CN1982259A - 多晶透明陶瓷制品及其制造方法 - Google Patents

多晶透明陶瓷制品及其制造方法 Download PDF

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CN1982259A
CN1982259A CNA2006100647093A CN200610064709A CN1982259A CN 1982259 A CN1982259 A CN 1982259A CN A2006100647093 A CNA2006100647093 A CN A2006100647093A CN 200610064709 A CN200610064709 A CN 200610064709A CN 1982259 A CN1982259 A CN 1982259A
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goods
molar fraction
oxide compound
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lutetium
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CN1982259B (zh
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K·M·克里斯纳
V·S·芬卡塔拉马尼
M·马诺哈兰
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General Electric Co
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General Electric Co
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Abstract

提出一种包括镥的多晶透明陶瓷制品。该制品包括结构式为ABO3、有A型晶格位置和B型晶格位置的氧化物。晶格位置A除镥之外还可进一步包括许多元素。B型晶格位置包括铝。提供包括镥基制品的图像装置、激光集合器和闪烁体。同时提供制造上述制品的方法。

Description

多晶透明陶瓷制品及其制造方法
技术领域
本发明一般性地涉及多晶透明陶瓷制品，特别涉及用于光学应用的镥基组合物。
背景技术
陶瓷材料，如镥基光学组合物，在闪烁体、激光和图像技术中有许多应用。光学应用经常需要材料的透明加工过的型态以减少由于散射和吸收的光损失。为此，加工过的型态一般要求有单相微结构。而且，在许多应用中要求材料在特殊波长范围内发射光或其它电磁辐射。通过一种或更多种掺杂物的选择性使用和通过调整材料中掺杂物的浓度，可以调节或“调谐”光学材料中例如发射的波长范围和光转化效率的光学特性。
当前应用经常使用单晶光学材料，它的制造相当昂贵和耗时。而且，由于在晶体形成期间掺杂的难度，单晶中的光学可调谐性经常难于实现。
一个替代的方法是使用多晶材料。与单晶材料相比多晶材料更容易掺杂。多晶材料的性能和应用部分取决于可以继而通过加工控制的组成材料的晶体的尺寸、形状和形态。
获得透明形态的多晶陶瓷材料的加工可能需要暴露于高温，期间想要的微结构可能由于诸如晶粒长大、相变和其它相关的机理等热激活过程而劣化。因此，需要解决这些问题以提供一种有效、经济和坚固的多晶光学组合物。
发明内容
