CN104893723A - Method for preparing YAG-Ce phosphor by using combustion method - Google Patents
Method for preparing YAG-Ce phosphor by using combustion method Download PDFInfo
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- CN104893723A CN104893723A CN201510197476.3A CN201510197476A CN104893723A CN 104893723 A CN104893723 A CN 104893723A CN 201510197476 A CN201510197476 A CN 201510197476A CN 104893723 A CN104893723 A CN 104893723A
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Abstract
The invention relates to a method for preparing YAG-Ce phosphor by using a combustion method. The method comprises: weighing a cosolvent, a combustion agent, and raw materials for preparing YAG-Ce phosphor; dissolving the raw materials in water; heating to a temperature of 80 DEG C, heating to a temperature of 300 DEG C by using a muffle furnace, carrying out thermal insulation for 3-6 h, carrying out calcining thermal insulation for 3-6 h at a temperature of 800 DEG C, and carrying out water washing or acid washing, suction filtration and drying; and placing the dried precursor under a reducing atmosphere, carrying out calcining thermal insulation for 3-6 h at a temperature of 900-1400 DEG C, cooling, taking out, and screening so as to obtained the required phosphor. According to the present invention, the starch or cellulose powder is adopted as the combustion agent, the combustion method is used to manufacture the YAG-Ce phosphor, the reaction temperature is lowered to about 900 DEG C from the traditional 1400-1700 DEG C, the obtained reaction product has characteristics of regular morphology and good uniformity, the method has characteristics of low temperature synthesis, simple process, low energy consumption, low equipment requirements and the like, and the phosphor has good light-emission intensity and is used for white light LED light source.
Description
Technical field
The present invention relates to the preparation field of fluorescent material, be specifically related to a kind of method that combustion method prepares fluorescent material.
Background technology
White light-emitting diode (light Emitting Diode, LED) attracts attention, and is applied to various set lights, as the taillight of pilot lamp, vehicle, ornament lamp, liquid crystal display device and backlight etc.It has the plurality of advantages such as efficiency is high, life-span length, energy saving standard, and application prospect is extensive.
At present, what realize that white light LEDs generally adopts is that blue-light LED chip and bloom are mixed to form white light LEDs, and its principle is that blue-ray LED excitated fluorescent powder produces the gold-tinted with blue light complementation, blue light and yellow light mix, and human eye can be made to produce the vision of white light.The yttrium aluminum garnet (YAG-Ce) that this fluorescent material is mainly activated by cerium, its chemical formula is Y
3a1
50
12: Ce
3+(US Patent No. 5998925 and European patent EP 862794).The YAG-Ce fluorescent material preparation method of current report mainly contains high temperature solid-state method, sol-gel method and coprecipitation method etc.Although industrial main employing high temperature solid-state method preparation, but it is temperature required is generally not less than 1400 DEG C and the sample prepared often needs through ball milling even secondary high-temperature reduction, sample surfaces defect is so not only caused to increase, fluorescence property reduces greatly, and high energy consumption, extend the production cycle, add production cost.And often produce some toxic substances in sol-gel method preparation process, and the fluorescent poor performance prepared.Although the sample that coprecipitation method is prepared can obtain the homogeneous particle of size, in preparation process, influence factor is numerous, wayward.
Publication number is the application for a patent for invention of CN103343006A, discloses one and prepares white light LEDs YAG-Ce fluorescent material preparation method: the raw material first taking incendiary material and preparation YAG-Ce fluorescent material: comprise aluminum compound, yttrium compound, cerium compound; By above-mentioned materials mix, grind even after, start heat temperature raising, between 300-600 DEG C, there is combustion phenomena, then heat up, insulation reaction for some time, then be down to room temperature, obtain yellow powder; By yellow powder ball milling, cross mesh sieve, obtain YAG-Ce fluorescent material.This technique incendiary material alcohols used is ethylene glycol, the not easily perfect combustion of this alcohol, and alcohol body itself and products of combustion poisonous to human body.
Summary of the invention
Technical problem to be solved by this invention is to provide that a kind of fluorescence property is good and preparation technology simple, Reactive Synthesis temperature low, free of contamination YAG-Ce fluorescent material preparation method.
