CN102585824A - Coprecipitation-rheological phase preparation method of rare earth-doped yttrium aluminum garnet fluorescent powder - Google Patents

Coprecipitation-rheological phase preparation method of rare earth-doped yttrium aluminum garnet fluorescent powder Download PDF

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CN102585824A
CN102585824A CN2011100056747A CN201110005674A CN102585824A CN 102585824 A CN102585824 A CN 102585824A CN 2011100056747 A CN2011100056747 A CN 2011100056747A CN 201110005674 A CN201110005674 A CN 201110005674A CN 102585824 A CN102585824 A CN 102585824A
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fluorescent powder
rare earth
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garnet fluorescent
aluminium garnet
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CN102585824B (en
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胡章贵
陆田野
龙震
宋浩亮
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Technical Institute of Physics and Chemistry of CAS
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Abstract

The invention relates to a coprecipitation-rheological phase preparation method of rare earth-doped yttrium aluminum garnet fluorescent powder, which comprises the following steps of: preparing a precursor, taking nanometer/micrometer YAG, SiO2 or SiC as a seed crystal and adjusting the seed crystal, the precursor and a dispersing agent into a rheological phase; then washing and removing impurities in the fluorescent powder through high-temperature heat treatment; and taking ammonium sulfate, polyethylene glycol, hydroxyethyl cellulose or dodecyltrimethylammonium bromide as the dispersing agent, taking deionized water, ethanol, acetic acid or oxalic acid as a rheological phase solvent and adding the seed crystal to reduce the reaction and activation energy and improve the luminous intensity through doping. The coprecipitation-rheological phase preparation method is suitable for the preparation of LED (Light-Emitting Diode) fluorescent powder, trichromatic fluorescent powder, long afterglow fluorescent powder and PDP (Plasma Display Panel) fluorescent powder. The grain size of the fluorescent powder prepared by the invention is between nanometer and micrometer and can be adjusted through the seed crystal and the calcination temperature. The method has the advantages of simplicity, low equipment cost and large treatment amount and is suitable for the preparation of the fluorescent powder for various indication, display or illumination.

Description

The co-precipitation of rare earth doping yttrium aluminium garnet fluorescent powder-rheology phase preparation method
Technical field
The present invention relates to a kind of preparation method of fluorescent material; Be particularly related to a kind of co-precipitation-rheology phase preparation method of the rare earth doping yttrium aluminium garnet fluorescent powder that can effectively be excited by UV-light, purple light or blue light, this method is with the nanometer and a micron YAG, SiO of regular shape 2Or SiC etc. makes crystal seed, and with co-precipitation-rheology phase method preparation, this fluorescent material can be widely used in white light emitting diode (LED).
Background technology
Fluorescent material is one of critical material of demonstration and lighting field.The performance of powder is mainly by decisions such as its phase structure, granule-morphology and the characteristics of luminescences.In order to prepare high-quality fluorescent material, need innovate the preparation method.
On the preparation method of fluorescent material, carried out a lot of explorations both at home and abroad.About the yttrium aluminium garnet fluorescent powder preparation, be in early days with high temperature solid-state method (ZL 02800161.3) synthetizing phosphor powder powder.The fluorescent material preparation method of report mainly contains the precipitator method (CN 101134896A at present; ZL 200510071958.0; ZL 02130949.3; ZL 98124953.1; US 20060145124; US 6869544; US 20040173807; US 4034257; US 6409938; WOI04/079790); Sol-gel method (ZL 02136705.1); Hydrothermal method (ZL03112160.8); Microemulsion method (ZL 200710118422.9); Combustion method; Vapor phase process (ZL 200510122254.1) etc.Solid phase method product granularity is big, lack of homogeneity; Sol-gel method prepares raw materials cost height in the process and productive rate is low; Various defectives below additive method also exists: can not improve light decay, brightness and coating property simultaneously.The precipitator method can remedy the deficiency of aforesaid method.
