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A kind of preparation method of small size red phosphor

A technology of red fluorescent powder and small size, which can be used in chemical instruments and methods, luminescent materials, etc. It can solve the problems of fluorides such as moisture resistance, poor heat resistance, lively properties, and high requirements for packaging technology, and achieve regular shape and variety. Easy to obtain, the effect of improving the mass transfer effect

Active Publication Date: 2020-09-22
BEIJING UNIV OF CHEM TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Such as the preparation of Mn4+ doped fluoride phosphor in patent CN106634989A. Although fluoride has excellent luminous performance, due to the poor moisture resistance and heat resistance of fluoride, and its lively nature, the performance of encapsulation glue is relatively high.

Method used

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  • A kind of preparation method of small size red phosphor
  • A kind of preparation method of small size red phosphor
  • A kind of preparation method of small size red phosphor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] According to the different doping amounts of GdBO3:Eu, weigh corresponding amounts of gadolinium oxide (3.26g), europium oxide (0.352g), boric acid (1.428g), nitric acid (2.84g), surfactant (PEG-1000) (4.43g ), mixed with 100ml of deionized water, put it into a high-gravity rotating packed bed at 2000r / min and mixed thoroughly for 20min; measured 4.32ml of acetylacetone and 36g of urea in a graduated cylinder and mixed them fully, heated at 90°C for 1h; the solution was reduced to After room temperature, the centrifuge was centrifuged at 11000r / min, the product was washed twice with deionized water and absolute ethanol, and then dried in an oven at 80°C for 12 hours; after drying, it was fully ground with a mortar and put into an alumina crucible, muffle Furnace 1200°C heating rate 5°C / min, holding time 4h; after cooling down to room temperature, take out the product and grind it;

Embodiment 2

[0032] According to the different doping amounts of GdBO3:Eu, weigh corresponding amounts of gadolinium oxide (3.26g), europium oxide (0.352g), boric acid (1.428g), nitric acid (2.84g), surfactant (PEG-1000) (4.43g ), take 100ml of deionized water and mix it, put it into a high-gravity rotating packed bed at 2000r / min and mix it thoroughly for 10-50min, take a sample every 10min, and mark 20ml of each sample as 1, 2, 3, 4, 5; Take out the solution measuring cylinder and measure 0.864ml acetylacetone, weigh 7.2g urea and mix it fully with the solution, heat at 90°C for 1 hour; after the solution cools down to room temperature, centrifuge at 11000r / min, wash with deionized water and absolute ethanol twice respectively Dry in an oven at 80°C for 12 hours. After drying, fully grind it with a mortar and put it into an alumina crucible. The heating rate of the muffle furnace is 1200 °C at 5 °C / min, and the holding time is 4 h; when the temperature is lowered to room temperature, the...

Embodiment 3

[0034]According to the different doping amounts of GdBO3:Eu, weigh corresponding amounts of gadolinium oxide (3.26g), europium oxide (0.352g), boric acid (1.428g), nitric acid (2.84g), surfactant (PEG-1000) (4.43g ), mixed with 100ml of deionized water, put into the high-gravity rotating packed bed at 2000r / min and fully mixed for 20min; measure 4.32ml of acetylacetone in a graduated cylinder and mix well, then divide the solution into eight parts, each 25ml part is marked as 2mol / L , 4mol / L, 6mol / L, 8mol / L, 10mol / L Weigh 2.4g, 4.8g, 7.2g, 9.6g, 12g of urea and mix them thoroughly with the solution, heat at 90°C for 1h; after the solution drops to room temperature, centrifuge Centrifuged at 11000r / min, the product was washed twice with deionized water and absolute ethanol, and then dried in an oven at 80°C for 12h. After drying, fully grind it with a mortar and put it into an alumina crucible. The heating rate of the muffle furnace is 1200 °C at 5 °C / min, and the holding time ...

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Abstract

The invention discloses a preparation method of small-size red fluorescent powder. Compared with a direct solid-phase burning method for preparing commercial fluorescent powder at present, the method has obvious improvement in the aspects of nano particle size controllability, simplicity and convenience of operation process and quality stability of large batches. A rotating packed bed reactor has great advantages in enhancing mixing and improving mass transfer effect. The rotating packed bed reactor further optimizes product morphology, improves doping effect, ensures product uniformity and good repeatability between different batches of products, and more importantly greatly shortens reaction time. In the process, urea is used as a precipitant. Compared with the original precipitant ammonia, the urea is less irritating, less volatile and easy to store and transport, and provides convenient conditions for experimental operation and large-scale synthesis.

Description

technical field [0001] The invention relates to the field of material synthesis, and more specifically relates to a process for preparing small-sized red fluorescent powder by uniform precipitation coupled with high-temperature burning technology in supergravity. Background technique [0002] Solid State Light Emitting Diode (LED for short) is currently the most common light source for commercial lighting displays due to its energy saving, environmental protection, long life, and good stability. LED devices are mainly composed of chips, encapsulants, and phosphors. There are two ways to synthesize white light: (1) use a blue light chip to excite yellow phosphors, and the yellow light generated by the excitation and the blue light of the chip together form white light; (2) ) Use the ultraviolet chip to excite and add red, green and blue three-color phosphors, and use the principle of three primary colors to form white light. Both approaches have their own advantages and disa...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/78
CPCC09K11/7797
Inventor 王丹崔思敏何相磊蒲源王洁欣陈建峰
Owner BEIJING UNIV OF CHEM TECH
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