CN110473771B - 直接转换x射线探测材料的制备方法 - Google Patents
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Abstract
本发明公开了一种直接转换X射线探测材料的制备方法，用于解决现有方法难以直接在TFT直接沉积CdZnTe多晶薄膜的技术问题。技术方案是采用布里奇曼法生长Cd1‑xZnxTe多晶锭切片作为生长源。将TFT衬底和生长源放入生长腔室，通过石英柱子调整好生长源与衬底之间的距离，关闭炉门，先开启机械泵抽真空，使腔室内真空度小于10pa，开启分子泵调节室内气压。开启水冷和温度控制系统，缓慢升温到设定温度，低温形核，采取重复生长方式，防止TFT衬底损坏，生长结束后，缓慢降温到一定温度然后自然冷却，由于采用了低温形核和重复生长方式，解决了背景技术方法难以直接在TFT衬底上真空沉积CdZnTe多晶薄膜问题。
Description
技术领域
本发明涉及一种X射线探测材料的制备方法，特别涉及一种直接转换X射线探测材料的制备方法。
背景技术
随着数字化时代的发展，常规X射线成像技术也在向数字化发展。传统的胶片-扫描仪已经被数字化X摄影技术(Digital Radiography，简称DR)所取代。DR以其更快的成像速度、更便捷的操作、更高的成像分辨率等显著优点，成为数字X摄影技术的主导方向，DR的技术核心是平板探测器(Flat panel detector，简称FPD)，按能量转换方式可以分为间接转换平板探测器和直接转换平板探测器。目前FPD材料主要有闪烁体和半导体非晶硒。以碘化铯、碘化钠闪烁体为代表的间接转换材料由于要经过X射线—可见光—电信号的转变，可见光的散射会造成空间分辨率的下降。直接接转换材料非晶硒具有很高的空间分辨率，但是其稳定性受温度波动影响大。FPD的发展急需要一种可以室温工作、高灵敏、高空间分辨的材料，长远来看，直接转换模式的高Z半导体材料是未来平板探测器的发展方向。
Cd1-xZnxTe(简称为CZT)是从碲化镉(CdTe)晶体发展而来的一种新型Ⅱ－Ⅵ固体化合物半导体。具有较大的禁带宽度(Eg随x在1.4～2.26可调)、较高的电阻率(室温下ρ>1010Ω·cm)、优异的载流子传输特性(电子迁移率μe>1000cm2/V·s，寿命τe>10-5s)、工作时漏电流小、噪声较低等优良特性，是制备室温X射线探测器的理想材料。但是由于CZT单晶成本昂贵，尺寸受限制，这影响了CZT在平板探测器上的发展。相比多晶薄膜，外延对工艺要求高，并且为了保证晶格匹配，必须选择价格昂贵的GaAs作为衬底材料，不符合CZT薄膜探测器工业化低成本的要求，采用近空间升华技术可以获取大面积的CdZnTe多晶薄膜，而均匀、致密的CdZnTe多晶薄膜可以替代非晶硒成为新的直接转换X射线探测材料。“Tokuda S,Kishihara H,AdachiS,et al.Preparation and characterization of polycrystallineCdZnTe films for large-area,high-sensitivity X-ray detectors.Journal ofMaterials Science:Materials in Electronics,2004,15(1):1-8.”日本岛津公司的Stoshi Tokuda等人用CSS法在氧化铝上沉积CdZnTe多晶薄膜，将CdZnTe多晶薄膜倒装在TFT上制成探测器，但此方法存在成本高，厚度不均匀，并且难以直接在TFT直接沉积CdZnTe多晶薄膜。
发明内容
为了克服现有方法难以直接在TFT直接沉积CdZnTe多晶薄膜的不足，本发明提供一种直接转换X射线探测材料的制备方法。该方法采用布里奇曼法生长出Cd1-xZnxTe多晶锭，将Cd1-xZnxTe多晶锭切成大小厚度一样的切片作为生长源。将TFT衬底和生长源放入生长腔室，通过石英柱子调整好生长源与衬底之间的距离，关闭炉门，先开启机械泵抽真空，使腔室内真空度小于10pa，开启分子泵调节室内气压。开启水冷和温度控制系统，缓慢升温到设定温度，低温形核，采取重复生长方式，防止TFT衬底损坏，生长结束后，缓慢降温到一定温度然后自然冷却，由于采用了低温形核和重复生长方式，解决了背景技术方法难以直接在TFT衬底上真空沉积CdZnTe多晶薄膜问题。