Summary of the invention
The object of the present invention is to provide a kind of co-precipitation-rheology phase preparation method of rare earth doping yttrium aluminium garnet fluorescent powder, promptly with the nanometer of regular shape or micron YAG, SiO 2Or SiC etc. is equipped with Y as crystal seed with co-precipitation-rheology phase legal system 3Al 5O 12: Ce fluorescent material, its shape of product rule, grain diameter (d 50) 0.1～20 μ, size distribution is even, chemical property is stable, good luminous performance, can effectively be excited by blue light.
Technical scheme of the present invention is following:
Rare-earth-dopping yttrium aluminum garnet (Y provided by the invention 3Al 5O 12: the Ce) co-precipitation of fluorescent material-rheology phase preparation method, it is with the nanometer of regular shape or micron YAG, SiO 2Or SiC is equipped with rare earth doping yttrium aluminium garnet fluorescent powder as crystal seed with co-precipitation-rheology phase legal system; Preparation process is following:
1) preparation Y 3Al 5O 12: Ce fluorescent material presoma:
1.1) preparing metal ion mixed solution:
Taking by weighing purity by stoichiometric ratio is that the MOX powder of 4N-7N adds in the entry; Preparing metal oxide compound suspension liquid; Add concentrated nitric acid again; Be heated to the MOX powder and dissolve fully, being mixed with concentration is the mixing solutions of the pH value 6-7 of 0.02～0.15mol/l, adds Al (NO by stoichiometric ratio to this mixing solutions again 3) 3, make the metals ion mixed solution; Described MOX powder is the mixed powder of yttrium oxide powder and cerium oxide powder;
1.2) compound concentration is the precipitant solution of 1.0～3.0mol/l, said precipitation agent is at least a in ammonium bicarbonate soln, urea, ammoniacal liquor and the oxalic acid solution;
1.3) preparation precipitation by metallic ion thing:
With step 1.1) the metals ion mixed solution is added to step 1.2 with the speed of 1ml/min～10ml/min) in the precipitant solution that makes, carry out precipitin reaction, still aging throw out;
In the said metals ion mixed solution in metals ion total moles and the said precipitant solution mole number proportioning of precipitation agent be 1: 20;
1.4) use deionized water and absolute ethanol washing gained throw out more successively, get white Y 3Al 5O 12: Ce fluorescent material presoma, and to said Y 3Al 5O 12: Ce fluorescent material presoma carries out drying treatment;
2) with crystal seed and step 1.4) Y 3Al 5O 12: Ce fluorescent material presoma mixes, and in this mixture, adds dispersion agent again, and and solvent, said mixture is adjusted to the rheology phase, and this rheology phase mixture is carried out drying treatment;
Described crystal seed is YAG crystal seed, SiO 2Crystal seed or SiC crystal seed;
Said dispersion agent is an ammonium sulfate, at least a in polyoxyethylene glycol, hydroxylated cellulose and the Trimethyllaurylammonium bromide;
Said solvent is deionized water, ethanol, acetate or oxalic acid;
Said crystal seed, said dispersion agent and Y 3Al 5O 12: the weight part proportioning of Ce fluorescent material presoma is 0.1～5: 0.1～0.5: 100;
3) in step 2) the rheology phase mixture after drying treatment in add the fusing assistant of the 1-20wt% of this rheology phase mixture gross weight; Evenly form compound through ground and mixed; In reducing atmosphere, said compound is carried out roasting and get product of roasting, said maturing temperature is 900 ℃～1600 ℃;
Described fusing assistant is an alkali metal halide, alkaline earth metal halide, boric acid, at least a in ammonium halogenide, alkaline carbonate and the alkaline earth metal carbonate;
4) product of roasting that step 3) is obtained washs successively again, removal of impurities, oven dry and classification, makes rare earth doping yttrium aluminium garnet fluorescent powder.
