CN101001936B - 低余辉的紧凑快速闪烁体材料 - Google Patents
低余辉的紧凑快速闪烁体材料 Download PDFInfo
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- 239000000203 mixture Substances 0.000 description 26
- 229910052684 Cerium Inorganic materials 0.000 description 6
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- 229910052791 calcium Inorganic materials 0.000 description 4
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
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- 229910052733 gallium Inorganic materials 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- ADOANNTYRWJJIS-UHFFFAOYSA-N lutetium silicic acid Chemical compound [Lu].[Si](O)(O)(O)O ADOANNTYRWJJIS-UHFFFAOYSA-N 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
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Abstract
本发明涉及式Lu(2-y)Y(y-z-x)CexMzSi(1-v)M’vO5的无机闪烁体材料，式中：M代表二价碱金属离子，M’代表三价金属，(z+v)大于或等于0.0001而小于或等于0.2；z大于或等于0而小于或等于0.2；v大于或等于0而小于或等于0.2；x大于或等于0.0001并小于0.1；和y是(x+z)至1。特别地，这种材料可以装备这些闪烁探测器应用于工业、医疗领域(扫描仪)和/或石油钻探探测中。晶体中存在的Ca减少了余辉，同时保持高能辐射的高阻止本领。
Description
本发明涉及闪烁体材料，能够获得这些材料的生产方法与所述材料的用途，尤其是在γ射线和/或X-射线探测器中的用途。
这些闪烁体材料广泛地用于γ射线、X射线、宇宙射线和其能量约1keV与高于这个值的粒子的探测器中。
闪烁体材料是一种在闪烁波长范围内透明的材料，它对发射光脉冲的入射辐射有响应。
使用这样一些材料，一般而言单晶材料，可以制造探测器，其中该探测器的晶体所发射的光与光探测器件联接，产生与收到光脉冲数及其强度成比例的电信号。这样一些探测器特别地用于测定厚度和每平方米克重的工业，以及用于核医学、物理、化学和石油研究领域。
一组使用的已知闪烁体晶体是掺杂铈的硅酸镥。US4958080描述了掺杂铈的Lu2SiO5，专利US6624420描述了Ce2x(Lu1-yYy)2(1-x)SiO5。最后，US6437336涉及Lu2(1-x)M2xSi2O7类组成，其中M至少部分地是铈。这些各种各样的闪烁体组成全都共同地具有高能量辐射的高阻止本领，引起有非常快光脉冲的强光发射。
一个可期望的附加性能是在入射辐射停止后减少发射光量(或延迟发光或余辉)。在物理学上，本技术领域的技术人员所熟知的这个现象可用材料晶体学结构中存在的电子陷阱进行解释。闪烁现象取决于光电效应，光电效应在闪光体材料中产生一个电子空穴对。该电子在活性部位(上述闪烁体中的Ce3+部位)再结合时发射光子，其过程通常远低于一微秒。上述特别快速的闪烁器导致脉冲时间降低，其一级指数常数约40ns。然而，捕获的电子不会产生光，但热激发(包括在室温)的去捕获作用导致发射光子，余辉，它在一秒多的时间里依然也是可测量的。
这个现象在寻求通过非常短的开窗分开每个脉冲的应用中可能是不可接受的。在医学和工业部门中熟知的计算机化断层摄影(CT扫描仪)的应用便是这种情况。CT系统与PET(正电子发射断层摄影法)扫描仪联接时，这已成为工业中的标准，CT的分辨率较差影响整个系统的性能，因此影响了临床医生解释完整PET/CT系统结果的能力。人们知道余辉对于这些应用是完全不能接受的。
人们知道US4958080(LSO：Ce类，根据本技术领域的技术人员使用的符号)和US6624420(LYSO：Ce类)列举的硅酸镥类组成产生明显的余辉。相反地，US6437336所描述组成(LPS:Ce类)的优点是余辉弱得多。例如由L.Pidol、A.Kahn-Harari、B.Viana、B.Ferrand、P.Dorenbos、J.deHaas、C.W.E.vanEijk和E.Virey在“Lu2Si2O7:Ce3+的闪烁性质，快速而紧凑的闪烁结晶”，《物理杂志》：凝聚态物质(JournalofPhysics：CondensedMatter)，2003，15，2091-2102中给出了这些结果。图1所示曲线摘录于这篇文章，表示在X射线激发几小时下，每mg闪烁材料以事件(或计数)数形式检测的光量随时间的变化。LPS:Ce组成给出了明显更好的余辉结果。
