CN108384532B - 含铀化合物作为闪烁体的应用 - Google Patents
含铀化合物作为闪烁体的应用 Download PDFInfo
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- 229910052770 Uranium Inorganic materials 0.000 title claims abstract description 60
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 150000001875 compounds Chemical class 0.000 title claims abstract description 19
- 239000000126 substance Substances 0.000 claims abstract description 10
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- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 4
- 239000002253 acid Substances 0.000 claims abstract description 4
- 150000007942 carboxylates Chemical class 0.000 claims abstract description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 4
- 239000010452 phosphate Substances 0.000 claims abstract description 4
- 150000004820 halides Chemical class 0.000 claims abstract description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 125000000217 alkyl group Chemical group 0.000 claims description 14
- 229910001868 water Inorganic materials 0.000 claims description 14
- 125000005289 uranyl group Chemical group 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 11
- QMKYBPDZANOJGF-UHFFFAOYSA-N benzene-1,3,5-tricarboxylic acid Chemical compound OC(=O)C1=CC(C(O)=O)=CC(C(O)=O)=C1 QMKYBPDZANOJGF-UHFFFAOYSA-N 0.000 claims description 10
- 229910002007 uranyl nitrate Inorganic materials 0.000 claims description 8
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 6
- 239000004327 boric acid Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 4
- QEMXHQIAXOOASZ-UHFFFAOYSA-N tetramethylammonium Chemical compound C[N+](C)(C)C QEMXHQIAXOOASZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052796 boron Inorganic materials 0.000 claims description 3
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 2
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
