CN108018040A - A kind of fluorescent ceramic material, its preparation method and a kind of low color temperature white light LED - Google Patents

A kind of fluorescent ceramic material, its preparation method and a kind of low color temperature white light LED Download PDF

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CN108018040A
CN108018040A CN201711321597.XA CN201711321597A CN108018040A CN 108018040 A CN108018040 A CN 108018040A CN 201711321597 A CN201711321597 A CN 201711321597A CN 108018040 A CN108018040 A CN 108018040A
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fluorescence ceramics
powder
ceramic material
sintering
white light
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孙鹏
刘永福
蒋俊
江浩川
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Ningbo Institute of Material Technology and Engineering of CAS
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Ningbo Institute of Material Technology and Engineering of CAS
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Abstract

The present invention provides a kind of fluorescent ceramic material, its chemical formula is:(A2‑xRexM)(Mg2D3)O12, wherein A is at least one of for Y, Lu, Sc, Gd, Ga, at least one of Re Eu, Ce, Pr, Sm, Dy, Tm, Tb, Nd, at least one of M Ca, Sr, Ba, at least one of D Ti, Si, Ge, 0.001≤x<2.The fluorescence ceramics can effectively be excited by blue chip, and low color temperature white light LED can be made with reference to blue chip;At the same time, the fluorescence ceramics have the incomparable machinery of fluorescent powder and mechanical property, can directly it be packaged with blue chip, substitute the encapsulation mode that current fluorescent powder adds organic material, efficiently solve organic packaging materials weak heat-dissipating, the problem of light efficiency reduction caused by continuous high temperature and color drift, significantly extend the white light LED part service life.

Description

A kind of fluorescent ceramic material, its preparation method and a kind of low color temperature white light LED
Technical field
The present invention relates to transparent fluorescent ceramic material, particularly a kind of fluorescent ceramic material, its preparation method and use it Prepare the application of low color temperature white light LED.
Background technology
White light LEDs as forth generation lighting source have the advantages of energy-saving and environmental protection, long lifespan and response are rapid, The development to attract people's attention is achieved, is widely used in various light scenes.The manufacture method of commercialization white light LEDs is usually adopted at present More than one fluorescent powder is encapsulated on blue chip using organic materials such as epoxy resin or silica gel with encapsulation technology, by Shine and the unnecessary blue light of blue chip excitated fluorescent powder obtain white light.But this packaged type is in actual use It there are problems that:First, organic packaging materials heat dissipation performance is poor, and prolonged periods, which light lower temperature, can be higher than 150 DEG C, Organic material easily aged deterioration at high temperature, causes luminous efficiency of source reduction and color drift, greatly reduces the use of white light LEDs Service life;Secondly as the heat dissipation performance of encapsulating material is poor, fluorescent powder is also constantly in hot environment in encapsulating material, causes Fluorescent powder aging, causes temperature quenching, equally causes light efficiency to reduce and color drift phenomenon;Furthermore fluorescent powder is in encapsulating material It is scattered uneven, when particularly high-volume makes, fluorescent powder is in epoxy resin and silica gel since precipitation causes scattered inequality It is even, cause light source luminescent irregular colour even.The application and popularization of white light LEDs of the above problem all strong influences, also limit Its development in large power white light LED field.
2006, Anant A.Setlur et al. reported Lu first2CaMg2(Si,Ge)3O12:Ce3+Orange fluorescent powder (refer to document Crystal Chemistry and Luminescence of Ce3+-Doped Lu2CaMg2(Si,Ge)3O12And Its Use in LED Based Lighting, Chem.Mater.2006,18,3314-3322), since it is unique Luminescent properties, propose to be applied in white light LEDs field.2016, Wei Xia et al. also ground this fluorescent powder Study carefully (Synthesis and luminescence properties of (Lu0.95-xCe0.05)2Ca1+ 2xMg2Si3O12silicate garnet phosphors and its applications,Functional Materials Letters Vol.9, No.3 (2016)), and it is subjected to single powder encapsulation with traditional YAG fluorescent powder and is contrasted, in chromaticity coordinates and light For effect under conditions of, the white light LED color temperature of the fluorescent powder packaging is lower.But white light LEDs prepared by the orange fluorescent powder It is difficult to avoid the above problem.
