CN102391871A - Preparation method of nano yttrium aluminum garnet fluorescent powder - Google Patents
Preparation method of nano yttrium aluminum garnet fluorescent powder Download PDFInfo
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Abstract
The invention discloses a preparation method of a nano yttrium aluminum garnet fluorescent powder, comprising the following steps of: preparing raw materials such as aluminium nitrate, yttrium nitrate and nitrate of the rare earth elements into mother liquor of which the total cation concentration is 0.1-1.0mol/L according to the proportion of 5: (3-X): X, wherein X is 0-0.1, reacting the evenly-mixed mother liquor in a depositing way by the means that weak base alcohol water solution or ammonia is added into an ultra-gravity field, and controlling the pH value at 7.0-8.0 so as to obtain turbid liquid; performing aging, extraction filtering, and microwave drying on the turbid liquid so as to obtain a precursor body; and putting the precursor body in a microwave field, and calcinating the precursor body so as to obtain a yttrium aluminum garnet fluorescent powder which is good in dispersity and has the particle size of 20-100 nanometers. Compared with the prior art, the preparation method has the advantages that the product has the mean grain size of about 20-100 nanometers, and the product is narrow in particle size distribution, free of conglobation, good in dispersity, high in crystallization degree, and free of transient phase. Furthermore, the preparation method is simple in technology, and can be used for quickly producing the nano yttrium aluminum garnet fluorescent powder in batches.
Description
Technical field
The present invention relates to a kind of method for preparing fluorescent material, particularly relate to a kind of novel method for preparing nanometer yttrium aluminum garnet fluorescent material.
Background technology
" green illumination " plan of electricity-saving lamp has successively been released and banned use of incandescent light, promoted the use of in global in recent years a plurality of countries; See from global range; The development trend that electricity-saving lamp replaces incandescent light is irreversible, and expectation will drive the fast development of China's electricity-saving lamp industry.In field of display, along with popularizing of panel display screens such as LCD, PDP, replace traditional C RT market, estimate to show and will rise year by year with the rare earth luminescent material market requirement.According to national fluorescent RE powder, the prediction of lamp coorporative network; By 2013; China's electricity-saving lamp output will reach nearly 7,000,000,000, and flat panel TV will be above 13,000 ten thousand; Also with reaching 2.93 hundred million, 1.59 hundred million and 8.80 hundred million respectively, the rare earth luminescent material market requirement will be above 14000 tons for the output of notebook computer, liquid-crystal display and mobile phone.
China's rare earth luminescent material enterprise competitiveness power a little less than.China's rare earth luminescent material industry is traditional small workshop mode manufacturing enterprise and modern large-scale production enterprise at present and deposits in addition; Owing to receive the influence of factors such as production technology level and foreign vendor's downstream corner on the market; Use rare earth luminescent material field with rare earth luminescent material, FPD with rare earth luminescent material and special source at high-end electricity-saving lamp, domestic have only industry-leading enterprise such as the permanent share of section to possess relevant art deposit and capability of industrialization.Therefore, accelerate technological improvement, autonomous innovation, active research development and preparation efficient LED is with the novel process and the new phosphors of fluorescent material; Emphasis is to using the research of performance, mass-producing, industrialization; Improve stability, the consistence of product overall applicability performance and product, break the monopolization of Japan, the U.S., have real environment, economy and social effect the LED industry; Also be instant task, extremely urgent.
