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CN100999662A - Preparation process of fluorescent powder for white light LED excited by blue light - Google Patents

Preparation process of fluorescent powder for white light LED excited by blue light Download PDF

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Publication number
CN100999662A
CN100999662A CNA2006101733861A CN200610173386A CN100999662A CN 100999662 A CN100999662 A CN 100999662A CN A2006101733861 A CNA2006101733861 A CN A2006101733861A CN 200610173386 A CN200610173386 A CN 200610173386A CN 100999662 A CN100999662 A CN 100999662A
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crucible
white light
blue light
inner crucible
cover
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尤洪鹏
李文
洪广言
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Changchun Institute of Applied Chemistry of CAS
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Changchun Institute of Applied Chemistry of CAS
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
    • Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps

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Abstract

本发明涉及一种蓝光激发的白光LED用荧光粉的制备方法，所述的荧光粉化学式为(R3－x－yCexLny)A5O12，其中，R为Y，La，Gd，Tb，Lu，Sc中至少一种，Ln为Pr，Dy，Nd，Sm，Dy，Bi中至少一种；A为B，Al，Ga，Si，Mn，Mg中至少一种；0.01≤x≤1.2；0≤y≤0.2。其制备方法是将上述结构式中的各个元素的氧化物、氢氧化物或相应的盐类与适量的助熔剂混合均匀后，把混合物放在内坩埚内，内坩埚加上非密封盖，石墨或碳放入外坩埚与内坩埚之间，外坩埚盖上密封盖，然后放入高温炉内灼烧，灼烧温度为1350～1700℃，灼烧时间为1～8小时，冷却取出，经粉碎，水洗，烘干后得粉末荧光体。The invention relates to a method for preparing phosphor powder for white LEDs excited by blue light. The chemical formula of the phosphor powder is (R 3-x-y Cex Ln y )A 5 O 12 , wherein R is Y, La, Gd , at least one of Tb, Lu, Sc, Ln is at least one of Pr, Dy, Nd, Sm, Dy, Bi; A is at least one of B, Al, Ga, Si, Mn, Mg; 0.01≤x ≤1.2; 0≤y≤0.2. Its preparation method is to mix the oxides, hydroxides or corresponding salts of each element in the above structural formula evenly with an appropriate amount of flux, then put the mixture in the inner crucible, add a non-sealed cover to the inner crucible, graphite or Put the carbon between the outer crucible and the inner crucible, cover the outer crucible with a sealing cover, and then put it into a high-temperature furnace for burning. The burning temperature is 1350-1700°C, and the burning time is 1-8 hours. After cooling, take it out and crush it. , washed with water, and dried to obtain a powder phosphor.

