WO2021000623A1 - 一种稀土离子掺杂氧化镧镥超快闪烁晶体及其制备方法和应用 - Google Patents

一种稀土离子掺杂氧化镧镥超快闪烁晶体及其制备方法和应用 Download PDF

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WO2021000623A1
WO2021000623A1 PCT/CN2020/084480 CN2020084480W WO2021000623A1 WO 2021000623 A1 WO2021000623 A1 WO 2021000623A1 CN 2020084480 W CN2020084480 W CN 2020084480W WO 2021000623 A1 WO2021000623 A1 WO 2021000623A1
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crystal
rare earth
growth
oxide
scintillation crystal
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赵衡煜
徐军
王东海
李东振
王庆国
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南京同溧晶体材料研究院有限公司
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
    • C09K11/7767—Chalcogenides
    • C09K11/7769—Oxides
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/16—Oxides
    • C30B29/22—Complex oxides

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  • the invention belongs to the field of rare earth ion crystal growth, and in particular relates to a rare earth ion doped lanthanum lutetium oxide ultrafast scintillation crystal and a preparation method and application thereof.
  • a scintillation material is a material that can absorb high-energy particles or rays to emit visible photons.
  • the ultrafast scintillation material refers to a scintillator material with a response time of less than 4ns (10 -9 s).
  • Such materials play a pivotal role in pulsed radiation detection, solar neutrino detection, and reaction dynamics, inertial confinement of nuclear fusion, and cosmic ray research.
  • the scintillator is used to detect ionizing radiation in most applications, so the scintillator is required to have a high blocking ability against ionizing radiation, that is, the scintillator is required to have high Density and contains elements with high atomic number.
  • Lanthanum lutetium oxide (LuLaO 3 ) has a very high density (8.87g/cm 3 ), which is the third-density matrix material in currently known scintillators, only slightly lower than hafnium oxide crystal HfO 2 (9.68g/cm 3 ) And lutetium oxide Lu 2 O 3 crystals (9.42g/cm 3 ). This makes it very high in stopping various rays (x-rays, ⁇ -rays) and is a potential scintillation material.
  • the melting point of the above-mentioned hafnium oxide crystal is 2830°C
  • the melting point of lutetium oxide crystal is 2450°C, which are higher than the melting points of common crucible materials platinum (Pt), iridium (Ir), and molybdenum (Mo).
  • platinum Pt
  • Ir iridium
  • Mo molybdenum
  • the melting point of lanthanum lutetium oxide is 2120°C, and molybdenum crucible can be used for large-scale growth.
  • lanthanum lutetium oxide has the potential for commercial development and application, and it is an excellent oxide scintillation crystal with high melting point and high damage threshold that has been neglected for a long time.
  • LaLuO 3 belongs to perovskite oxide crystals. Compared with the above-mentioned halide perovskite crystals, LaLuO 3 has the advantages of high melting point and high density.
  • Ce 3+ ions are a good scintillator luminescence center, which can usually achieve an ultra-fast response time of 0.2-1ns, and has good commercial applications in LYSO:Ce crystals.
  • Yb 3+ in doped scintillation crystals has achieved ultra-fast scintillation reports of the order of 1-5 ns in YAG, LuAG, YAP and other crystals.
  • ultrafast photomultiplier tubes reaching 0.4ns, the shortcomings of the low light yield of Yb 3+ ion scintillation crystals (usually around 500Ph) have been greatly improved.
  • the rare earth ion doped lanthanum lutetium oxide ultra-fast scintillation crystal uses intrinsic defects or rare earth ions as activating ions.
  • the rare earth ion is any one of Yb 3+ , Eu 3+ , Pr 3+ , Ce 3+
  • the density of the ultrafast scintillation crystal is 8.87g/cm 3
  • the melting point is 2100°C
  • the modulated ion can be any one of Ca 2+ , Mg 2+ , Ga 2+ , Er 3+ , Tb 3+ , Si 4+ , and Ge 4+ .
  • the scintillation crystal includes a single crystal and a single crystal fiber.