At present, the main method for preparing yttrium aluminium garnet fluorescent powder both at home and abroad comprises solid phase method, liquid phase method, vapor phase process.Solid phase method is simple to operate, but the Granularity Distribution of preparation is uneven, is prone to reunite; Liquid phase method is the most frequently used method of present synthesizing nano-particle, and so it introduces impurity easily, and product purity is not high; The vapor phase process product is reunited few, good dispersivity, and particle diameter is little, narrowly distributing, but productive rate is low, and powder is easily collecting not.To sum up can know, prepare still difficulty relatively of nanometer yttrium aluminum garnet fluorescent material, its reason one is that YAG fluorescent material particle in the crystal conversion process can reunite, and is difficult to reach nano level; Next is that not high, the assorted peak of crystalline phase purity is many; The temperature requirement that is sintered into YAG fluorescent material is more than 1000 ℃; The TR that is sintered into YAG fluorescent material through different compound methods so will reach higher percent crystallinity between 1000 to 1500 ℃, must improve calcining temperature; Increase calcination time, general common heating mode is difficult to meet the demands.In addition, general preparing method's production cycle is long, is unfavorable for suitability for industrialized production
Therefore, proposed following improving one's methods, but still problem has separately been arranged, existing about the patent of preparation nanometer yttrium aluminum garnet fluorescent material aspect and the problem or the weak point of existence:
Chinese patent CN1907860A discloses a kind of preparation method who prepares nanometer yttrium aluminium garnet powder; Its main raw material(s) aluminum nitrate, Yttrium trinitrate and other nitrate of rare earth element; Wherein adopted alcohol-water compounded solvents coprecipitation method, that this preparation method has is controlled, can stablize advantages such as obtaining monophasic nanometer yttrium aluminium garnet powder, and its weak point is that the titration process time is longer; Production cycle is longer, and preparation cost is high.
Chinese patent CN101289218A discloses a kind of preparation method who prepares nanometer yttrium aluminium garnet powder; Its main raw material(s) aluminum nitrate, Yttrium trinitrate; Wherein adopt the mode of spraying, be added drop-wise to the mixing solutions of aluminum nitrate and Yttrium trinitrate in the urea soln presoma that obtains; After calcining, obtain the nanometer yttrium aluminum garnet powder, its weak point is that the powder of gained has obvious agglomeration.
In known up to now preparation method, its weak point is: the bad dispersibility of the yttrium aluminum garnet powder of gained, particle shape heterogeneity, and size distribution is wide, and particle is difficult to be controlled at nanoscale.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, a kind of good dispersivity, particle shape homogeneous are provided, narrow diameter distribution, particle are controlled at nanoscale, the novel method for preparing the nanometer yttrium aluminum garnet powder easily.
The present invention realizes through following mode: its main raw material(s) is aluminum nitrate, Yttrium trinitrate and other nitrate of rare earth element, in super gravity field, carries out precipitin reaction, said method comprising the steps of:
(1) with aluminum nitrate, Yttrium trinitrate and other nitrate of rare earth element according to 5: (3-X): the X ratio is made into the mother liquor that total cation concentration is 0.1-1.0mol/L, and X is 0-0.1, uniform mixing; The mother liquor that mixes in super gravity field, adds the weak base alcohol solution or ammonia carries out precipitin reaction, and control pH value obtains suspension liquid at 7.0-8.0;
(2) step (1) gained suspension liquid was worn out 2-6 hour at 40-80 degree Celsius, suction filtration obtains filter cake 3-5 time with deionized water wash then; Filter cake is joined in the 100-300 milliliter absolute ethyl alcohol, and ultrasonic concussion is the back suction filtration evenly.40-80 degree microwave drying Celsius 2-6 hour, obtain the precursor of 15-90 nanometer;
(3) step (2) gained precursor is placed microwave field, under 700-1100 degree Celsius, calcining the granularity that obtained good dispersivity in 0.5-4 hour is the yttrium aluminium garnet fluorescent powder of 20-100 nanometer; The chemical formula of described yttrium aluminium garnet fluorescent powder is Y
1-xAl
5O
12: Me
x, wherein one or more among Me=Ce, La, Tb, Gb, Si, the Nb and combination thereof.
Said suspension liquid prepares with the liquid-liquid reactions method under the super gravity field environment.
Said suspension liquid prepares with the gas-liquid reaction method under the super gravity field environment.
The equipment of said super gravity field is RPB, rotating bed with helix channel or other hypergravity reaction unit.
Described microwave field calcining directly heats up to control to calcine changes brilliant.
Described microwave field calcination procedure heats up and controls calcining commentaries on classics crystalline substance.
Said microwave high-temperature calcining precursor obtains nanometer yttrium aluminum garnet fluorescent material, regulates and control nanometer yttrium aluminum garnet fluorescent powder grain size through the particle diameter of control nanometer precursor.
Compared with prior art, the present invention has the following advantages: the product median size is about the 20-100 nanometer, and narrow diameter distribution does not have and reunites, good dispersivity, percent crystallinity height and complete in crystal formation, no transition phase.And this method technology is simple, but rapid batch is produced nanometer yttrium aluminum garnet fluorescent material.
