伏薄膜。对得到的薄膜进行XRD测试，结果如图1所示，表明该低带隙KBNNO铁电光伏薄膜具有正交钙钛矿结构，结晶性良好并沿(101)方向择优取向生长，良好的结晶性能为其铁电性研究和在光电领域应用提供了可能。该薄膜吸收系数平方与入射光子能量关系曲线如图2所示，从中可得出其带隙约为1.5eV。
实施例5
采用Pt/Ti/SiO2/Si(100)作为衬底，依次用丙酮、无水乙醇、去离子水经超声波清洗器清洗10分钟，超声波清洗器工作频率40kHz，然后用氮气吹干并立即装入真空腔内。设定靶台与样品台间距为55mm、衬底温度为700℃、真空室氧压为0.3Pa、激光脉冲能量为300mJ、脉冲激光频率为5Hz、样品台和靶台自转速度分别为10r/min和5r/min、沉积时间为20分钟条件下，制备(KNbO3)0.9(BaNi0.5Nb0.5O3)0.1铁电光伏薄膜。所得到的薄膜结构如图1XRD图谱所示，该薄膜具有正交钙钛矿结构，结晶性良好并具有(101)择优取向；其禁带宽度可从图2所示的吸收系数平方与入射光子能量关系曲线得出，约为1.5eV。
实施例6
采用Pt/Ti/SiO2/Si(100)作为衬底，依次用丙酮、无水乙醇、去离子水经超声波清洗器清洗10分钟，超声波清洗器工作频率40kHz，然后用氮气吹干并立即装入真空腔内。设定靶台与样品台间距为55mm、衬底温度为700℃、真空室氧压为0.5Pa、激光脉冲能量为300mJ、脉冲激光频率为10Hz、样品台和靶台自转速度分别为10r/min和5r/min、沉积时间为60分钟条件下，制备得到低带隙(KNbO3)0.9(BaNi0.5Nb0.5O3)0.1铁电光伏薄膜。所得到的薄膜结构如图1XRD图谱所示，该薄膜具有正交钙钛矿结构，结晶性良好并具有(101)择优取向；其禁带宽度可从图2所示的吸收系数平方与入射光子能量关系曲线得出，约为1.6eV。
实施例7
采用Pt/Ti/SiO2/Si(100)作为衬底，依次用丙酮、无水乙醇、去离子水经超声波清洗器清洗10分钟，超声波清洗器工作频率40kHz，然后用氮气吹干并立即装入真空腔内。设定靶台与样品台间距为60mm、衬底温度为800℃、真空室氧压为0.5Pa、激光脉冲能量为300mJ、脉冲激光频率为10Hz、样品台和靶台自转速度分别为10r/min和5r/min、沉积时间为60分钟条件下，制备得到低带隙(KNbO3)0.9(BaNi0.5Nb0.5O3)0.1(KBNNO)铁电光伏薄膜。
实施例8
采用Pt/Ti/SiO2/Si(100)作为衬底，依次用丙酮、无水乙醇、去离子水经超声波清洗器清洗10分钟，超声波清洗器工作频率40kHz，然后用氮气吹干并立即装入真空腔内。设定靶台与样品台间距为60mm、衬底温度为800℃、真空室氧压为5Pa、激光脉冲能量为500mJ、脉冲激光频率为20Hz、样品台和靶台自转速度分别为10r/min和5r/min、沉积时间为100分钟条件下，制备得到低带隙(KNbO3)0.9(BaNi0.5Nb0.5O3)0.1(KBNNO)铁电光伏薄膜材料。
Claims (5)
1.脉冲激光沉积制备低带隙铁电光伏薄膜的方法，其特征在于，包括以下步骤：
(1)将(KNbO3)0.9(BaNi0.5Nb0.5O3)0.1陶瓷靶材和清洗后的衬底分别固定在靶台和样品台上装入真空室，调整样品台与靶台间距；
(2)调节样品台加热器功率，升温并稳定在生长低带隙薄膜所需的衬底温度值；
(3)通过调节氧气进气角阀和旁抽阀，使真空室中的氧气压强稳定在生长低带隙薄膜所需的氧压值；
(4)设定激光器的工作模式为恒能模式，并选择所需的激光脉冲能量、激光脉冲频率参数；
(5)先启动样品台和靶台的自转，再开启激光器高压，激光预溅射靶材3分钟，然后旋开样品台的挡板，开始沉积薄膜，薄膜沉积结束后关闭激光器、氧气进气角阀，样品自然冷却至室温后再取出真空室。
2.根据权利要求1所述的脉冲激光沉积制备低带隙铁电光伏薄膜的方法，其特征在于，步骤(1)中，选用的衬底为Pt/Ti/SiO2/Si(100)，将所述Pt/Ti/SiO2/Si(100)衬底依次用丙酮、无水乙醇、去离子水经超声波清洗器清洗10分钟，超声波清洗器工作频率40kHz，用氮气吹干衬底后立即装入真空腔内，并调节样品台与靶台间距为30～60mm。
3.根据权利要求1所述的脉冲激光沉积制备低带隙铁电光伏薄膜的方法，其特征在于，步骤(2)中，生长低带隙薄膜所需的衬底温度值为600～800℃。
4.根据权利要求1所述的脉冲激光沉积制备低带隙铁电光伏薄膜的方法，其特征在于，步骤(3)中，生长低带隙薄膜所需的氧压值为0～5Pa。
5.根据权利要求1所述的脉冲激光沉积制备低带隙铁电光伏薄膜的方法，其特征在于，步骤(4)中，激光脉冲能量为100～500mJ，激光脉冲频率为1～20Hz。
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