CN105315995A - Fluxing agent and method for preparing YAG fluorescent powder - Google Patents
Fluxing agent and method for preparing YAG fluorescent powder Download PDFInfo
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Abstract
The invention provides a fluxing agent and a method for preparing YAG fluorescent powder. The fluxing agent for preparing YAG fluorescent powder comprises a substance of which the chemical formula is AxHyPO4, and further comprises an oxide of Bi2O3, B2O3 and BaO; in the formula of AxHyPO4, A is NH4, Li, Na or K, x is greater than or equal to 1 and less than or equal to 3, and x+y=3. When the YAG fluorescent powder is prepared, the combined fluxing agent is added into a fluorescent powder raw material and uniformly mixed; by adjusting the ratio of phosphate to oxides in the fluxing agent and by adjusting the ratio of the fluxing agent to the fluorescent powder raw material, the size of YAG fluorescent powder granules can be controlled; by sintering the fluxing agent and the fluorescent powder raw material after being mixed, the sintering temperature can be reduced, and the crystallinity and homogeneity of YAG fluorescent powder granules can be improved; the fluorescent powder prepared from the fluxing agent is environment-friendly, easy in aftertreatment, high in brightness, uniform in granularity and good in dispersity.
Description
Technical field
The present invention relates to a kind of fluorescent material preparation method, specifically a kind of fusing assistant and method preparing YAG fluorescent powder.
Background technology
Electric energy can be converted into luminous energy by LED photodiode, and it has, and efficiency of conversion is high, long service life, the advantage such as energy-conservation, is widely used in fields such as illumination, displays.In recent years, blue and near-ultraviolet light LED develops rapidly, adopting yellow fluorescent powder to join blue chip, to realize white light be current packaged type the most widely, the fluorescent material of yttrium aluminum garnet (being called for short YAG) structure has the advantage that luminous efficiency is high and chemical stability is good, is a kind of desirable LED fluorescent material.
Along with developing rapidly of LED, the requirement of people to fluorescent material performance (as crystallinity, granular size etc.) is also more and more higher.YAG fluorescent powder uses maximum a kind of fluorescent material, and the performance improving YAG fluorescent powder obviously can promote package quality, and the principal element limiting YAG fluorescent powder performance at present has the type etc. of the purity of raw material, sintering process and fusing assistant.
In the choosing of fusing assistant, normally used have boric acid, borate, fluorochemical etc., as disclosed a kind of method of synthesized high-performance LED fluorescent powder in patent CN201310387833.3, fusing assistant adopts the auxiliary combination producing bifluoride in bifluoride and reaction process, good acidic atmosphere is kept in reaction process, be conducive to improving brightness, this kind of fusing assistant causes sintering temperature more than 1500 DEG C, after sintering there is skewness in grain graininess, the problems such as crystallinity is poor, finally cause luminosity low, poor stability, antidamping ability, the existence of fluorochemical simultaneously causes difficulty to aftertreatment.Patent CN201210063056.2 discloses a kind of fusing assistant of yellow fluorescent powder, on the basis of fluorochemical and borate compositions, with the addition of carbonate, obtain good dispersity, crystallization is crystal grain that is spherical or elliposoidal, but the size-grade distribution of particle, brightness are all well improved.Patent CN201210141988.4 discloses a kind of fusing assistant of LED yellow fluorescent powder, with NaF, KPF
6, SrCl
2common proportioning obtains the comparatively uniform fluorescent material of size distribution, and improve original intensity, but in product, fine particle is more, the homogeneity of particle is still poor, and product yield is low.The use of fusing assistant fluorochemical, causes it unstable under the high temperature conditions, produces fluorine-containing poison gas, easy contaminate environment, easily works the mischief to the person in production process.
Summary of the invention
An object of the present invention is just to provide a kind of fusing assistant preparing YAG fluorescent powder, there is not fluorochemical in this fusing assistant, and aftertreatment is simple, free from environmental pollution.
Two of object of the present invention is just to provide a kind of method preparing YAG fluorescent powder, the process employs above-mentioned fusing assistant, and prepares gained YAG fluorescent powder even particle size distribution, and brightness is higher.
An object of the present invention is achieved in that a kind of fusing assistant preparing YAG fluorescent powder, and it is A that this fusing assistant comprises chemical general formula
xh
ypO
4material, also comprise Bi
2o
3, B
2o
3with a kind of oxide compound in BaO; General formula A
xh
ypO
4in, A is NH
4, Li, Na or K, 1≤x≤3, and x+y=3.