In order to solve this technical problem, preparation YAG-Ce fluorescent material, comprises the steps:
(1) with aluminium salt, yttrium salt, cerium salt for raw material, mixed with the solubility promoter of its 1.5 ~ 4 times of weight by above-mentioned raw materials and be placed in ceramic crucible or corundum crucible, add distilled water, mixing solutions temperature control stirring equipment is heated to 80 DEG C;
Described aluminium salt, yttrium salt, cerium salt, it is Y:Al:Ce=3:5:(0.01 ~ 0.12 that its consumption controls mol ratio);
Described aluminium salt can be the one in aluminum chloride or Tai-Ace S 150;
Described yttrium salt is the one in Yttrium trichloride or yttrium sulfate;
Described cerium salt is the one in Cerium II Chloride or cerous sulfate;
Described aluminium salt, yttrium salt, cerium salt are+3 valence states;
Described solubility promoter is NH
4at least one in Cl or LiCl;
Described temperature control stirring equipment is a kind of in intelligent temperature control magnetic stirring apparatus or thermostat water bath.
(2) add 1 ~ 2 times of incendiary material of mixing salt weight, continue to be stirred to evenly, it is first placed in retort furnace and is heated to 300 DEG C of insulations 3 ~ 6 hours, then colloidal sol calcination insulation taking-up after 3 ~ 6 hours at 800 DEG C will be obtained;
At least one in described incendiary material starch or cellulose powder.
(3) washing or pickling remove solubility promoter, suction filtration, dry;
In described removing solubility promoter process, until wash this fluorescent material obtain washing the specific conductivity < 15ps/cm of remaining solution, when PH is 7.0 ± 0.1; Washing terminates.
(4) dried precursor grinding is placed in lower 900 DEG C ~ 1400 DEG C calcination insulation of reducing atmosphere after 3 ~ 6 hours, cooling is taken out, and crosses mesh sieve and namely obtains required fluorescent material.
Described reducing atmosphere is CO atmosphere, or is nitrogen and hydrogen mixture atmosphere, and the volume ratio of hydrogen and nitrogen is 1:9; Or be argon hydrogen mixed atmosphere, hydrogen and argon gas volume ratio are 1:9.
The present invention has the following advantages compared with existing preparation technology:
1, in mixing salt solution and starch or cellulose powder Hybrid Heating process, its reticulated structure formed, intergranular agglomeration can be hindered, refinement of particle size, there is preparation technology simple, cycle is short, light agglomeration, and product grain diameter is little to 100nm ~ 120nm and the feature be evenly distributed.
2, compared with high temperature solid-state method, doing in the preparation method of incendiary material with starch or Mierocrystalline cellulose, the thermolysis of starch or Mierocrystalline cellulose self can promote the carrying out reacted, thus can significantly reduce Reactive Synthesis temperature, general comparable traditional high temperature solid-state method reduces temperature of reaction more than 500 DEG C, about 900 DEG C of the inventive method can be reduced to from traditional 1400 DEG C ~ 1700 DEG C, reach the effect of low temperature synthesis.
Accompanying drawing explanation
Fig. 1 is the X-ray diffraction spectrogram (XRD) that the embodiment of the present invention 1 calcines the sample that 900 DEG C of insulations obtained after 6 hours.
Fig. 2 is the scanning electron microscope (SEM) photograph (SEM) that the embodiment of the present invention 4 calcines the sample that 1400 DEG C of insulations obtained after 3 hours.
Embodiment
For making the object of the invention and technical scheme advantage clearly, the present invention will be further illustrated by embodiment below.But the present invention is not limited to embodiment, every do according to technical spirit of the present invention any simple modification, equivalent variations and modification, all fall in the protection domain of technical solution of the present invention.