Description of drawings
Fig. 1 is the XRD figure of the nanometer presoma of preparation among the embodiment 1
Fig. 2 be the nanometer presoma of preparation among the embodiment 1 SEM figure+
Fig. 3 is the XRD figure of the nano yttrium aluminum garnet powder of preparation among the embodiment 1
Fig. 4 is the SEM figure of the nano yttrium aluminum garnet powder of preparation among the embodiment 1
Fig. 5 is the SEM figure of the nano yttrium aluminum garnet powder of preparation in the reference examples 1
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is further described.
The main raw material(s) of method of the present invention is aluminum nitrate, Yttrium trinitrate and other nitrate of rare earth element, in super gravity field, carries out precipitin reaction, said method comprising the steps of:
(1) with aluminum nitrate, Yttrium trinitrate and other nitrate of rare earth element according to 5: (3-X): the X ratio is made into the mother liquor that total cation concentration is 0.1-1.0mol/L, and X is 0-0.1, uniform mixing; The mother liquor that mixes in super gravity field, adds the weak base alcohol solution or ammonia carries out precipitin reaction, and control pH value obtains suspension liquid at 7.0-8.0; The preferred 0.3-0.5 of X.
(2) step (1) gained suspension liquid was worn out 2-6 hour at 40-80 degree Celsius, suction filtration obtains filter cake 3-5 time with deionized water wash then; Filter cake is joined in the 100-300 milliliter absolute ethyl alcohol, and ultrasonic concussion is the back suction filtration evenly.40-80 degree microwave drying Celsius 2-6 hour, obtain the precursor of 15-90 nanometer;
(3) step (2) gained precursor is placed microwave field, under 700-1100 degree Celsius, calcining the granularity that obtained good dispersivity in 0.5-4 hour is the yttrium aluminium garnet fluorescent powder of 20-100 nanometer; The chemical formula of described yttrium aluminium garnet fluorescent powder is Y
1-xAl
5O
12: Mex, wherein one or more among Me=Ce, La, Tb, Gb, Si, the Nb and combination thereof.
Said suspension liquid prepares with the liquid-liquid reactions method under the super gravity field environment.
Said suspension liquid prepares with the gas-liquid reaction method under the super gravity field environment.
The equipment of said super gravity field is RPB, rotating bed with helix channel or other hypergravity reaction unit.
Described microwave field calcining directly heats up to control to calcine changes brilliant.
Described microwave field calcination procedure heats up and controls calcining commentaries on classics crystalline substance.
Said microwave high-temperature calcining precursor obtains nanometer yttrium aluminum garnet fluorescent material, regulates and control nanometer yttrium aluminum garnet fluorescent powder grain size through the particle diameter of control nanometer precursor.
The embodiment explanation:
1, the transformation temperature of presoma:
Adopt TGAQ50 type thermogravimetric analyzer, at N
2Sample was warming up to 1200 ℃ with the speed of 10 ℃/min under atmosphere was enclosed, heavy (TGA/DSC) curve of record differential thermal difference.
2, material phase analysis:
Adopt Japanese motor D of science/MAX-3C type X-ray diffractometer to test (CuK α target; Wavelength is 0.154nm; Graphite monochromator, pipe pressure=50KV, pipe stream=100mA); The thing that the contrast of gained spectrogram and standard card can be confirmed material mutually and crystalline structure can calculate the crystal block size according to the Scherrer formula.
D-grain-size angle
The K-constant, K=0.89
λ-wavelength, λ=0.15406nm
The wideization degree at half place of L-diffracted ray intensity
3, morphology analysis:
Adopt observation morphology microstructure, crystallization lines, the Micro-Structure Analysis of JSM-6360LV type electron-microscope scanning appearance (SEM) and JEM 2010 type transmission electron microscopes (TEM) and estimate particle size.