本发明的实施方案针对这些和其它需要。根据一种实施方案，制品包含含有A型晶格位置和B型晶格位置的具有多晶结构的氧化物。该氧化物有ABO3的结构式，其中A表示占据A型晶格位置的材料，B表示占据B型晶格位置的材料。这里，A包括包括镥在内的许多元素，镥以至少为氧化物的约0.5摩尔分数的量存在，B包括铝。在这里给出的其它实施方案包括具有包含所述制品的发射介质的激光集合器，和包含含所述制品的闪烁体的图像装置。
附图说明
当参考相应附图阅读下列详细描述时，本发明的这些和其它特征、方面和优点将变得更透彻，其中：
图1是Lu0.8Gd0.15Y0.05AlO3的XRD图；和
图2是有大约200nm晶粒尺寸的Lu0.8Gd0.15Y0.05AlO3的典型SEM照片。
具体实施方式
作为这里使用的冠词“一个”、“一种”和“该”应该被理解成表示“至少一个”。
作为这里使用的术语“约”应该被理解成表示正或负0.001％(+/-0.001％)。作为这里使用的术语“辐射”指电磁辐射的整个光谱。作为这里使用的术语“光”指电磁光谱的可见区。
根据一个实施方案，提供了包括有A型晶格位置和B型晶格位置的多晶结构的氧化物的制品。该氧化物有ABO3的结构式，A表示占据A型晶格位置的材料，B表示占据B型晶格位置的材料。在一个实施方案中，A除了镥(Lu)之外还包括许多元素，B包括铝(Al)。镥以至少为氧化物的约0.5摩尔分数的量存在。
除非特别指明，此后将用到的术语“制品”应该被理解成表示上面描述过的制品。除非特别指明，此后术语“氧化物”应该被理解成表示上面描述过的氧化物。
氧化物中镥的高浓度有助于给予制品所需程度的密度。在许多光学应用中，高密度有助于材料的辐射阻止能力，这提高例如闪烁体等产品的性能。在某些实施方案中，Lu的浓度在约0.5摩尔分数到约0.995摩尔分数的范围内。在特殊的实施方案中，Lu以在约0.8到约0.995摩尔分数的范围内的量存在。
在一个实施方案中，具有所述氧化物的所述制品在A型晶格位置除镥之外还包括稀土元素(RE)。在特殊的实施方案中，稀土元素包括钆(Gd)、铽(Tb)和镱(Yb)中的一个或多个。下面将讨论，RE的加入可以帮助稳定想要的晶体结构。在一个实施方案中，RE的浓度大于约0.005摩尔分数。在某些实施方案中，RE以约0.005摩尔分数到约0.5摩尔分数的量存在。
在某些实施方案中，含有氧化物的制品进一步包括例如钇(Y)的过渡金属在A型晶格位置。钇的加入可以帮助获得想要的晶体结构。更进一步，钇的存在可以降低制品的进一步加工需要的温度。在一个实施方案中，钇的浓度大于约0.005摩尔分数。在某些实施方案中，钇的浓度在约0.005摩尔分数到约0.5摩尔分数的范围内。
在具体的实施例中，除了已经存在于晶格中的镥，含有氧化物的制品还有浓度在约0.0025摩尔分数到约0.5摩尔分数范围内的钇在A型晶格位置，和浓度在约0.0025摩尔分数到约0.5摩尔分数范围内的另一种稀土元素在A型晶格位置。在特殊的实施方案中，钇的浓度在约0.0025摩尔分数到约0.1摩尔分数的范围内。氧化物中镥的浓度可以在约0.5到约0.995摩尔分数的范围内。如上面描述过的，可以混合在ABO3中的合适稀土元素包括Gd、Tb、Yb和它们的组合。示例性组合物是Lu0.5Y0.25Gd0.25AlO3和Lu0.995Y0.0025Gd0.0025AlO3。制品的另一个示例性组合物包括Lu0.8Y0.05Gd0.15AlO3。
在一个实施方案中，结构式为ABO3的多晶氧化物有钙钛矿结构。有钙钛矿结构的材料是某些光学应用想要的。例如，在闪烁体探测器中具有钙钛矿结构的基质材料的使用与例如具有石榴石结构的基质材料相比能改善分散于基质材料中的掺杂物的衰减时间。而且，具有钙钛矿结构的材料改善闪烁体的阻止能力。
钙钛矿结构通常由有A型晶格位置和B型晶格位置的通式为ABX3的组合物形成。这里用到的“A位置”或“A晶格位置”指具有阴离子配位大于9(例如，举例来说，那些有配位数12的位置)的钙钛矿晶格内的位置，“B位置”或“B晶格位置”指阴离子配位为6的钙钛矿晶格内的位置。
钙钛矿结构的形成和稳定性大部分取决于组分离子的离子尺寸。作为众所周知的镧系收缩现象的结果，镥阳离子有不易于使其本身形成钙钛矿结构的尺寸。在A型晶格位置的其它元素的存在给予钙钛矿结构稳定性。
确定钙钛矿结构稳定性的因素是所谓的容许系数，它由方程式 T = ( R A + R X ) R B + R X 给出。这里，RA，RB和RX分别表示在A晶格位置、B晶格位置和在X晶格位置的元素的平均离子半径。这里，X表示ABO3中的氧。
一般地，钙钛矿结构在大约大于0.94的容许系数下是稳定的。下面的表格给出了在示例性组合物的不同摩尔分数下的容许系数，其中稀土元素Gd或过渡元素Y代替在A型晶格位置，和晶体结构中的Lu一起致力于稳定钙钛矿结构。
摩尔分数Lu 摩尔分数Gd 平均半径 容许系数
1 0 1.15 0.934
0.9 0.1 1.159 0.938
0.7 0.3 1.177 0.944
0.5 0.5 1.195 0.951
0.3 0.7 1.213 0.957
0.1 0.9 1.231 0.964
0 1 1.24 0.967
 摩尔分数Lu   摩尔分数Y   平均半径   容许系数
1 0 1.15 0.934
0.9 0.1 1.163 0.939
0.7 0.3 1.189 0.949
0.5 0.5 1.215 0.958
0.3 0.7 1.241 0.968
0.1 0.9 1.267 0.977
0 1 1.28 0.982
从以上的表格，基于容许系数的分析提出在钙钛矿结构中纯LuAlO3可能是不稳定的，而YAlO3和GdAlO3是稳定的。分析进一步提出添加Y和/或Gd到LuAlO3有利地可以用来稳定这种钙钛矿结构的材料。
在高于室温(约25℃)和低于约2400℃的氧化物的熔融温度，包括具有钙钛矿结构相的多晶氧化物的制品是稳定的。氧化物ABO3的钙钛矿结构甚至在高压下得以保存。甚至在中等高的温度和压力下钙钛矿结构相的保存是有利的性质，因为它能减少加工期间制品中相反的结构转换的风险。在某些实施方案中，氧化物在约1个大气压力到约500MPa的范围内的压力下是稳定的。在特殊的实施方案中，氧化物在约1个大气压力到约500GPa的范围内的压力下是稳定的。
具有氧化物的制品可包括碱土元素(AE)在A型晶格位置。在A型晶格位置包括碱土元素由于碱土元素的较大阳离子尺寸而给予钙钛矿结构稳定性。晶格中AE的加入可以降低加工需要的温度。在特殊的实施方案中，AE包括选自钙、锶、钡或镁的至少一种碱土元素。
如果不加限制，在A型晶格位置包括不同于镥的价态的离子将导致电荷不均衡；这种情况通过在B型晶格位置的代替离子可以抵销。例如，在A型晶格位置二价钙离子代替三价镥可能需要四价离子(如铪)在B型晶格位置来抵销氧阴离子上的电荷。包括离子的一般实例组合物可被表示成(Lu，RE，Y)1-m(AE)mCmAl1-mO3，其中C是四价离子。这里，Lu、RE和Y代表在A型晶格位置的镥(Lu)、稀土元素(RE)或钇(Y)中的一个或多个。碱土元素(AE)代替在A型晶格位置，而C即四价离子代替在B型晶格位置，以抵销电荷不均衡。Lu维持在约0.5摩尔分数到约0.995摩尔分数的浓度。AE的浓度可从约0.001到约0.5变化，这意味“m”是在约0.001摩尔分数到约0.5摩尔分数的范围内。在一个实施例中，钙的浓度可以是约0.2摩尔分数，这意味“m”是0.2。在某些实施方案中，锶浓度可以高达0.3，而钡浓度可以是约0.15。