Embodiment 1
(1) 6.667g aluminum chloride is first taken, 8.949g Yttrium trichloride, 0.186g Cerium II Chloride, its consumption controls mol ratio: Y:Al:Ce=3:5:0.05, the LiCl mixing of above-mentioned mixing salt and its 1.5 times of weight and 23.703g is placed in ceramic crucible, add appropriate distilled water, crucible is placed in water-bath and is heated to 80 DEG C while stirring;
(2) in crucible, add 15.802g starch as incendiary material, continue to be stirred to evenly, it is first placed in retort furnace and is heated to 300 DEG C, be incubated 3 hours, then will obtain taking out after colloidal sol calcination at 800 DEG C is incubated 3 hours;
(3) LiCl in precursor is removed in washing, until wash this fluorescent material obtain washing remaining solution specific conductivity when be 12ps/cm, pH being 7.0; Washing terminates, and suction filtration, is placed in 80 DEG C of dry 12h of loft drier;
(4) volume dried precursor powder mull being placed in hydrogen and nitrogen is under the reducing atmosphere of 1:9, and 900 DEG C of calcination are after 6 hours, and cooling is taken out, and crosses 300 mesh sieves and namely obtains required fluorescent material.
Accompanying drawing 1 calcines the X-ray diffraction spectrogram (XRD) of sample that 900 DEG C of insulations obtain after 6 hours for the present embodiment.As shown in Figure 1, with Y
3al
5o
12standard card contrasts, and the YAG-Ce phosphor material powder synthesis single-phase structure that the present invention obtains, not only has higher diffraction peak, and do not occur assorted peak.
Embodiment 2
(1) first take 6.667g aluminum chloride, 8.888g Yttrium trichloride, 0.260g Cerium II Chloride, its consumption controls mol ratio and is: Y:Al:Ce=3:5:0.07; The LiCl mixing of above-mentioned mixing salt and 31.63g is placed in ceramic crucible, and add appropriate distilled water, crucible is placed in water-bath and is heated to 80 DEG C while stirring;
(2) in crucible, add 15.82g starch, continue to be stirred to evenly, it is first placed in retort furnace and is heated to 300 DEG C of insulations 3 hours, then will obtain taking out after colloidal sol calcination at 800 DEG C is incubated 3 hours;
(3) with dilute hydrochloric acid cleaning, LiCl in precursor is removed, until to wash specific conductivity that this fluorescent material institute obtains washing remaining solution be 8ps/cm, pH when being 6.9, washing end, suction filtration, is placed in 80 DEG C of dry 12h of loft drier;
(4) volume dried precursor powder mull being placed in hydrogen and nitrogen is under the reducing atmosphere of 1:9, and 1000 DEG C of calcination are after 4 hours, and cooling is taken out, and crosses 300 mesh sieves and namely obtains required fluorescent material
Embodiment 3
(1) 6.667g aluminum chloride is first taken, 9.009g Yttrium trichloride, 0.111g Cerium II Chloride, its consumption controls mol ratio: Y:Al:Ce=3:5:0.03, above-mentioned mixing salt is placed in ceramic crucible with 63.148g LiCl mixing, add appropriate distilled water, crucible is placed in water-bath and is heated to 80 DEG C while stirring;
(2) in crucible, add 15.787g starch as incendiary material, continue to be stirred to evenly, it is first placed in retort furnace and is heated to 300 DEG C of insulations 3 hours, then will obtain taking out after colloidal sol calcination at 800 DEG C is incubated 3 hours;
(3) LiCl in precursor is removed in washing, until to wash specific conductivity that this fluorescent material institute obtains washing remaining solution be 13ps/cm, pH when being 7.1, and washing end, suction filtration, is placed in 80 DEG C of dry 12h of loft drier;
(4) volume dried precursor powder mull being placed in hydrogen and nitrogen is under the reducing atmosphere of 1:9, and 1200 DEG C of calcination are after 3 hours, and cooling is taken out, and crosses 300 mesh sieves and namely obtains required fluorescent material.
Embodiment 4
(1) 6.667g aluminum chloride is first taken, 8.949g Yttrium trichloride, 0.186g Cerium II Chloride, its consumption controls mol ratio: Y:Al:Ce=3:5:0.05, the LiCl mixing of above-mentioned mixing salt and 32.864g is placed in ceramic crucible, add appropriate distilled water, crucible is placed in water-bath and is heated to 80 DEG C while stirring;
(2) in crucible, add 32.864g starch as incendiary material, continue to be stirred to evenly, it is first placed in retort furnace and is heated to 300 DEG C of insulations 3 hours, then will obtain taking out after colloidal sol calcination at 800 DEG C is incubated 3 hours;
(3) LiCl in precursor is removed in dilute hydrochloric acid pickling, until to wash specific conductivity that this fluorescent material institute obtains washing remaining solution be 10ps/cm, pH when being 7.0, and washing end; Suction filtration, is placed in 80 DEG C of dry 12h of loft drier;
(4) volume dried precursor powder mull being placed in hydrogen and nitrogen is under the reducing atmosphere of 1:9, and 1400 DEG C of calcination are after 3 hours, and cooling is taken out, and crosses 300 mesh sieves and namely obtains required fluorescent material.