Description

A kind of preparation method of blue-light excited phosphor for white light LED
Technical field
The present invention relates to a kind of preparation method of phosphor for white light LED of blue excitation.
Background technology
In recent years, has all solid state White-light LED illumination light source that plurality of advantages such as energy-saving and environmental protection, long lifetime, radiationless, adverse environment resistant, time of response be short are integrated in one, its Application Areas constantly enlarges, progressively replace incandescent light and luminescent lamp, will become the new generation of green lighting source and show wide application prospect and huge development potentiality from " special lighting ".Its widespread use will cause a revolution of lighting industry, and will drive the develop rapidly of large quantities of related industrieies.The high-brightness white-light that the garnet combination that practical at present white light LEDs is made up of gallium nitride light-emitting diode blue light that sends and the multiple rare earth that can effectively absorb blue light produces.The luminescent material of garnet structure has the luminous efficiency height, good stability, plurality of advantages such as life-span length.Therefore, this high efficient luminous material has been widely used among the LED that emits white light, and its technology of preparing causes people's extensive concern always.
Yttrium aluminum garnet is the compound that is at high temperature reacted generation by yttrium oxide and aluminum oxide, its fusing point height, hardness is big, has good chemical stability, thereby can easily mix other rare earth ion and obtain different purposes laser and luminescent material, disclose the high efficient luminous material of cerium activated garnet structure as U.S. Pat 702675682.The formation of this cerium activated high efficient luminous material is at high temperature to finish, because trivalent cerium ion is easy to be oxidized to the quadrivalent cerium ion, pyroreaction is difficult to obtain high efficient luminous material in the air.Therefore, obtain cerium activated high efficient luminous material, also need reducing atmosphere.The reducing atmosphere that adopts is the mixed gas of nitrogen and hydrogen at present.U.S. Pat 20050099786A1 discloses the preparation process of the luminescent material of cerium activated garnet structure, and it forms cerium at high temperature N 2And H 2Mixing reducing atmosphere forms down.Adopt the mixed gas calcination conditional request strictness of nitrogen and hydrogen, calcination time is long, and preparation cycle is long, and cost is higher, and in preparation process owing to the existence of hydrogen, set off an explosion easily.Chinese patent CN1730607A discloses the preparation method of the luminescent material of cerium activated garnet structure, this patent is carbon dust to be blended directly in the starting material obtain, this preparation method is owing to carbon directly is added in the starting material, if the quantity not sufficient that carbon adds, the quadrivalent cerium ion can not reduce effectively, if it is excessive to add carbon, can cause carbon directly to pollute, very difficult acquisition is luminescent material efficiently.Therefore, this preparation method can not satisfy demand of practical production well.
Summary of the invention
The object of the present invention is to provide a kind of simple, safe, practical, prepare the method for garnet structure high-efficiency fluorescence powder cheaply.
The preparation method of fluorescent material of the present invention adopts two crucible graphite or carbon reduction method preparation, wanting the reductive sample to be placed in the interior crucible, and put non-tight lid at interior crucible, graphite or carbon are put between outer crucible and the crucible, outer crucible covers sealing cover, puts into High Temperature Furnaces Heating Apparatus then, and calcination at high temperature produces reducing atmosphere, with the sample reduction, thereby make needed high efficient luminous material.
The chemical formula that the present invention relates to fluor is:
(R 3-x-yCe xLn y)A 5O 12
Wherein, R is Y, La, and Gd, Tb, Lu, at least a among the Sc; Ln is Pr, Nd, Sm, Dy, Bi, at least a; A is B, Al, and Ga, Si, Mn, at least a among the Mg; 0.01≤x≤1.2; 0≤y≤0.2.
The starting material that adopted are the oxide compound of each element in the above-mentioned chemical formula, the salt that oxyhydroxide maybe can transform corresponding oxide.
Fusing assistant is boron oxide, boric acid, Neutral ammonium fluoride, aluminum fluoride, in alkaline-earth metal fluoride, the rare earth metal fluorochemical one or more, the addition of fusing assistant account for the starting material gross weight per-cent be 0～8wt%.
By proportioning starting material are placed in the interior crucible, and put the non-tight lid at interior crucible, graphite or carbon are put between outer crucible and the crucible, outer crucible covers sealing cover, put into High Temperature Furnaces Heating Apparatus then, calcination temperature is 1350～1700 ℃, and calcination time is 1～8 hour, calcination at high temperature produces reducing atmosphere and reduces, cooling is taken out, through pulverizing washing, oven dry obtains a kind of blue-light excited phosphor for white light LED.
Adopt the present invention to prepare the high-efficiency fluorescence body following characteristics arranged:
1, when the above-mentioned luminescent material of preparation, crucible is a high temperature sintering in air, and preparation technology is simple, and is safe and reliable, and working condition is controlled easily, can perform well in actual production.
2, owing to adopt two crucibles reduction, sample and graphite or carbon are separated, can either prevent graphite or Prevent Carbon Contamination sample effectively, the effective cerium ion in the reducing material again simultaneously, so can obtain blue-light excited white light LEDs luminescent material.
3, can continuous production, with short production cycle, a large amount of save energy reduce production costs.
Embodiment
Embodiment 1
Take by weighing Y 2O 39.991g, Al 2O 37.647g, AlF 30.4g, CeO 20.258g.Utilize ball mill to carry out abundant ground and mixed, put into a less alumina crucible, cover the non-tight lid, then it is put into a bigger alumina crucible, China ink or carbon are put between outer crucible and the crucible, and outer crucible covers sealing cover, put into High Temperature Furnaces Heating Apparatus, 1400 ℃, calcination 4 hours, cooling is taken out, remove China ink or carbon, after the Ball milling, after scouring sieves, oven dry then obtains to consist of Y 2.95Ce 0.05Al 5O 12The white light LEDs fluor, it is 108 that 460nm excites down luminosity.
Embodiment 2
Take by weighing Y 2O 39.991g, Al 2O 37.647g, CeO 20.258g, H 3BO 30.2g.Other condition obtains to consist of Y with embodiment 1 2.95Ce 0.05Al 5O 12The white light LEDs fluor, it is 105 that 460nm excites down luminosity.
Embodiment 3
Take by weighing Y 2O 39.991g, Al 2O 37.647g, MgF 20.3g, CeO 20.258g.Other condition obtains to consist of Y with embodiment 1 2.95Ce 0.05Al 5O 12The white light LEDs fluor, it is 105 that 460nm excites down luminosity.
Embodiment 4
Take by weighing Y 2O 39.991g, Al 2O 37.647g, B 2O 3, 0.1g,, CaF 20.3g, CeO 20.258g.Other condition must consist of Y with embodiment 1 2.95Ce 0.05Al 5O 12The white light LEDs fluor, it is 106 that 460nm excites down luminosity.
Embodiment 5
Take by weighing Y 2O 39.991g, Al 2O3 7.647g, BaF 20.5g, CeO 2O.258g.Other condition obtains to consist of Y with implementing 1 2.95Ce 0.05Al 5O 12The white light LEDs fluor, it is 106 that 460nm excites down luminosity.
Embodiment 6
Take by weighing Y 2O 39.991g, Al 2O 37.647g, YF 30.5g, CeO 20.258g.Other condition obtains to consist of Y with embodiment 1 2.95Ce 0.05Al 5O 12The white light LEDs fluor, it is 107 that 460nm excites down luminosity.
Embodiment 7
Take by weighing Y 2O 39.991g, Al 2O 37.647g, BaF 20.3g, H 3BO 30.1g, CeO 20.258g.Other condition obtains to consist of Y with embodiment 1 2.95Ce 0.05Al 5O 12The white light LEDs fluor, it is 106 that 460nm excites down luminosity.
Embodiment 8
Take by weighing Y 2O 39.991g, Al 2O 37.647g, H 3BO 30.1g,, AlF 30.4g, CeO 20.258g.Other condition obtains to consist of Y with embodiment 1 2.95Ce 0.05Al 5O 12The white light LEDs fluor, it is 105 that 460nm excites down luminosity.
Embodiment 9
Take by weighing Y 2O 39.991g, Al 2O 37.647g, B 2O 30.1g,, SrF 20.4g, CeO 20.258g.Other condition obtains to consist of Y with embodiment 1 2.95Ce 0.05Al 5O 12The white light LEDs fluor, it is 106 that 460nm excites down luminosity.
Embodiment 10
Take by weighing Y 2O 39.991g, Al 2O 37.647g, NH4F 0.3g, CeO 20.258g.Calcination temperature is 1500 ℃, and other condition obtains to consist of Y with embodiment 1 2.95Ce 0.05Al 5O 12The white light LEDs fluor, it is 106 that 460nm excites down luminosity.
Embodiment 11
Take by weighing Y 2O 39.991g, Al 2O 37.647g, CeO 20.258g.Calcination temperature is 1700 ℃, and the time is 1 hour, and other condition obtains to consist of Y with embodiment 1 2.95Ce 0.05Al 5O 12The white light LEDs fluor of efficient blue excitation, it is 106 that 460nm excites down luminosity.
Embodiment 12
Take by weighing Y 2O 39.991g, Al 2O 37.647g, AlF 30.6g, CeO 20.258g.Calcination temperature is 1350 ℃, and the time is 8 hours, and other condition obtains to consist of Y with embodiment 1 2.95Ce 0.05Al 5O 12The white light LEDs fluor, it is 103 that 460nm excites down luminosity.
Embodiment 13～embodiment 40
Change the component of fluorescent material among the embodiment 1, its concrete composition sees Table 1, and other condition is with embodiment 1, and the luminosity of the fluorescent material that is obtained under 460nm excites listed in table 1.
Table 1
Embodiment Molecular formula Relative brightness (%)
13 ?Y 2.75Gd 0.2Ce 0.05Al 5O 12 ?110
14 ?Y 2.35Gd 0.6Ce 0.05Al 5O 12 ?112
15 ?Y 2.95Gd 1.0Ce 0.05Al 5O 12 ?113
16 ?Y 1.15Gd 1.8Ce 0.05Al 5O 12 ?110
17 ?Y 1.13Gd 1.8Ce 0.07Al 5O 12 ?111
18 ?Y 1.17Gd 1.8Ce 0.03Al 5O 12 ?106
19 ?Y 1.09Gd 1.8Ce 0.11Al 5O 12 ?109
20 ?Y 2.75La 0.2Ce 0.01Al 5O 12 ?101
21 ?Y 2.86Pr 0.1Ce 0.04Al 5O 12 ?110
22 ?Y 2.78Tb 0.15Ce 0.07Al 5O 12 ?112
23 ?Y 2.64Lu 0.3Ce 0.06Al 5O 12 ?115
24 ?Y 2.75Sc 0.2Ce 0.05Al 5O 12 ?113
25 ?Y 2.9Sm 0.01Ce 0.09Al 5O 12 ?109
26 ?Y 2.88Nd 0.02Ce 0.1Al 5O 12 ?112
27 ?Y 2.89Dy 0.03Ce 0.08Al 5O 12 ?111
28 ?Y 2.86Bi 0.02Ce 0.12Al 5O 12 ?108
29 ?Y 2.2Gd 0.6La 0.15Ce 0.05Al 5O 12 ?110
30 ?Y 2.0Gd 0.6Lu 0.35Ce 0.05Al 5O 12 ?119
31 ?Y 2.Gd 0.8Sc 0.15Ce 0.05Al 5O 12 ?118
32 ?Y 2.0Gd 0.7La 0.1Lu 0.15Ce 0.05Al 5O 12 ?116
33 ?Y 2.92Ce 0.08Al 4.5Ga 0.5O 12 ?117
34 ?Y 2.92Ce 0.08Al 4Ga 1O 12 ?118
35 ?Y 2.91Ce 0.09Al 4.9B 0.1O 12 ?113
36 ?Y 2.91Ce 0.09Al 4.5B 0.5O 12 ?115
37 ?Y 2.8Gd 0.15Ce 0.05Al 4.99Mg 0.01O 12 ?113
38 ?Y 2.96Ce 0.04Al 4.98Mg 0.01Mn 0.01O 12 ?112
39 ?Y 2.93Ce 0.07Mg 0.01Al 4.98Si 0.01O 12 ?115
40 ?Y 2.35Gd 0.5Sc 0.1Ce 0.05Al 3.9Ga 1B 0.1O 12 ?117