Grinding in the said step 3) is for to grind in ethanol, acetone or water.The roasting time of described step 4) is 2～30 hours.The removal of impurities of in the said step 4) said product of roasting being carried out is to its pickling, alkali cleaning or washing.Be classified as a kind of classification or several kinds of mixing-classifyings in settling process classification, method of sieving classification, hydraulic elutria-tion method classification and the classification of air classification method to what said product of roasting carried out in the said step 4).
The co-precipitation of rare earth doping yttrium aluminium garnet fluorescent powder provided by the invention-rheology phase preparation method has following characteristics:
The inventive method is in the co-precipitation presoma, to add uniform nanometer or the micron inorganic particulate crystal seed as precipitin reaction; Add various tensio-active agents simultaneously; And the adding solvent adjustment becomes the rheology phase, the rare earth doping yttrium aluminium garnet fluorescent powder regular shape that obtains, even, the grain diameter (d of particle diameter 50) 0.1～20 μ, size distribution is even, chemical property is stable, good luminous performance, can effectively be excited by blue light; Can be applicable to blue-light LED chip.
Embodiment
Below further describe the present invention through specific embodiment, but protection scope of the present invention does not receive the qualification of these embodiment.
Embodiment 1
The preparation molecule is Y 3Al 5O 12: the rare earth doping yttrium aluminium garnet fluorescent powder of Ce, its preparation process is following:
Take by weighing 3.331gY 2O 3(4N) and 0.086gCeO 2(4N) add in the entry, use volume ratio to be the concentrated nitric acid heating for dissolving of 1ml: 1ml it, the pH that is mixed with concentration and is 0.08mol/l is 6 yttrium cerium nitrate mixed solution; Add 18.756gAl (NO to this mixing solutions again 3) 39H 2O processes metallic ion mixed liquor (female salts solution);
Take by weighing 6.320g NH 4HCO 3, be mixed with the precipitant solution that concentration is 1.5mol/l;
At room temperature, female salts solution is dripped (drop rate 5ml/min) to the NH that stirs with the anti-method of dripping 4HCO 3In the solution, until whole generation depositions; Use deionized water and absolute ethanol washing throw out more successively; Get the white depositions presoma, this white depositions presoma is carried out drying treatment;
With being added in the above-mentioned white depositions presoma after 0.6umYAG crystal seed 0.060g and dispersion agent (Trimethyllaurylammonium bromide) the 0.01g mixing, be adjusted to the rheology attitude with ethanol;
Above-mentioned rheology phase material 100 ℃ of insulations 6 hours, is obtained drying product;
Add fusing assistant (0.060g fluoridize receive and the 0.060g mebor) mix grinding in the product in oven dry then; 1600 ℃ of roastings got product of roasting in 2 hours in reducing atmosphere (nitrogen-hydrogen mixed gas) again;
Again the gained product of roasting is carried out comminution by gas stream, pickling, alkali cleaning, washing removal of impurities, oven dry and classification of sedimentation etc. successively, obtain the YAG:Ce (Y that particle diameter is about 1.5um 3Al 5O 12: Ce) rare earth doping yttrium aluminium garnet fluorescent powder.