Accompanying drawing 2 is the scanning electron microscope (SEM) photograph (SEM) that embodiment 4 calcines the sample that 1400 DEG C of insulations obtained after 3 hours.As shown in Figure 2, can find out, the less and size uniformity of the YAG-Ce fluorescent powder product particle size that the present invention obtains, granule-morphology rule, good dispersion property.
Embodiment 5
(1) 6.667g aluminum chloride is first taken, 8.949g Yttrium trichloride, 0.186g Cerium II Chloride, its consumption controls mol ratio: Y:Al:Ce=3:5:0.05, the LiCl mixing of above-mentioned mixing salt and 23.703g is placed in ceramic crucible, add appropriate distilled water, crucible is placed in water-bath and is heated to 80 DEG C while stirring;
(2) in crucible, add 31.604g cellulose powder, continue to be stirred to evenly, it is first placed in retort furnace and is heated to 300 DEG C of insulations 3 hours, then will obtain taking out after colloidal sol calcination at 800 DEG C is incubated 3 hours;
(3) LiCl in precursor is removed in washing, until when to wash specific conductivity that this fluorescent material institute obtains washing remaining solution be 14ps/cm, pH=7.1, and washing end, suction filtration, is placed in 80 DEG C of dry 12h of loft drier;
(4) volume dried precursor powder mull being placed in hydrogen and nitrogen is under the reducing atmosphere of 1:9, and 900 DEG C of calcination are after 6 hours, and cooling is taken out, and crosses 300 mesh sieves and namely obtains required fluorescent material.
Embodiment 6
(1) first take 6.667g aluminum chloride, 8.888g Yttrium trichloride, 0.260g Cerium II Chloride, the LiCl mixing of above-mentioned mixing salt and 47.445g is placed in ceramic crucible, and add appropriate distilled water, crucible is placed in water-bath and is heated to 80 DEG C while stirring;
(2) in crucible, add the cellulose powder of 15.815g as incendiary material, continue to be stirred to evenly, it is first placed in retort furnace and is heated to 300 DEG C of insulations 3 hours, then will obtain taking out after colloidal sol calcination at 800 DEG C is incubated 3 hours;
(3) LiCl in precursor is removed in dilute hydrochloric acid pickling, until to wash specific conductivity that this fluorescent material institute obtains washing remaining solution be 12ps/cm, pH when being 6.97, and washing end; Suction filtration, is placed in 80 DEG C of dry 12h of loft drier;
(4) volume dried precursor powder mull being placed in hydrogen and nitrogen is under the reducing atmosphere of 1:9, and 1400 DEG C of calcination are after 3 hours, and cooling is taken out, and crosses 300 mesh sieves and namely obtains required fluorescent material.
Claims (7)
1. prepare a method for YAG-Ce fluorescent material by combustion method, it is characterized in that: comprise the steps:
(1) adopt be the aluminium salt of+3 valence states, yttrium salt, cerium salt is raw material, it is Y:Al:Ce=3:5:(0.01 ~ 0.12 that the consumption of aluminium salt, yttrium salt, cerium salt controls mol ratio); The solubility promoter mixing of the mixing salt weighed up and its 1.5 ~ 4 times of weight is placed in ceramic crucible or corundum crucible, and add distilled water, mixing solutions temperature control stirring equipment is heated to 80 DEG C;
(2) add 1 ~ 2 times of incendiary material of mixing salt weight, described incendiary material is at least one in starch or cellulose powder; Continue to be stirred to evenly, it is first placed in retort furnace and is heated to 300 DEG C of insulations 3 ~ 6 hours, then colloidal sol calcination insulation taking-up after 3 ~ 6 hours at 800 DEG C will be obtained;
(3) washing or pickling remove solubility promoter, suction filtration, dry;
(4) dried precursor is placed in lower 900 DEG C ~ 1400 DEG C calcination insulation of reducing atmosphere after 3 ~ 6 hours, cooling is taken out, and crosses mesh sieve and namely obtains required fluorescent material.