  • the preparation method steps are as follows:
  • crystal growth methods including but not limited to floating zone method, cold crucible method, micro-drawing method, warm extraction method, heat exchange method, descending method Either, use high melting point metals as crucibles, crystal growth temperature is 2000-2200°C, seed crystal inoculation temperature is 2150-2200°C, growth atmosphere is pure Ar gas, (1-10%) H 2 + (90- 99%) Ar, (0.1-1%) O 2 + (99-99.9%) H 2 .
  • the crucible in step (2) is a crucible made of tungsten, rhenium, tantalum or any combination of alloys.
  • the crucible when the floating zone method is used in step (2), the crucible is not used, and the growth atmosphere also includes an air atmosphere or a reducing atmosphere with a higher proportion of oxygen partial pressure.
  • the present invention provides a rare earth ion doped lanthanum lutetium oxide ultra-fast scintillation crystal, which is a perovskite ABO3 structure with intrinsic defects or rare earth ions as active ions, or rare earth ions as the main active ions and doped with modulated ions ,
  • the scintillation crystal obtained by a suitable production method, the production cost is reduced, and the performance of the scintillation crystal can be guaranteed.
  • it has stable and excellent optical performance.
  • 340nm wavelength fluorescent light has a short response time.
  • Crystal growth use the pulling method for crystal growth, put the raw materials into the molybdenum metal crucible, and use pure Ar gas for protection.
  • the temperature is increased to 2150°C to fully melt, and it is kept for about 10 minutes for the melt to form non-forced convection.
  • the speed is 5rad/, and the seeds are slowly inserted into the melt after 10 minutes of roasting. After they are stabilized, they are slowly lifted to release the shoulders at a rate of 2mm/h. When the shoulders reach the diameter of 40mm, it enters the equal diameter stage, and the pulling speed is 1mm/h.
  • the isodiametric duration is 100 hours. Then enter the neck and pull off. After pulling off, the crystal is suspended 5 cm above the melt and enters the in-situ annealing stage. After 100 hours of annealing, the dislocation and thermal stress in the crystal lattice are fully eliminated and the crystal quality is improved.
  • Crystal growth using the floating zone method for crystal growth, using a high-power floating zone furnace from Sci-direct, with a slit efficiency of 12% incipient melting, 14% of the upper rod and the lower rod butt, and the speed of 5rad/s. After it is stable, keep the spot position unchanged, lower the upper rod and the lower rod at a rate of 10mm/h, and the crystal grows upward at a rate of 10mm/h until the crystal growth is completed.
  • Crystal growth use the pulling method for crystal growth, put the raw materials into the molybdenum metal crucible, and use pure Ar gas for protection.
  • the temperature is increased to 2150°C to fully melt, and it is kept for about 10 minutes for the melt to form non-forced convection.
  • the speed is 5rad/, and the seeds are slowly inserted into the melt after 10 minutes of roasting. After they are stabilized, they are slowly lifted to release the shoulders at a rate of 2mm/h. When the shoulders reach the diameter of 40mm, it enters the equal diameter stage, and the pulling speed is 1mm/h.
  • the isodiametric duration is 100 hours. Then enter the neck and pull off. After pulling off, the crystal is suspended 5 cm above the melt and enters the in-situ annealing stage. After 100 hours of annealing, the dislocation and thermal stress in the crystal lattice are fully eliminated and the crystal quality is improved.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Metallurgy (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Luminescent Compositions (AREA)
  • Measurement Of Radiation (AREA)

Abstract

稀土离子掺杂氧化镧镥超快闪烁晶体，为以本征缺陷或稀土离子作为激活离子，或以稀土离子为主要激活离子并掺调制离子的钙钛矿ABO3结构，提供了闪烁晶体的制备方法，在高能射线探测领域中，在激发状态下，获得340nm波长荧光发光时相应时间短。