The content of the invention
The present invention provides a kind of fluorescent ceramic material, can be stimulated by blue light, and has the characteristic of the high colour developing of low colour temperature, can use , can directly and blue light simultaneously because with the incomparable machinery of fluorescent powder and mechanical property in making low color temperature white light LED Chip is packaged, and substitutes the encapsulation mode that current fluorescent powder adds organic material, so as to effectively solve organic packaging materials heat dissipation The problem of difference, light efficiency reduction caused by continuous high temperature and color drift, it can significantly extend the white light LED part service life.
The technical scheme is that:A kind of fluorescent ceramic material, its chemical formula are (A2-xRexM)(Mg2D3)O12, in, A For the combination of a kind of element or two or more elements in Y, Lu, Sc, Gd, Ga, Re is rare earth element Eu, Ce, Pr, Sm, Dy, The combination of a kind of element or two or more elements in Tm, Tb, Nd, a kind of element or two or more members in M Ca, Sr, Ba The combination of element, the combination of a kind of element or two or more elements in D Ti, Si, Ge;Also, 0.001≤x≤0.2, as It is preferred that 0.01≤x≤0.1.
The fluorescent ceramic material is garnet structure, belongs to cubic system, space group Ia3d.
The excitation wavelength of the fluorescent ceramic material can be effectively excited by blue light in 400-550nm, is issued in blue light excitation It is 500-700nm to penetrate wave-length coverage.
The spectrum of the fluorescent ceramic material can be adjusted by the species and concentration for adjusting matrix components and rare earth element, is reached Develop the color to low colour temperature is high.
Present invention also offers a kind of method for preparing above-mentioned fluorescent ceramic material, include the following steps:
(1) (A is pressed2-xRexM)(Mg2D3)O12Stoichiometric ratio, by the oxide of A or corresponding salt, the oxide of Re Either corresponding salt, the oxide of M or corresponding salt, the oxide of D or corresponding salt, magnesia or the corresponding salt of magnesium Mixed, obtain nanometer or the other powder of submicron order;
(2) by the powder calcination, the organic matter and volatile matter in powder are removed, and carries out tabletting and makes biscuit of ceramics;
(3) biscuit of ceramics is sintered and annealed, obtain fluorescence ceramics;
(4) fluorescence ceramics are processed by shot blasting, to improve transmitance, control thickness.
In the step (1), the method for obtaining powder is unlimited, including ball-milling method, sol-gal process or sluggish precipitation etc..
In the step (2), preferably, calcining heat is 600 DEG C -1200 DEG C.
In the step (2), biscuit production method is unlimited, including isometric unidirectional, isometric bidirectional pressing and isostatic cool pressing Deng.
In the step (3), sintering method is unlimited, including vacuum-sintering, reducing atmosphere sintering, hot pressed sintering and heat etc. Static pressure sintering etc..Preferably, sintering process to be warming up to 600 DEG C -1200 DEG C, keeps the temperature 1h-24h, then heat to 1300 DEG C - 1450 DEG C, insulation 2h-24h is cooled to room temperature afterwards.
In the step (3), method for annealing is unlimited, including carries out in atmosphere, in reducing atmosphere, in oxygen atmosphere, moves back Fiery temperature is preferably 900 DEG C -1300 DEG C, and the preferred 2h-20h of soaking time, is cooled to room temperature, obtains fluorescence ceramics afterwards.
Compared with prior art, the present invention has the advantages that:
(1) block shape fluorescent ceramic material is obtained by the adjustment of matrix components and the species and concentration of rare earth element, with Fluorescent powder is compared, which has excellent machinery and mechanical property, can be directly packaged with blue chip, Substitute current fluorescent powder and add the encapsulation mode of organic material, so as to efficiently solve organic packaging materials weak heat-dissipating, continuous high temperature The problem of caused light efficiency reduction and color drift, it can significantly extend the white light LED part service life.Meanwhile compared with fluorescent powder, it is glimmering The packaged type of light ceramic has more preferable uniformity, ensures light source uniform in light emission.
