Growing method of lithium gadolinium borate crystal

A crystal growth, lithium gadolinium borate technology, applied in crystal growth, single crystal growth, single crystal growth, etc., can solve the problems of limited crystal size, crystal growth cannot be carried out, and crystal erosion

Inactive Publication Date: 2012-10-03
上海上硅中试基地科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] By analyzing the convection conditions of the melt during the growth of lithium gadolinium borate crystals, it is found that when the diameter of the crystals increases to a certain extent, the forced convection of the melt will transfer the heat from the bottom of the crucible to the solid-liquid interface of crystal growth. The temperature at the center of the crystal growth is too high, so that the crystal growth cannot proceed, and even the grown crystal will be ablated, resulting in a concave interface, which makes the crystal growth interface flipped, so that the crystal cannot grow long, and the size of the crystal is limited.

Method used

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  • Growing method of lithium gadolinium borate crystal
  • Growing method of lithium gadolinium borate crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Li according to the composition 6 Ce 0.01 Gd 0.99 B 3 o 9 Weigh Li 2 CO 3 (purity 99.99%) 270g, Gd 2 o 3 (purity is 99.99%) 217.2g, H 3 BO 3 (99.99%) 228.6g and CeO 2 (99.99%) 2.06g, mix evenly, press into a cylindrical block with a diameter of 50mm, put it into a corundum cup, sinter at 450°C for 10 hours, take it out, grind it again, press it into a block again, put it in a horse Sintered at 700°C for 10 hours in a Furnace. After taking it out, put it into a special-shaped iridium gold crucible (the cross-section is shown in figure 1 As shown in ), the single crystal of lithium gadolinium borate is used as the seed crystal, the crystal growth temperature is 800°C, the rotation speed is 3rpm, the pulling speed is 0.5mm / h, and the cooling rate is 0.8°C / h. After 80 hours of growth, it can grow A lithium gadolinium borate single crystal with a diameter of 32 mm and a length of about 40 mm was obtained.

Embodiment 2

[0034] Li according to the composition 6 Ce 0.01 Gd 0.99 B 3 o 9 Weigh Li 2 CO 3 (99.99%) 270g, Gd 2 o 3 (99.99%) 217.2g, H 3 BO3 (99.99%) 237.7g and CeO 2 (99.99%) 2.06g, mix evenly, press into a cylindrical block with a diameter of 50mm, put it into a corundum cup, sinter at 440°C for 11 hours, take it out, grind it again, press it into a block again, put it in a horse Sintered at 750°C for 9 hours in a Furnace. After taking it out, put it into a special-shaped platinum crucible (the cross-section is shown in figure 2 As shown), a piece of iridium gold ring with an inner diameter of 45mm and an outer diameter of 80mm is placed at the mouth of the crucible as a post-heating device. With cerium-doped gadolinium lithium borate single crystal as the seed crystal, the crystal growth temperature is 865°C, the rotation speed is 10rpm, the pulling speed is 0.1mm / h, and the cooling rate is 0.4°C / h. After 60 hours of growth, a diameter of Cerium-doped lithium gadolinium b...

Embodiment 3

[0036] Li according to the composition 6 Ce 0.1 Gd 0.9 B 3 o 9 Weigh LiOH (99.99%) 175.2g, Gd 2 o 3 (99.99%) 199.1g, B 2 o 3 (99.99%) 127.8g and Ce(NO 3 ) 3 (99.99%) 39.8g, mix evenly, press into a cylindrical block with a diameter of 50mm, put it into a corundum cup, sinter at 440°C for 11 hours, take it out, grind it again, press it into a block again, put it in a horse Sintered at 650°C for 11 hours in a Furnace. After taking it out, put it into a special-shaped platinum crucible (the cross-section is shown in figure 2 As shown), a piece of iridium ring with an inner diameter of 50mm and an outer diameter of 80mm is placed at the mouth of the crucible as a post-heating device. Using platinum wire as the seed crystal, the crystal growth temperature is 865°C, the rotation speed is 10rpm, the pulling speed is 0.1mm / h, and the cooling rate is 0.4°C / h. After 60 hours of growth, a diameter of 41mm and a length of 28mm can be grown. Left and right cerium-doped lithium...

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Abstract

The invention discloses a growing method of lithium gadolinium borate crystal, relating to the field of crystal growth. The invention is characterized in that crystal growing material is developed by using a pulling method; the chemical formula of the lithium gadolinium borate crystal is Li6CexGd1-xB3O9, wherein, x is larger than 0 and is 0.1 at most; when the crystal is developed by using the pulling method, a special graphite in which the lower part is in arc shaped or the bottom is tapered serves as a growing graphite. The invention uses the special graphite and a post heating device to overcome the defect that the lithium gadolinium borate crystal developed by using the pulling method is easy to form a concave interface or is hard to grow into big diameter while common cylindrical graphite is used. The crystal developed by using the method has the advantages of big size, high optical quality and the like, can be used for neutron detection and can be used for detecting alpha, beta, gamma rays and the like.

Description

technical field [0001] The invention relates to the field of crystal growth, in particular to a crystal growth method of lithium gadolinium borate crystal. Background technique [0002] Lithium gadolinium borate crystal (the molecular formula is Li 6 Ce x Gd 1-x B 3 o 9 ) detects neutrons by reacting the enriched lithium-6 or boron-10 or gadolinium-155 or gadolinium-157 isotopes in the crystal with neutrons, first reported by J.B.Czirr of the United States in 1996 as neutron detection scintillation Potential uses of crystals. As a new neutron detection scintillation crystal, Li 6 Ce x Gd 1-x B 3 o 9 Has the following advantages: [0003] (1) Elements containing Li, B and Gd three isotopes with large capture cross-sections for neutrons can choose different isotope enrichment combinations according to different detection requirements, and optimize the design of crystal components with higher detection efficiency , so the crystal has strong adaptability. [0004] (...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/22C30B15/00
Inventor 潘尚可杨帆任国浩丁栋舟陆晟张卫东
Owner 上海上硅中试基地科技有限公司
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