2. method according to claim 1, is characterized in that: the solubility promoter in described step (1) is NH
4at least one in Cl or LiCl; Temperature control stirring equipment used is a kind of in intelligent temperature control magnetic stirring apparatus or thermostat water bath.
3. method according to claim 1, it is characterized in that: in described step (3), remove in solubility promoter process, until wash the specific conductivity < 15ps/cm that this fluorescent material institute obtains washing remaining solution, washing end when pH is 7.0 ± 0.1.
4. method according to claim 1, is characterized in that: in described step (4), reducing atmosphere is CO atmosphere.
5. method according to claim 1, is characterized in that: in described step (4), reducing atmosphere is nitrogen and hydrogen mixture atmosphere, and the volume ratio of hydrogen and nitrogen is 1:9; Or be argon hydrogen mixed atmosphere, hydrogen and argon gas volume ratio are 1:9.
6. method according to claim 1, is characterized in that: described aluminium salt is the one in aluminum chloride or Tai-Ace S 150; Described yttrium salt is the one in Yttrium trichloride or yttrium sulfate; Described cerium salt is the one in Cerium II Chloride or cerous sulfate.
7. according to the YAG-Ce fluorescent material that method described in claim 1 obtains.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107978666A (en) * | 2017-11-30 | 2018-05-01 | 重庆文理学院 | A kind of translucent YAG shines the semi-free molding method of thin ceramics |
| CN109135746A (en) * | 2018-10-08 | 2019-01-04 | 广州市伟圣实业有限公司 | A kind of environment-friendly type fluorescent powder |
| CN111170355A (en) * | 2019-12-27 | 2020-05-19 | 合肥学院 | Method for synthesizing Fe/ZnO nanoparticles based on euphorbia helioscopia extracting solution through low-temperature combustion |
| CN112300785A (en) * | 2020-10-28 | 2021-02-02 | 陕西彩虹新材料有限公司 | Preparation method of fluorescent slurry |
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| CN101597164A (en) * | 2009-07-01 | 2009-12-09 | 南京工业大学 | Preparation method of double-doped yttrium aluminum garnet transparent ceramic powder |
| WO2011102566A1 (en) * | 2010-02-16 | 2011-08-25 | The Industry & Academic Cooperation In Chungnam National University (Iac) | Rapid solid-state synthesis of yttrium aluminum garnet yellow-emitting phosphors |
| CN102367383A (en) * | 2011-10-29 | 2012-03-07 | 南昌大学 | Preparation method of yttrium aluminum garnet yellow fluorescent powder for white light LED |
| CN103343006A (en) * | 2013-07-03 | 2013-10-09 | 惠州学院 | Method for preparing YAG-Ce fluorescent powder for white-light LED (light-emitting diode) |
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2015
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Patent Citations (4)
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| CN101597164A (en) * | 2009-07-01 | 2009-12-09 | 南京工业大学 | Preparation method of double-doped yttrium aluminum garnet transparent ceramic powder |
| WO2011102566A1 (en) * | 2010-02-16 | 2011-08-25 | The Industry & Academic Cooperation In Chungnam National University (Iac) | Rapid solid-state synthesis of yttrium aluminum garnet yellow-emitting phosphors |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107978666A (en) * | 2017-11-30 | 2018-05-01 | 重庆文理学院 | A kind of translucent YAG shines the semi-free molding method of thin ceramics |
| CN109135746A (en) * | 2018-10-08 | 2019-01-04 | 广州市伟圣实业有限公司 | A kind of environment-friendly type fluorescent powder |
| CN111170355A (en) * | 2019-12-27 | 2020-05-19 | 合肥学院 | Method for synthesizing Fe/ZnO nanoparticles based on euphorbia helioscopia extracting solution through low-temperature combustion |
| CN112300785A (en) * | 2020-10-28 | 2021-02-02 | 陕西彩虹新材料有限公司 | Preparation method of fluorescent slurry |
| CN112300785B (en) * | 2020-10-28 | 2024-02-13 | 陕西彩虹新材料有限公司 | Preparation method of fluorescent slurry |
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