(2) fluorescent ceramic material and the white light LED part colour temperature that blue chip assembles are relatively low, in 2600-3000K Between, colour rendering index and YAG close with incandescent lamps light color temperature:Ce3+Fluorescence ceramics are compared to being obviously improved, in high-power height Performance white light LEDs have good application prospect in field.
Brief description of the drawings
Fig. 1 is the excitation and emission spectra figure of fluorescence ceramics piece in the embodiment of the present invention 1;
Fig. 2 is the XRD spectra of fluorescence ceramics piece in the embodiment of the present invention 1;
Fig. 3 is the excitation and emission spectra figure of fluorescence ceramics piece in the embodiment of the present invention 2;
Fig. 4 is the excitation and emission spectra figure of fluorescence ceramics piece in the embodiment of the present invention 3;
Fig. 5 is the pictorial diagram of the fluorescence ceramics piece in the embodiment of the present invention 4.
Embodiment
The present invention is described in further detail with reference to embodiment, it should be pointed out that embodiment described below purport Easy to the understanding of the present invention, and any restriction effect is not played to it.
Embodiment 1:
Fluorescence ceramics piece (Lu1.99Ce0.01Ca)(Mg2Si3)O12Preparation method it is as follows:
(1) Lu is stoichiometrically weighed2O3:3.9594g CeO2:0.0172g, CaCO3:1.0087g MgO: 0.8061g, SiO2:1.8025g;With grinding pot plus agate ball, it is ground by abrasive media of absolute ethyl alcohol with mixing, until Powder average grain diameter is less than 1 μm;
(2) it is gained slurry is dry and sieve, the 1000 DEG C of insulation 2h in atmosphere of the powder after sieving are removed in powder Organic matter, and allow CaCO3Fully decompose;2min is kept using the isometric unidirectional 10Mpa pressure that applies after gained powder is sieved, It is dry-pressing formed, it is pressed into biscuit, pressure 200MPa, dwell time 2min in isostatic cool pressing equipment;
(3) gained biscuit of ceramics is sintered in a vacuum furnace, 1 DEG C/min of heating rate, 4h is kept the temperature at 1200 DEG C, 1350 DEG C of insulation 10h, complete solid phase reaction, exclude stomata and reach densification;By sample after vacuum-sintering in 5%H2/ 95%N2's The lower 1200 DEG C of insulations 6h of reducing atmosphere, reduces rare earth element;
(4) fluorescent ceramic material after step (3) is annealed is processed by shot blasting, obtains (Lu1.99Ce0.01Ca) (Mg2Si3)O12Fluorescence ceramics piece, its thickness are 1mm.
The excitation and emission spectra figure of fluorescence ceramics piece obtained above is as shown in Figure 1, excitation peak shows the fluorescence ceramics Can effectively it be excited by blue light, emission peak positions are to be orange-yellow under 585nm, blue light excitation, and colour temperature is relatively low, and colour rendering index is higher.
The XRD spectra of fluorescence ceramics piece obtained above belongs to as shown in Fig. 2, show that the ceramic material is garnet structure In cubic system, space group Ia3d.
To fluorescence ceramics piece obtained above carry out Data Detection, as a result for:Chromaticity coordinate:X=0.5261, y= 0.4689, colour temperature 2347K, colour rendering index 62.
Embodiment 2:
Fluorescence ceramics piece (Lu1.99Ce0.01Ca0.9Ba0.1)(Mg2Si3)O12Preparation method it is as follows:
(1) Lu is stoichiometrically weighed2O3:3.9594g CeO2:0.0172g, CaCO3:0.9074g, BaCO3: 0.0164g, MgO:0.8061g, SiO2:1.8025g.With grinding pot plus agate ball, ground by abrasive media of absolute ethyl alcohol Mill is with mixing, until powder average grain diameter is less than 1 μm;
(2) it is gained slurry is dry and sieve, the 1000 DEG C of insulation 2h in atmosphere of the powder after sieving are removed in powder Organic matter, and allow CaCO3Fully decompose;2min is kept using the isometric unidirectional 10Mpa pressure that applies after gained powder is sieved, It is dry-pressing formed, it is pressed into biscuit, pressure 200MPa, dwell time 2min in isostatic cool pressing equipment;
(3) gained biscuit of ceramics is sintered in a vacuum furnace, 1 DEG C/min of heating rate, 4h is kept the temperature at 900 DEG C, 1450 DEG C of insulation 10h, complete solid phase reaction, exclude stomata and reach densification;By sample after vacuum-sintering under reducing atmosphere 5% H2/ 95%N2, 1300 DEG C of insulation 6h, reduce activator;
(4) fluorescent ceramic material after step (3) is annealed is processed by shot blasting, obtains (Lu1.99Ce0.01Ca0.9Ba0.1) (Mg2Si3)O12Fluorescence ceramics piece, its thickness are 1mm.
