CN115274921A - 基于ATe3O8单晶的X射线探测器及其制备方法 - Google Patents
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Abstract
本发明涉及基于ATe3O8单晶的X射线探测器及其制备方法，将ATe3O8单晶顶面溅射金属金作为正极，在该单晶底面溅射金属金作为负极，从而得到基于ATe3O8单晶的X射线探测器。相比于现有的单晶X射线探测器，本发明的探测器制备过程更简单，成本更低。得到的探测器可以实现高的灵敏度，超低的检测线、极好的稳定性、高迁移率寿命积，低暗电流漂移和更高的热稳定性。
Description
技术领域
本发明涉及基于ATe3O8单晶的X射线探测器及其制备方法，属于X射线探测器领域。
背景技术
近年来，X射线探测器在工业无损检测、安检、医学检验、科学研究和太空探索等领域有着重要而广泛的应用。根据光电转化过程的不同，X射线探测器可以分为间接型X射线探测器和直接型X射线探测器。相比间接型X射线探测器，直接型X射线探测器中光电转换层直接将X射线转化为电信号，可以实现更好的空间分辨率和探测最低限制。高探测灵敏度和低探测极限被认为是X射线探测器的关键指标，在实际应用中需要减少总的X射线照射剂量。低检测线可大大降低常规医学检查中与辐射相关的健康风险。高电阻率有利于降低X射线探测器的暗电流，从而更容易获得低检测线的X射线探测器。并且高灵敏度的X射线探测器也可以通过低剂量成像来减小辐射危险。而引入含孤对电子的阳离子可以提高X射线探测器的灵敏度。优异的半导体X射线探测器需要材料同时具备高的光吸收系数、高迁移率寿命(μτ)、高电阻率、合适的带隙，以及稳定的物理和化学性能和优良的晶体生长习性。而目前，有价值的直接型X射线探测材料包括非晶态硒(α-Se)，硅，CdZnTe和钙钛矿，然而，这些材料在晶体生长中都会存在固有的缺陷或持续的未解决的问题。因此，探索具有综合性能的新型X射线探测材料已经成为当今材料领域的热点。
重金属碲具有丰富的构型，包括TeO3、TeO4、TeO5和TeO6多面体。亚碲酸盐(Te4+)的电子结构为5s2p0，在最外层的电子轨道上有两个未成键的电子。在高能X射线下，亚碲酸盐(Te4+)的存在有望提供更多的电子-空穴对，从而提高X射线探测器的灵敏度。此外，Te4+阳离子的引入很可能保留由孤对电子的s轨道引起的反键特性。氧化物晶体表现出稳定的物理化学性质和良好的晶体生长习性，通过助熔剂法可以生长出高质量的氧化物晶体。因此，亚碲酸盐氧化物晶体有望成为X射线探测器的理想材料。
发明内容
针对现有技术的不足，本发明提供一种基于ATe3O8单晶的X射线探测器及其制备方法。本发明的X射线探测器实现了高灵敏度和超低检测限。
本发明是通过以下技术方案实现的：
基于ATe3O8单晶的X射线探测器的制备方法，包括步骤：
将ATe3O8单晶顶面溅射金属金作为正极，在该单晶底面溅射金属金作为负极，从而得到基于ATe3O8单晶的X射线探测器。
根据本发明优选的，ATe3O8单晶为正方体形状，边长为4mm，厚度为1mm。
根据本发明优选的，在制备X射线探测器之前，先将ATe3O8单晶在X射线定向仪上进行定向，之后进行晶体切割，切割速度为0.1mm/h，最后将切割后的ATe3O8晶片进行抛光处理，抛光工艺如下：首先采用1000目砂纸进行手工粗抛10分钟，之后采用7000目砂纸进行手工粗抛15分钟，最后采用9091超细纤维布作为抛光垫，以0.05μmAl2O3抛光粉和0.5g去离子水作为抛光液，进行抛光10分钟。
X射线定向仪为丹东辽东射线有限公司YX-2型X射线定向仪，现有技术。
晶体切割采用沈阳科晶自动化设备有限公司STX-202A型金刚石线切割机进行，现有技术。
根据本发明优选的，顶面金电极的厚度为50-150nm，底面金电极的厚度为50-150nm。
根据本发明优选的，所述的ATe3O8单晶，A＝Ti，Zr或Sn。