A in described fusing assistant
xh
ypO
4with the mol ratio of oxide compound be: 1:5 ~ 5:1.
The usage quantity of described fusing assistant accounts for 0.3% ~ 10% of the raw materials used total mass of preparation YAG fluorescent powder.
Two of object of the present invention is achieved in that a kind of method preparing YAG fluorescent powder, comprises the steps:
A, according to chemical general formula Y
3-a-mm
aal
5-bga
bo
12: in mLn, the stoichiometric ratio of each element takes oxide compound corresponding to each element respectively; In general formula, M is the one in Sc and Gd, and Ln is the one in Ce, Eu and Lu, 0≤a≤2,0≤b < 5,0.03≤m≤0.35;
B, take fusing assistant, described fusing assistant is by A
xh
ypO
4form with oxide compound, the oxide compound in described fusing assistant is Bi
2o
3, B
2o
3with the one in BaO; A is NH
4, Li, Na or K, 1≤x≤3, and x+y=3; The quality of the fusing assistant taken accounts for 0.3% ~ 10% of all raw material total masses taken in step a, and in fusing assistant, A
xh
ypO
4with the mol ratio of oxide compound be: 1:5 ~ 5:1;
C, the fusing assistant taken in the raw material taken in step a and step b is mixed after put into crucible, be heated to temperature T under reducing atmosphere, soaking time t under temperature T, is down to room temperature afterwards, obtains sintered product;
D, by sintered product take out, after ball milling, pickling, washing, filtration, oven dry, obtain YAG fluorescent powder.
In step c, described temperature T meets: 1300 DEG C≤T≤1450 DEG C.
In step c, described time t meets: 4h≤t≤6h.
In step c, reducing atmosphere is the mixed gas of nitrogen and hydrogen.
Fusing assistant provided by the present invention is A
xh
ypO
4with the mixed flux of oxide compound, this mixed flux uses when preparing YAG fluorescent powder, can improve the brightness of YAG fluorescent powder, improve the particle size distribution of powder, crystallinity and dispersiveness; Sintering temperature can also be reduced while the good luminous performance of guarantee YAG fluorescent powder; And fusing assistant used is conventional phosphate and conventional oxide, can not produce the objectionable impurities of welding, can not impact human body, aftertreatment is easy, environmentally friendly.
Accompanying drawing explanation
Fig. 1 is the Y prepared by the embodiment of the present invention 1
2.96al
5o
12: the SEM figure of 0.04Ce fluorescent material.
Fig. 2 is the Y prepared by the embodiment of the present invention 1
2.96al
5o
12: the utilizing emitted light spectrogram of 0.04Ce fluorescent material.
Fig. 3 is the Y prepared by comparative example 1 of the present invention
2.96al
5o
12: the SEM figure of 0.04Ce fluorescent material.
Embodiment
The fusing assistant of preparation YAG fluorescent powder provided by the present invention, by A
xh
ypO
4form with combination of oxides, oxide compound is Bi
2o
3, B
2o
3with the one in BaO; General formula A
xh
ypO
4in, A is NH
4, Li, Na or K, 1≤x≤3, and x+y=3.A in fusing assistant
xh
ypO
4with the mol ratio of oxide compound be: 1:5 ~ 5:1.The amount of the fusing assistant used when preparing YAG fluorescent powder generally accounts for 0.3% ~ 10% of the raw materials used total mass of preparation YAG fluorescent powder, by the ratio of phosphoric acid salt and oxide compound in adjustment fusing assistant, adjust solubility promoter and proportioning raw materials used during preparation YAG fluorescent powder simultaneously, and then the size of YAG fluorescent powder particle can be controlled.
The chemical general formula of YAG fluorescent powder prepared in the present invention is Y
3-a-mm
aal
5-bga
bo
12: mLn, in general formula, M is the one in Sc and Gd, and Ln is the one in Ce, Eu and Lu, 0≤a≤2,0≤b < 5,0.03≤m≤0.35.Its medium trace element Sc, Gd, Ga add, and can modify the lattice imperfection of fluorescent material, improve the luminous intensity of this system fluorescent material.Fusing assistant can reduce the sintering temperature of fluorescent material, and promote that activator enters intracell, the phosphoric acid salt in fusing assistant has dissemination, and activator can be prevented oxidized, the oxide compound in fusing assistant can promote the growth of crystal grain simultaneously.
The method preparing YAG fluorescent powder is described in the present invention below in detail with specific embodiment.
Embodiment 1:Y
2.96al
5o
12: the preparation of 0.04Ce fluorescent material.
