CN102173773A - Transparent ceramic for high-brightness white light emitting diode and preparation method thereof - Google Patents
Transparent ceramic for high-brightness white light emitting diode and preparation method thereof Download PDFInfo
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- 238000000034 method Methods 0.000 claims abstract description 62
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- 229910052777 Praseodymium Inorganic materials 0.000 claims abstract description 38
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- 229910052771 Terbium Inorganic materials 0.000 claims abstract description 36
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 36
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- 239000002994 raw material Substances 0.000 claims abstract description 17
- 239000000126 substance Substances 0.000 claims abstract description 16
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- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 4
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- 239000011222 crystalline ceramic Substances 0.000 claims description 80
- 229910002106 crystalline ceramic Inorganic materials 0.000 claims description 80
- 150000002500 ions Chemical class 0.000 claims description 12
- 229910002651 NO3 Inorganic materials 0.000 claims description 11
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 9
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 9
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 9
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- 238000005303 weighing Methods 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 6
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- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 5
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 5
- 230000006690 co-activation Effects 0.000 claims description 5
- -1 poly(oxyethylene glycol) Polymers 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
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- 238000003825 pressing Methods 0.000 claims description 4
- 238000009877 rendering Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 3
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
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- 150000001875 compounds Chemical class 0.000 claims description 2
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Abstract
A transparent ceramic for high-brightness white LED and its preparing process, wherein the chemical formula can be written as (Y)3-x-y-zCexLiyRz)(Al5-nMn)O12Wherein R can be at least one of La, Pr, Sm, Gd, Tb and Dy, M is at least one of Sc, Ti, V, Cr and Mn, the value ranges of x, y, z and n are respectively that x is more than or equal to 0.003 and less than or equal to 0.06, y is more than or equal to 0.003 and less than or equal to 0.06, z is more than or equal to 0 and less than or equal to 0.75, and n is more than or equal to 0 and less than or equal to 0.75. The raw material powder prepared by a solid phase ball milling method or a wet chemical method is subjected to forming, cold isostatic pressing and vacuum sintering to obtain transparent ceramic with fine and uniform crystal grains and extremely low porosity. The transparent ceramic has the characteristics of high transmittance, high thermal conductivity, good chemical and thermal stability and high fluorescence conversion efficiency.
Description
Technical field
The present invention relates to crystalline ceramics, particularly a kind of crystalline ceramics that is used for high-brightness white-light photodiode (being designated hereinafter simply as LED) and preparation method thereof belongs to extraordinary light function ceramics preparing technical field.
Background technology
Compare with the traditional lighting light source, white light LEDs has that volume is little, less energy consumption, response is fast, the life-span is long, characteristics such as pollution-free, have great market outlook in fields such as landscape light in city, indoor and outdoor general lighting, signal lamp, flat pannel display and backlights, generally believed it is the new light sources that substitutes the traditional lighting device, be subjected to domestic and international great attention, particularly under the situation that global energy conservation and environmental protection becomes increasingly conspicuous, it is very great to develop energy-efficient semiconductor solid lighting meaning.
The method of at present the most general making white light LEDs is to send blue-light excited cerium activated yttrium aluminum garnet Y with efficient InGaN/GaN base blue-light LED chip
3Al
5O
12: Ce (YAG:Ce) fluorescent material, adopt the encapsulation of Resins, epoxy or silica gel, promptly YAG:Ce fluorescent material is distributed in Resins, epoxy or the silica gel.YAG:Ce fluorescent material and blue chip matching are good, the luminous efficiency height, but have problems such as ruddiness composition deficiency, colour rendering index are low, usually add some rare earth ions (for example gadolinium Gd, praseodymium Pr etc.) as doping agent for addressing these problems, the lattice distortion that increases the YAG structure makes Ce
3+Ion perhaps directly replenishes the luminous of red spectral band in the luminous red shift of yellow band, improves the color developing of white light LEDs.But white light LEDs for high-power and high-luminance, do transition material with traditional fluorescent material and have more serious problem: blue-light LED chip is lighted the meeting persistent fever big the injection under the electric current, and Resins, epoxy or silica gel shell do not reach the heat radiation requirement led chip temperature will be raise, and luminous efficiency descends; Fluorescent material efficiency of conversion when temperature raises descends on the other hand, and the meeting accelerated deterioration under the accumulation of continuous heat of Resins, epoxy or silica gel shell, the efficiency of conversion of fluorescent material is also descended, cause high-brightness white-light LED thermic light decay phenomenon to occur, influence its practicality.Crystalline ceramics has than Resins, epoxy or much higher thermal conductivity and the thermostability of silica gel, and have higher mechanical properties such as hardness, use transparent fluorescence ceramics to come Wavelength-converting simultaneously as package casing, can alleviate the heat dissipation problem of high-brightness white-light LED greatly, prolong its work-ing life, have high economic benefit.