其它有代表性的组合物包括(Lu，RE，Y)3-3m(AE)3mDmE2mAl3-3mO9，其中D和E是二价和五价的离子，且其中A型晶格位置有Lu、RE、Y或AE中的一个或多个，B型晶格位置可包括D和E，以抵销电荷不均衡。在B位置实例离子包括二价镁(Mg)、五价钽(Ta)和四价锆(Zr)、铪(Hf)、硅(Si)和锗(Ge)。
在某些实施方案中，离子代替在B晶格位置。以其它离子例如镁在B位置替换铝，能降低进一步加工需要的温度。代替在B位置的合适材料包括选自由过渡元素、稀土元素、半金属元素和碱土元素组成的组的元素的离子。在特殊的实施方案中，离子选自镁(Mg)、锌(Zn)、钪(Sc)、硅(Si)、锗(Ge)、钛(Ti)、锆(Zr)、铪(Hf)、铌(Nb)和钽(Ta)中的一个或多个。在非限制性的实施例中，在B位置的铝阳离子可被二价镁阳离子和四价铪阳离子替换以维持电荷平衡。典型的组合物可被表示成(Lu，RE，Y)Al1-mDm/2Cm/2O3，其中D和C分别是二价和四价离子。其它组合物可被表示成(Lu，RE，Y)Al1-3m/2DmEm/2O3，其中D和E分别是二价和五价离子。这里，Lu、RE和Y代表在A型晶格位置的镥(Lu)、稀土元素(RE)或钇(Y)中的一个或多个。Lu维持在约0.5摩尔分数到约0.995摩尔分数的浓度。“m”在约0.001摩尔分数到约0.5摩尔分数的范围内。在A位置和B位置离子的代替能在宽温度范围上稳定钙钛矿结构和能在更低温度下增强加工，因此减少有害的晶粒生长的风险。
制品可进一步被一种或多种掺杂物掺杂。掺杂物可给予制品有用的光学特性和可例如用于闪烁体、激光装置和检测器。在一些实施方案中，掺杂物包括稀土元素。稀土元素掺杂物的合适的例子包括铈(Ce)、钕(Nd)、铕(Eu)、铽(Tb)、镱(Yb)、铥(Tm)、钬(Ho)和镨(Pr)。在某些实施方案中，掺杂物是包括钛或铬中的一个或多个的过渡金属元素。
可调整掺杂物的浓度以控制氧化物的光学特性。例如，激光应用可能需要相对高浓度的掺杂物来获得需要的发射特性。在某些实施方案中，掺杂物浓度少于约15摩尔百分数。在特殊的实施方案中，浓度在约0.005摩尔百分数到约15摩尔百分数的范围内。在一个实施方案中，掺杂物的浓度在约0.005摩尔百分数到约6摩尔百分数的范围内。
多晶制品有许多晶粒。晶粒的平均尺寸可从纳米到微米改变。在A位置镥的高浓度需要高的形成温度和因而可导致更大的晶粒尺寸。然而，大晶粒降低使用所述制品制成的多晶制品的光学特性，如透明度。晶粒的尺寸取决于形成期间可控制的因素。在非限制性的实施例中，使用燃料助溶合成形成的晶粒的尺寸(在下面更详细地描述)部分取决于反应过程期间燃料添加的量。在一个实施方案中，晶粒尺寸小于约10微米。在另一个实施方案中，晶粒尺寸在约0.1微米到约10微米的范围内。在某些实施方案中，晶粒尺寸在约10纳米到约0.1微米的范围内。
粉末形状的材料，如上面描述过的通过燃料助溶合成形成的材料，可被进一步加工形成固体陶瓷制品。在一个实施方案中，作为具有许多晶粒的多晶粉末而形成的氧化物被烧结以形成透明陶瓷制品。烧结的过程是本领域众所周知的，且控制过程和其制品的各种方法是常用的，将在下面讨论。在非限制性的实施例中，制品是用于激光集合器的发射介质。在另一实施例中制品是闪烁体。