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- 238000000034 method Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- -1 lanthanide silicates Chemical class 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
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- 230000015572 biosynthetic process Effects 0.000 description 2
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- DCLUBAHWHZHUKW-UHFFFAOYSA-N (3-oxo-2,4-dioxa-3lambda5-phosphabicyclo[3.3.1]nona-1(9),5,7-trien-3-yl) dihydrogen phosphate Chemical compound C1=CC2=CC(=C1)OP(=O)(O2)OP(=O)(O)O DCLUBAHWHZHUKW-UHFFFAOYSA-N 0.000 description 1
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- 229910014323 Lanthanum(III) bromide Inorganic materials 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 229910004619 Na2MoO4 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
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- 229910052785 arsenic Inorganic materials 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
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- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium oxide Inorganic materials O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 150000002602 lanthanoids Chemical class 0.000 description 1
- XKUYOJZZLGFZTC-UHFFFAOYSA-K lanthanum(iii) bromide Chemical compound Br[La](Br)Br XKUYOJZZLGFZTC-UHFFFAOYSA-K 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
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- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000009206 nuclear medicine Methods 0.000 description 1
- 230000005658 nuclear physics Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
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- 229910052702 rhenium Inorganic materials 0.000 description 1
- 239000011684 sodium molybdate Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- GPHXJBZAVNFMKX-UHFFFAOYSA-M triethyl(phenyl)azanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)C1=CC=CC=C1 GPHXJBZAVNFMKX-UHFFFAOYSA-M 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 238000012800 visualization Methods 0.000 description 1