Description

一种稀土离子掺杂氧化镧镥超快闪烁晶体及其制备方法和应用 技术领域
本发明属于稀土离子晶体生长领域，特别涉及一种稀土离子掺杂氧化镧镥超快闪烁晶体及其制备方法和应用。
背景技术
闪烁材料是一种能吸收高能粒子或射线而发出可见光子的材料，其中超快闪烁材料是指响应时间小于4ns(10 -9s)的闪烁体材料。此类材料在脉冲辐射探测(Pulsed radiation detection),太阳中微子探测，和反应动力学，惯性约束核聚变，宇宙射线研究中发挥着支柱性的作用。
尽管不同的应用对闪烁体会提出不同的要求，但闪烁体在绝大多数应用中都被用于检测电离辐射，所以要求闪烁体对电离辐射要有高的阻断能力，即要求闪烁体具有高密度并含有原子序数大的元素。
氧化镧镥(LuLaO 3)具有极高的密度(8.87g/cm 3)，是目前已知的闪烁体中密度第三的基质材料，仅略低于氧化铪晶体HfO 2(9.68g/cm 3)和氧化镥Lu 2O 3晶体(9.42g/cm 3).这使得它对各类射线(x射线、γ射线)的阻止本领相当高，是有潜力的闪烁材料。此外，上述氧化铪晶体的熔点为2830℃，氧化镥晶体的熔点为2450℃，均高于常见的坩埚材料铂金(Pt),铱金(Ir),钼(Mo)的熔点，在实验室中使用昂贵的铼金属坩埚，成本价格为4万人民币/公斤，且仅能获得厘米级尺寸的完整单晶,上述不利因素极大的限制了商业应用的预期。氧化镧镥的熔点温度为2120℃，可以使用钼坩埚进行大尺寸生长。综上所述，氧化镧镥具备商业开发应用的可能，是长期以来被忽视的优良的高熔点高损伤阈值的氧化物闪烁晶体。
表1超快闪烁体性能(按密度排序)
Figure PCTCN2020084480-appb-000001
Figure PCTCN2020084480-appb-000002
最近，具有ABC 3结构的钙钛矿结构的闪烁晶体收到了极大的关注，国际上先后报道了RhPbCl 3，CsPbCl 3等晶体的闪烁性能。LaLuO 3属于钙钛矿氧化物晶体，相较于上述卤化物钙钛矿晶体，具有熔点高，密度大的优点。
在超快闪烁应用领域，Ce 3+离子是良好的闪烁体发光中心，通常可以实现0.2-1ns级的超快响应时间，并在在LYSO:Ce晶体有良好的商业应用。Yb 3+在掺杂的闪烁晶体在YAG，LuAG，YAP等晶体中实现了1-5ns量级的超快闪烁报道。随着超快光电倍增管的发展达到了0.4ns，Yb 3+离子闪烁晶体的光产额较低(通常500Ph左右)的缺点得到了极大的改善。
发明内容
为了克服上述现有技术存在的不足，获得一种低成本且光学性能优良的闪烁晶体，本发明提供的稀土离子掺杂氧化镧镥超快闪烁晶体，为以本征缺陷或稀土离子作为激活离子，或以稀土离子为主要激活离子并掺调制离子的钙钛矿ABO 3结构，LaLuO 3氧化物晶体为基质。
作为改进，稀土离子为Yb 3+，Eu 3+，Pr 3+，Ce 3+中任一种，所述超快闪烁晶体的密度为8.87g/cm 3，熔点为2100℃，采用生长技术覆盖浮区法，提拉法，导模法，热交换法，下降法中任一种高温晶体生长方法进行生长。
作为改进，所述调制离子Ca 2+，Mg 2+,Ga 2+,Er 3+，Tb 3+，Si 4+,Ge 4+中任一种。
同时，提供了一种稀土离子掺杂氧化镧镥闪烁晶体的生长方法，闪烁晶体包括单晶和单晶光纤，制备方法步骤如下：
(1)按照化学通式La 1-xLu xO 3称取化学计量比的99.999％纯度氧化镧和99.99％纯的氧化镥原料，99.99％氧化镱或所需的稀土离子氧化物，氧化镧在180-220℃烘烧除水；混合均匀后，根据需要等静压成料饼或料棒，等静压压力为100-220MPa，烧结温度为1350-1650℃，恒温2-12小时；
(2)选用氧化镧镥陶瓷棒或单晶作为籽晶进行晶体生长，采用晶体生长方法包括但不限于浮区法，冷坩埚法，微下拉法，温提法，热交换法，下降法中任一种，使用等高熔点金属作为坩埚，晶体生长温度为2000-2200℃，籽晶接种温度为2150-2200℃，生长气氛为纯Ar气，(1-10％)H 2+(90-99％)Ar，(0.1-1％)O 2+(99-99.9％)H 2。
作为改进，步骤(2)中所述坩埚为钨，铼，钽任一种金属或任一组合的合金制成的坩埚。
作为改进，步骤(2)中采用浮区法时，不选用属于坩埚，生长氛围还包括空气气氛或含有较高比例氧气分压的还原性气氛。
同时，还提供了上述超快闪烁晶体在高能射线探测的闪烁材料中的应用。