Corresponding Y is taken respectively in molar ratio for Y:Al:Ce=2.96:5:0.04
2o
3, Al
2o
3and CeO
2as the raw material of preparation YAG fluorescent powder, then take the Na of total raw material quality 10%
3pO
4and B
2o
3as fusing assistant, in fusing assistant, the mass ratio of phosphoric acid salt and oxide compound is Na
3pO
4: B
2o
3=3:1, mixes raw material and fusing assistant and loads in corundum crucible, be heated to 1450 DEG C, be incubated and be cooled to room temperature after 5 hours, obtain sintered product in the reducing atmosphere that nitrogen mixes with hydrogen (volume ratio is 7:3).Sintered product was pulverized 150 mesh sieves, then carry out ball milling with the agate ball of 6mm and water, then carry out warm pickling with hydrochloric acid, then wash, moisture is washed till specific conductivity and is less than 10 μ S/cm, filters, and obtains required sample after drying through 100 DEG C.Carry out sem test to obtained sample, acquired results is shown in Fig. 1, as seen from Figure 1, and the good dispersity of powder granule, good uniformity.Through particle size analyzer test, the particle diameter (medium particle diameter, i.e. D50) of powder is 7.58 μm.Adopt the light source of 460nm to prepared Y
2.96al
4.9ga
0.1o
12: 0.04Ce fluorescent material excites, and gained emmission spectrum is as shown in Figure 2.As seen from Figure 2, its emission peak is about 550nm, is Yellow luminous fluorescent material.
Embodiment 2-17, according to the processing condition in embodiment 1, step, accounting for the ratio of the mass ratio of phosphor raw material, phosphoric acid salt and oxide compound, preparing different fluorescent material by changing fusing assistant in fusing assistant.Obtained fluorescent material is carried out to the test of relative brightness and particle diameter, acquired results is in table 1.
Table 1
As can be seen from Table 1, fusing assistant account for raw material ratio in 0.3% ~ 10% scope time, along with the increase of fusing assistant addition, particle reduce, homogeneity is better; Fusing assistant account for raw material ratio lower than 0.3% time, particle brightness is lower, reason be fusing assistant less time, it is more difficult that activator Ce enters crystals; Fusing assistant account for raw material ratio more than 10% after, crystal morphology be deteriorated, cause brightness to decline, the homogeneity of particle also can decline.Embodiment 11-14 gives the situation that combination fusing assistant ratio exceeds proportional range given in the present invention, and when combining fusing assistant ratio and going beyond the scope, can cause the appearance of irregular particle, particle uniformity also can decline.
Embodiment 18-45, according to the processing condition in embodiment 1, step, the addition of fusing assistant, changes the stoichiometric ratio of each element of fluorescent material, prepares different fluorescent material.Obtained fluorescent material is carried out to the test of relative brightness and particle diameter, acquired results is in table 2.
Table 2
| Embodiment | Fluorescent material chemical general formula | Relative brightness | D50 | (D90-D10)/D50 |
| 18 | Y 2.97Al 5O 12:0.03Ce | 101.4 | 11.53 | 1.1482 |
| 19 | Y 2.84Al 5O 12:0.16Ce | 103.7 | 15.46 | 1.0485 |
| 20 | Y 2.8Al 5O 12:0.2Ce | 103.2 | 18.99 | 0.9473 |
| 21 | Y 2.65Al 5O 12:0.35Ce | 101.9 | 20.47 | 1.0468 |
| 22 | Y 2.971Al 5O 12:0.029Ce | 88.7 | 12.45 | 1.297 |
| 23 | Y 2.6Al 5O 12:0.4Ce | 79.8 | 16.59 | 1.276 |