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Abstract
本发明公开了含铀化合物作为闪烁体的应用，含铀化合物为含铀有机无机杂化物或含铀无机物，含铀有机无机杂化物为含铀有机羧酸盐或含铀有机磷酸盐：含铀无机物为含铀非金属酸盐、含铀金属盐或含铀卤化物。本发明公开了含铀有机无机化合物或含铀无机物具有本征闪烁能力，为利用铀元素进行各类型化学组成与形态(有机无机、无机)的闪烁体开发提供了新理念。
Description
技术领域
本发明涉及闪烁体技术领域，尤其涉及一种含铀化合物作为闪烁体的应用。
背景技术
辐射闪烁性能是指材料吸收高能粒子(α、β粒子)或射线(X、γ)后发射可见光的过程，具备这种性质的材料通常被称为“闪烁体”，由于其能够对辐射进行“可视化”过程(射线-可见光-光电转换-成像)，因此此类材料在高能物理和核物理实验、空间和天体物理、医学成像、环境监测、安全检查、核不扩散检测、工业无损检测、石油测井和地质勘探等领域均具有广泛应用。
目前大规模使用的闪烁体为无机闪烁体。早期无机闪烁体包含ZnS，NaI，CsI等晶体，此类纯无机盐晶体发光效率较低，在无机盐晶体中加入少量激活剂如Tl+离子等能进一步提高发光效率，目前已发展的高荧光强度的闪烁体有NaI:Tl、CsI:Tl等，但此类离子型材料较易吸湿，在实际制作产品过程需额外的处理方式。此外，以掺杂发光体Ce3+离子为主的镧系硅酸盐具有高的稳定性、较大的光输出，也被广泛应用，但此类材料单晶生长技术仍不够成熟，例如Y2Si2O7:Ce不一致融化，生长大尺寸单晶仍是难题。另外一类非常重要的闪烁体为锗酸铋晶体(Bi4Ge3O12，BGO)，其密度约为7g/cm3，使得此类晶体具有较高的射线吸收能力，目前广泛应用于高能物理、核医学成像等装置。但合成前体GeO2价格较为昂贵，寻找廉价、高性能闪烁体仍是闪烁体发展的重要内容。
一般来说辐射探测材料应具备以下几点：(1)高光输出；(2)快速响应时间；(3)良好的辐射和湿度稳定性；(4)较好的能量分辨率等性能；(5)强的射线阻止能力。虽然各类闪烁体已经被广泛使用，但是每种闪烁体在实际应用过程中仅限于特定需求，因此，闪烁体材料开发很大程度上以应用为导向。当前闪烁体材料开发以重元素组成的晶格基质(硅酸盐、铝酸盐、硼酸盐等)掺杂发光元素Ce3+、Eu2+等为主，力求获得较好的材料性能；另外一方面，闪烁体材料发展也着力生长LaBr3:Ce3+、PbWO4、Bi4Ge3O12(BGO)等高质量晶体。
发明内容
为解决上述技术问题，本发明的目的是提供一种含铀化合物作为闪烁体的应用，本发明公开了含铀有机无机化合物或含铀无机物具有本征闪烁能力，作为射线闪烁体，提高了闪烁体的性能，为利用铀元素进行各类型化学组成与形态(有机无机、无机)的闪烁体开发提供了新理念。
本发明公开了含铀化合物作为闪烁体的应用，含铀化合物为含铀有机无机杂化物或含铀无机物，含铀有机无机杂化物为式(Ⅰ)的含铀有机羧酸盐或式(Ⅱ)的含铀有机磷酸盐：
含铀无机物为式(Ⅲ)的含铀非金属酸盐、式(Ⅳ)的含铀金属盐或式(Ⅴ)的含铀卤化物：
其中，
式(Ⅰ)中的R1选自苯基、取代苯基或烷基；优选地，烷基为C1-C8烷基；n＝1或2；
式(Ⅱ)中的R2选自苯基、取代苯基或烷基；优选地，烷基为C1-C8烷基；n＝1或2；
式(Ⅲ)的M选自B、N、Si、Se、P、As、S或Te元素；n＝1或2；
式(Ⅳ)的Y选自Mo、V、Cr、Nb、W、Re、Ga、Ge、Sb或Sn元素；m为1，则n为2；m为2，则n为1；
式(Ⅴ)的X选自F元素、Cl元素、Br元素或I元素；
式(Ⅱ)、式(Ⅲ)和式(Ⅳ)的An+独立地选自四甲基铵阳离子、Na+、K+、NH4 +、Li+、Rb+、Cs+、Mg2+、Ca2+、Sr2+、Ba2+、Pb2+或Bi2+；
式(Ⅴ)的B+选自Na+、K+、Li+、Rb+、Cs+或
其中，R3、R4、R5和R6独立地选自氢、烷基、苯基、苯基或含氮苯基。
进一步地，R1为苯基或烷基。
进一步地，式(Ⅰ)的含铀有机羧酸盐为UO2(C9O6H4)(H2O)，以下简称SCU-9，其结构式如下：
传统闪烁体多以离子键结合(如CsI:Tl)，本发明提供的铀酰有机无机杂化材料SCU-9以共价方式键合，具有较高的辐射抗性和水稳定性。SCU-9的密度仅有2.85g/cm3，但其在医学射线成像应用范围内(＞20KeV)对射线阻止能力明显优于目前商用材料CsI:Tl(其密度4.85g/cm3)，因此以铀酰为发光中心的材料对射线阻止能力可通过材料设计进一步提高。
