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Method for growing Ce: YAG monocrystal fluorescent material

A fluorescent material and single crystal technology, applied in the direction of single crystal growth, crystal growth, single crystal growth, etc., can solve the problems of small segregation coefficient, difficult to increase Ce doping concentration, high dislocation density, etc., and achieve crystal internal defects less, simple growth method, large crystal size effect

Inactive Publication Date: 2013-12-25
KUSN KAIWEI ELECTRONICS
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AI Technical Summary

Problems solved by technology

Among them, the pulling method is currently the most widely used method in the growth of Ce:YAG crystals. However, this method has the following problems in practical applications: 1) The crystals grown by the pulling method have many internal defects and high dislocation density; There is forced convection in the melt during the pulling process, and the segregation coefficient of Ce ions in the YAG crystal is small (about 0.2), so it is difficult to increase the doping concentration of Ce in the crystal; 3) The pulling method usually uses an iridium pot, The cost investment is too high; 4) The crystal size grown by the pulling method is limited
The Ce:YAG crystal grown by the temperature gradient method has a large size, with a diameter of more than 100 mm and a small dislocation density. However, the temperature gradient method requires high process requirements, and graphite heating elements are usually used, which is easy to cause carbon pollution.

Method used

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  • Method for growing Ce: YAG monocrystal fluorescent material
  • Method for growing Ce: YAG monocrystal fluorescent material

Examples

Experimental program
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Effect test

Embodiment 1

[0031] According to the chemical formula (Y 1-m Ce m ) 3 al 5 o 12 (m=0.01) raw material Y 2 o 3 、Al 2 o 3 , CeO 2 The molar ratio of the powder is weighed and proportioned, the total weight is 2.7Kg, mixed evenly, pressed into agglomerates, sintered at 1200°C for 12h; put into a crucible after sintering; the diameter of the crucible is 80mm, the length is 150mm; the orientation of the seed crystal is Put the crucible into the bottom of the crucible, put the crucible into the descending furnace, keep the furnace temperature at 1950°C, and keep the constant temperature for 5 hours; descend the crucible at a constant rate, the descending rate is 0.4mm / h, and the temperature gradient of the solid-liquid interface in the descending direction of the crucible is 25°C / cm; after the crystal growth is completed, control the furnace temperature to drop, the initial cooling rate is 1°C / h, and the cooling speed is accelerated from slow to fast, and the final cooling rate is 50°C / h,...

Embodiment 2

[0033] According to the chemical formula (Y 1-m Ce m ) 3 al 5 o 12 (m=0.008) raw material Y 2 o 3 、Al 2 o 3 , CeO 2 The molar ratio of the powder is weighed and proportioned, the total weight is 7.5Kg, mixed evenly, pressed into a block, sintered at 1200°C for 12h; put into a crucible after sintering; the diameter of the crucible is 120mm, the length is 220mm; the orientation of the seed crystal is Put the crucible into the bottom of the crucible, put the crucible into the descending furnace, keep the furnace temperature at 1950°C, and keep the constant temperature for 5 hours; descend the crucible at a constant rate, the descending rate is 0.2mm / h, and the temperature gradient of the solid-liquid interface in the descending direction of the crucible is 25°C / cm; control the temperature drop of the furnace, the initial cooling rate is 0.2°C / h, accelerate the cooling from slow to fast, and the final cooling rate is 30°C / h, and the cooling process is 180h; after the crysta...

Embodiment 3

[0035] According to the chemical formula (Y 0.99 Ce 0.01 ) 3 (Al 0.998 mn 0.002 ) 5 o 12 Weighing and proportioning, the total weight is 5Kg, mixed evenly, pressed into blocks, sintered at 1200°C for 12 hours; put into a crucible after sintering; the diameter of the crucible is 100mm, and the length is 200mm; put the seed crystal orientation into the bottom of the crucible , put the crucible into the descending furnace, keep the furnace temperature at 1950°C, and keep the constant temperature for 5 hours; descend the crucible at a constant rate, the descending rate is 0.3mm / h, and the temperature gradient of the solid-liquid interface in the descending direction of the crucible is 25°C / cm; Control the temperature drop of the furnace. The initial cooling rate is 0.5°C / h, and the cooling rate is accelerated from slow to fast. The final cooling rate is 35°C / h, and the cooling process is 120h. After the crystal growth is completed, the furnace body is naturally cooled to roo...

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Abstract

The invention discloses a method for growing a Ce: YAG monocrystal fluorescent material. The chemical formula of the Ce: YAG monocrystal fluorescent material is (Y<1-x-m>AxCem)3(Al<1-y>By)5O12, wherein x is not less than 0 and not greater than 1, y is not less than 0 and not greater than 1, m is not less than 0 and not greater than 0.05, A is one type from Lu, Tb, Pr, La and Gd, and B is one type from Ga, Ti, Mn, Cr and Zr. The furnace temperature range for crystal growth is 1900 to 2000 DEG C, the temperature gradient of a solid liquid interface in the descending direction of a crucible is 10-50 DEG C / cm, the descending speed of the crucible is 0.1-5mm / h, the directions of (111), (100) and (001) can be adopted for seed crystals, the diameter of the crucible is 30-120 mm, and the height of the crucible is 50-200mm. Through adoption of the Bridgman-Stockbarger method, the method for growing the Ce: YAG monocrystal fluorescent material has the advantages of simplicity in operation, low cost, large size of grown Ce: YAG crystals, less internal defects, high doping concentration and the like.

Description

technical field [0001] The invention relates to the field of LED production and manufacturing, in particular to a method for growing a Ce:YAG single crystal fluorescent material by a crucible descending method. Background technique [0002] LED is a solid-state semiconductor device that can directly convert electrical energy into light energy. Compared with traditional incandescent lamps and fluorescent lamps, white LEDs have the advantages of low power consumption, high luminous efficiency, long service life, energy saving and environmental protection. Therefore, they are not only widely used in the field of daily lighting, but also enter the field of display equipment. Currently, technologies for obtaining white LEDs can be divided into two categories: (1) using a mixture of three LED chips that emit red, green, and blue light; (2) using blue or ultraviolet LED chips to excite appropriate fluorescent materials. At present, white LEDs mainly use blue LED chips and phosphor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/28C30B11/00C30B11/14
Inventor 曹顿华董永军梁月山
Owner KUSN KAIWEI ELECTRONICS
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