从这个观点来看，LYSO的性质与LSO非常接近。限制这种余辉成为本申请的目的。
通过热致发光可以从根本上证明这种余辉性质(参见S.W.S.McKeever，《固体的热致发光》，剑桥大学出版社(1985))。这个特征在于在辐射后以热方法激发样品并测定光发射。在接近室温的300K下光峰会随其强度(去捕获)表现出或多或少很大的余辉。在更高的温度下光峰表现出更深而在室温下不太能热激发的捕获作用的存在。图2说明了这一点，该图取自上述L.Pidol等人撰写的文章，它还证明了LPS类组成在余辉方面的优点。
但是，LPS类组成的缺陷是其阻止本领不如LSO或LYSO类组成。这种情况可简单地由化合物的平均原子数与相关相的密度推导出来。
可以使用RISO(丹麦)生产的TL-DA-15自动化仪器进行热致发光测定，该仪器示于图3。能够使样品定位的加热器、热电偶和“升降器(ascenseur)”与光电倍增管(PM)和滤光片对准。在有氮气流的分析室内，一个用电动机驱动的旋转台(旋转样品台)或者在辐照步骤可以将样品定位在放射源处(放在铅容器内)，或者在热致发光测定时可以将样品定位在加热器和光电倍增管之间。在每次测定前，这些厚度约1mm的晶体在672K加热几分钟。然后它们进行辐照，再记录在氮气流下在313-672K之间不变加热速率的热致发光曲线。因黑体辐射(由以白热方式加热的物质自然发射的光称之黑体辐射)在更高温度的测定变得不可能。每条曲线是相对于产物质量进行标准化的。
在我们的申请中，我们感兴趣的发射是铈离子在约350-450nm的发射。我们已选择在光电倍增管入口的合适滤光器(HA3和7-59)。为了定量测定，使用在空气中提供剂量3.6Gray/h的90Sr/90Yβ-源进行原地辐照。TL(热致发光)测定时可改变的参数是剂量(辐照时间，在这里是20s)和加热速率(在这里是0.5K/s)。
本申请人已发现，往LYSO类组成中添加二价碱土金属M和/或三价金属M’能够非常显著地减少余辉。特别地，M可以是Ca、Mg或Sr(呈二价阳离子形态)。特别地，M’可以是Al、Ga或In(呈三价阳离子形态)。元素M取代Y或Lu，元素M’取代Si。
本发明的产品由于添加了M，特别是Ca，令人惊奇地能够减少余辉，而不会影响在这些考虑的比例范围内的密度。
本发明的闪烁体材料是式：
Lu(2-y)Y(y-z-x)CexMzSi(1-v)M’vO5(式1)
式中：
M代表二价碱土金属，如Ca、Mg或Sr，M’代表三价金属，如Al、Ga或In，
(z+v)大于或等于0.0001而小于或等于0.2；
z大于或等于0而小于或等于0.2；
v大于或等于0而小于或等于0.2；
x大于或等于0.0001而小于0.1；
y是(x+z)至1。
优选地，(z+v)大于或等于0.0002。
优选地，(z+v)小于或等于0.05，更优选地小于或等于0.01，甚至小于0.001。
优选地，x大于0.0001并小于0.001。
特别地，v可以是0(没有M’)，在这种情况中，z是至少0.0001。
特别地，本发明的闪烁体材料可以是v为0这样的材料。同样，本发明的闪烁体材料可以是M为Ca的材料，这相应于特别合适的组成。v为0与M为Ca的组合是特别合适的。那么，本发明的组成具有下式：
Lu(2-y)Y(y-z-x)CexCazSiO5(式II)
同样，本发明闪烁体材料还特别地可以是z为0的组成。同样，本发明闪烁体材料还特别地可以是M’为Al的组成。z为0与M’为Al的组合是特别合适的。那么，本发明的组成具有下式：
Lu(2-y)Y(y-x)CexAlvSi(1-v)O5(式III)
元素O的摩尔含量基本上是(Si+M’)摩尔含量的五倍，其条件是这个值可以变化约±2％。
采用Czochralski生长法可以得到本发明呈单晶形式的闪烁体材料。
本发明还涉及本发明闪烁体材料作为辐射探测器，特别地γ射线和/或X-射线探测器的器件的用途，尤其在计算机化断层摄影(CT)扫描仪中作为辐射探测器的用途。
本发明还涉及本发明闪烁体材料作为闪烁探测器器件的用途，尤其在工业、医疗领域和/或石油钻探探测中作为闪烁探测器器件的用途。特别地，还涉及连续采集的所有闪烁器系统(它包括断层摄影CT，即计算机化断层摄影)。还涉及正电子发射断层摄影类的任何闪烁器系统，尤其有飞行时间，如果必要与发射段层摄影结合的闪烁器系统。
本中请人没有被任何理论论据所束缚，假设引入二价碱土金属离子M取代三价稀土离子，或引入三价金属离子M’取代四价硅原子，因此产生正电荷不足，这样限制了捕获造成余辉的电子。
实施例
在与上述这些专利所描述的相同条件下，根据Czochralski方法制备三种直径1英寸的LYSO:Ce单晶。为此，使用相应于下述这些组成的原料：
对照(没有Ca)：
Lu1.8Y0.1978Ce0.0022SiO4.9961
组成1：
