CN107230735B - 具有缓冲层的CdZnTe薄膜光电探测器的制备方法 - Google Patents
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Abstract
本发明涉及一种具有缓冲层的CdZnTe薄膜光电探测器的制备方法，属于薄膜光电探测器部件制造工艺技术领域。本发明的目的是通过在采用近空间升华法制备CdZnTe薄膜之前先引入缓冲层（ZnTe/CdTe），从而达到提高CdZnTe薄膜质量的目的，给CdZnTe薄膜在光电探测器设备中的实际应用提供了新的方案。本发明是一种具有缓冲层的CdZnTe薄膜光电探测器的制备方法,其特点在于基于高真空近空间升华与磁控溅射镀膜一体化工艺设备，以预处理过的单晶Si为衬底，先溅射ZnTe/CdTe作为缓冲层，再传输到升华腔内用CdZnTe单晶的粉末源沉积一层CdZnTe薄膜，之后对CdZnTe薄膜进行退火及腐蚀等后处理，并通过电子束沉积叉指型的金电极获得理想欧姆接触，最终制得薄膜光电探测器部件。
Description
技术领域
本发明涉及具有缓冲层的CdZnTe薄膜光电探测器的制备方法，属于属于光电探测器器件制造工艺技术领域。
背景技术
CdZnTe晶体是直接带隙的II-VI族化合物半导体，可以看作是由CdTe和ZnTe的固溶成。
CdZnTe禁带宽度可随着Zn含量的不同而从1.45eV到2.2eV变化，在室温下使用可以省去昂贵、复杂的冷却系统，可以降低整个系统的成本。CdZnTe的电阻率高因此在高温下也能有较小的漏电流，并且CdZnTe的极化效应比CdTe晶体要低很多，辐射探测衰减现象比CdTe弱，有利于探测。此外CdZnTe光灵敏度高，平均原子序数高，可以有较高的探测效率。
CdZnTe单晶在室温高能射线探测器中被认为最有潜力的的材料，具有较好的探测效率和能量分辨率。但是随着大面积探测器的不断发展，对CdZnTe单晶质量和尺寸的要求不断提高，使得晶体生长带来很大困难。对于大尺寸CdZnTe探测器的应用，CdZnTe薄膜相对于晶体具有优势。CdZnTe薄膜的制备技术简单，成本更低，最重要的是容易得到大面的CdZnTe薄膜。获得CdZnTe薄膜的方法有很多，如：热蒸发，磁控溅射，化学气相沉积，近空间升华法等。其中近空间升华法制备CdZnTe薄膜成本低、质量高、速度快，适用于大面积沉积薄膜是目前最有前途的方法，可以获得高质量、高电阻率的CdZnTe薄膜。
目前，近空间升华法制备的CdZnTe薄膜主要沉积在单晶硅、普通玻璃、FTO或者ITO涂层的玻璃上，这些衬底和CdZnTe薄膜之间存在较大的晶格失配，这样一定程度上限制了CdZnTe薄膜的质量提高和实际的器件应用。缓冲层是一种被用来减小薄膜与衬底减晶格失配的常用方法，但是在高质量CdZnTe薄膜的制备过程中，采用缓冲层的方法还非常少见。ZnTe和CdTe的晶格常数分别为6.11和6.48，非常接近于CdZnTe薄膜的晶格常数（接近于6.44）。因此我们通过引入ZnTe/CdTe作为缓冲层来减小CdZnTe薄膜与衬底之间的晶格失配，制备高质量探测器用CdZnTe薄膜。
发明内容
本发明的目的是通过在采用近空间升华法制备CdZnTe薄膜之前先引入缓冲层（ZnTe/CdTe），从而达到提高CdZnTe薄膜质量的目的，给CdZnTe薄膜在光电探测器设备中的实际应用提供了新的方案。
本发明采用如下技术方案。
本发明是一种具有缓冲层的CdZnTe薄膜光电探测器的制备方法，其特征在于该方法包括如下过程和步骤：
a. 衬底Si片的预处理：采用本征单晶Si片做为衬底，将衬底先用曲拉通去除表面的油污，再用去离子水、丙酮和乙醇分别超声清洗5~20分钟，去除衬底表面的有机物与杂质，最后将衬底放在在氢氟酸的稀释浓液中浸泡10~15分钟去除表面的SiO2，烘干后放入高真空近空间升华与磁控溅射镀膜设备的磁控溅射腔内；