Comparative example 1
The preparation molecule is Y 2.95Al 5O 12: Ce 0.05Rare earth doping yttrium aluminium garnet fluorescent powder, it prepares as follows:
Take by weighing 3.331gY 2O 3(4N) and 0.086gCeO 2(4N) add in the entry, use volume ratio to be the concentrated nitric acid heating for dissolving of 1ml: 1ml it, the pH that is mixed with concentration and is 0.08mol/l is 6 yttrium cerium nitrate mixed solution; Add 18.756gAl (NO to this mixing solutions again 3) 39H 2O processes metallic ion mixed liquor (female salts solution);
Take by weighing 6.320g NH 4HCO 3, be mixed with the precipitant solution that concentration is 1.5mol/l;
At room temperature, female salts solution is dripped (drop rate 5ml/min) to the NH that stirs with the anti-method of dripping 4HCO 3In the solution, until whole generation depositions; Use deionized water and absolute ethanol washing throw out more successively; Get the white depositions presoma, this white depositions presoma is carried out drying treatment;
0.6umYAG crystal seed 0.060g and dispersion agent (Trimethyllaurylammonium bromide) 0.01g are added in the above-mentioned throw out presoma, add fusing assistant (0.060g fluoridize receive and the 0.060g mebor) mix grinding in the product in oven dry then; 1600 ℃ of roastings got product of roasting in 2 hours in reducing atmosphere (nitrogen-hydrogen mixed gas) again;
Again the gained product of roasting is carried out comminution by gas stream, pickling, alkali cleaning, washing removal of impurities, oven dry and classification of sedimentation etc. successively, obtain the YAG:Ce fluorescent material that particle diameter is about 2.5um.
Comparative example 2
Take by weighing 3.331gY 2O 3(4N) and 0.086gCeO 2(4N) add in the entry, use volume ratio to be the concentrated nitric acid heating for dissolving of 1ml: 1ml it, the pH that is mixed with concentration and is 0.08mol/l is 6 yttrium cerium nitrate mixed solution; Add 18.756gAl (NO to this mixing solutions again 3) 39H 2O processes metallic ion mixed liquor (female salts solution);
Take by weighing 6.320g NH 4HCO 3, be mixed with the precipitant solution that concentration is 1.5mol/l;
At room temperature, female salts solution is dripped (drop rate 5ml/min) to the NH that stirs with the anti-method of dripping 4HCO 3In the solution, until whole generation depositions; Use deionized water and absolute ethanol washing throw out more successively; Get the white depositions presoma, this white depositions presoma is carried out drying treatment;
0.01g is added in the above-mentioned throw out presoma with dispersion agent (Trimethyllaurylammonium bromide), is adjusted to the rheology attitude with ethanol;
Above-mentioned rheology phase material 100 ℃ of insulations 6 hours, is obtained drying product;
Add fusing assistant (0.060g fluoridize receive and the 0.060g mebor) mix grinding in the product in oven dry then; 1600 ℃ of roastings got product of roasting in 2 hours in reducing atmosphere (nitrogen-hydrogen mixed gas) again;
Again the gained product of roasting is carried out comminution by gas stream, pickling, alkali cleaning, washing removal of impurities, oven dry and classification of sedimentation etc. successively, obtain the YAG:Ce fluorescent material that particle diameter is about 1.0um.
Embodiment 1 with the difference of two comparative examples is: embodiment 1 adopts co-precipitation-rheology of the present invention method (adding crystal seed) mutually, comparative example 1 usefulness coprecipitation method (adding crystal seed), comparative example 2 usefulness coprecipitation method-rheology phase method (not adding crystal seed).
The emission peak wavelength of embodiment 1 and two made fluorescent material of comparative example, relative luminous intensity are as shown in the table:
Sample Emission peak wavelength (nm) Relative luminous intensity (%)
Embodiment 1 540 112
Comparative example 1 541 100
Comparative example 2 540 90
By on can know that with the prepared YAG:Ce fluorescent material of method of the present invention, regular shape, particle diameter are even, be easy to apply, be well positioned to meet application requiring (chemical property is stable, good luminous performance, can effectively be excited) by blue light; Can be widely used in blue-light LED chip.