Lu1.8Y0.1778Ca0.02Ce0.0022SiO4.9961
组成2：
Lu1.8Y0.1878Ca0.01Ce0.0022SiO4.9961
为了得到这些期望式而使用相应的氧化物(Ca、Ce、Lu、Y氧化物)制备这些物料。在晶体生长过程中因偏析的原因，最终晶体中Ce和Ca的真实浓度低于由原料加入的Ce和Ca浓度。
最终得到其式Lu(2-y)Y(y-z-x)CexCazSiO5的单晶在样品顶部具有下述组成：
组成1发出的余辉比对照组成(通常的LYSO类组成)明显低，在137Csγ射线源的激发下，估计光能级达到20000光子/Mev，即略低于LPS组成(26000光子/Mev)、LYSO组成(34000光子/Mev)和LSO组成(约28000光子/Mev)。对于大多数的应用，这样的光能级是完全不会造成严重阻碍的。非常通常使用的锗酸铋(Bi4Ge3O12)仅发射9000光子/Mev。总之，组成1能够保持LYSO类组成的阻止本领，而不会明显损失光能级，同时还明显降低余辉。
组成2更有意义，余辉还低得多，光产率是27000光子/Mev。
图4比较了组成1和2与通常LSO(对照)的余辉值。
Claims (17)
1.式Lu(2-y)Y(y-z-x)CexCazSiO5的无机闪烁体材料，其中：
z大于或等于0.0001而小于或等于0.2；
x大于或等于0.0001而小于0.1；
y是(x+z)至1。
2.根据上述权利要求所述的材料，其特征在于z大于或等于0.0002。
3.根据上述权利要求中任一项权利要求所述的材料，其特征在于z小于或等于0.05。
4.根据权利要求3所述的材料，其特征在于z小于或等于0.01。
5.根据权利要求4所述的材料，其特征在于z小于或等于0.001。
6.根据权利要求1或2所述的材料，其特征在于x大于0.0001而小于0.001。
7.根据权利要求1或2所述的材料，其特征在于z小于0.05。
8.根据权利要求7所述的材料，其特征在于z小于0.01。
9.根据权利要求7所述的材料，其特征在于z小于0.001。
10.根据权利要求1或2所述的闪烁体材料，其特征在于它是单晶。
11.一种权利要求10所述单晶闪烁体材料的生长方法，其特征在于它是采用Czochralski法得到的。
12.包括权利要求1-10中任一权利要求所述的无机闪烁体材料的闪烁探测器。
13.包括权利要求12所述的闪烁探测器的计算机化断层摄影扫描仪。
14.权利要求1-10中任一项权利要求所述的闪烁体材料作为闪烁探测器部件的用途。
15.权利要求14的用途，其特征在于所述闪烁探测器部件是作为工业应用，医疗领域或石油钻探探测的闪烁探测器部件。
16.权利要求1-10中任一权利要求所述的闪烁体材料作为计算机化断层摄影扫描仪元件或正电子发射断层摄影扫描仪元件的用途。
17.权利要求16的用途，其特征在于所述正电子发射断层摄影扫描仪元件是有飞行时间的正电子发射断层摄影扫描仪元件。
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| FR0451815A FR2874021B1 (fr) | 2004-08-09 | 2004-08-09 | Materiau scintillateur dense et rapide a faible luminescence retardee |
| FR0451815 | 2004-08-09 | ||
| PCT/FR2005/050658 WO2006018586A1 (fr) | 2004-08-09 | 2005-08-08 | Materiau scintillateur dense et rapide a faible luminescence retardee |
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| CN101001936A CN101001936A (zh) | 2007-07-18 |
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| EP (1) | EP1781757B1 (zh) |
| JP (2) | JP5390095B2 (zh) |
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| FR (1) | FR2874021B1 (zh) |
| PL (1) | PL1781757T3 (zh) |
| UA (1) | UA93484C2 (zh) |
| WO (1) | WO2006018586A1 (zh) |
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- 2005-08-08 JP JP2007525327A patent/JP5390095B2/ja active Active
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