The XRD spectra of fluorescence ceramics piece obtained above is similar to Figure 2, and it is garnet structure to show the ceramic material, Belong to cubic system, space group Ia3d.
The excitation and emission spectra figure of fluorescence ceramics piece obtained above is as shown in figure 3, excitation peak shows the fluorescence ceramics Can effectively it be excited by blue light, emission peak positions are to be orange-yellow under 581nm, blue light excitation, and colour temperature is relatively low, and colour rendering index is higher.
To fluorescence ceramics piece obtained above carry out Data Detection, as a result for:Chromaticity coordinate is:X=0.5230, y= 0.4711, colour temperature 2384K, colour rendering index 64.
Embodiment 3:
Fluorescence ceramics piece (Lu1.99Ce0.005Pr0.005Ca)(Mg2Si3)O12Preparation method it is as follows:
(1) Lu is stoichiometrically weighed2O3:3.9594g CeO2:0.0086, Pr6O11:0.0085g, CaCO3: 1.0087g MgO:0.8061g, SiO2:1.8025g.With grinding pot plus agate ball, ground by abrasive media of absolute ethyl alcohol Mill is with mixing, until powder average grain diameter is less than 1 μm;
(2) it is gained slurry is dry and sieve, the 900 DEG C of insulation 2h in atmosphere of the powder after sieving are removed in powder Organic matter, and allow CaCO3Fully decompose;2min is kept using the isometric unidirectional 10Mpa pressure that applies after gained powder is sieved, It is dry-pressing formed, it is pressed into biscuit, pressure 200MPa, dwell time 2min in isostatic cool pressing equipment;
(3) gained biscuit of ceramics is sintered in a vacuum furnace, 1 DEG C/min of heating rate, 2h is kept the temperature at 600 DEG C, 1350 DEG C of insulation 10h, complete solid phase reaction, exclude stomata and reach densification;Will sample 5%H under reducing atmosphere after sintering2/ 95%N2, 1200 DEG C of insulation 6h, reduce activator;
(4) fluorescence ceramics after step (3) is annealed are processed by shot blasting, obtain (Lu1.99Ce0.005Pr0.005Ca) (Mg2Si3)O12Fluorescence ceramics piece, its thickness are 1mm.
The XRD spectra of fluorescence ceramics piece obtained above is similar to Figure 2, and it is garnet structure to show the ceramic material, Belong to cubic system, space group Ia3d.
The excitation and emission spectra figure of above-mentioned fluorescence ceramics is as shown in figure 4, excitation peak shows that the fluorescence ceramics can be by blue light Effectively excitation, emission peak positions have the characteristic peak of Pr ions in 563nm, and it is greenish orange yellow that blue light excitation is lower, and colour temperature is relatively low, Colour rendering index is higher.
To fluorescence ceramics piece obtained above carry out Data Detection, as a result for:Chromaticity coordinate is:X=0.5084, y= 0.4528, colour temperature 2412K, colour rendering index 56.
