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CN102786932B - Novel preparation process of LED (light-emitting diode) - Google Patents

Novel preparation process of LED (light-emitting diode) Download PDF

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Publication number
CN102786932B
CN102786932B CN 201210297412 CN201210297412A CN102786932B CN 102786932 B CN102786932 B CN 102786932B CN 201210297412 CN201210297412 CN 201210297412 CN 201210297412 A CN201210297412 A CN 201210297412A CN 102786932 B CN102786932 B CN 102786932B
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led
preparation process
hours
high temperature
powder
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CN102786932A (en
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宋碧清
崔西成
倪广春
宗明立
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JINFENG HANBAO LLC
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JINFENG HANBAO LLC
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Abstract

The invention discloses a novel preparation process of an LED (light-emitting diode). The preparation process comprises the following steps of: preparing raw material powder and restoring in a rotary kiln at high temperature, wherein the step of preparing the material powder is as follows: weighing 55.59g of Y2O3, 21.73g of CeO, 42.69g of Al2O3, 31g of H3BO, and 21g of BaF according to the stoichiometric proportion, and adding an agate ball to mix for 72 hours in a material mixer, and the step of restoring the material powder in the rotary kiln at the high temperature is as follows: uniformly mixing and putting a sample into a 500cc of crucible, covering in atmosphere of N2 and 3H2, and preserving the heat for 6 hours at 1500 DEG C; and crushing and sieving, ball-milling or airstream crushing, wetly sieving, cleaning and centrifugally dripping. The novel preparation process has the advantages that the novel preparation process of the LED adopts a tri-color blue powder kiln to directly restore, crush, wash, clean and bake the product at the high temperature; and the granularity of LED fluorescent powder is controlled by adjusting the temperature of a furnace, the heat preservation time and the adding quantity of a fluxing agent, and the advantages of small energy consumption and high yield are achieved.

Description

A kind of New LED preparation technology
Technical field
The present invention relates to a kind of luminescent material, relate in particular to a kind of New LED preparation technology.
Background technology
1997, the Nakamura of Japanese Ri Ya company applied YAG:Ce at blue light InGaN/GaN chip 3+Yellow fluorescent powder, the blue light that the gold-tinted that is sent by fluorescent material and worker nGaN/GaN chip send forms white light, thereby has caused the revolution of a lighting system.White light LEDs is compared with luminescent lamp with respect to conventional incandescent, has volume little (particle is little, easily combination), thermal value low (non-thermal radiation), power consumption is little, the life-span is long (greater than 10000 hours), reaction soon, environmental protection advantages such as (no mercury pollution, recyclable).YAG:Ce 3+Fluorescent material plays a part very crucial in white light LEDs.
YAG:Ce 3+The matrix of fluorescent material is yttrium aluminum garnet, has the favorable mechanical performance, physical and chemical performance, and high temperature resistant irradiation and electron-bombardment ability are a kind of good luminescent materials.Present YAG:Ce 3+Fluorescent material is because flow process is longer, and process is wayward, and yield is lower, energy consumption is big, product is unstable, production cost is higher.
Summary of the invention
The technical process that the present invention is directed to traditional LED production technique is longer, and process is wayward, and yield is lower, energy consumption is big, product is unstable, the production cost problem of higher, has made the improvement on technology and the prescription; Provide a kind of energy consumption little, yield height, a kind of New LED preparation technology that production cost is low.
For achieving the above object, the technical scheme that adopts of the utility model is:
A kind of New LED preparation technology, comprising following steps: the preparation of raw material powder, the kiln high temperature reduction, its characteristics are: the preparation of described raw material powder is according to Y 3Al 5O 12: 0.06Ce 3+Chemical formula calculates and takes by weighing Al 2O 3(99.99%), Y 2O 3(99.999%), CeO 2(99.99%) and add 1%H 3BO 3And BaF 2(take by weighing Y according to stoichiometric ratio as fusing assistant 2O 355.59g, CeO 21.73g, Al 2O 342.69g, H 3BO 3Lg, BaF 21g), add agate ball batch mixing 72 hours in blender.Described kiln high temperature reduction is that sample behind the mixing is placed in the 500cc crucible, adds a cover at N 2+ 3H 2Atmosphere in, with 1500 ℃ the insulation 6 hours.This New LED preparation technology comprises that also fragmentation sieves, ball milling or comminution by gas stream, wet sieving cleaned centrifuge dripping, namely with crusher with the fluorescent material fragmentation after, with the sample washing, in order to remove impurity in the sample.This New LED preparation technology also comprises oven dry, and ultrasonic wave is selected powder, is about to fluorescent material and is placed in the baking oven with 120 ℃ of insulations 17 hours; After the oven dry, LED fluorescent material is crossed 500 order vibration of ultrasonic wave sieve.
Advantage of the present invention is: this New LED preparation technology adopts the direct high temperature reduction of three primary colours blue powder kiln, pulverizes, selects powder, cleaning, oven dry finished product one cover flow process; By regulating furnace temperature, the add-on of soaking time and fusing assistant is controlled the granularity of LED fluorescent material, and it is little to reach energy consumption, yield height, the advantage that production cost is low.
Description of drawings
Fig. 1 is process flow diagram of the present invention.
Embodiment
Below in conjunction with accompanying drawing and specific embodiment the present invention is further described:
A kind of New LED preparation technology, as shown in Figure 1, comprising following steps: the preparation of raw material powder, the kiln high temperature reduction, its characteristics are: the preparation of described raw material powder is according to Y 3Al 5O 12: 0.06Ce 3+Chemical formula calculates and takes by weighing Al 2O 3(99.99%), Y 2O 3(99.999%), CeO 2(99.99%) and add 1%H 3BO 3And BaF 2(take by weighing Y according to stoichiometric ratio as fusing assistant 2O 355.59g, CeO 21.73g, Al 2O 342.69g, H 3BO 3Lg, BaF 21g), add agate ball batch mixing 72 hours in blender.Described kiln high temperature reduction is that sample behind the mixing is placed in the 500cc crucible, adds a cover at N 2+ 3H 2Atmosphere in, with 1500 ℃ the insulation 6 hours.This New LED preparation technology comprises that also fragmentation sieves, ball milling or comminution by gas stream, wet sieving cleaned centrifuge dripping, namely with crusher with the fluorescent material fragmentation after, with the sample washing, in order to remove impurity in the sample.This New LED preparation technology also comprises oven dry, and ultrasonic wave is selected powder, is about to fluorescent material and is placed in the baking oven with 120 ℃ of insulations 17 hours; After the oven dry, LED fluorescent material is crossed 500 order vibration of ultrasonic wave sieve; Employing distant place spectroscopic analysis system, and the American-European laser particle size analyzer that restrains is tested every index that tristimulus coordinates, relative brightness, the granularity of LED fluorescent material all can reach (or surpassing) traditional technology production LED fluorescent material respectively.
The invention has the beneficial effects as follows:
(1) cuts down the consumption of energy greatly, improve yield.
(2) be convenient to the control of LED MODEL OF THE PHOSPHOR PARTICLE SIZE.By regulating furnace temperature, the add-on of soaking time and fusing assistant can obtain required granular powder easily.
(3) significantly reduced production cost.
(4) every index of the every index of fluorescent material of this method production and traditional technology production does not reduce.
Figure BSA00000766185100031
Embodiment recited above is described preferred implementation of the present invention; be not that design of the present invention and protection domain are limited; under the prerequisite that does not break away from design concept of the present invention; common engineering technical personnel make technical scheme of the present invention in this area various modification and improvement all should fall into protection scope of the present invention.

