CN102105557B - 用于CT应用中的Gd2O2S材料 - Google Patents

用于CT应用中的Gd2O2S材料 Download PDF

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CN102105557B
CN102105557B CN2009801287519A CN200980128751A CN102105557B CN 102105557 B CN102105557 B CN 102105557B CN 2009801287519 A CN2009801287519 A CN 2009801287519A CN 200980128751 A CN200980128751 A CN 200980128751A CN 102105557 B CN102105557 B CN 102105557B
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C·R·龙达
G·蔡特勒
H·施赖讷马赫尔
N·康拉茨
D·U·维歇特
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Abstract

本发明涉及用于CT应用中的Gd2O2S材料。具体地说，本发明涉及Gd2O2S:Nd荧光材料以及Nd3+在合适的材料中作为发射体的用途。

Description

用于CT应用中的Gd2O2S材料
技术领域
本发明涉及尤其是用于CT和/或X-射线应用中的包含荧光钆的粉末。 
本发明还涉及使用单轴热压制备荧光陶瓷的方法。 
本发明还涉及用于检测电离辐射的检测器。 
本发明还涉及所述检测器用于检测电离辐射的用途。 
背景技术
用于检测高能辐射的荧光元件包括能吸收辐射并将其转化为可见光的荧光材料。由此产生的发光是电子器件要求的，并借助于光敏系统如光电二极管或光电倍增管进行评价。所述荧光元件可以由单晶材料，如掺杂的碱金属卤化物制备。非单晶材料可以用作粉末化的荧光材料或以由其制备的陶瓷元件的形式采用。 
用于检测高能辐射的典型的荧光陶瓷材料是Pr-掺杂的Gd2O2S。另一材料是Eu-掺杂的(Y，Gd)2O3。 
尽管在现有领域中所用的材料具有一些优点，但是对于可用作CT和/或X-射线应用中的荧光材料的其它替代材料仍不断有需求。 
发明内容
本发明的第一目的是提供用于CT和/或X-射线应用中的闪烁材料。 
所述目的通过如本发明权利要求1所述的荧光材料而实现。相应地，提供了Gd2O2S:Nd荧光材料。 
所述目的通过在一种或多种如下材料中使用Nd作为发射体而进一步得以实现：Gd2O2S、(Y，Gd)2O3、Lu3Al5O12、Y3Al5O12、Lu3Ga5O12。 
本发明意义上的术语“发射体”尤其是指和/或包括在入射X-射线辐射时Nd能在400-1200 nm波长范围内发射光。 
本发明人出人意料地发现在Gd2O2S和/或(Y，Gd)2O3、Lu3Al5O12、 Y3Al5O12、Lu3Ga5O12材料中加入Nd获得了具有良好的发射特性的荧光材料。特别地，一个优点是在本发明的多数应用中没有或几乎没有“余辉”。 
需要指出的是本发明的材料会被其它的稀土离子污染。典型的例子是Pr、Dy、Sm、Ce、Eu、Yb。这些离子的浓度应该优选地保持非常低，优选低于0.5摩尔ppm。 
根据本发明的一个优选实施方式，将Gd2O2S:Nd荧光材料和/或其中Nd用作发射体的材料的基质材料提供为陶瓷材料。 
本发明意义上的术语“陶瓷材料”是指和/或包括特别地晶体或多晶体的压实材料、或具有控制数量的孔或无孔的复合材料。   
本发明意义上的术语“多晶材料”是指和/或包括特别地体积密度大于主要成分的90％的材料，所述材料包括大于80％的单晶域，其中各域的直径大于0.5 μm并具有不同的晶体学取向。所述单晶域可以通过无定形或玻璃状材料或另外的晶体成分连接。 
利用相应盐：NdCl3、NdBr3、NdI3、Nd(NO3)3、Nd2(SO4)3等的水溶液进行Nd离子的引入。或者，在机械混合含有钆的粉末，如Gd2O2S，与包括掺杂剂，例如氧化物如Nd2O3的不溶性组合物的期间可以进行掺杂离子的引入。 