进一步地，UO2(C9O6H4)(H2O)的制备方法包括以下步骤：
将硝酸双氧铀(UO2(NO3)2·6H2O)、硼酸(H3BO3)和均苯三酸溶于水，在密闭条件下于190-250℃下反应，冷却、洗涤后得到UO2(C9O6H4)(H2O)。
进一步地，硝酸双氧铀、硼酸和均苯三酸的摩尔比为0.8-1:1-10:1-2。
进一步地，在式(Ⅱ)中，n＝1，R2为苯基，An+为四甲基铵阳离子。
进一步地，式(Ⅱ)的含铀有机磷酸盐的结构式如下：
进一步地，在式(Ⅲ)中，n＝1，M为B元素，An+为Na+。其分子式为Na[(UO2)B6O10(OH)]，以下简称为NaBUO-4。
进一步地，在式(Ⅳ)中，n＝1，m＝2，Y为Mo元素，An+为Na+、Li+、K+、Rb+或Cs+；
或n＝2，m＝1，Y为Mo元素，An+为Mg2+、Ca2+、Sr2+、Ba2+、Pb2+或Bi2+。
进一步地，在式(Ⅴ)中，X为Cl元素，B+为
其中，R3、R4、R5和R6独立地选自氢、烷基、苯基、苯基或含氮苯基。优选地，B+为NH4 +或
本发明提出了含铀化合物的新用途，含铀化合物作为闪烁体，铀具备优异的发光和材料可设计性能，是闪烁体研究与开发仍然未引入的一个发光元素。铀元素最稳定价态为六价，其化学形式为铀酰(UO2 2+)，其重要特点是铀酰分子轨道跃迁导致的绿色荧光发射，与镧系发光元素相比，铀酰发光为本征发光，不需引入传递能量的配体，可直接由激发源能量传递至元素本身发光。同时，铀是地球上存在的最后一个稳定元素，本身具有较高的密度和射线阻止能力。如图1所示，与主流闪烁体核心元素W、Pb、Bi、Tl等相比，铀具有最强的射线阻止能力。
借由上述方案，本发明至少具有以下优点：
本发明提出了利用铀元素作为闪烁体的方法和概念，包括含铀有机无机杂化物或含铀无机物，材料性能优越、设计空间大，提供了一种全新的闪烁体材料设计理念。
上述说明仅是本发明技术方案的概述，为了能够更清楚了解本发明的技术手段，并可依照说明书的内容予以实施，以下以本发明的较佳实施例并配合附图详细说明如后。
附图说明
图1是元素密度与射线阻滞能力图；
图2是X射线测试实验装置结构图；
图3是不同物质的X射线荧光光谱图；
图4是不同X射线功率与SCU-9荧光强度的关系图；
图5为SCU-9和CsI:Tl辐照稳定性对比结果及辐照稳定性变化趋势；
图6为SCU-9和CsI:Tl湿度稳定性对比结果及湿度稳定性变化趋势；
图7是30eV-30KeV X射线能量范围内，SCU-9和CsI:Tl材料对于射线的阻止能力测试结果。
具体实施方式
下面结合附图和实施例，对本发明的具体实施方式作进一步详细描述。以下实施例用于说明本发明，但不用来限制本发明的范围。
实施例1SCU-9晶体的合成
将反应物UO2(NO3)2·6H2O、H3BO3和均苯三酸以摩尔比为1:10:1的比例置入聚四氟乙烯反应釜中，加少量去离子水溶解，密封，升温至200℃，加热3天，后逐渐冷却至室温，产物用大量沸水洗涤，至硼酸全部溶解，所得晶体产物用乙醇洗涤，后于室温下晾干，得到SCU-9晶体。该产物晶体的中心金属UO2 2+与羧酸配位形成的一维链状聚合物，密度为2.85g/cm3。
采用X射线测试实验装置测试SCU-9晶体在X射线荧光光谱图，其中，X射线测试实验装置结构如图2所示，图中样品在本实施例中即为SCU-9晶体，测试结果如图3中上方曲线所示。
此外，测试不同X射线功率与SCU-9荧光强度的关系，以CsI:Tl作为对照，实验结果表明随着X射线能量的增加，样品荧光强度也会增加(图4b，其中电压均为40kV)，并且两者呈线性关系(图4a)，符合闪烁体应用的特征。
辐射下的发光稳定性是闪烁体性能的另一个特性，图5a为SCU-9和CsI:Tl辐照稳定性对比结果，图5b、c分别为SCU-9和CsI:Tl的辐照稳定性变化趋势，随着剂量的增加，SCU-9和CsI:Tl的发光输出均呈下降趋势，结果显示在最终的53Gy剂量辐射下SCU-9仍然保持65％的发光输出，相同条件下的CsI:Tl仅为20％左右。同样为了扩大应用范围，高湿度下闪烁体的稳定性也是一项必测得性质，实验结果如图6所示，图6a为SCU-9和CsI:Tl湿度稳定性对比结果，图6b、c分别为SCU-9和CsI:Tl的湿度稳定性变化趋势，随着相对湿度的增加，SCU-9和CsI:Tl的发光输出均呈下降趋势，在95％湿度下，CsI:Tl光输出减小到10％以下，而SCU-9仍保持80％左右的光输出量。
计算30eV-30KeV X射线能量范围内，SCU-9和CsI:Tl材料对于射线的阻止能力，如图7所示，20KeV以上，SCU-9化合物对射线的阻止能力强于商用产品CsI:Tl。