Embodiment 2
The preparation molecule is Y 3Al 5O 12: the rare earth doping yttrium aluminium garnet fluorescent powder of Ce, it prepares as follows:
Take by weighing 3.331gY 2O 3(5N) and 0.086gCeO 2(5N) add in the entry, use volume ratio to be the concentrated nitric acid heating for dissolving of 1ml: 1ml it, the pH that is mixed with concentration and is 0.02mol/l is 7 yttrium cerium nitrate mixed solution; Add 18.756gAl (NO to this mixing solutions again 3) 39H 2O processes metallic ion mixed liquor (female salts solution);
Take by weighing 6.320g NH 4HCO 3, be mixed with the precipitant solution that concentration is 1.0mol/l;
At room temperature, female salts solution is dripped (drop rate 1ml/min) to the NH that stirs with the anti-method of dripping 4HCO 3In the solution, until whole generation depositions; Use deionized water and absolute ethanol washing throw out more successively; Get the white depositions presoma, this white depositions presoma is carried out drying treatment;
0.05umSiC crystal seed 0.30g and dispersion agent (polyoxyethylene glycol) 0.006g are added in the above-mentioned throw out presoma, are adjusted to the rheology attitude with deionized water;
Above-mentioned rheology phase material 100 ℃ of insulations 6 hours, is obtained drying product;
Add fusing assistant (0.120g fluoridize receive) mix grinding in the product in oven dry then; 900 ℃ of roastings got product of roasting in 2 hours in reducing atmosphere (nitrogen-hydrogen mixed gas) again;
Again the gained product of roasting is carried out comminution by gas stream, pickling, alkali cleaning, washing removal of impurities, oven dry and classification of sedimentation etc. successively, obtain the YAG:Ce fluorescent material that particle diameter is about 0.1um.
Embodiment 3
The preparation molecule is Y 3Al 5O 12: the rare earth doping yttrium aluminium garnet fluorescent powder of Ce, it prepares as follows:
Take by weighing 3.331gY 2O 3(6N) and 0.086gCeO 2(6N) add in the entry, use volume ratio to be the concentrated nitric acid heating for dissolving of 1ml: 1ml it, the pH that is mixed with concentration and is 0.15mol/l is 6 yttrium cerium nitrate mixed solution; Add 18.756gAl (NO to this mixing solutions again 3) 39H 2O processes metallic ion mixed liquor (female salts solution);
Take by weighing 6.320g NH 4HCO 3, be mixed with the precipitant solution that concentration is 3.0mol/l;
At room temperature, female salts solution is dripped (drop rate 10ml/min) to the NH that stirs with the anti-method of dripping 4HCO 3In the solution, until whole generation depositions; Use deionized water and absolute ethanol washing throw out more successively; Get the white depositions presoma, this white depositions presoma is carried out drying treatment;
With 0.1um SiO 2Crystal seed 0.006g and dispersion agent (ammonium sulfate) 0.02g is added in the above-mentioned throw out presoma, is adjusted to the rheology attitude with acetate;
Above-mentioned rheology phase material 100 ℃ of insulations 6 hours, is obtained drying product;
In the oven dry product, add fusing assistant (0.120g boric acid) mix grinding then; 1200 ℃ of roastings got product of roasting in 10 hours in reducing atmosphere (nitrogen-hydrogen mixed gas) again;
Again the gained product of roasting is carried out comminution by gas stream, pickling, alkali cleaning, washing removal of impurities, oven dry and classification of sedimentation etc. successively, obtain the YAG:Ce fluorescent material that particle diameter is about 1.0um.