或者，含钆的粉末，如Gd2O2S粉末，可以与Nd的水不溶性盐，如NdF3、Nd2S3、Nd2O2S、Nd2(CO3)3、Nd2(C2O4)3等机械混合。 
根据本发明的一个优选实施方式，Gd2O2S的掺杂颜料粉末具有BET表面积为≥0.01m2/g和≤1m2/g的范围，优选≥0.05m2/g和≤0.5m2/g，更优选≥0.1m2/g和≤0.2m2/g。 
根据本发明的一个优选实施方式，基质材料中的Nd3+的浓度为≥10和≤2000重量ppm，优选≥100和≤1000重量ppm，最优选≥500和≤1000重量ppm。这些范围在实践中显示是适合于本发明的。 
根据本发明的一个优选实施方式，根据本发明的Gd2O2S:Nd荧光陶瓷材料显示为＞120％的范围的相对光产率，和优选相对于CdWO4的光输出大于230％。 
利用Hamamatsu Photodiode和National Instruments ADC测量光输出和 余辉。在120kV/100mA，80cm FDD(18-20mGy/s)，2s脉冲下测量余辉。在用聚硅氧烷粘附至光电二极管的4×4mm2的像素上测量信号值(光输出)。在关闭X-射线脉冲后测量余辉。 
根据本发明的一个优选实施方式，Gd2O2S:Nd荧光材料是透明的。应该注意在存在Ce的情形中，Gd2O2S:Nd荧光材料可以是黄色的。 
根据本发明的一个优选实施方式，相对于1.6mm的层厚度，Gd2O2S:Nd荧光材料在光谱范围880-1200nm中的自发射波长下的透射率为10％-70％，优选20％-60％，更优选≥40％，最优选≥50％。使用Perkin Elmer光谱仪进行总透射的测量。 
本发明的另一目的涉及用于制备根据本发明的Gd2O2S:Nd荧光材料中的含有钆的颜料粉末。 
本发明人出人意料地发现如果如上所述使用其中含有Nd的含钆颜料粉末，可以获得具有减少的余辉的Gd2O2S:Nd荧光材料。 
优选地，含钆的颜料粉末可以选自Gd2O3、Gd2O2S和/或Gd2O2S:Nd。 
本发明的另一目的涉及利用热压制备根据本发明的一个实施方式的荧光陶瓷材料的方法，所述方法包括如下步骤： 
a)选择如上所述的Gd2O2S:Nd的颜料粉末，其中，用于热压的所述粉末的粒径为1μm-20μm，所述热压在如下条件下进行： 
-温度为1000℃-1400℃，和/或 
-压力为100MPa-300MPa； 
b)在温度为700℃-1200℃下进行空气退火0.5小时-30小时，在步骤a)和步骤b)之间，任选地进行步骤c)，其中，步骤c)包括在真空下温度为1000℃-1400℃退火荧光陶瓷0.5小时至30小时。 
已发现在空气中化学稳定的相对粗糙的粒状粉末可以成功地被压制以形成具有改善的特性的荧光晶体。 
因此，根据本发明，优选的是压制模式按如下进行： 
-温度为1000℃-1400℃，优选1100℃-1300℃，更优选1150℃-1250℃，和/或 
-压力为100MPa-300MPa，优选180MPa-280MPa，更优选200MPa-250MPa。优选地，在根据本发明的单轴压制步骤期间的真空是≤100Pa和 ≥0.01Pa。 
根据本发明，可以在如下范围内调节真空：≥0.01Pa和≤50Pa，优选≥0.01Pa和≤10Pa，最优选将真空调节至≥0.01Pa和＜1Pa的范围。 
在真空下的热压步骤之后，荧光陶瓷可以进一步在温度700℃-1200℃，优选800℃-1100℃，更优选900℃-1000℃下通过空气退火被处理，其中，空气退火处理的时间是0.5小时至30小时，优选1小时至20小时，更优选2小时至10小时，最优选2小时至4小时. 
在一个实施方式中，优选的是根据本发明使用的Gd2O2S颜料粉末具有的平均粒径在1μm-20μm的范围，更优选2μm-10μm，最优选4μm-6 μm。 
根据本发明，有利的是引入真空退火步骤，以再进一步提高所得陶瓷的光学性能。在该步骤期间，在陶瓷中进行了进一步的晶粒生长，由于孔隙率的降低而进一步改进了透明度。除此之外，由于晶粒生长，在氧硫化物的晶格中掺杂原子的额外扩散使得进一步改善了陶瓷的闪烁性质。 