Domesticly some research work have also been done with the fluorescence transition material about white light LEDs, as Chinese patent CN1815765 a kind of YAG chip-type white-light light-emitting-diode and method for packing thereof are proposed, rear-earth-doped YAG wafer is used as fluorescent material, but compare with crystalline ceramics, the growth temperature of monocrystalline and preparation cost are all higher, and aspect machinery, mechanical stability, have deficiency, limited the handiness of processing and manufacturing.And the segregation coefficient of active ions in the YAG monocrystalline is very low in this technical scheme, and bigger doping will cause crystal mass seriously to descend, and restrict its efficiency of conversion.Chinese patent CN101338879A discloses the method that a kind of YAG of utilization crystalline ceramics prepares white light LEDs, is actually the polycrystalline particle coat, and particle size is at 1～300nm, rather than block body ceramic material, and is little with conventional fluorescent powder difference.At present adopt YAG:Ce system (comprising doping Gd, Pr, Sm, Dy etc.) though crystalline ceramics can be used as the transition material of white light LEDs, its efficiency of conversion has still been compared gap with the fluorescent material of traditional YAG:Ce system.
In the research to the transparent fluorescence ceramics of high conversion efficiency, we find to work as very small amount of co-activation ion such as Li
+Be incorporated into the luminous intensity that can significantly strengthen fluor in the matrix.We think, with Li
+Can play sintering aid on the one hand as the co-activation ion, can improve crystalline quality, improve the luminous intensity of active ions; On the other hand, Li
+Ionic is introduced also can produce an amount of oxygen room, and the oxygen room can be used as the sensitizing agent of useful energy transmission.
Summary of the invention
The object of the invention is to provide a kind of crystalline ceramics that is used for high-brightness white-light photodiode (being designated hereinafter simply as LED) and preparation method thereof, the crystalline ceramics that this method makes should have transmitance height, thermal conductivity height, chemistry and Heat stability is good and the high characteristics of fluorescence conversion efficiency.
Technical solution of the present invention is as follows:
A kind of high-brightness white-light LED crystalline ceramics, its characteristics are that the chemical formula of this crystalline ceramics is: (Y
3-x-y-zCe
xLi
yR
z) (Al
5-nM
n) O
12, wherein R can be at least a among La, Pr, Sm, Gd, Tb and the Dy, and M is at least a among Sc, Ti, V, Cr and the Mn, and the span of x, y, z and n is 0.003≤x≤0.06,0.003≤y≤0.06,0≤z≤0.75,0≤n≤0.75.
The described high-brightness white-light LED preparation method of crystalline ceramics, this method comprises the steps:
1. select the chemical formula of the crystalline ceramics of required preparation:
Selected chemical formula (Y
3-x-y-zCe
xLi
yR
z) (Al
5-nM
n) O
12In the element that refers to of R and M and the value of x, y, z and n, wherein R is at least a among La, Pr, Sm, Gd, Tb and the Dy, M is at least a among Sc, Ti, V, Cr and the Mn;
2. by the selected required powder raw material of the accurate weighing of chemical formula, adopt the solid phase ball milled or the urea precipitator method to make the superfine powder raw material;
3. moulding: described superfine powder raw material single shaft is molded, obtain having the green sheet of certain intensity again with 200MPa or above pressure isostatic cool pressing;
4. sintering: described green sheet is put into vacuum oven in 1400～1800 ℃ of following sintering 5～30 hours, and its vacuum tightness is not less than 3 * 10
-3Pa, thus the needed predetermined chemical formula (Y that has obtained
3-x-y-zCe
xLi
yR
z) (Al
5-nM
n) O
12Crystalline ceramics.