根据本发明优选的，所述的ATe3O8单晶为TiTe3O8，ZrTe3O8或SnTe3O8。
根据本发明优选的，所述的ATe3O8单晶是按如下方法制备得到：
将纯相ATe3O8多晶粉末置于助熔剂体系中，混合均匀，放置铂金坩埚中，升温使之完全熔化，搅拌混合均匀，降温至饱和点，下入籽晶并转动，以0.01-5℃的速率降温使晶体生长，生长周期为15-30天。
进一步优选的，纯相ATe3O8多晶粉末为TiO2、ZrO2或者SnO2与TeO2按化学计量比混合得到的混合物。
进一步优选的，助熔剂体系为Li2CO3-TeO2。
根据本发明优选的，纯相ATe3O8多晶粉末与助熔剂体系的质量比为10-24％。
根据本发明优选的，籽晶为(100)方向，转速速度30rpm。
本发明通过助熔剂法生长得到ATe3O8单晶，接着通过溅射方式制作Au电极，完成基于ATe3O8单晶的X射线探测器的制备。与现有技术相比，本发明具有如下优点：
1、本发明基于ATe3O8单晶的X射线探测器具有高的灵敏度和超低的检测线，此外，由于其高的热稳定性，SnTe3O8单晶X射线探测器在高温下也具有优异的X射线探测性能。
2、本发明基于ATe3O8单晶的X射线探测器采用金属Au作为X射线探测器的正极和负极，有效地提升性能、简化器件制作工艺，且降低成本。
3、本发明采用的ATe3O8单晶结晶性好、形貌规整，具有高X射线吸收系数、合适的带隙、高的电阻率、高迁移率寿命积、低暗电流漂移、更好的热稳定性等优势，因而得到的X射线探测器可以实现高的灵敏度，超低的检测线和极好的稳定性。
4、本发明采用助熔剂法制备ATe3O8(A＝Ti，Zr和Sn)单晶，制备工艺简单、通用，且成本低。制备出的单晶质量较高，单晶无裂纹，晶莹剔透，单晶内部无明显的缺陷。
附图说明
图1为ATe3O8(A＝Ti，Zr和Sn)单晶的实物照片；
图2为ATe3O8(A＝Ti，Zr和Sn)单晶的XRD图；
图3为基于ATe3O8(A＝Ti，Zr和Sn)单晶的X射线探测器的结构示意图；
图4为基于ATe3O8(A＝Ti，Zr和Sn)单晶的X射线探测器的X射线吸收系数；
图5为基于ATe3O8(A＝Ti，Zr和Sn)单晶的X射线探测器的不同剂量下的光电流曲线；
图6为基于ATe3O8(A＝Ti，Zr和Sn)单晶的X射线探测器的灵敏度测试图；
图7为基于ATe3O8(A＝Ti，Zr和Sn)单晶的X射线探测器的检测线测试图；
图8为基于ATe3O8(A＝Ti，Zr和Sn)单晶的X射线探测器的暗电流漂移曲线图。
具体实施方式
以下结合附图对本发明涉及的ATe3O8(A＝Ti，Zr和Sn)单晶X射线探测器的具体实施方案进行详细地说明。
实施例1：
(1)SnTe3O8单晶的制备：
将原料SnO2和TeO2按化学计量比配料，混合均匀，直接加入到助熔剂体系Li2CO3-TeO2中，装入容积为Φ50mm×70mm的铂金坩埚中，升温至原料熔化并形成均一溶液；降温至饱和点，此时把预热过的籽晶下入溶液中，并以0.01-3℃/h的降温速率降温，生长周期15天，即可得到块状SnTe3O8单晶，记作STO；定向加工(100)晶片(图1)，测试其X射线衍射图，与理论计算一致(图2)，证明得到的是立方晶系的晶体；
(2)基于SnTe3O8单晶的X射线探测器的制备：
选取SnTe3O8单晶的(100)晶片上下对应的平面，两面利用溅射法沉积Au电极，电极厚度为100nm；制得结构为Au/SnTe3O8单晶/Au的X射线探测器(图3)。
实验例1
120keV X射线产生的光电流和探测器的X射线剂量率的关系如表1所示。
表1. 120keV X射线能量下光电流和剂量率关系
实施例1制备的基于SnTe3O8单晶的X射线探测器在不同剂量下的光电流曲线如图5所示。
实施例1制备的基于SnTe3O8单晶的X射线探测器X射线能量下的灵敏度如图6所示，SnTe3O8单晶X射线探测器的灵敏度为436μC Gyair -1cm-2，SnTe3O8单晶X射线探测器在高温448K的灵敏度为617μC Gyair -1cm-2；说明SnTe3O8单晶X射线探测器在高温下也具有优异的X射线探测性能。