同时，还提供了采用上述生长方法获得的晶体在高能射线探测的闪烁材料中的应 用。
有益效果：本发明中提供了稀土离子掺杂氧化镧镥超快闪烁晶体，为以本征缺陷或稀土离子作为激活离子，或以稀土离子为主要激活离子并掺调制离子的钙钛矿ABO3结构，还通过提供了合适的生产方法获得的闪烁晶体，降低了生产成本同时，还可以保证闪烁晶体的性能，尤其在高能射线探测领域中，具有稳定且优良的光学性能，具有激发状态下，获得340nm波长荧光发光时响应时间短的特性。
具体实施方式
下面对本发明作出进一步说明。
实施例1
1)配制料块：采用纯度为99.99％的Yb 2O 3和Lu 2O 3，经200℃烘烧的99.999％的La 2O 3作为初始原料，并按摩尔比3：44.5：52.5进行配料。原料经过充分球磨混合后用等静压机压制成料饼，装入氧化铝陶瓷坩埚投入马弗炉中进行烧结。烧料温度为1500℃，恒温10小时，升降温速率100℃/h。
2)晶体生长：使用提拉法进行晶体生长，将原料投入钼金属坩埚内，采用纯Ar气体保护。升温至2150℃充分熔化，保持约10分钟是熔体形成非强迫对流。籽晶下降至熔体液面上方1-3cm进行烤种后,转速为5rad/，烤种10分钟后缓慢插入熔体中，待稳定后缓缓提起放肩，放肩速率为2mm/h。放肩至直径40mm时进入等径阶段，此时拉速为1mm/h。等径持续时间为100小时。之后进入缩颈并拉脱。拉脱后，晶体悬挂于熔体上方5cm并进入原位退火阶段，经过100小时退火，充分消除晶格内的位错及热应力，提高晶体质量。
3)所获晶体为无色透明。经XRD测定为单晶钙钛矿相。在X射线激发发光30kV加速电压，10keV X-ray激发下，出现～340nm的荧光发光。响应时间为2ns。
实施例2
1)配制料块：采用纯度为99.99％的Ce 2O 3和Lu 2O 3，经200℃烘烧的99.999％的La 2O 3作为初始原料，并按摩尔比0.2：47.3：52.5进行配料。原料经过充分球磨混合后用等静压机压制成细棒，尺寸为φ8*70mm，装入氧化铝陶瓷坩埚投入马弗炉中进行烧结。烧料温度为1500℃，恒温10小时，升降温速率100℃/h。煅烧完毕后，对料棒进行加工滚圆，制成φ5*70mm料棒2根，分别作为浮区法长晶用的料棒和籽晶棒。
2)晶体生长：使用浮区法进行晶体生长，使用Sci-direct公司高功率浮区炉，狭缝效率为12％初熔化，14％上棒与下棒对接，转速5rad/s。待稳定后，保持光斑位置不变，以10mm/h速率下降上棒与下棒，晶体以10mm/h速率向上生长，直至长晶完成。
3)所获0.2％Ce：LaLuO 3晶体为淡红色透明。经XRD测定为单晶钙钛矿相。经过定向后，沿着(100)方向切割晶体并抛光制样。在X射线激发发光其中30kV加速电压，10keV X-ray激发下，出现～340nm的荧光发光。响应时间为1ns。
实施例3
1)配制料块：采用纯度为99.99％的Yb 2O 3，CaCO 3和Lu 2O 3，经200℃烘烧的99.999％的La 2O 3作为初始原料，并按摩尔比3：0.5：44：52.5进行配料。原料经过充分球磨混合后用等静压机压制成料饼，装入氧化铝陶瓷坩埚投入马弗炉中进行烧结。烧料温度为1500℃，恒温10小时，升降温速率100℃/h。
2)晶体生长：使用提拉法进行晶体生长，将原料投入钼金属坩埚内，采用纯Ar气体保护。升温至2150℃充分熔化，保持约10分钟是熔体形成非强迫对流。籽晶下降至熔体液面上方1-3cm进行烤种后,转速为5rad/，烤种10分钟后缓慢插入熔体中，待稳定后缓缓提起放肩，放肩速率为2mm/h。放肩至直径40mm时进入等径阶段，此时拉速为1mm/h。等径持续时间为100小时。之后进入缩颈并拉脱。拉脱后，晶体悬挂于熔体上方5cm并进入原位退火阶段，经过100小时退火，充分消除晶格内的位错及热应力，提高晶体质量。
3)所获3％Yb,0.5Ca：LaLuO3晶体为无色透明。经XRD测定为单晶钙钛矿相。在X射线激发发光(30kV加速电压,10keV X-ray)激发下，出现～340nm的荧光发光。响应时间为2ns。
以上所述实施例仅表达了本发明的几种实施方式，其描述较为具体和详细，但并不能因此而理解为对发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。因此，本发明专利的保护范围应以所附权利要求为准。

