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Growth method of scorched yttrium silicate scintillation single crystal by means of floating zone

A technology of yttrium disilicate and growth method, which is applied in the direction of single crystal growth, single crystal growth, crystal growth, etc., can solve the problems that hinder the single crystal growth and application of YPS, prone to phase transition, crystal polycrystal, etc., and achieve Large application value, large subcooling degree, and low cost effect

Inactive Publication Date: 2012-01-25
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the prior art, the growth technology of YPS single crystal mainly contains following two schemes: one is according to phase diagram (referring to RussianChemistry Bulletin 1961, the 10th volume, the 502nd page), the YPS of chemical dose ratio (Y 2 o 3 : SiO 2 =1:2) peritectic reaction will occur during the cooling process; the second is that YPS has 5 (or 6) different structural phases in the temperature range of 1535-1225 °C (see Journal of Solid State Chemistry 2000, No. 16 Volume, p. 149), where the relationship between the four phases at high temperature is: It can be seen from the relationship that YPS has a relatively complex phase transition relationship, which can easily lead to the crushing of the material rod during the pre-sintering process of the raw material, and the phase transition is very easy to occur during the cooling process after the crystal growth, which in turn leads to polycrystalline crystals. and cracking
The above two problems hinder the growth and application of single crystal of YPS

Method used

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  • Growth method of scorched yttrium silicate scintillation single crystal by means of floating zone
  • Growth method of scorched yttrium silicate scintillation single crystal by means of floating zone
  • Growth method of scorched yttrium silicate scintillation single crystal by means of floating zone

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Growth of pure YPS single crystal:

[0031] (1) SiO with a raw material purity of 4N 2 and Y 2 o 3 , pre-fire the raw material at 200°C under an air atmosphere to remove H in the raw material 2 O and CO 2 , press Y 2 o3 100mol%, SiO 2 The mole percentage is compounded at 205 mol%.

[0032] (2) After the raw materials are fully mixed, put them into a Φ10mm rubber tube and seal them, and press them into a relatively dense material rod under the pressure of 100Mpa by isostatic pressing, and then hang it in the muffle furnace with Pt wire for pre-sintering. The sintering temperature is 1200° C., and the sintering time is 20 hours to produce a polycrystalline rod.

[0033] (3) Hang the polycrystalline rod on the upper end of the floating zone furnace with a nickel-chromium wire, and install the seed crystal on the lower end. After installation, seal it with a quartz tube and let in argon gas, then heat up until the rod and seed crystal melt, and at the same time, the ...

Embodiment 2

[0038] Ce-doped YPS single crystal (Ce 0.005 Y 0.995 ) 2 Si 2 o 7 of growth:

[0039] (1) The raw material purity is 4N SiO 2 , Y 2 o 3 and CeO 2 , pre-fire the raw material at 200°C under an air atmosphere to remove H in the raw material 2 O and CO 2 , press Y 2 o 3 100mol%, SiO 2 105mol% and CeO 2 It is compounded at a molar percentage of 0.5 mol%.

[0040] (2) After the raw materials are fully mixed, put them into a Φ10mm rubber tube and seal them, and press them into a relatively dense material rod under the pressure of 100Mpa by isostatic pressing, and then hang it in the muffle furnace with Pt wire for pre-sintering. The sintering temperature is 1200° C., and the sintering time is 20 hours to produce a polycrystalline rod.

[0041] (3) Hang the polycrystalline rod on the upper end of the floating zone furnace with a nickel-chromium wire, and install the seed crystal on the lower end. After installation, seal it with a quartz tube and let in argon gas, then...

Embodiment 3

[0046] Growth of pure YPS single crystal:

[0047] (1) SiO with a raw material purity of 4N 2 and Y 2 o 3 , pre-fire the raw material at 200°C under an air atmosphere to remove H in the raw material 2 O and CO 2 , press Y 2 o 3 with SiO 2 The ratio of ingredients is 1:2.

[0048] (2) After the raw materials are fully mixed, put them into a Φ10mm rubber tube and seal them, and press them into denser rods under the pressure of 200Mpa by isostatic pressing, and then hang them in the muffle furnace with Pt wires for pre-sintering and sintering. The temperature is 1000° C., and the sintering time is 100 hours to produce a polycrystalline rod.

[0049] (3) Hang the polycrystalline rod on the upper end of the floating zone furnace with a nickel-chromium wire, and install the seed crystal on the lower end. After installation, seal it with a quartz tube and let in argon gas, then heat up until the rod and seed crystal melt, and at the same time, the rod Rotate in the opposite ...

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Abstract

The invention belongs to the technical fields of inorganic compound crystal and production, in particular to a growth method of scorched yttrium silicate scintillation single crystal by means of a floating zone. The method comprises the steps of: raw materials synthesizing, melting, inoculating, growing and temperature reducing, wherein in the process of temperature reducing after the crystal growing, when being over the temperature of a transformation point, the temperature reducing velocity is 30-50 DEG C / minute, and when being below the temperature of the transformation point, the temperature reducing velocity is 100-200 DEG C. The growth method solves the problems of nonconforming fusion and phase change in the process of the growth of the YPS crystal, and can obtain YPS high temperature Delta phase crystal with better quality.

Description

technical field [0001] The invention belongs to the technical field of inorganic compound crystals and their manufacture, and in particular relates to a method for growing a yttrium disilicate scintillation single crystal by a floating zone method. Background technique [0002] Rare earth doped yttrium disilicate Y 2 Si 2 o 7 (referred to as YPS) single crystal belongs to the hexagonal crystal system, the space group is Pna2 1 , lattice constant a=13.66 b=5.016 c=8.149 The melting point is 1775°C. [0003] In the prior art, the growth technology of YPS single crystal mainly contains following two schemes: one is according to phase diagram (referring to RussianChemistry Bulletin 1961, the 10th volume, the 502nd page), the YPS of chemical dose ratio (Y 2 o 3 : SiO 2 =1:2) peritectic reaction will occur during the cooling process; the second is that YPS has 5 (or 6) different structural phases in the temperature range of 1535-1225 °C (see Journal of Solid State Chem...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/34C30B13/00
Inventor 冯鹤丁栋舟任国浩潘尚可陆晟张卫东
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI