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Preparation method of nitride fluorescent transparent ceramics for LEDs (light-emitting diodes)

A technology of nitride phosphor powder and transparent ceramics, which is applied in the field of preparation of nitride fluorescent transparent ceramics for LEDs. It can solve problems such as destruction, reduction of luminous intensity, and defects in nitride crystal structure, and achieve high efficiency, increase transmittance, and thickness. shape controllable effect

Active Publication Date: 2016-12-21
JIANGSU LUOHUA NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Due to the high requirements of rare earth ions on the crystal matrix structure in the preparation process of nitride phosphors, when mixed with ceramic raw materials for heat treatment, it is easy to cause defects and damage to the nitride crystal structure, which greatly reduces the luminous intensity, thus limiting its application.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] In a nitrogen-protected glove box, weigh Si 3 N 4 5.65g, Al 3 N 4 5.53g, Ca 2 N 3 7.09g, Eu 2 O 3 0.85g, NH 4 Grind and mix evenly with 0.76g of Cl, transfer it to a corundum pot, immediately put it into a vacuum sintering furnace, raise the temperature to 1700°C at 2°C / min, keep it warm for 3 hours, and keep the nitrogen pressure at 0.65MPa. After the furnace cools down, take out the sample and grind it Pass through a 120-mesh sieve to obtain a nitride phosphor; weigh SiO2 31.8g, Al 2 o 3 7.5g, Bi 2 o 3 22.6g, B 2 o 3 15.9g, ZnO 9.7g, CaCO 3 Mix 6.8g, a small amount of metal particles and 8g nitride phosphor evenly, then dry press the mixture at 100MPa pressure for 5min to obtain a green body, put the green body into a rubber mold and hold the pressure in a cold isostatic press at 200MPa for 5min to obtain Biscuit, heat the biscuit in a high-temperature resistance furnace at 8°C / min to 1200°C, keep it for 2 hours, then heat it at 6°C / min to 1000°C for an...

Embodiment 2

[0045] In a nitrogen-protected glove box, weigh Si 3 N 4 5.65g, Al 3 N 4 5.53g, Ca 2 N 3 6.79g, Eu 2 o 3 0.91g, NH 4 Grind and mix evenly with 0.94g of Cl, transfer it to a corundum pot, immediately put it into a vacuum sintering furnace, raise the temperature to 1600°C at 3°C / min, keep it warm for 4 hours, and keep the nitrogen pressure at 0.45MPa. After the furnace cools down, take out the sample and grind it Pass through a 120-mesh sieve to obtain a nitride phosphor; weigh SiO 2 32.7g, Al 2 o 3 6.2g, Bi 2 o 3 23.6g, B 2 o 3 16.7g, ZnO 7.7g, CaCO 3 4.3 g, a small amount of metal particles and 10 g of nitride phosphor are uniformly mixed, and then the mixture is dry pressed at 100 MPa for 10 minutes to obtain a green body, and the green body is put into a plastic mold and held in a cold isostatic press with a pressure of 200 MPa for 10 minutes to obtain Biscuit, heat the biscuit in a high-temperature resistance furnace at 10°C / min to 1000°C, keep it for 2 hour...

Embodiment 3

[0047] In a nitrogen-protected glove box, weigh Si 3 N 4 5.65g, Al 3 N 4 5.53g, Ca 2 N 3 8.12g, Eu 2 o 3 0.65g, NH 4 Grind and mix evenly with 0.4g of Cl, transfer it to a corundum pot, immediately put it into a vacuum sintering furnace, raise the temperature to 1800°C at 2°C / min, keep it warm for 3 hours, and keep the nitrogen pressure at 0.5MPa, wait for the furnace to cool down, take out the sample for grinding Pass through a 120-mesh sieve to obtain a nitride phosphor; weigh SiO 2 26.4g, Al 2 o 3 3.6g, P 2 o 5 21.8g, B 2 o 3 12.9g, ZnO 4.8g, CaCO 3 2.8g, a small amount of metal particles and 5g of nitride phosphor are evenly mixed, and then the mixture is dry pressed at 150MPa for 5 minutes to obtain a green body, and the green body is put into a plastic mold and held in a cold isostatic press with a pressure of 150MPa for 10 minutes to obtain Biscuit, heat the biscuit in a high-temperature resistance furnace at 9°C / min to 1100°C, hold it for 2 hours, then ...

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Abstract

The invention discloses a preparation method of nitride fluorescent transparent ceramics for LEDs (light-emitting diodes). The method comprises the following steps: 1. in a glove box in a nitrogen protective atmosphere, weighing the raw materials, mixing and grinding; 2. putting the ground powder in the step 1 into a corundum crucible, putting into a vacuum pressure sintering-quick cooling furnace, sintering and cooling; 3. carrying out grinding and crushing on the product obtained in the step 2, and passing through a 120-mesh screen to obtain nitride fluorescent powder; 4. proportionally weighing ceramic powder and the fluorescent powder, adding into a mortar, and uniformly mixing to obtain a mixture; 5. carrying out pelleting treatment on the mixture to obtain a billet; 6. putting the billet into a mold, and flattening with a cold isostatic press to obtain a biscuit; 7. carrying out high-temperature sintering on the biscuit in a high temperature resistance furnace to obtain a sample; 8. and carrying out annealing treatment on the sample to obtain the fluorescent transparent ceramics. The preparation method has the advantages of simple technique, low cost and high efficiency. The prepared nitride fluorescent ceramics have the advantages of high density, high luminescence efficiency, favorable uniformity and controllable thickness and shape.

Description

technical field [0001] The present disclosure generally relates to the technical field of solid lighting materials, and in particular to a method for preparing nitride fluorescent transparent ceramics for LEDs. Background technique [0002] High-power LED is the current research focus, and with the increase of LED power, heat production increases, and the heat is concentrated on a small chip. The temperature inside the chip is getting higher and higher, which will accelerate the aging of the device and even burn the chip. In addition, currently resin and silica gel are mostly used as binders for phosphor packaging, but both have poor high temperature resistance and UV resistance. Long-term exposure to high temperature environments or ultraviolet radiation will cause aging, cracking, and yellowing, resulting in LEDs appearing Decrease in brightness, drift in color temperature, and shortened lifespan have seriously affected the development of high-power white LEDs. In respons...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/14C04B35/622C04B35/58C04B35/626
CPCC04B35/14C04B35/58C04B35/622C04B35/62645C04B2235/3208C04B2235/3217C04B2235/3224C04B2235/3284C04B2235/3298C04B2235/34C04B2235/3409C04B2235/3852C04B2235/3865C04B2235/3873C04B2235/444C04B2235/9646C04B2235/9653
Inventor 罗雪方张甜甜罗子杰陈文娟
Owner JIANGSU LUOHUA NEW MATERIAL
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