Embodiment 4
The preparation molecule is Y 3Al 5O 12: the rare earth doping yttrium aluminium garnet fluorescent powder of Ce, it prepares as follows:
Take by weighing 3.331gY 2O 3(7N) and 0.086gCeO 2(7N) add in the entry, use volume ratio to be the concentrated nitric acid heating for dissolving of 1ml: 1ml it, the pH that is mixed with concentration and is 0.08mol/l is 6 yttrium cerium nitrate mixed solution; Add 18.756gAl (NO to this mixing solutions again 3) 39H 2O processes metallic ion mixed liquor (female salts solution);
Take by weighing 9.612g urea, be mixed with the precipitant solution that concentration is 1.5mol/l;
At room temperature, female salts solution is dripped (drop rate 3ml/min) to the urea soln that stirs with the anti-method of dripping, until whole generation depositions; Use deionized water and absolute ethanol washing throw out more successively; Get the white depositions presoma, this white depositions presoma is carried out drying treatment;
0.6umYAG crystal seed 0.12g and dispersion agent (polyoxyethylene glycol) 0.03g are added in the above-mentioned throw out presoma, are adjusted to the rheology attitude with oxalic acid;
Above-mentioned rheology phase material 100 ℃ of insulations 6 hours, is obtained drying product;
In the oven dry product, add fusing assistant (1.20g barium fluoride) mix grinding then; 1600 ℃ of roastings got product of roasting in 30 hours in reducing atmosphere (nitrogen-hydrogen mixed gas) again;
Again the gained product of roasting is carried out comminution by gas stream, pickling, alkali cleaning, washing removal of impurities, oven dry and classification of sedimentation etc. successively, obtain the YAG:Ce fluorescent material that particle diameter is about 20um.
Embodiment 5
The preparation molecule is Y 3Al 5O 12: the rare earth doping yttrium aluminium garnet fluorescent powder of Ce, it prepares as follows:
Take by weighing 3.331gY 2O 3(5N) and 0.086gCeO 2(5N) add in the entry, use volume ratio to be the concentrated nitric acid heating for dissolving of 1ml: 1ml it, the pH that is mixed with concentration and is 0.08mol/l is 7 yttrium cerium nitrate mixed solution; Add 18.756gAl (NO to this mixing solutions again 3) 39H 2O processes metallic ion mixed liquor (female salts solution);
Take by weighing 2.724g ammoniacal liquor, be mixed with the precipitant solution that concentration is 1.5mol/l;
At room temperature, female salts solution is dripped (drop rate 6ml/min) to the ammonia soln that stirs with the anti-method of dripping, until whole generation depositions; Use deionized water and absolute ethanol washing throw out more successively; Get the white depositions presoma, this white depositions presoma is carried out drying treatment;
0.6umYAG crystal seed 0.12g and dispersion agent (hydroxylated cellulose) 0.01g are added in the above-mentioned throw out presoma, are adjusted to the rheology attitude with ethanol;
Above-mentioned rheology phase material 100 ℃ of insulations 6 hours, is obtained drying product;
In the oven dry product, add fusing assistant (0.06g Neutral ammonium fluoride) mix grinding then; 1500 ℃ of roastings got product of roasting in 15 hours in reducing atmosphere (nitrogen-hydrogen mixed gas) again;
Again the gained product of roasting is carried out comminution by gas stream, pickling, alkali cleaning, washing removal of impurities, oven dry and classification of sedimentation etc. successively, obtain the YAG:Ce fluorescent material that particle diameter is about 10um.
Embodiment 6
The preparation molecule is Y 3Al 5O 12: the rare earth doping yttrium aluminium garnet fluorescent powder of Ce, it prepares as follows:
Take by weighing 3.331gY 2O 3(5N) and 0.086gCeO 2(5N) add in the entry, use volume ratio to be the concentrated nitric acid heating for dissolving of 1ml: 1ml it, the pH that is mixed with concentration and is 0.08mol/l is 7 yttrium cerium nitrate mixed solution; Add 18.756gAl (NO to this mixing solutions again 3) 39H 2O processes metallic ion mixed liquor (female salts solution);
Take by weighing 20.171g oxalic acid, be mixed with the precipitant solution that concentration is 2.0mol/;
At room temperature, female salts solution is dripped (drop rate 10ml/min) to the oxalic acid solution that stirs with the anti-method of dripping, until whole generation depositions; Use deionized water and absolute ethanol washing throw out more successively; Get the white depositions presoma, this white depositions presoma is carried out drying treatment;
0.1umYAG crystal seed 0.20g and dispersion agent (hydroxylated cellulose) 0.01g are added in the above-mentioned throw out presoma, are adjusted to the rheology attitude with oxalic acid;
Above-mentioned rheology phase material 100 ℃ of insulations 6 hours, is obtained drying product;
In the oven dry product, add fusing assistant (0.80g yellow soda ash) mix grinding then; 1600 ℃ of roastings got product of roasting in 5 hours in reducing atmosphere (nitrogen-hydrogen mixed gas) again;
Again the gained product of roasting is carried out comminution by gas stream, pickling, alkali cleaning, washing removal of impurities, oven dry and classification of sedimentation etc. successively, obtain the YAG:Ce fluorescent material that particle diameter is about 5.0um.