| 24 | Y 2.75Sc 0.05Al 5O 12:0.2Ce | 103.8 | 10.75 | 0.897 |
| 25 | Y 1.45Sc 1.35Al 5O 12:0.2Ce | 103.5 | 11.97 | 0.972 |
| 26 | Y 1.3Sc 1.5Al 5O 12:0.2Ce | 103.9 | 15.67 | 0.897 |
| 27 | Y 0.8Sc 2Al 5O 12:0.2Ce | 104.5 | 13.59 | 1.019 |
| 28 | Y 0.6Sc 2.2Al 5O 12:0.2Ce | 87.2 | 15.19 | 0.978 |
| 29 | Y 2.75Gd 0.05Al 5O 12:0.2Ce | 103.5 | 8.79 | 0.798 |
| 30 | Y 1.8Gd 1Al 5O 12:0.2Ce | 104.1 | 7.92 | 0.849 |
| 31 | Y 0.8Gd 2Al 5O 12:0.2Ce | 102.5 | 12.51 | 0.749 |
| 32 | Y 0.6Gd 2.2Al 5O 12:0.2Ce | 89.2 | 13.41 | 1.200 |
| 33 | Y 0.8Gd 2Al 4GaO 12:0.2Ce | 102.4 | 12.42 | 0.802 |
| 34 | Y 0.8Gd 2Al 3.4Ga 1.6O 12:0.2Ce | 103.2 | 11.57 | 0.889 |
| 35 | Y 0.8Gd 2Al 4.7Ga 0.3O 12:0.2Ce | 104.9 | 12.68 | 0.924 |
| 36 | Y 2.96Al 5O 12:0.04Lu | 102.3 | 6.21 | 1.0251 |
| 37 | Y 2.93Al 5O 12:0.07Lu | 104.7 | 13.74 | 0.9952 |
| 38 | Y 2.65Al 5O 12:0.35Lu | 103.8 | 15.38 | 0.8957 |
| 39 | Y 2.8Al 4.3Ga 0.7O 12:0.2Lu | 104.9 | 11.58 | 0.9984 |
| 40 | Y 2.93Al 3.4Ga 1.6O 12:0.07Lu | 103.1 | 12.46 | 1.495 |
| 41 | Y 0.8Gd 2Al 4GaO 12:0.2Lu | 103.3 | 12.23 | 0.9037 |
| 42 | Y 1.65Sc 0.75Al 5O 12:0.6Lu | 102.0 | 17.89 | 1.089 |
| 43 | Y 2.93Al 5O 12:0.07Eu | 98.5 | 12.25 | 1.023 |
| 44 | Y 2.7Al 5O 12:0.3Eu | 100.7 | 12.38 | 0.9048 |
| 45 | Y 2.4Gd 0.5Al 5O 12:0.1Eu | 101.4 | 15.90 | 1.0592 |
In embodiment 18-23, the concentration of activator can affect the luminous intensity of fluorescent material, and activator content is increased to after 0.35, and portion of energy is not outside quantity of radiant energy in activator internal delivery, causes the reduction of luminosity.In theory, particle is larger, luminescence center is more, and particle light-emitting intensity is higher, in embodiment 24-35, rare earth Sc, the adding of Gd, Ga, the crystallinity of crystal grain is improved, and luminous intensity has the raising of part, but when the add-on of Sc, Gd is greater than 2, lattice defect increases, and luminous intensity reduces.
Embodiment 46-54, according to the addition of the fluorescent material mol ratio in embodiment 1, fusing assistant, changes the sintering temperature in fluorescent material preparation process and soaking time, prepares different fluorescent material.Obtained fluorescent material is carried out to the test of relative brightness and particle diameter, acquired results is in table 3.
Table 3
| Embodiment | Sintering temperature/DEG C | Sintering time/h | Relative brightness | D50/μm | (D90-D10)/D50 |
| 1 | 1450 | 5 | 102.2 | 7.58 | 0.7968 |
| 46 | 1300 | 5 | 101.2 | 8.28 | 0.8182 |
| 47 | 1380 | 5 | 101.5 | 8.10 | 0.8102 |
| 48 | 1290 | 5 | 88 | 12.51 | 1.852 |
| 49 | 1460 | 5 | 102.0 | 7.64 | 1.025 |
| 50 | 1380 | 3.5 | 98.0 | 10.13 | 1.885 |
| 51 | 1380 | 4 | 102.0 | 8.11 | 0.8412 |
| 52 | 1380 | 6 | 102.5 | 8.00 | 0.7842 |
| 53 | 1380 | 6.5 | 101.2 | 8.12 | 0.9700 |
| 54 | 1380 | 7 | 101.0 | 8.05 | 0.8584 |
In embodiment 1, embodiment 46-54, when temperature is less than 1300 DEG C, the crystal structure of fluorescent material is poor, and homogeneity is lower, causes particle light-emitting low lightness; When temperature is higher than 1450 DEG C, temperature is too high, and the particle shape obtained is irregular, and particle uniformity is poor.When sintering time is less than 4h, the non-complete reaction of raw material, granular size is uneven, and luminescence center is uneven, and luminous intensity is low; Sintering time is greater than 6h, there is no larger improvement to the performance of fluorescent material, and therefore sintering time is best between 4h-6h.
