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Multi-crucible fused mass growth technique of lithium aluminate and doped lithium aluminate crystal

A technology of crystal growth, lithium aluminate, applied in the direction of crystal growth, single crystal growth, single crystal growth, etc.

Inactive Publication Date: 2011-01-26
上海博晶光电科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, the high melting point of lithium aluminate and the serious lithium volatilization near the melting point limit the growth of lithium aluminate crystals, (see J.Cryst.Growth., 1998, 193: 127), and the multi-crucible descent method is suitable for high melting point crystals. In addition, there is no disturbance in the melt during the growth process, and there is no large-scale flow of the air flow, which can effectively prevent the volatilization of volatile substances in the crystal growth process. The present invention provides an effective lithium aluminate crystal growth technology

Method used

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  • Multi-crucible fused mass growth technique of lithium aluminate and doped lithium aluminate crystal
  • Multi-crucible fused mass growth technique of lithium aluminate and doped lithium aluminate crystal

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Experimental program
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Effect test

Embodiment 1

[0034] Will Al 2 o 3 and Li 2 CO 3 The powder raw materials are fully mixed according to the molar ratio of 1:1, compacted, solid-state sintered in the air at 1200°C for 10 hours, and then loaded with , direction seeds into rectangular columns and cylinders respectively. Shaped 2 molybdenum crucibles. At the same time, it is placed in the high-temperature drop furnace of two stations. After the whole system is sealed, it is powered on and heated up, and the mechanical pump and diffusion pump are started successively to evacuate to 10 -3 Pa, when the furnace temperature reaches 800°C, fill it with argon, continue to heat up to 1600°C, keep it warm for 1 hour, adjust the position of the crucible, melt the top of the raw material and the seed crystal, adjust the temperature gradient of the solid-liquid interface to 10°C / cm, and then start The lowering device starts crystal growth, and the lowering rate of the crucible is 0.1mm / h. After the crystal growth is completed, the t...

Embodiment 2

[0036] separately synthesized by molten salt hydrolysis method doped with Eu 3++ Lithium aluminate powder with a concentration of 0.001, 0.01, 0.1 and 0.8, briquette, loaded into 4 iridium crucibles of rectangular column, cylindrical, cubic column and ellipsoid, and the orientations were , respectively, The seed crystals of , and are placed in the bottom of the above crucible in sequence, and then the blocks are placed in the crucible and adjusted to the appropriate position in the furnace. After the whole system is sealed, the power is turned on to heat up, and the mechanical pump and diffusion pump are started successively to evacuate to 5×10 -4 Pa, after the furnace temperature reaches 1000 °C, fill with argon, continue to heat up to 1800 °C, hold for 2 hours, melt the raw material and the top of the seed crystal, adjust the position of the crucible for inoculation, and keep the temperature gradient of the solid-liquid interface at about 20 °C / cm, start The device was lo...

Embodiment 3

[0038] synthesized by sol-gel method and doped with Ce 3+ Lithium aluminate powder with a concentration of 0.001, 0.01, 0.1, 0.4 and 0.8, briquette, prepare five tungsten-molybdenum alloy crucibles in the shape of rectangular column, cylinder, cubic column, ellipsoid and cone, and the orientations are The seed crystals of , , , and are placed in the bottom of the above crucible in sequence, and then the blocks are placed in the crucible and adjusted to the appropriate position in the furnace. After the whole system is sealed, the power is turned on to heat up, and the mechanical pump and diffusion pump are started successively to evacuate to 10 -4 Pa, after the furnace temperature reaches 1200 °C, fill with argon gas, continue to heat up to 1900 °C, hold for 4 hours, melt the raw material and the top of the seed crystal, adjust the position of the crucible for inoculation, keep the temperature gradient of the solid-liquid interface at 50 °C / cm, and start the descent device,...

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Abstract

The invention provides a multi-crucible fused mass growth technique for growing lithium aluminate (gamma-LiAlO2) monocrystal and doped lithium aluminate crystal, comprising the following steps of (1) synthesizing a lithium aluminate raw material; (2) putting the synthesized lithium aluminate raw material and the directed seed crystal into a crucible, transferring into a high-temperature descending furnace, sealing the whole system and electrifying for raising temperature, sequentially starting a mechanical pump and a diffusion pump, vacuumizing to 10<-3>Pa to 10<-4>Pa, charging inert protective gas when the furnace temperature is up to 800-1200 DEG C, and continuously raising the temperature to the preset temperature of 1600-1900 DEG C; (3) after the furnace temperature is up to the preset temperature, holding for 1-4 hours, regulating the temperature of a hearth and the position of the crucible to ensure that the raw material and the top of the seed crystal are smelted so as to realize the inoculation growth, setting the temperature gradient of solid liquid interface within 10-50 DEG C / cm, and controlling the descending speed of the crucible within 0.1-3.0mm / h; and (4) after crystals finishes the growth, carrying out the in0situ annealing treatment. The invention has the following technical characteristics of special temperature field design, multi-crucible technique, in-situ annealing treatment and the like, and has the advantages of stable temperature field, adjustable temperature gradient, convenient operation, low average energy consumption, one-furnace multiple-products and beneficial to industrial production.

Description

technical field [0001] The technical fields of the invention are: GaN-based or ZnO-based LEDs and LDs; preparation of GaN self-supporting substrates by HVPE and other technologies; preparation of non-polarized M-plane and A-plane GaN; preparation of new GaN-based fluorescent substrates; substrate peeling technology . It has broad application prospect and market potential. Background technique [0002] In recent years, blue-green light-emitting diodes, lasers and related devices have become research hotspots due to their huge market application prospects, among which the research on GaN-based series materials is the most prominent. At present, GaN-based blue-green LEDs have been commercialized. In 1997, the continuous working life of the blu-ray LD developed by Nichia Company using GaN exceeded 10000h. However, at present, the luminous efficiency and lifetime of LEDs and LDs are difficult to be greatly improved, mainly because the lattice mismatch and thermal mismatch betw...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B11/00C30B29/22
Inventor 李扬向卫东苏小龙
Owner 上海博晶光电科技有限公司
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