Even, the grain diameter (d of rare earth doping yttrium aluminium garnet fluorescent powder regular shape, particle diameter of the inventive method preparation 50) 0.1～20 μ, size distribution is even, chemical property is stable, good luminous performance, can effectively be excited by blue light; Can be applicable to blue-light LED chip.

Claims (5)

1. the co-precipitation of a rare earth doping yttrium aluminium garnet fluorescent powder-rheology phase preparation method, it is with the nanometer of regular shape or micron YAG, SiO 2Or SiC is equipped with rare earth doping yttrium aluminium garnet fluorescent powder as crystal seed with co-precipitation-rheology phase legal system; Preparation process is following:
1) preparation rare earth doping yttrium aluminium garnet fluorescent powder presoma:
1.1) preparing metal ion mixed solution:
Taking by weighing purity by stoichiometric ratio is that the MOX powder of 4N-7N adds in the entry; Preparing metal oxide compound suspension liquid; Add concentrated nitric acid again; Be heated to the MOX powder and dissolve fully, being mixed with concentration is the mixing solutions of the pH value 6-7 of 0.02～0.15mol/l, adds Al (NO by stoichiometric ratio to this mixing solutions again 3) 3, make the metals ion mixed solution; Described MOX powder is the mixed powder of yttrium oxide powder and cerium oxide powder;
1.2) compound concentration is the precipitant solution of 1.0～3.0mol/l, said precipitation agent is at least a in ammonium bicarbonate soln, urea, ammoniacal liquor and the oxalic acid solution;
1.3) preparation precipitation by metallic ion thing:
With step 1.1) the metals ion mixed solution is added to step 1.2 with the speed of 1ml/min～10ml/min) in the precipitant solution that makes, carry out precipitin reaction, still aging throw out;
In the said metals ion mixed solution in metals ion total moles and the said precipitant solution mole number proportioning of precipitation agent be 1: 20;
1.4) use deionized water and absolute ethanol washing gained throw out more successively, get white rare earth doping yttrium aluminium garnet fluorescent powder presoma, and said rare earth doping yttrium aluminium garnet fluorescent powder presoma is carried out drying treatment;
2) with crystal seed and step 1.4) the rare earth doping yttrium aluminium garnet fluorescent powder presoma mix, in this mixture, add dispersion agent again, and and solvent, said mixture is adjusted to the rheology phase, and this rheology phase mixture is carried out drying treatment;
Described crystal seed is YAG crystal seed, SiO 2Crystal seed or SiC crystal seed;
Said dispersion agent is an ammonium sulfate, at least a in polyoxyethylene glycol, hydroxylated cellulose and the Trimethyllaurylammonium bromide;
Said solvent is deionized water, ethanol, acetate or oxalic acid;
Said crystal seed, said dispersion agent and Y 3Al 5O 12: the weight part proportioning of Ce fluorescent material presoma is 0.1～5: 0.1～0.5: 100;
3) in step 2) the rheology phase mixture after drying treatment in add the fusing assistant of the 1-20wt% of this rheology phase mixture gross weight; Evenly form compound through ground and mixed; In reducing atmosphere, said compound is carried out roasting and get product of roasting, said maturing temperature is 900 ℃～1600 ℃;
Described fusing assistant is an alkali metal halide, alkaline earth metal halide, boric acid, at least a in ammonium halogenide, alkaline carbonate and the alkaline earth metal carbonate;
4) product of roasting that step 3) is obtained washs successively again, removal of impurities, oven dry and classification, makes rare earth doping yttrium aluminium garnet fluorescent powder.