提供了具有发射介质的激光集合器，其中发射介质包括上面描述过的氧化物。在一个实施方案中，多晶氧化物有钙钛矿结构。氧化物可形成配置在激光集合器活性介质中的透明、致密制品。制品可进一步被例如钕(Nd)掺杂。其它合适的掺杂物包括其它稀土元素，如铕(Eu)、镨(Pr)、钬(Ho)、铥(Tm)和镱(Yb)；和过渡金属元素，如钛和铬。在一个实施方案中，掺杂浓度少于约15摩尔百分数。在另一个实施方案中，掺杂浓度在约0.005到约15摩尔百分数的范围内。
术语“闪烁体”在本领域通常被理解为指暴露于辐射时发射可见光的材料或制品。在许多图像应用中，闪烁体通常被设计成吸收X-射线和发射可见光。示例性闪烁体应用是正电子发射断层扫描(PET)。利用闪烁体的其它图像应用包括X-射线检测器、伽马射线检测器和中子检测器。
PET使用有助于病人的放射性标记物质，使用合适的光电探测器通过跟随放射性标记物质的衰减而随后对该放射性物质进行示踪。放射性衰减导致辐射的发射。作为临床图像技术的PET的价值很大程度上依赖光电探测器的性能。光电探测器包括闪烁体材料，其在暴露于辐射时发射在可见光区的光线。理想的是具有优良的阻止能力、高光输出和快衰减时间的闪烁体材料。
如前面讨论过的，由于镥的高密度而期望包括镥的闪烁体材料有优良的阻止力量。在一个实施方案中，闪烁体包括由这里前面描述过的氧化物制成的基质材料。在一个实施方案中，多晶氧化物有钙钛矿结构。氧化物可被进一步加工以形成透明制品。包括氧化物的基质材料可被铕、镨、铈和钕中的一个或多个进一步掺杂。一般地掺杂物的浓度最高为约15摩尔百分数。在一些实施例中，掺杂物的浓度可从约0.005摩尔百分数到约15摩尔百分数变化。
根据一个实施方案，提供一种使用燃料助溶合成(FASS)制作氧化物的方法。混合镥和铝的前体以形成均匀化的前体溶液。在某些实施方案中，包括稀土元素和钇的可代替在A晶格位置的材料和可代替在B晶格位置的材料的前体可被包括在前体溶液中。在一个实施例中，将掺杂物前体加入到前体溶液中。示例性前体包括金属的氧化物、硝酸盐、醋酸盐和碳酸盐。不是硝酸盐的前体溶解于有效量的硝酸中以转化为硝酸盐前体。
通过添加硝酸调整前体溶液的pH。在一个实施方案中，pH在约0.5到约5的范围内。一种关系存在于晶粒或随后的颗粒的形态和均匀化的前体溶液的pH之间。例如，对于pH值小于约1.0获得类似球体的形态。
然后将燃料与前体溶液混合。合适的燃料的例子包括但不仅限于甘氨酸、尿素和肼。可变化前体与燃料的比以控制晶粒或随后的颗粒的尺寸。在一个实施例中，约2∶1.4的前体与燃料的比可导致颗粒尺寸在约0.5微米到约1微米的范围内。在另一个实施例中，约2∶0.7的前体与燃料的比可导致颗粒尺寸在约10纳米到约200纳米的范围内。通常，较小的晶粒尺寸是进一步加工成透明制品所需要的。
包括燃料的前体溶液自燃或在约300℃到约400℃下分解以形成材料的粉末。选择性地，在FASS期间通过增加燃料与前体摩尔的比可实现颗粒或晶粒形成，但是不利地它由于较少的反应控制可能形成较大的颗粒。
所述方法进一步包括加工这样获得的粉末。使用本领域公知的方法，例如研磨、粉磨等等，使粉末均匀化。对均化的粉末进行本领域技术人员公知的受控制的煅烧，导致具有如尺寸、形状和形态等所需性能的纯相组合物。在一个实施例中，对粉末进行介于1小时到约12小时的各种热处理或煅烧。在一个实施例中，温度在约600℃到约1700℃的范围内。在特殊的实施例中，温度在约800℃到约1200℃的范围内。