The solid phase ball milled of described superfine powder raw material is as follows:
By the selected required high-purity Y of the accurate weighing of chemical formula
2O
3, Al
2O
3, CeO
2, Li
2CO
3, R
2O
3And the oxide powder of M, its purity is not less than 99.9%, be ball-milling medium then with the dehydrated alcohol, the high purity aluminium oxide ball is an abrading-ball, positive tetraethyl orthosilicate is a sintering aid, poly(oxyethylene glycol) 400 is a dispersion agent, in planetary ball mill high speed ball milling, ball milling finishes after drying, grinds, sieve, obtain the high-purity powder of submicron order, this powder forms corresponding oxide compound 700～800 ℃ of calcinings 3 hours to remove remaining organism and decomposing carbonate, sieve once more after the calcining, obtain the high-purity superfine powder raw material of submicron order.
The urea precipitator method of described superfine powder raw material are as follows:
By the selected required high-purity Y of the accurate weighing of chemical formula
2O
3, Al
2O
3, CeO
2, Li
2CO
3, R
2O
3And the oxide powder of M, its purity is not less than 99.9%, be dissolved in the respective amount nitric acid and be made into nitrate solution, this nitrate solution and urea soln, ammoniumsulphate soln are mixed, wherein, urea content is 50～100 times of nitrate concentration, and the molar weight of ammonium sulfate and the molar weight of nitrate are equal to, and adding deionized water at last is 0.001～0.03mol/L with the concentration that mixing solutions is diluted to nitrate; Place 80～99 ℃ of isoperibols to react 2～5 hours mixing solutions, leave standstill after taking out then, filter the collecting precipitation thing, washing, the precursor powder that obtains after the drying and grinding obtained the submicron-grade superfine powder raw material in 2～5 hours in 800～1100 ℃ of high-temperature calcinations.
Among the present invention, variously treat that the selection of doped element and doping thereof has considerable influence to sintering process, for example mix the La amount more for a long time, can suitably reduce sintering temperature or shorten soaking time, and mix the Sc amount more for a long time, need suitably to improve sintering temperature or prolong soaking time.And other ion pair sintering process influence is little, changes its doping, and the gained pottery is still in transparent scope.
Technique effect of the present invention is as follows:
The present invention is with Ce
3+Be main active ions, Li
+Crystalline ceramics for the co-activation ion makes can improve degree of crystallinity, improves Ce
3+The ionic luminous intensity, the even grain size of the crystalline ceramics that obtains, void content is extremely low; And doping La
3+, Pr
3+, Sm
3+, Gd
3+, Tb
3+, Dy
3+Or Sc
3+, Ti
3+, V
3+, Cr
3+, Mn
3+In one or more increase lattice distortion, make Ce
3+The red shift of ionic light emitting region, this crystalline ceramics is by blue-ray LED fluorescence excitation efficiency of conversion height, and the white light colour temperature that obtains is low, the colour rendering index height, and thermal conductivity and Heat stability is good, the material for transformation of wave length and the package casing that therefore can be used as high-brightness white-light LED use.
Description of drawings
Fig. 1 mixes YAG crystalline ceramics and the correlated fluorescence spectrum of the YAG crystalline ceramics of singly mixing Ce (identical experiment condition) fluorescence intensity altogether for the embodiment of the invention 25 Ce, Li.
Embodiment
The invention will be further described below in conjunction with embodiment, but should not limit protection scope of the present invention with this.