2. by the co-precipitation-rheology phase preparation method of the described rare earth doping yttrium aluminium garnet fluorescent powder of claim 1, it is characterized in that the grinding in the said step 3) is for to grind in ethanol, acetone or water.
3. by the co-precipitation-rheology phase preparation method of the described rare earth doping yttrium aluminium garnet fluorescent powder of claim 3, it is characterized in that the roasting time of described step 4) is 2～30 hours.
4. by the co-precipitation-rheology phase preparation method of the described rare earth doping yttrium aluminium garnet fluorescent powder of claim 1, it is characterized in that the removal of impurities of in the said step 4) said product of roasting being carried out is to its pickling, alkali cleaning or washing.
5. press the co-precipitation-rheology phase preparation method of the described rare earth doping yttrium aluminium garnet fluorescent powder of claim 1,
It is characterized in that, be classified as a kind of classification or several kinds of mixing-classifyings in settling process classification, method of sieving classification, hydraulic elutria-tion method classification and the classification of air classification method to what said product of roasting carried out in the said step 4).
CN201110005674.7A 2011-01-07 2011-01-07 Coprecipitation-rheological phase preparation method of rare earth-doped yttrium aluminum garnet fluorescent powder Expired - Fee Related CN102585824B (en)

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CN102899045A (en) * 2012-10-25 2013-01-30 江苏博睿光电有限公司 Preparation method for yellow fluorescent powder for LED (Light Emitting Diode)
CN103641149A (en) * 2013-12-14 2014-03-19 福建师范大学 Method of synthesizing monodisperse hexagonal rare earth fluoride nanosheet by adopting rheological phase reaction method
CN104045103A (en) * 2014-06-24 2014-09-17 中国工程物理研究院化工材料研究所 Yttrium aluminium garnet nano-powder and preparation method thereof
CN104119910A (en) * 2013-04-28 2014-10-29 广东超越光电科技有限公司 Fluorescent powder for light-emitting diode
CN104341152A (en) * 2013-07-25 2015-02-11 中国科学院宁波材料技术与工程研究所 Preparation method for garnet phase nano-powder
CN111057547A (en) * 2019-12-27 2020-04-24 江苏师范大学 Silicon carbide modified YAG (yttrium aluminum garnet) Ce fluorescent powder and preparation method thereof

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102899045A (en) * 2012-10-25 2013-01-30 江苏博睿光电有限公司 Preparation method for yellow fluorescent powder for LED (Light Emitting Diode)
CN104119910A (en) * 2013-04-28 2014-10-29 广东超越光电科技有限公司 Fluorescent powder for light-emitting diode
CN104341152A (en) * 2013-07-25 2015-02-11 中国科学院宁波材料技术与工程研究所 Preparation method for garnet phase nano-powder
CN103641149A (en) * 2013-12-14 2014-03-19 福建师范大学 Method of synthesizing monodisperse hexagonal rare earth fluoride nanosheet by adopting rheological phase reaction method
CN103641149B (en) * 2013-12-14 2015-06-17 福建师范大学 Method of synthesizing monodisperse hexagonal rare earth fluoride nanosheet by adopting rheological phase reaction method
CN104045103A (en) * 2014-06-24 2014-09-17 中国工程物理研究院化工材料研究所 Yttrium aluminium garnet nano-powder and preparation method thereof
CN111057547A (en) * 2019-12-27 2020-04-24 江苏师范大学 Silicon carbide modified YAG (yttrium aluminum garnet) Ce fluorescent powder and preparation method thereof

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