实施例1制备的基于SnTe3O8单晶的X射线探测器的检测线如图7所示，SnTe3O8单晶X射线探测器的最低检测限为8.19nGyair s-1。
实施例1制备的基于SnTe3O8单晶的X射线探测器的暗电流漂移曲线如图8所示，SnTe3O8单晶X射线探测器的暗电流漂移为2.44×10-9nA cm-1s-1V-1。
实施例2：
(1)TiTe3O8单晶的制备：
将原料TiO2和TeO2按化学计量比配料，混合均匀，直接加入到助熔剂体系Li2CO3-TeO2中，装入容积为Φ50mm×70mm的铂金坩埚中，升温至原料熔化并形成均一溶液；降温至饱和点，此时把预热过的籽晶下入溶液中，并以0.01-3℃/h的降温速率降温，生长周期15天，即可得到块状TiTe3O8单晶，记作TTO；定向加工(100)晶片(图1)，测试其X射线衍射图，与理论计算一致(图2)，证明得到的是立方晶系的晶体；
(2)基于TiTe3O8单晶的X射线探测器的制备：
选取TiTe3O8单晶的(100)晶片上下对应的平面，两面利用溅射法沉积Au电极，电极厚度为100m；制得结构为Au/TiTe3O8单晶/Au的X射线探测器(图3)。
实验例2
实施例2制备的基于TiTe3O8单晶的X射线探测器在不同剂量下的光电流曲线如图5所示。
实施例2制备的基于TiTe3O8单晶的X射线探测器X射线能量下的灵敏度如图6所示，TiTe3O8单晶X射线探测器的灵敏度为329μC Gyair -1cm-2。
实施例2制备的基于SnTe3O8单晶的X射线探测器的检测线如图7所示，TiTe3O8单晶X射线探测器的最低检测限为27.2nGyair s-1。
实施例2制备的基于SnTe3O8单晶的X射线探测器的暗电流漂移曲线如图8所示，TiTe3O8单晶X射线探测器的暗电流漂移为1.97×10-8nA cm-1 s-1V-1。
实施例3：
(1)ZrTe3O8单晶的制备：
将原料ZrO2和TeO2按化学计量比配料，混合均匀，直接加入到助熔剂体系Li2CO3-TeO2中，装入容积为Φ50mm×70mm的铂金坩埚中，升温至原料熔化并形成均一溶液；降温至饱和点，此时把预热过的籽晶下入溶液中，并以0.01-3℃/h的降温速率降温，生长周期15天，即可得到块状ZrTe3O8单晶，记作ZTO，定向加工(100)晶片(图1)，测试其X射线衍射图，与理论计算一致(图2)，证明得到的是立方晶系的晶体；
(2)基于ZrTe3O8单晶的X射线探测器的制备：
选取ZrTe3O8单晶的(100)晶片上下对应的平面，两面利用溅射法沉积Au电极，电极厚度为100nm；制得结构为Au/ZrTe3O8单晶/Au的X射线探测器(图3)。
实验例3
实施例3制备的基于ZrTe3O8单晶的X射线探测器在不同剂量下的光电流曲线如图5所示。
实施例3制备的基于ZrTe3O8单晶的X射线探测器X射线能量下的灵敏度如图6所示，ZrTe3O8单晶X射线探测器的灵敏度为348μC Gyair -1cm-2。
实施例3制备的基于SnTe3O8单晶的X射线探测器的检测线如图7所示，ZrTe3O8单晶X射线探测器的最低检测限为15.4nGyairs-1。
实施例3制备的基于SnTe3O8单晶的X射线探测器的暗电流漂移曲线如图8所示，ZrTe3O8单晶X射线探测器的暗电流漂移为3.16×10-9nA cm-1s-1V-1。
以上所述实施例仅是对本发明技术方案所做的举例说明。本发明所涉及的基于ATe3O8(A＝Ti，Zr和Sn)系列单晶的X射线探测器及其制备方法并不仅仅限定于在上述实施例中所描述的内容，而是以权利要求所限定的范围为准。本发明所属领域技术人员在精神和原则之内所作的任何修改、补充、等同替换或改进等，均应包含在本发明的保护范围之内。
Claims (10)
1.基于ATe3O8单晶的X射线探测器的制备方法，包括步骤：
将ATe3O8单晶顶面溅射金属金作为正极，在该单晶底面溅射金属金作为负极，从而得到基于ATe3O8单晶的X射线探测器。