Embodiment 1
Get aluminum nitrate 21.30 grams, Yttrium trinitrate 16.5 gram uniform mixing according to 5: 3 mol ratios; Add the mixed solution that deionized water is mixed with 2L; Be made into the mother liquor that total cation concentration is 0.16mol/L, use the rotating bed with helix channel supergravity reactor to produce super gravity field, in super gravity field, react and circulate; In the super gravity field reactor drum, add the weak base alcohol solution, pH value of solution is controlled at 7.0-8.0 obtains suspension liquid.With gained suspension liquid suction filtration behind 60 ℃ of aging 2h, with deionized water wash 3 times.Filter cake is joined in the 200ml absolute ethyl alcohol, and ultrasonic concussion is the back suction filtration evenly.At 60 ℃ of microwave drying 4h, the precursor that obtains loosening.The gained precursor is placed microwave field, and 15 ℃/min program is warming up to 1000 ℃ of insulation 2h from room temperature and obtains loose yttrium aluminium garnet fluorescent powder.Presoma and performance of products by XRD and SEM detected result referring to Fig. 1, Fig. 2, Fig. 3 and Fig. 4.From XRD and SEM figure, can know, the pure phase YAG powder of products obtained therefrom, spherical in shape, median size does not have and reunites at 50nm.
Microwave calcination:
Its method is following: get precursor 2-50g and place corundum crucible, put into microwave Muffle furnace and calcine, temperature programming, calcining temperature 700-1200 ℃, calcination time 0.5-4h.
Reference examples 1
Get aluminum nitrate 21.30 grams, Yttrium trinitrate 16.50 gram uniform mixing according to 5: 3 mol ratios; Add the mixed solution that deionized water is mixed with 2L; Be made into the mother liquor that total cation concentration is 0.16mol/L; In super gravity field, circulate, add the weak base alcohol solution, the pH value of solution value is controlled at 7.0-8.0 obtains suspension liquid.With gained suspension liquid suction filtration behind 60 ℃ of aging 2h, with deionized water wash 3 times.Filter cake is joined in the 200ml absolute ethyl alcohol, and ultrasonic concussion is the back suction filtration evenly.At 60 ℃ of microwave drying 4h, the precursor that obtains loosening.The gained precursor is got 2-50g place corundum crucible, place common retort furnace, calcine 2h down at 1000 ℃ and obtain yttrium aluminium garnet fluorescent powder.Performance of products is by SEM check and analysis Fig. 5, can know that by SEM figure particle has adhesion phenomenon, powder dispersed relatively poor, and median size is about 85 nanometers.
When in common retort furnace, calcining precursor, calcining temperature 950-1400 ℃, calcination time 0.5-4h, calcining temperature is high, and energy consumption is big, and preparation cost is high.
Get aluminum nitrate 21.30 grams, Yttrium trinitrate 16.50 gram uniform mixing according to 5: 3 mol ratios; Add the mixed solution that deionized water is mixed with 2L; Be made into the mother liquor that total cation concentration is 0.16mol/L; In super gravity field, circulate, add the weak base alcohol solution, the pH value of solution value is controlled at 7.0-8.0 obtains suspension liquid.With gained suspension liquid suction filtration behind 60 ℃ of aging 2h, with deionized water wash 3 times.Filter cake is joined in the 200ml absolute ethyl alcohol, and ultrasonic concussion is the back suction filtration evenly.At 60 ℃ of microwave drying 4h, the precursor that obtains loosening.The gained precursor is placed microwave field, and fast directly heating mode is from room temperature to 1000 ℃, and insulation 2h obtains loose yttrium aluminium garnet fluorescent powder.
Microwave calcination:
Its method is following: gets precursor 2-50g and places corundum crucible, put into microwave Muffle furnace and calcine, directly heat up fast, and calcining temperature 700-1200 ℃, calcination time 0.5-4h.
Embodiment 3
Prepare nanometer yttrium aluminum garnet fluorescent material according to embodiment 1 identical method, different is: soaking time is made as 0.5h.
Embodiment 4
Prepare nanometer yttrium aluminum garnet fluorescent material according to embodiment 1 identical method, different is: soaking time is made as 4h.
Embodiment 5
Prepare nanometer yttrium aluminum garnet fluorescent material according to embodiment 1 identical method, different is: calcining temperature is made as 1100 ℃.