本发明解决其技术问题所采用的技术方案：一种直接转换X射线探测材料的制备方法，其特点是包括以下步骤：
步骤一、将TFT基板用丙酮、乙醇和去离子水各超声清洗10～20分钟，去除表面杂质和有机物，最后用氮气吹干放入真空箱中备用。
步骤二、将高纯的Cd、Zn、Te放入石英管中，采用布里奇曼法生长出Cd1-xZnxTe多晶锭切片，将生长好的Cd1-xZnxTe多晶体切片作为生长源，使用前进行砂纸磨抛处理，去除表面氧化物，最后用酒精、丙酮、蒸馏水各清洗10～20分钟，氮气吹干，放入干燥箱中备用。
步骤三、将生长源和TFT基板从干燥箱和真空箱取出，分别放到用石英柱子支撑的石墨圆盘上和AlN圆盘上，通过石英柱子调控源基距为5～10mm，先开机械泵抽真空，气压抽到5～10Pa，启动分子泵，生长过程通入氩气调节室内气压。然后开启水冷和启动温度系统，分别将生长源和TFT基板升温到200～300℃和50～100℃，预热30min，最后将生长源和TFT基板分别缓慢加热到600～720℃和200～300℃，升温速度10℃/min，生长时间1～2h，然后将生长源温度缓慢降温到200～300℃，保温30min，再缓慢加热到600～700℃，生长时间2h，生长结束后TFT基板以1～2℃/min的降温速率缓慢降到100℃，然后自然冷却到室温，得到X射线探测材料。
本发明的有益效果是：该方法采用布里奇曼法生长出Cd1-xZnxTe多晶锭，将Cd1- xZnxTe多晶锭切成大小厚度一样的切片作为生长源。将TFT衬底和生长源放入生长腔室，通过石英柱子调整好生长源与衬底之间的距离，关闭炉门，先开启机械泵抽真空，使腔室内真空度小于10pa，开启分子泵调节室内气压。开启水冷和温度控制系统，缓慢升温到设定温度，低温形核，采取重复生长方式，防止TFT衬底损坏，生长结束后，缓慢降温到一定温度然后自然冷却，由于采用了低温形核和重复生长方式，解决了背景技术方法难以直接在TFT衬底上真空沉积CdZnTe多晶薄膜问题。
下面结合附图和具体实施方式对本发明作详细说明。
附图说明
图1是本发明方法实施例1生长的CdZnTe多晶薄膜在不同剂量的X射线下的光电流台阶图。
图2是本发明方法实施例1生长的CdZnTe多晶薄膜的厚度分布图。
具体实施方式
以下实施例参照图1-2。
实施例1：
(1)将TFT基板用丙酮、乙醇、去离子水各超声清洗15分钟，去除表面杂质和有机物，最后用氮气吹干放入真空箱中备用。
(2)将高纯的Cd、Zn、Te放入石英管中，采用布里奇曼法生长出质量好、成分分布相对均匀、无大块Te夹杂的Cd1-xZnxTe多晶锭切片，其中Zn含量可调，将生长好的晶体切片作为生长源，使用前进行砂纸磨抛处理，去除表面氧化物，最后用酒精、丙酮、蒸馏水各清洗15分钟，氮气吹干，放入干燥箱中备用。
(3)将步骤(1)清洗的TFT和步骤(2)制备的原料，从干燥箱和真空箱取出，分别放到用石英柱子支撑的石墨圆盘上和AlN圆盘上，通过石英柱子调控源基距为5mm，先开机械泵抽真空，气压抽到8帕，启动分子泵，生长过程可通入氩气调节室内气压。然后开启水冷和启动温度系统，分别将生长源和衬底升温到250℃和70℃，预热30min，最后将生长源和衬底分别缓慢加热到650℃和200℃，升温速度5℃/min，生长时间2h，然后将源温缓慢降温到250℃，保温30min，缓慢加热到650℃，生长时间2h，生长结束后衬底以1℃/min的降温速率缓慢降到100°，然后自然冷却到室温，薄膜的平均厚度266um，符合用作平板探测器的厚度，生长源可重复性利用。
从图1中可以看出，在不同剂量下X射线具有良好的响应，光电流与X射线剂量成正比例关系增加且平台平稳，适用于平板探测器。