实施例2(NaBUO-4)的合成
将NaNO3、H3BO3和UO2(NO3)2·6H2O以3:15:1摩尔比置入聚四氟乙烯反应釜中，加少量去离子水溶解，密封，升温至190℃，加热1天，后逐渐冷却至室温，产物用大量沸水洗涤，至硼酸全部溶解，所得晶体产物用乙醇洗涤，后于室温下晾干，得到(NaBUO-4)。
按照实施例1中的方法，测试(NaBUO-4)的X射线荧光光谱图，结果如图3中下方曲线所示。
实施例3
式(Ⅱ)的含铀有机磷酸盐的结构式如下，以下简称([TMA][(UO2)2(1,3-pbpH)(1,3-pbpH2)])：
将间苯二磷酸(1,3-bppH4)、四甲基氢氧化铵和UO2(NO3)2·6H2O以2:2:1摩尔比置入聚四氟乙烯反应釜中，加1滴HF酸，加1mL去离子水溶解，密封，升温至200℃，加热3天，后逐渐冷却至室温，产物用水洗涤，后所得晶体产物用乙醇洗涤，后于室温下晾干，得到[TMA][(UO2)2(1,3-pbpH)(1,3-pbpH2)]化合物。该化合物可作为闪烁体使用。
实施例4
式(Ⅳ)的含铀金属盐结构式如下，其中，n＝1，m＝2，Y为Mo元素，An+为Na+，以下简称Na2UO2(MoO4)2H2O：
将Na2MoO4和UO2(NO3)2·6H2O以1:4摩尔比置入聚四氟乙烯反应釜中，加少量去离子水溶解，密封，升温至200℃，加热3天，后逐渐冷却至室温，产物用大量沸水洗涤，后所得晶体产物用乙醇洗涤，后于室温下晾干，得到Na2UO2(MoO4)2H2O。该化合物可作为闪烁体使用。
实施例4
式(Ⅴ)的X为Cl元素，B+为
其结构式如下，以下简称[BTA]2[UO2Cl4]化合物：
UO2(CH3COOH)2·2H2O和苯基三乙基氢氧化铵以1:2.9摩尔比置入烧杯中，加2mL盐酸，再加10mL去离子水溶解，后在室温下挥发5-7天，至有晶体析出，产物用水洗涤，后所得晶体产物用乙醇洗涤，后于室温下晾干，得到[BTA]2[UO2Cl4]化合物。该化合物可作为闪烁体使用。
以上所述仅是本发明的优选实施方式，并不用于限制本发明，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明技术原理的前提下，还可以做出若干改进和变型，这些改进和变型也应视为本发明的保护范围。
Claims (8)
1.含铀化合物作为闪烁体的应用，其特征在于：所述含铀化合物为含铀有机无机杂化物或含铀无机物，所述含铀有机无机杂化物为式(Ⅰ)的含铀有机羧酸盐或式(Ⅱ)的含铀有机磷酸盐：
所述含铀无机物为式(Ⅲ)的含铀非金属酸盐、式(Ⅳ)的含铀金属盐或式(Ⅴ)的含铀卤化物：
其中，m为1或2；n为1或2；
式(Ⅰ)中的R1选自苯基、取代苯基或烷基；
式(Ⅱ)中的R2选自苯基、取代苯基或烷基；
式(Ⅴ)的X选自F元素、Cl元素、Br元素或I元素；
式(Ⅱ)的An+独立地选自四甲基铵阳离子、Na+、K+、NH4 +、Li+、Rb+、Cs+、Mg2+、Ca2+、Sr2+、Ba2 +、Pb2+或Bi2+；
式(Ⅴ)的B+选自Na+、K+、Li+、Rb+、Cs+或
其中，R3、R4、R5和R6独立地选自氢、烷基、苯基或含氮苯基；
在式(Ⅲ)中，n＝1，M为B元素，An+为Na+；
在式(Ⅳ)中，n＝1，m＝2，Y为Mo元素，An+为Na+、Li+、K+、Rb+或Cs+；
或n＝2，m＝1，Y为Mo元素，An+为Mg2+、Ca2+、Sr2+、Ba2+、Pb2+或Bi2+。
2.根据权利要求1所述的应用，其特征在于：R1为苯基或烷基。
3.根据权利要求2所述的应用，其特征在于，式(Ⅰ)的含铀有机羧酸盐为UO2(C9O6H4)(H2O)，其结构式如下：
4.根据权利要求3所述的应用，其特征在于，UO2(C9O6H4)(H2O)的制备方法包括以下步骤：
将硝酸双氧铀、硼酸和均苯三甲酸溶于水，在密闭条件下于190-250℃下反应，冷却、洗涤后得到UO2(C9O6H4)(H2O)。
5.根据权利要求4所述的应用，其特征在于：所述硝酸双氧铀、硼酸和均苯三甲酸的摩尔比为0.8-1:1-10:1-2。
6.根据权利要求1所述的应用，其特征在于：在式(Ⅱ)中，n＝1，R2为苯基，An+为四甲基铵阳离子。
7.根据权利要求6所述的应用，其特征在于，式(Ⅱ)的含铀有机磷酸盐的结构式如下：
8.根据权利要求1所述的应用，其特征在于：在式(Ⅴ)中，X为Cl元素，B+为
其中，R3、R4、R5和R6独立地选自氢、烷基、苯基或含氮苯基。
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