2.根据权利要求1所述的制备方法，其特征在于，ATe3O8单晶为正方体形状，边长为4mm，厚度为1mm。
3.根据权利要求1所述的制备方法，其特征在于，在制备X射线探测器之前，先将ATe3O8单晶在X射线定向仪上进行定向，之后进行晶体切割，切割速度为0.1mm/h，最后将切割后的ATe3O8晶片进行抛光处理，抛光工艺如下：首先采用1000目砂纸进行手工粗抛10分钟，之后采用7000目砂纸进行手工粗抛15分钟，最后采用9091超细纤维布作为抛光垫，以0.05μmAl2O3抛光粉和0.5g去离子水作为抛光液，抛光10分钟。
4.根据权利要求1所述的制备方法，其特征在于，顶面金电极的厚度为50-150nm，底面金电极的厚度为50-150nm。
5.根据权利要求1所述的制备方法，其特征在于，所述的ATe3O8单晶，A＝Ti,Zr或Sn。
6.根据权利要求1所述的制备方法，其特征在于，所述的ATe3O8单晶为TiTe3O8，ZrTe3O8或SnTe3O8。
7.根据权利要求1所述的制备方法，其特征在于，所述的ATe3O8单晶是按如下方法制备得到：
将纯相ATe3O8多晶粉末置于助熔剂体系中，混合均匀，放置铂金坩埚中，升温使之完全熔化，搅拌混合均匀，降温至饱和点，下入籽晶并转动，以0.01-5℃的速率降温使晶体生长，生长周期为15-30天。
8.根据权利要求7所述的制备方法，其特征在于，纯相ATe3O8多晶粉末为TiO2、ZrO2或者SnO2与TeO2按化学计量比混合得到的混合物。
9.根据权利要求1所述的制备方法，其特征在于，助熔剂体系为Li2CO3-TeO2，纯相ATe3O8多晶粉末与助熔剂体系的质量比为10-24％，籽晶为(100)方向，转速速度30rpm。
10.一种基于ATe3O8单晶的X射线探测器，是由权利要求1所述的方法制备得到。
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| JPH0632632A (ja) * | 1992-05-18 | 1994-02-08 | Sumitomo Electric Ind Ltd | 光学材料及びその製造方法 |
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| WO2014117409A1 (zh) * | 2013-02-04 | 2014-08-07 | 深圳首创光伏有限公司 | 晶体硅太阳能电池正面电极导电浆料及其制备方法 |
| KR101608851B1 (ko) * | 2014-10-31 | 2016-04-05 | 중앙대학교 산학협력단 | 신규한 혼합금속산화물 |
| CN106676635A (zh) * | 2017-01-12 | 2017-05-17 | 山东大学 | 一类碲酸盐晶体及其生长方法与应用 |
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| JPH0632632A (ja) * | 1992-05-18 | 1994-02-08 | Sumitomo Electric Ind Ltd | 光学材料及びその製造方法 |
| WO2014117409A1 (zh) * | 2013-02-04 | 2014-08-07 | 深圳首创光伏有限公司 | 晶体硅太阳能电池正面电极导电浆料及其制备方法 |
| CN103865540A (zh) * | 2014-02-27 | 2014-06-18 | 重庆邮电大学 | 一种碲酸盐玻璃基质下转换材料及制备方法 |
| KR101608851B1 (ko) * | 2014-10-31 | 2016-04-05 | 중앙대학교 산학협력단 | 신규한 혼합금속산화물 |
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