Embodiment 4:
Fluorescence ceramics piece (Lu1.99Ce0.01Ca)(Mg2Si1Ge2)O12Preparation method it is as follows:
(1) Lu is stoichiometrically weighed2O3:3.9594g CeO2:0.0172g, CaCO3:1.0087g MgO: 0.8061g, SiO2:0.6008g, GeO2:2.0928.With grinding pot plus agate ball, it is ground by abrasive media of absolute ethyl alcohol With mixing, until powder average grain diameter is less than 1 μm;
(2) it is gained slurry is dry and sieve, the 1000 DEG C of insulation 2h in atmosphere of the powder after sieving are removed in powder Organic matter, and allow CaCO3Fully decompose;2min is kept using the isometric unidirectional 10Mpa pressure that applies after gained powder is sieved, It is dry-pressing formed, it is pressed into biscuit, pressure 200MPa, dwell time 2min in isostatic cool pressing equipment;
(3) gained biscuit of ceramics is sintered in a vacuum furnace, 1 DEG C/min of heating rate, 4h is kept the temperature at 1100 DEG C, 1400 DEG C of insulation 10h, complete solid phase reaction, exclude stomata and reach densification;In atmosphere, 1200 DEG C keep the temperature sample after sintering 6h anneals;
(4) fluorescence ceramics after step (3) is annealed are processed by shot blasting, obtain (Lu1.99Ce0.01Ca)(Mg2Si1Ge2) O12Fluorescence ceramics piece, its thickness are 1mm.
The XRD spectra of fluorescence ceramics piece obtained above is similar to Figure 2, and it is garnet structure to show the ceramic material, Belong to cubic system, space group Ia3d.
Circular portion in Fig. 5 is the material object of above-mentioned fluorescence ceramics piece, as shown in figure 5, the potsherd is with higher Transmitance, through the potsherd it can be seen that pattern on square shape paper.
Obtained potsherd can prepare the warm white LED device of the high colour developing of low colour temperature by detection.
Embodiment 5:
Fluorescence ceramics piece (YLu0.99Ce0.01Ca)(Mg2Si3)O12Preparation method it is as follows:
(1) Y is stoichiometrically weighed2O3:1.129g Lu2O3:1.9698g CeO2:0.0172g, CaCO3: 1.0087g MgO:0.8061g, SiO2:1.8025g.With grinding pot plus agate ball, ground by abrasive media of absolute ethyl alcohol Mill is with mixing, until powder average grain diameter is less than 1 μm;
(2) it is gained slurry is dry and sieve, the 1000 DEG C of insulation 2h in atmosphere of the powder after sieving are removed in powder Organic matter, and allow CaCO3Fully decompose;2min is kept using the isometric unidirectional 10Mpa pressure that applies after gained powder is sieved, It is dry-pressing formed, it is pressed into biscuit, pressure 200MPa, dwell time 2min in isostatic cool pressing equipment;
(3) gained biscuit of ceramics is sintered in a vacuum furnace, 1 DEG C/min of heating rate, 10h is kept the temperature at 1350 DEG C, Solid phase reaction is completed, stomata is excluded and reaches densification;By the 5%H under reducing atmosphere of sample after vacuum-sintering2/ 95%N2, 1000 DEG C of insulation 2h, 1300 DEG C of insulation 6h, reduce activator;
(4) fluorescence ceramics after step (3) is annealed are processed by shot blasting, obtain (YLu0.99Ce0.01Ca)(Mg2Si3)O12 Fluorescence ceramics piece, its thickness are 2mm.
The XRD spectra of fluorescence ceramics piece obtained above is similar to Figure 2, and it is garnet structure to show the ceramic material, Belong to cubic system, space group Ia3d.
Obtained potsherd can prepare the warm white LED device of the high colour developing of low colour temperature by detection.