Claims (1)

1. LED preparation technology, comprising following steps: the preparation of raw material powder, the kiln high temperature reduction is characterized in that: the preparation of described raw material powder is according to Y 3Al 5O 12: 0.06Ce 3+Chemical formula calculates and to take by weighing purity is 99.99% Al 2O 3, purity is 99.99% Y 2O 3, purity is 99.99% CeO 2And adding 1%H 3BO 3And BaF 2As fusing assistant, specifically take by weighing Y according to stoichiometric ratio 2O 355.59g, CeO 21.73g, Al 2O 342.69g, H 3BO 31g, BaF 21g adds agate ball batch mixing 72 hours in blender; Described kiln high temperature reduction is that sample behind the mixing is placed in the 500cc crucible, adds a cover at N 2+ 3H 2Atmosphere in, with 1500 ℃ the insulation 6 hours; Preparation technology comprises that also fragmentation sieves, ball milling or comminution by gas stream, wet sieving cleaned centrifuge dripping, namely with crusher with the fluorescent material fragmentation after, with the sample washing, in order to remove impurity in the sample; Preparation technology also comprises oven dry, and ultrasonic wave is selected powder, is about to fluorescent material and is placed in the baking oven with 120 ℃ of insulations 17 hours; After the oven dry, LED fluorescent material is crossed 500 order vibration of ultrasonic wave sieve.
CN 201210297412 2012-08-11 2012-08-11 Novel preparation process of LED (light-emitting diode) Expired - Fee Related CN102786932B (en)

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Application Number Priority Date Filing Date Title
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CN102786932B true CN102786932B (en) 2013-08-14

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1482208A (en) * 2002-09-13 2004-03-17 北京有色金属研究总院 Blue light-excitated white phosphor powder for LED and production method thereof
CN1687307A (en) * 2005-05-27 2005-10-26 王锦高 Luminescent powder of light emitting diode for semiconductor white light illumination, and preparation method thereof
CN101376522A (en) * 2008-10-09 2009-03-04 天津大学 Fluorescent powder for white light LED and preparation thereof
CN101445729A (en) * 2008-12-22 2009-06-03 江门市科恒实业股份有限公司 Preparation method of phosphor powder for white LED

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI265916B (en) * 2004-12-31 2006-11-11 Ind Tech Res Inst Process of making YAG fluorescence powder

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1482208A (en) * 2002-09-13 2004-03-17 北京有色金属研究总院 Blue light-excitated white phosphor powder for LED and production method thereof
CN1687307A (en) * 2005-05-27 2005-10-26 王锦高 Luminescent powder of light emitting diode for semiconductor white light illumination, and preparation method thereof
CN101376522A (en) * 2008-10-09 2009-03-04 天津大学 Fluorescent powder for white light LED and preparation thereof
CN101445729A (en) * 2008-12-22 2009-06-03 江门市科恒实业股份有限公司 Preparation method of phosphor powder for white LED

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
助熔剂对Y3Al5O12:Ce荧光粉性能的影响;张书生等;《中国稀土学报》;20021231;第20卷(第6期);605-607 *
张书生等.助熔剂对Y3Al5O12:Ce荧光粉性能的影响.《中国稀土学报》.2002,第20卷(第6期),605-607.

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