b. 磁控溅射缓冲层：以Si为衬底采用磁控溅射法依次溅射ZnTe和CdTe薄膜作为CdZnTe薄膜生长的缓冲层；靶材分别为纯度为99.99%的ZnTe和CdTe；ZnTe和CdTe的溅射条件相同即溅射气氛为氩气，溅射气压为1~6 mTorr，溅射功率50~200 W,溅射时间20~100min；ZnTe和CdTe的膜厚分别在0.05~1 mm。缓冲层制备好以后，通过设备自带的机械手将衬底传输到近空间升华腔内；
c. 真空沉积CdZnTe薄膜：首先是CdZnTe单晶粉末升华源的准备，即采用移动加热法生长出质量好、成分均匀且Zn含量为2~20%的CdZnTe单晶；生长好的单晶被切片然后研磨成粉末做为升华源；然后是薄膜的生长：开机械泵抽真空保持升华腔内的气压在2Pa以下；加热升华源和衬底的温度分别为650 ℃和400 ℃；生长3 h后，关闭升华源和衬底的加热；冷却样品至室温；关机械泵，取出样品；薄膜的厚度在300 mm左右；
d. CdZnTe薄膜的退火及腐蚀：样品在氮气保护下慢速退火30~90 min，退火温度为300~450 ℃。将退火样品放在0.1~0.2%的溴甲醇浓液中腐蚀5~40 S，然后将样品依次放入无水甲醇和去离子水中清洗吹干；
e. 叉指电极的制备：通过光刻工艺等制作叉指电极掩膜板，利用掩膜板在样品的表面采用电子束蒸发法在样品的表面沉积金电极；然后在真空中退火15~45 min，退火温度为100~450 ℃，使得薄膜和电极之间形成良好的欧姆接触；最终制得薄膜光电探测器部件。
同现有的技术相比，本发明具有如下显著优点：
（1）采用高真空近空间升华与磁控溅射镀膜一体化工艺设备，通过机械手将样品从磁控溅射腔传到升华腔，避免在CdZnTe薄膜沉积前，缓冲层被污染，从而影响薄膜质量。
（2）在Si衬底和CdZnTe薄膜之间引入ZnTe/CdTe缓冲层，有效地减小了Si衬底和CdZnTe薄膜之间的晶格失配，提高了CdZnTe薄膜的质量，有有利于制备高性能的光电探测器件。
附图说明
图1为本发明具有缓冲层的CdZnTe薄膜光电探测器和一般CdZnTe薄膜光电探测器的结构示意图。
图2为本发明具有缓冲层的CdZnTe薄膜光电探测器和一般CdZnTe薄膜制备的光电探测器对X射线的IV响应图谱。
具体实施方式，现将本发明的具体实施例叙述于后。
实施例1
本实施例的制备过程和步骤如下：
a. 衬底Si片的预处理：采用本征单晶Si片做为衬底，将衬底先用曲拉通去除表面的油污，再用去离子水、丙酮和乙醇分别超声清洗10 min，去除衬底表面的有机物与杂质，最后在氢氟酸的稀释浓液中浸泡10 min去除表面的SiO2，烘干后放入高真空近空间升华与磁控溅射镀膜设备的磁控溅射腔内。
b. 磁控溅射缓冲层：以Si为衬底采用磁控溅射法依次溅射ZnTe和CdTe薄膜作为CdZnTe薄膜生长的缓冲层。靶材分别为纯度为99.99%的ZnTe和CdTe。ZnTe和CdTe的溅射条件相同即溅射气氛为氮气，溅射气压为6 mTorr，溅射功率150 W,溅射时间20 min。ZnTe和CdTe的膜厚分别在0.1 mm。缓冲层制备好以后，通过设备自带的机械手将衬底传输到升华腔内。
c. 真空沉积CdZnTe薄膜：首先是CdZnTe单晶粉末升华源的准备即采用移动加热法生长出质量好、成分均匀且Zn含量为10%的CdZnTe单晶。生长好的单晶被切片然后研磨成粉末做为升华源。然后是薄膜的生长，开机械泵抽真空保持升华腔内的气压在2Pa以下；加热升华源和衬底的温度分别为650 ℃和400 ℃；生长3 h后，关闭升华源和衬底的加热，冷却样品至室温，关机械泵，取出样品，薄膜的厚度在300 mm。
d. CdZnTe薄膜的退火及腐蚀：样品在氮气保护下慢速退火40 min，退火温度为350 ℃。将退火样品放在0.1%的溴甲醇浓液中腐蚀20 S，然后将样品依次放入无水甲醇和去离子水中清洗吹干。
e. 叉指电极的制备：通过光刻工艺等制作叉指电极掩膜板，利用掩膜板在样品的表面采用电子束蒸发法在样品的表面沉积金电极，然后在真空中退火30 min，退火温度为300 ℃，使得薄膜和电极之间形成良好的欧姆接触。最终制备薄膜光电探测器部件。