从图2中可以看出，本实施例生长的CdZnTe多晶薄膜厚度分布均匀，最高和最低相差25um。
实施例2：
(1)将TFT基板用丙酮、乙醇、去离子水各超声清洗20分钟，去除表面杂质和有机物，最后用氮气吹干放入真空箱中备用。
(2)将高纯的Cd、Zn、Te放入石英管中，采用布里奇曼法生长出质量好、成分分布相对均匀、无大块Te夹杂的Cd1-xZnxTe多晶锭切片，其中Zn含量可调，将生长好的晶体切片作为生长源，使用前进行砂纸磨抛处理，去除表面氧化物，最后用酒精、丙酮、蒸馏水各清洗20分钟，氮气吹干，放入干燥箱中备用。
(3)将步骤(1)清洗的TFT和步骤(2)制备的原料，从干燥箱和真空箱取出，分别放到用石英柱子支撑的石墨圆盘上和AlN圆盘上，通过石英柱子调控源基距为10mm，先开机械泵抽真空，气压抽到10帕，启动分子泵，生长过程可通入氩气调节室内气压。然后开启水冷和启动温度系统，分别将生长源和衬底升温到300℃和100℃，预热30min，最后将生长源和衬底分别缓慢加热到700℃和250℃，升温速度7℃/min，生长时间1h，然后将源温缓慢降温到300℃，保温30min，缓慢加热到700℃，生长时间2h，生长结束后衬底以1℃/min的降温速率缓慢降到100°，然后自然冷却到室温。
实施例3：
(1)将TFT基板用丙酮、乙醇、去离子水各超声清洗10分钟，去除表面杂质和有机物，最后用氮气吹干放入真空箱中备用。
(2)将高纯的Cd、Zn、Te放入石英管中，采用布里奇曼法生长出质量好、成分分布相对均匀、无大块Te夹杂的Cd1-xZnxTe多晶锭切片，其中Zn含量可调，将生长好的晶体切片作为生长源，使用前进行砂纸磨抛处理，去除表面氧化物，最后用酒精、丙酮、蒸馏水各清洗10分钟，氮气吹干，放入干燥箱中备用。
(3)将步骤(1)清洗的TFT和步骤(2)制备的原料，从干燥箱和真空箱取出，分别放到用石英柱子支撑的石墨圆盘上和AlN圆盘上，通过石英柱子调控源基距为8mm，先开机械泵抽真空，气压抽到5帕，启动分子泵，生长过程可通入氩气调节室内气压。然后开启水冷和启动温度系统，分别将生长源和衬底升温到200℃和50℃，预热30min，最后将生长源和衬底分别缓慢加热到600℃和300℃，升温速度10℃/min，生长时间1.5h，然后将源温缓慢降温到250℃，保温30min，缓慢加热到680℃，生长时间3h，然后将源温缓慢降温到200℃，保温30min，缓慢加热到600℃，生长时间2h，生长结束后衬底以1℃/min的降温速率缓慢降到100°，然后自然冷却到室温。
Claims (1)
1.一种直接转换X射线探测材料的制备方法，其特征在于包括以下步骤：
步骤一、将TFT基板用丙酮、乙醇和去离子水各超声清洗10～20分钟，去除表面杂质和有机物，最后用氮气吹干放入真空箱中备用；
步骤二、将高纯的Cd、Zn、Te放入石英管中，采用布里奇曼法生长出Cd1-xZnxTe多晶锭切片，将生长好的Cd1-xZnxTe多晶体切片作为生长源，使用前进行砂纸磨抛处理，去除表面氧化物，最后用酒精、丙酮、蒸馏水各清洗10～20分钟，氮气吹干，放入干燥箱中备用；
步骤三、将生长源和TFT基板从干燥箱和真空箱取出，分别放到用石英柱子支撑的石墨圆盘上和AlN圆盘上，通过石英柱子调控源基距为5～10mm，先开机械泵抽真空，气压抽到5～10Pa，启动分子泵，生长过程通入氩气调节室内气压；然后开启水冷和启动温度系统，分别将生长源和TFT基板升温到200～300℃和50～100℃，预热30min，最后将生长源和TFT基板分别缓慢加热到600～720℃和200～300℃，升温速度10℃/min，生长时间1～2h，然后将生长源温度缓慢降温到200～300℃，保温30min，再缓慢加热到600～700℃，生长时间2h，生长结束后TFT基板以1～2℃/min的降温速率缓慢降到100℃，然后自然冷却到室温，得到X射线探测材料。
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