Comparative example 1:Y
2.96al
5o
12: the preparation of 0.04Ce fluorescent material.
Corresponding Y is taken respectively in molar ratio for Y:Al:Ce=2.96:5:0.04
2o
3, Al
2o
3and CeO
2as the raw material of preparation YAG fluorescent powder, then take the H of total raw material quality 2.5%
3bO
3, NaF, AlF
3and Na
2cO
3as fusing assistant, in fusing assistant, the mass ratio of each material is H
3bO
3: NaF:AlF
3: Na
2cO
3=1:0.4:0.6:0.5.Raw material and fusing assistant are loaded in ball grinder, ball mill mixes, reinstalls in corundum crucible, in nitrogen and hydrogen (volume ratio is 95:5) mixed reducing atmosphere, be heated to 1550 DEG C, be incubated and be cooled to room temperature after 2 hours, obtain sintered product.Sintered product was pulverized 150 mesh sieves, and then carried out ball milling with the agate ball of 6mm and water, be washed till specific conductivity through four moisture and be less than 10 μ S/cm, filter, after drying through 120 DEG C, obtained required sample.Carry out sem test to obtained sample, acquired results is shown in Fig. 3, and as seen from Figure 3, the particle diameter of powder is approximately 13-15 μm.
Because in documents 1, fusing assistant have employed NaF and AlF
3, therefore aftertreatment is more difficult, has larger harm to environment.And also can find out from Fig. 3, the particle uniformity of the fluorescent material prepared by documents 1 is poor, powder reuniting phenomenon is comparatively serious, bad dispersibility.And adopt fluorescent material (see Fig. 1) granule-morphology prepared by the present invention good, particle surface zero defect, the homogeneity of particle and good dispersity.In documents 1, sintering temperature is 1550 DEG C, and the temperature that the present invention prepares fluorescent material is lower, is 1300 DEG C ~ 1450 DEG C, reduces sintering temperature.
Claims (7)
1. prepare a fusing assistant for YAG fluorescent powder, it is characterized in that, it is A that this fusing assistant comprises chemical general formula
xh
ypO
4material, also comprise Bi
2o
3, B
2o
3with a kind of oxide compound in BaO; General formula A
xh
ypO
4in, A is NH
4, Li, Na or K, 1≤x≤3, and x+y=3.
2. the fusing assistant of preparation YAG fluorescent powder according to claim 1, is characterized in that, A in described fusing assistant
xh
ypO
4with the mol ratio of oxide compound be: 1:5 ~ 5:1.
3. the fusing assistant of preparation YAG fluorescent powder according to claim 1, is characterized in that, the usage quantity of described fusing assistant accounts for 0.3% ~ 10% of preparation YAG fluorescent powder raw material total mass.
4. prepare a method for YAG fluorescent powder, it is characterized in that, comprise the steps:
A, according to chemical general formula Y
3-a-mm
aal
5-bga
bo
12: in mLn, the stoichiometric ratio of each element takes oxide compound corresponding to each element respectively; In general formula, M is the one in Sc and Gd, and Ln is the one in Ce, Eu and Lu, 0≤a≤2,0≤b < 5,0.03≤m≤0.35;
B, take fusing assistant, described fusing assistant is by A
xh
ypO
4form with oxide compound, the oxide compound in described fusing assistant is Bi
2o
3, B
2o
3with the one in BaO; A is NH
4, Li, Na or K, 1≤x≤3, and x+y=3; The quality of the fusing assistant taken accounts for 0.3% ~ 10% of all raw material total masses taken in step a, and in fusing assistant, A
xh
ypO
4with the mol ratio of oxide compound be: 1:5 ~ 5:1;
C, the fusing assistant taken in the raw material taken in step a and step b is mixed after put into crucible, be heated to temperature T under reducing atmosphere, soaking time t under temperature T, is down to room temperature afterwards, obtains sintered product;
D, by sintered product take out, after ball milling, pickling, washing, filtration, oven dry, obtain YAG fluorescent powder.
5. the method preparing YAG fluorescent powder according to claim 4, is characterized in that, in step c, described temperature T meets: 1300 DEG C≤T≤1450 DEG C.
6. the method preparing YAG fluorescent powder according to claim 4, is characterized in that, in step c, described time t meets: 4h≤t≤6h.
7. the method preparing YAG fluorescent powder according to claim 4, is characterized in that, in step c, reducing atmosphere is the mixed atmosphere of nitrogen and hydrogen.
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| Publication number | Publication date |
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| CN105315995B (en) | 2017-08-04 |
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