Claims (8)

  1. 一种稀土离子掺杂氧化镧镥的超快闪烁晶体，其特征在于：为以本征缺陷或稀土离子作为激活离子，或以稀土离子为主要激活离子并掺调制离子的钙钛矿ABO 3结构，LaLuO 3氧化物晶体为基质。
  2. 根据权利要求1所述超快闪烁晶体，其特征在于：稀土离子为Yb 3+，Eu 3+，Pr 3+，Ce 3+中任一种，所述超快闪烁晶体的密度为8.87g/cm 3，熔点为2100℃，采用生长技术覆盖浮区法，提拉法，导模法，热交换法，下降法中任一种高温晶体生长方法进行生长。
  3. 根据权利要求1所述超快闪烁晶体，其特征在于：所述调制离子Ca 2+，Mg 2+,Ga 2+,Er 3+，Tb 3+，Si 4+,Ge 4+中任一种。
  4. 一种稀土离子掺杂氧化镧镥闪烁晶体的生长方法，其特征在于：闪烁晶体包括单晶和单晶光纤，制备方法步骤如下：
    (1)按照化学通式La 1-xLu xO 3称取化学计量比的99.999％纯度氧化镧和99.99％纯的氧化镥原料，99.99％氧化镱或所需的稀土离子氧化物，氧化镧在180-220℃烘烧除水；混合均匀后，根据需要等静压成料饼或料棒，等静压压力为100-220MPa，烧结温度为1350-1650℃，恒温2-12小时；
    (2)选用氧化镧镥陶瓷棒或单晶作为籽晶进行晶体生长，采用晶体生长方法包括但不限于浮区法，冷坩埚法，微下拉法，温提法，热交换法，下降法中任一种，使用等高熔点金属作为坩埚，晶体生长温度为2000-2200℃，籽晶接种温度为2150-2200℃，生长气氛为纯Ar气，(1-10％)H 2+(90-99％)Ar，(0.1-1％)O 2+(99-99.9％)H 2。
  5. 根据权利要求4所述生长方法，其特征在于：步骤(2)中所述坩埚为钨，铼，钽任一种金属或任一组合的合金制成的坩埚。
  6. 根据权利要求4所述生长方法，其特征在于：步骤(2)中采用浮区法时，不选用属于坩埚，生长氛围还包括空气气氛或含有较高比例氧气分压的还原性气氛。
  7. 根据权利要求1-3中任一所述超快闪烁晶体在高能射线探测的闪烁材料中的应用。
  8. 根据权利要求4-6任一所述生长方法获得的晶体在高能射线探测的闪烁材料中的应用。
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