Embodiment 6:
Fluorescence ceramics piece (Lu1.8Ce0.1Pr0.05Tb0.05Ca)(Mg2Si3)O12Preparation method it is as follows:
(1) Lu is stoichiometrically weighed2O3:3.5768g CeO2:0.172g, Pr6O11:0.085g, Tb2O3: 0.0914g, CaCO3:1.0087g MgO:0.8061g, SiO2:1.8025g.With grinding pot plus agate ball, using absolute ethyl alcohol to grind Grinding media is ground with mixing, until powder average grain diameter is less than 1 μm;
(2) it is gained slurry is dry and sieve, the 1000 DEG C of insulation 2h in atmosphere of the powder after sieving are removed in powder Organic matter, and allow CaCO3Fully decompose;2min is kept using the isometric unidirectional 10Mpa pressure that applies after gained powder is sieved, It is dry-pressing formed, it is pressed into biscuit, pressure 200MPa, dwell time 2min in isostatic cool pressing equipment;
(3) gained biscuit of ceramics is sintered in a vacuum furnace, 1 DEG C/min of heating rate, 3h is kept the temperature at 800 DEG C, 1450 DEG C of insulation 12h, complete solid phase reaction, exclude stomata and reach densification;By sample after vacuum-sintering in decomposed ammonia, 1100 DEG C of insulation 6h, reduce activator;
(4) fluorescence ceramics after step (3) is annealed are processed by shot blasting, obtain (Lu1.8Ce0.1Pr0.05Tb0.05Ca) (Mg2Si3)O12Fluorescence ceramics piece, its thickness are 1mm.
The XRD spectra of fluorescence ceramics piece obtained above is similar to Figure 2, and it is garnet structure to show the ceramic material, Belong to cubic system, space group Ia3d.
Obtained potsherd can prepare the warm white LED device of the high colour developing of low colour temperature by detection.
Embodiment 7:
Fluorescence ceramics piece (Lu1.999Ce0.001Ca)(Mg2Si3)O12Preparation method it is as follows:
(1) Lu is stoichiometrically weighed2O3:3.9773g CeO2:0.00172g, CaCO3:1.0087g MgO: 0.8061g, SiO2:1.8025g.With grinding pot plus agate ball, it is ground by abrasive media of absolute ethyl alcohol with mixing, until Powder average grain diameter is less than 1 μm;
(2) it is gained slurry is dry and sieve, the 1000 DEG C of insulation 2h in atmosphere of the powder after sieving are removed in powder Organic matter, and allow CaCO3Fully decompose;2min is kept using the isometric unidirectional 10Mpa pressure that applies after gained powder is sieved, It is dry-pressing formed, it is pressed into biscuit, pressure 200MPa, dwell time 2min in isostatic cool pressing equipment;
(3) gained biscuit of ceramics is sintered in a vacuum furnace, 1 DEG C/min of heating rate, 4h is kept the temperature at 1200 DEG C, 1350 DEG C of insulation 10h, complete solid phase reaction, exclude stomata and reach densification;By sample after vacuum-sintering under reducing atmosphere 5% H2/ 95%N2, 1100 DEG C of insulation 6h, reduce activator;
(4) fluorescence ceramics after step (3) is annealed are processed by shot blasting, obtain (Lu1.999Ce0.001Ca)(Mg2Si3)O12 Fluorescence ceramics piece, its thickness are 2mm.
The XRD spectra of fluorescence ceramics piece obtained above is similar to Figure 2, and it is garnet structure to show the ceramic material, Belong to cubic system, space group Ia3d.
Obtained potsherd can prepare the warm white LED device of the high colour developing of low colour temperature by detection.
Embodiment 8:
Fluorescence ceramics piece (GdLu0.99Ce0.01Ca)(Mg2Si3)O12Preparation method it is as follows:
(1) Gd is stoichiometrically weighed2O3:1.8125g Lu2O3:1.9698g CeO2:0.0172g, CaCO3: 1.0087g MgO:0.8061g, SiO2:1.8025g.With grinding pot plus agate ball, ground by abrasive media of absolute ethyl alcohol Mill is with mixing, until powder average grain diameter is less than 1 μm;
(2) it is gained slurry is dry and sieve, the 1000 DEG C of insulation 2h in atmosphere of the powder after sieving are removed in powder Organic matter, and allow CaCO3Fully decompose;2min is kept using the isometric unidirectional 10Mpa pressure that applies after gained powder is sieved, It is dry-pressing formed, it is pressed into biscuit, pressure 200MPa, dwell time 2min in isostatic cool pressing equipment;
(3) gained biscuit of ceramics is sintered in a vacuum furnace, 1 DEG C/min of heating rate, 2h is kept the temperature at 700 DEG C, 1350 DEG C of insulation 10h, complete solid phase reaction, exclude stomata and reach densification;By sample after vacuum-sintering in atmosphere, 1200 DEG C Keep the temperature 6h;
(4) fluorescence ceramics after step (3) is annealed are processed by shot blasting, obtain (GdLu0.99Ce0.01Ca)(Mg2Si3) O12Fluorescence ceramics piece, its thickness are 1mm.