Claims (1)

1.一种蓝光激发的白光LED用荧光粉的制备方法，其特征在于：所述的荧光体的化学式为：1. A preparation method of phosphor powder for white LEDs excited by blue light, characterized in that: the chemical formula of the phosphor is: (R3-x-yCexLny)A5O12 (R 3-xy C x Ln y )A 5 O 12 其中，R为Y，La，Gd，Tb，Lu，Sc中至少一种；Ln为Pr，Nd，Sm，Dy，Bi，中至少一种；A为B，Al，Ga，Si，Mn，Mg中至少一种；0.01≤x≤1.2；0≤y≤0.2；Among them, R is at least one of Y, La, Gd, Tb, Lu, Sc; Ln is at least one of Pr, Nd, Sm, Dy, Bi; A is B, Al, Ga, Si, Mn, Mg At least one of them; 0.01≤x≤1.2; 0≤y≤0.2; 所采用的原材料为上述化学式中各个元素的氧化物、氢氧化物或可以转化相应氧化物的盐类；The raw materials used are oxides, hydroxides or salts that can be converted to corresponding oxides of each element in the above chemical formula; 助熔剂为氧化硼、硼酸、氟化铵、氟化铝，碱土金属氟化物、稀土金属氟化物中一种或多种，助熔剂的添加量占原材料总重量的的百分比为0～8wt％；The fluxing agent is one or more of boron oxide, boric acid, ammonium fluoride, aluminum fluoride, alkaline-earth metal fluoride, and rare-earth metal fluoride, and the percentage of the fluxing agent added to the total weight of the raw materials is 0-8 wt%. 按配比把原材料放在内坩埚内，并在内坩埚放上非密封盖，石墨或碳放入外坩埚与内坩埚之间，外坩埚盖上密封盖，然后放入高温炉内，灼烧温度为1350～1700℃，灼烧时间为1～8小时，冷却取出，经粉碎，水洗，烘干，得到一种蓝光激发的白光LED用荧光粉。Put the raw materials in the inner crucible according to the ratio, and put a non-sealed cover on the inner crucible, put graphite or carbon between the outer crucible and the inner crucible, cover the outer crucible with a sealing cover, and then put it into a high-temperature furnace, the firing temperature The temperature is 1350-1700° C., the burning time is 1-8 hours, cooled, taken out, crushed, washed with water, and dried to obtain a phosphor powder for white LEDs excited by blue light.
CNA2006101733861A 2006-12-29 2006-12-29 Preparation process of fluorescent powder for white light LED excited by blue light Pending CN100999662A (en)

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