Embodiment 6
Get aluminum nitrate 21.30 grams, Yttrium trinitrate 16.17 grams and cerous nitrate 0.391 gram uniform mixing according to 5: 2.94: 0.06 mol ratios; Add deionized water 2L and be made into the mother liquor that total cation concentration is 0.16mol/L; In super gravity field, circulate; Add the weak base alcohol solution, pH value of solution is controlled at 7.0-8.0 forms suspension liquid.With gained suspension liquid suction filtration behind 60 ℃ of aging 2h, with deionized water wash 3 times.Filter cake is joined in the 200ml absolute ethyl alcohol, and ultrasonic concussion is the back suction filtration evenly.At 60 ℃ of microwave drying 4h, the precursor that obtains loosening.The gained precursor is placed microwave field, and 15 ℃/min temperature programming to 1000 a ℃ insulation 2h obtains loose YAG:Ce fluorescent material.
Embodiment 7
According to 5: 2.84: 0.06: 0.1 mol ratio was got aluminum nitrate 21.30 grams, Yttrium trinitrate 15.62 grams, cerous nitrate 0.391 gram and Lanthanum trinitrate 0.65 gram uniform mixing; Add deionized water 2L and be made into the mother liquor that total cation concentration is 0.16mol/L; In super gravity field, circulate; Add the weak base alcohol solution, pH value of solution is controlled at 7.0-8.0 forms suspension liquid.With gained suspension liquid suction filtration behind 60 ℃ of aging 2h, with deionized water wash 3 times.Filter cake is joined in the 200ml absolute ethyl alcohol, and ultrasonic concussion is the back suction filtration evenly.At 60 ℃ of microwave drying 4h, the precursor that obtains loosening.The gained precursor is placed microwave field, and 15 ℃/min temperature programming to 1000 a ℃ insulation 2h obtains loose YAG:Ce fluorescent material.
Embodiment 8:
According to 5: 2.84: 0.06: 0.1 mol ratio was got aluminum nitrate 21.30 grams, Yttrium trinitrate 15.62 grams, cerous nitrate 0.391 gram and Lanthanum trinitrate 0.65 gram uniform mixing; Add deionized water 2L and be made into the mother liquor that total cation concentration is 0.16mol/L; In super gravity field, circulate; Add the weak base alcohol solution, pH value of solution is controlled at 7.0-8.0 forms suspension liquid.With gained suspension liquid suction filtration behind 60 ℃ of aging 2h, with deionized water wash 3-4 time.Filter cake is joined in the 200ml absolute ethyl alcohol, and ultrasonic concussion is the back suction filtration evenly.At 70 ℃ of microwave drying 3h, the precursor that obtains loosening.The gained precursor is placed the roasting of microwave baboon stove microwave field, be warming up to 1050 ℃ of insulation 2h by 15 ℃/min speed program and obtain loose YAG:Ce fluorescent material.
Method of the present invention adopts the hypergravity legal system to be equipped with the presoma of nanometer yttrium aluminum garnet powder, adopts microwave high-temperature calcining presoma, obtains the nanometer yttrium aluminum garnet powder.This is a kind of novel method of utilizing hypergravity and microwave integrated technique to prepare the nanometer yttrium aluminum garnet powder.
The nanometer precursor can under the super gravity field environment, prepare with gas-liquid reaction or liquid-liquid reactions method or other method prepares.The super gravity field reactor drum comprises the hypergravity reaction unit of RPB (RPB), rotating bed with helix channel (RBHC) or other form.
The present invention utilizes that the high-temperature calcination presoma obtains the nanometer yttrium aluminum garnet powder in the microwave field.Microwave heating is different from common heating, and common method for calcinating is that heat energy passes through conduction pattern by entad portion's transmission of specimen surface, makes the specimen surface temperature be higher than inside.For microwave calcination, sample is inner to have the ability of equal absorption microwave with the surface, and external enwergy is simultaneously by even heating in the sample.Sample temperature inside gradient is little, can make the material built-in thermal stress reduce to minimum, can stop particulate to be reunited like this.And microwave heating is faster than the routine heating, save energy, and also pollution-free.
In sum, the present invention has following beneficial effect:
1, a kind of novel method for preparing the nanometer yttrium aluminum garnet powder can be provided; The size distribution that has overcome prior art for preparing nanometer yttrium aluminum garnet powder is uneven, is prone to reunite, and crystalline phase purity is low; The not high shortcoming of percent crystallinity; Can prepare nanometer yttrium aluminum garnet powder median size is the 20-100 nanometer, narrow diameter distribution, percent crystallinity height and complete in crystal formation.