在热处理之后，使用本领域技术人员公知的方法将均化的粉末烧结。在一个实施例中，在低于材料的熔融点的温度下使用热压，以形成透明陶瓷制品。
在一个实施例中，在颗粒生长添加剂如锂、镁、钙、硅或氟的存在下对期望的组合物的多晶粉末进行烧结，以形成烧结的陶瓷。烧结的陶瓷可以包含晶种，颗粒生长可在低于组合物熔融点的温度下从晶种进行外延。然后在约100GPa的恒压下对烧结的陶瓷进行热压以形成透明陶瓷制品。
实施例
制备有80摩尔％镥、5摩尔％钇、15摩尔％钆的镥钆钇铝酸盐(Lu0.8Gd0.15Y0.05AlO3)组合物一份10g。通过溶解镥氧化物(6.56g)、钇氧化物(0.23g)、钆氧化物(1.12g)和硝酸铝(15.46g)于水和硝酸的溶液20ml中制备前体溶液。然后将前体溶液搅拌均匀。通过添加水和硝酸将前体溶液的pH调整至0.5。前体溶液的最终体积是100ml。将甘氨酸(4.39g)加入到溶液中。将溶液放置在预热过的热板上并加热到约300℃的温度。通过加热，除去水和形成反应浓缩物。在进一步加热时，反应浓缩物的起泡就发生了。随着连续加热，起泡产品生成体积大的、蓬松的、灰暗的粉末。然后将粉末研磨使它均匀。然后将均化的粉末放置入氧化铝坩锅内并在马弗炉中在1200℃下在空气中加热2小时。对由合成产生的粉末以及热处理过的粉末实施各种表征技术如X-射线衍射(XRD)和扫描电子显微镜(SEM)。附图1是使用这里描述过的方法制备的组合物Lu0.8Gd0.15Y0.05AlO3的典型XRD图像。XRD图像显示组合物保持钙钛矿结构相。附图2是使用上面的方法但甘氨酸量减少至2.15g制备的Lu0.8Gd0.15Y0.05AlO3的典型SEM图像。图形表示晶粒有小于约200nm的平均尺寸。通过在控制的条件下烧结可对这种细微粉末进一步加工以形成透明陶瓷制品。
虽然已在这里举例说明和描述了只有某些本发明的特征，对那些本领域技术人员将发生许多改进和变化。因此，将被理解为附加权利要求想要覆盖所有这样的适合本发明真实精神的改进和变化。

Claims (10)

1.一种制品，包含：具有多晶结构和包含A型晶格位置和B型晶格位置的氧化物，该氧化物有结构式ABO3，其中A表示占据A型晶格位置的材料，B表示占据B型晶格位置的材料；其中A包括多种元素，该多种元素包括镥，其中镥以至少为氧化物的约0.5摩尔分数的量存在；和其中B包括铝。
2.权利要求1的制品，其中A包括选自由钆、铽、镱和它们的组合组成的组的稀土元素。
3.权利要求1的制品，其中A包括钇。
4.权利要求1的制品，其中A包括钇和稀土元素，其中钇以在约0.0025摩尔分数到约0.5摩尔分数的范围内的量存在，且稀土元素以在约0.0025摩尔分数到约0.5摩尔分数的范围内的量存在。
5.权利要求1的制品，其中A进一步包括碱土元素，其中碱土元素选自由钙、锶、钡、镁或它们的组合组成的组。
6.权利要求1的制品，其中B进一步包括选自由硅、锗、钛、锌、铪、铌、钽或它们的组合组成的组的至少一种附加的元素。
7.权利要求1的制品，其中该制品本质上由钙钛矿结构组成。
8.权利要求1的，进一步包含至少一种掺杂物，其中该至少一种掺杂物选自由铈、钕、铕、铽、镨、铥、钬、铬、钛或它们的组合组成的组，且其中该至少一种掺杂物的浓度在约0.005摩尔百分数到约15摩尔百分数的范围内。
9.权利要求1的制品，其中该制品进一步包含晶粒尺寸在约10纳米到约10微米范围内的许多晶粒。
10.权利要求1的制品，其中氧化物是透明的。
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