因此，根据本发明方法的一个实施方式，在步骤a)和步骤b)之间可以实施额外的步骤c)，其中步骤c)包括在真空下在1000℃-1400℃的温度下使荧光陶瓷退火0.5小时至30小时。 
优选地，退火温度被选择为1100℃-1300℃，更优选1200℃-1250℃。 
用于真空退火的时间优选设定为1小时至20小时，更优选为2小时至10小时，最优选为3小时至5小时。 
本发明还涉及用于检测电离辐射的检测器，所述检测器包括如本发明所述的荧光材料，其中，所述检测器优选是X-射线检测器、CT-检测器或电子射野影像检测器。 
根据本发明的荧光材料和/或检测器可以用于例如： 
-用于检测电离辐射，优选x-射线、γ射线和电子束的闪烁器或荧光元件；和/或 
-用于医学领域，优选计算机X射线断层摄影(CT)中的装置或设备。 
最优选的是根据本发明的至少一种荧光材料可以用于适用于医学成像的检测器或装置。 
然而，所述荧光材料可以用于医学领域中已知的任何检测器。这些检 测器例如是X-射线检测器、CT-检测器、电子射野影像检测器等。 
前述部件、权利要求书中的部件以及在所述实施方式中根据本发明所用的部件并不受限于其尺寸、形状、材料选择和技术概念，相关领域中已知的选择标准可以不受限制地应用。 
附图说明
本发明目的的另外的细节、特征和优点公开于从属权利要求、附图和以下关于附图和实施例的描述中，实施例以示例性的方式显示了本发明的优选实施方式。 
图1是显示根据本发明的两个不同实施例的两个光谱。 
实施例
实施例I 
在该实施例中，使用Nd浓度为0.1重量％的Gd2O2S:Nd颜料粉末。将3kg的所述颜料粉末与作为烧结和/或助熔剂的0.0055g的LiF混合。 
首先，以约20K/min升高温度直至达到800℃，此时进行25分钟的停留步骤。在停留步骤的部分期间，以2.5MPa/min升高压力，直至达到约50MPa。 
随后，以10K/min再次升高温度直至达到1050℃，随后以2K/min和1MPa/min同时升高温度和压力，直至达到最大压力150MPa和最高温度1250℃。 
此时，进行热压240分钟。 
在压制完成后，首先以5MPa/min降低压力，然后以3K/min降低温度，直至达到室温和常压。 
实施例II 
以与实施例1相同的方法，制备Nd浓度为2重量％的第二Gd2O2S:Nd陶瓷。 
图1显示实施例I(直线)和实施例II(虚线)的材料的发射光谱，其中，使用在230nm的X-射线作为入射光。可以很好地看出作为激活剂的Nd 满足成功用于CT和X-射线应用中的标准。 
上述具体实施方式中的元件和特性的特定结合仅是示例性的，在此可以用其它的教导互换和替换这些教导，并且本发明还包括通过引用加入本文的专利/申请。在不背离本发明的精神和范围下本领域技术人员会认识到关于在此描述的内容的各种改变、改进和其它的实施方式。因此，前述的说明书仅是示例性的而不是限制性的。本发明的范围由权利要求书及其等价物所限定。而且，本说明书和权利要求书中所用的附图标记并不限制本发明的范围。 

Claims (6)

1.Gd2O2S:Nd荧光材料，其中，Nd3+的浓度为≥100和≤1000重量ppm。
2.如权利要求1所述的Gd2O2S:Nd荧光材料，其中，所述Gd2O2S:Nd材料是陶瓷材料。
3.Nd的用途，其在一种或多种如下材料中用作发射体：Gd2O2S、(Y,Gd)2O3、Lu3Al5O12、Y3Al5O12、Lu3Ga5O12，其中，Nd3+的浓度为≥100和≤1000重量ppm。
4.如权利要求3所述的用途，其中，基质材料是陶瓷材料。
5.用于检测电离辐射的检测器，所述检测器包括如权利要求1-4任一项所述的荧光材料，其中，所述检测器优选是X-射线检测器、CT-检测器或电子射野影像检测器。
6.如权利要求5所述的检测器的用途，其用于适于医学成像的装置中，其中，所述检测器优选是X-射线检测器、CT-检测器或电子射野影像检测器。
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