2, the preparation method of nanometer presoma of the present invention is many.This nanometer precursor can obtain with solution-air (G-L) reaction or liquid-liquid (L-L) prepared in reaction under the hypergravity environment, perhaps prepares with other method.
3, adopt the size of the adjustable preparation cashier of super gravity field effect rice presoma particle diameter, thereby can prepare the nanometer yttrium aluminum garnet particle grain size through control precursor particle size.
4, utilize microwave high-temperature calcining preparation nanometer yttrium aluminum garnet powder, operation is simple.
5, method technology of the present invention is simple, but rapid batch is produced nanometer yttrium aluminum garnet fluorescent material.
Claims (10)
1. method for preparing nanometer yttrium aluminum garnet fluorescent material, main raw material(s) is aluminum nitrate, Yttrium trinitrate and other nitrate of rare earth element, in super gravity field, carries out precipitin reaction, it is characterized in that: said method comprising the steps of:
(1) with aluminum nitrate, Yttrium trinitrate and other nitrate of rare earth element according to 5: (3-X): the X ratio is made into the mother liquor that total cation concentration is 0.1-1.0mol/L, and X is 0-0.1, uniform mixing; The mother liquor that mixes in super gravity field, adds the weak base alcohol solution or ammonia carries out precipitin reaction, and control pH value obtains suspension liquid at 7.0-8.0;
(2) step (1) gained suspension liquid was worn out 2-6 hour at 40-80 degree Celsius, suction filtration obtains filter cake 3-5 time with deionized water wash then; Filter cake is joined in the 100-300 milliliter absolute ethyl alcohol, and ultrasonic concussion is the back suction filtration evenly.40-80 degree microwave drying Celsius 2-6 hour, obtain the precursor of 15-90 nanometer;
(3) step (2) gained precursor is placed microwave field, under 700-1100 degree Celsius, calcining the granularity that obtained good dispersivity in 0.5-4 hour is the yttrium aluminium garnet fluorescent powder of 20-100 nanometer; The chemical formula of described yttrium aluminium garnet fluorescent powder is Y
1-xAl
5O
12: Me
x, wherein one or more among Me=Ce, La, Tb, Gb, Si, the Nb and combination thereof.
2. the method for preparing nanometer yttrium aluminum garnet fluorescent material according to claim 1 is characterized in that: said suspension liquid prepares with the liquid-liquid reactions method under the super gravity field environment.
3. the method for preparing nanometer yttrium aluminum garnet fluorescent material according to claim 1 is characterized in that: said suspension liquid prepares with the gas-liquid reaction method under the super gravity field environment.
4. according to the optional described method for preparing nanometer yttrium aluminum garnet fluorescent material of claim 1-3, it is characterized in that: the equipment of said super gravity field is RPB, rotating bed with helix channel or other hypergravity reaction unit.
5. according to the optional described method for preparing nanometer yttrium aluminum garnet fluorescent material of claim 1-3, it is characterized in that: described microwave field calcining directly intensification control calcining changes brilliant.
6. according to the optional described method for preparing nanometer yttrium aluminum garnet fluorescent material of claim 1-3, it is characterized in that: described microwave field calcination procedure heats up to control to calcine changes brilliant.
7. the method for preparing nanometer yttrium aluminum garnet fluorescent material according to claim 4 is characterized in that: described microwave field calcining directly heats up to control to calcine changes brilliant.
8. the method for preparing nanometer yttrium aluminum garnet fluorescent material according to claim 4 is characterized in that: described microwave field calcination procedure heats up and controls calcining commentaries on classics crystalline substance.
9. according to the optional described method for preparing nanometer yttrium aluminum garnet fluorescent material of claim 1-3; It is characterized in that: said microwave high-temperature calcining precursor obtains nanometer yttrium aluminum garnet fluorescent material, regulates and control nanometer yttrium aluminum garnet fluorescent powder grain size through the particle diameter of control nanometer precursor.
10. the method for preparing nanometer yttrium aluminum garnet fluorescent material according to claim 4; It is characterized in that: said microwave high-temperature calcining precursor obtains nanometer yttrium aluminum garnet fluorescent material, regulates and control nanometer yttrium aluminum garnet fluorescent powder grain size through the particle diameter of control nanometer precursor.
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