实施例2：
本实施例的制备过程和步骤如下：
a. 衬底Si片的预处理：采用本征单晶Si片做为衬底，将衬底先用曲拉通表面的油污，再用去离子水、丙酮和乙醇分别超声清洗10 min，去除衬底表面的有机物与杂质，最后在氢氟酸的稀释浓液中浸泡10 min去除表面的SiO2，烘干后放入高真空近空间升华与磁控溅射镀膜设备的磁控溅射腔内。
b. 磁控溅射缓冲层：以Si为衬底采用磁控溅射法依次溅射ZnTe和CdTe薄膜作为CdZnTe薄膜生长的缓冲层。靶材分别为纯度为99.99%的ZnTe和CdTe。ZnTe和CdTe的溅射条件相同即溅射气氛为氮气，溅射气压为6 mTorr，溅射功率150 W,溅射时间40 min。ZnTe和CdTe的膜厚分别在0.25 mm。缓冲层制备好以后，通过设备自带的机械手将衬底传输到升华腔内。
c. 真空沉积CdZnTe薄膜：首先是CdZnTe单晶粉末升华源的准备即采用移动加热法生长出质量好、成分均匀且Zn含量为10%的CdZnTe单晶。生长好的单晶被切片然后研磨成粉末做为升华源。然后是薄膜的生长，开机械泵抽真空保持升华腔内的气压在2Pa以下；加热升华源和衬底的温度分别为650 ℃和400 ℃；生长3 h后，关闭升华源和衬底的加热，冷却样品至室温，关机械泵，取出样品，薄膜的厚度在300 mm。
d. CdZnTe薄膜的退火及腐蚀：样品在氮气保护下慢速退火40 min，退火温度为350 ℃。将退火样品放在0.1%的溴甲醇浓液中腐蚀20 S，然后将样品依次放入无水甲醇和去离子水中清洗吹干。
e. 叉指电极的制备：通过光刻工艺等制作叉指电极掩膜板，利用掩膜板在样品的表面采用电子束蒸发法在样品的表面沉积金电极，然后在真空中退火30 min，退火温度为300 ℃，使得薄膜和电极之间形成良好的欧姆接触。最终制备薄膜光电探测器部件。
Claims (1)
1.一种具有缓冲层的CdZnTe薄膜光电探测器的制备方法，其特征具有以下的过程和步骤：
a.衬底Si片的预处理：采用本征单晶Si片做为衬底，将衬底先用曲拉通去除表面的油污，再用去离子水、丙酮和乙醇分别超声清洗5～20分钟，去除衬底表面的有机物与杂质，最后将衬底放在氢氟酸的稀释溶液中浸泡10～15分钟去除表面的SiO2，烘干后放入高真空近空间升华与磁控溅射镀膜设备的磁控溅射腔内；
b.磁控溅射缓冲层：以Si为衬底采用磁控溅射法依次溅射ZnTe和CdTe薄膜作为CdZnTe薄膜生长的缓冲层；靶材分别为纯度为99.99％的ZnTe和CdTe；ZnTe和CdTe的溅射条件相同，即溅射气氛为氩气，溅射气压为1～6mTorr，溅射功率50～200W,溅射时间20～100min；ZnTe和CdTe的膜厚分别在0.05～1μm；缓冲层制备好以后，通过设备自带的机械手将衬底传输到近空间升华腔内；
c.真空沉积CdZnTe薄膜：首先是CdZnTe单晶粉末升华源的准备，即采用移动加热法生长出质量好、成分均匀且Zn含量为2～20％的CdZnTe单晶；生长好的单晶被切片然后研磨成粉末做为升华源；然后是薄膜的生长，开机械泵抽真空保持升华腔内的气压在2Pa以下；加热升华源和衬底的温度分别为650℃和400℃；生长3h后，关闭升华源和衬底的加热；冷却样品至室温；关机械泵，取出样品；薄膜的厚度在300μm左右；
d.CdZnTe薄膜的退火及腐蚀：样品在氮气保护下慢速退火30～90min，退火温度为300～450℃；将退火样品放在0.1～0.2％的溴甲醇浓液中腐蚀5～40S，然后将样品依次放入无水甲醇和去离子水中清洗吹干；
e.叉指电极的制备：通过光刻工艺制作叉指电极掩膜板，利用掩膜板在样品的表面采用电子束蒸发法在样品的表面沉积金电极；然后在真空中退火15～45min，退火温度为100～450℃，使得薄膜和电极之间形成良好的欧姆接触；最终制得薄膜光电探测器部件。
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