The XRD spectra of fluorescence ceramics piece obtained above is similar to Figure 2, and it is garnet structure to show the ceramic material, Belong to cubic system, space group Ia3d.
Obtained potsherd can prepare the warm white LED device of the high colour developing of low colour temperature by detection.
Technical scheme is described in detail in embodiment described above, it should be understood that the above is only For the specific embodiment of the present invention, it is not intended to limit the invention, all any modifications made in the spirit of the present invention, Supplement or similar fashion replacement etc., should all be included in the protection scope of the present invention.

Claims (10)

1. a kind of fluorescent ceramic material, it is characterised in that its chemical formula is:
(A2-xRexM)(Mg2D3)O12
Wherein, the combination of a kind of element or two or more elements in A Y, Lu, Sc, Gd, Ga;Re for rare earth element Eu, Ce, The combination of a kind of element or two or more elements in Pr, Sm, Dy, Tm, Tb, Nd;M is a kind of element or two in Ca, Sr, Ba The combination of kind above element;D is the combination of a kind of element or two or more elements in Ti, Si, Ge;Also, 0.001≤x<2.
2. fluorescence ceramics according to claim 1, it is characterised in that 0.001≤x≤0.2, preferably 0.01≤x≤ 0.1。
3. fluorescence ceramics according to claim 1, it is characterised in that the excitation wavelength of the fluorescent ceramic material is in 400- In the range of 550nm.
4. fluorescence ceramics according to claim 1, it is characterised in that the fluorescent ceramic material is launched under blue light excitation Wavelength is in the range of 500-700nm.
5. fluorescence ceramics according to claim 1, it is characterised in that the emission peak positions of the fluorescence ceramics can pass through Change the element in the chemical formula and rare earth element species and concentration is regulated and controled.
6. according to the preparation method of the fluorescence ceramics described in claim 1-5, it is characterised in that include the following steps:
(1) (A is pressed2-xRexM)(Mg2D3)O12Stoichiometric ratio, by the oxide of A either corresponding salt, Re oxide or Corresponding salt, either corresponding salt, the oxide of D or corresponding salt, magnesia or the corresponding salt of magnesium carry out the oxide of M Mixing, obtains nanometer or the other powder of submicron order;
(2) by the powder calcination, the organic matter and volatile matter in powder are removed, and carries out tabletting and makes biscuit of ceramics;
(3) biscuit of ceramics is sintered and annealed, obtain fluorescence ceramics;
(4) fluorescence ceramics are processed by shot blasting.
7. the preparation method of fluorescence ceramics according to claim 6, it is characterised in that in the step (1), obtain powder Method include ball-milling method, sol-gal process or sluggish precipitation;
Preferably, in the step (2), calcining heat is 600 DEG C -1200 DEG C, keeps the temperature 1h-24h.
Preferably, in the step (2), biscuit production method includes isometric unidirectional, isometric bidirectional pressing and isostatic cool pressing.
8. the preparation method of fluorescence ceramics according to claim 6, it is characterised in that in the step (3), sintering method Including vacuum-sintering, reducing atmosphere sintering, hot pressed sintering and HIP sintering;
Preferably, sintering process is is warming up to 600 DEG C -1200 DEG C, insulation 1h-24h, then heats to 1300 DEG C -1450 DEG C, Room temperature is cooled to after insulation 2h-24h;
Preferably, in the step (3), annealing temperature is 900 DEG C -1300 DEG C, the preferred 2h-20h of soaking time.
9. a kind of white light LEDs, are assembled as the fluorescent ceramic material described in any claim in claim 1-5 and blue chip Obtain.
10. white light LEDs according to claim 9, it is characterised in that it is characterized in that, colour temperature is between 2600-3000K.
CN201711321597.XA 2017-12-12 2017-12-12 A kind of fluorescent ceramic material, its preparation method and a kind of low color temperature white light LED Pending CN108018040A (en)

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Application publication date: 20180511