Embodiment one:
With purity greater than 99.9% Y
2O
3, Al
2O
3, CeO
2, Li
2CO
3, R
2O
3And the oxide powder of M is raw material, by molecular formula (Y
3-x-y-zCe
xLi
yR
z) (Al
5-nM
n) O
12Weighing and burden, x=0.003 wherein, y=0.003, z=0, n=0.With the dehydrated alcohol is ball-milling medium, and the high purity aluminium oxide ball is an abrading-ball, and positive tetraethyl orthosilicate is a sintering aid, poly(oxyethylene glycol) 400 is a dispersion agent, and high speed ball milling 24 hours placed loft drier dry 24 hours, grind, sieve, put into 600 ℃ of calcinings of retort furnace 3 hours, sieve once more, the molded green sheet of single shaft then, the 210MPa isostatic cool pressing places vacuum oven with green sheet, rise to 1700～1750 ℃ of insulations 20 hours, obtain required crystalline ceramics.
Embodiment two: what implementing process and the foregoing description one were inequality is x=0.003, y=0.003, z=0, n=0.75.Wherein at least a among the optional Sc of M, Ti, V, Cr and the Mn 1700～1800 ℃ of insulations 15～30 hours, obtains required crystalline ceramics.
Embodiment three: what implementing process and the foregoing description one were inequality is x=0.003, y=0.003, z=0.75, n=0.Wherein at least a among the optional La of R, Pr, Sm, Gd, Tb and the Dy 1400～1750 ℃ of insulations 5～30 hours, obtains required crystalline ceramics.
Embodiment four: what implementing process and the foregoing description one were inequality is x=0.003, y=0.003, z=0.75, n=0.75.At least a among the optional La of R, Pr, Sm, Gd, Tb and the Dy wherein, at least a among the optional Sc of M, Ti, V, Cr and the Mn 1400～1800 ℃ of insulations 5～30 hours, obtains required crystalline ceramics.
Embodiment five: what implementing process and the foregoing description one were inequality is x=0.003, y=0.06, z=0, n=0.1650～1750 ℃ of insulations 20 hours, obtain required crystalline ceramics.
Embodiment six: what implementing process and the foregoing description one were inequality is x=0.003, y=0.06, z=0, n=0.75.Wherein at least a among the optional Sc of M, Ti, V, Cr and the Mn 1650～1750 ℃ of insulations 15～20 hours, obtains required crystalline ceramics.
Embodiment seven: what implementing process and the foregoing description one were inequality is x=0.003, y=0.06, z=0.75, n=0.Wherein at least a among the optional La of R, Pr, Sm, Gd, Tb and the Dy 1400～1750 ℃ of insulations 5～20 hours, obtains required crystalline ceramics.
Embodiment eight: what implementing process and the foregoing description one were inequality is x=0.003, y=0.06, z=0.75, n=0.75.At least a among the optional La of R, Pr, Sm, Gd, Tb and the Dy wherein, at least a among the optional Sc of M, Ti, V, Cr and the Mn 1400～1750 ℃ of insulations 5～20 hours, obtains required crystalline ceramics.
Embodiment nine: what implementing process and the foregoing description one were inequality is x=0.06, y=0.003, z=0, n=0.1700～1750 ℃ of insulations 20 hours, obtain required crystalline ceramics.
Embodiment ten: what implementing process and the foregoing description one were inequality is x=0.06, y=0.003, z=0, n=0.75.Wherein at least a among the optional Sc of M, Ti, V, Cr and the Mn 1700～1800 ℃ of insulations 15～30 hours, obtains required crystalline ceramics.
Embodiment 11: what implementing process and the foregoing description one were inequality is x=0.06, y=0.003, z=0.75, n=0.75.Wherein at least a among the optional La of R, Pr, Sm, Gd, Tb and the Dy 1400～1750 ℃ of insulations 5～30 hours, obtains required crystalline ceramics.
Embodiment 12: what implementing process and the foregoing description one were inequality is x=0.06, y=0.003, z=0.75, n=0.75.At least a among the optional La of R, Pr, Sm, Gd, Tb and the Dy wherein, at least a among the optional Sc of M, Ti, V, Cr and the Mn 1400～1800 ℃ of insulations 5～30 hours, obtains required crystalline ceramics.
Embodiment 13: what implementing process and the foregoing description one were inequality is x=0.06, y=0.06, z=0, n=0.1650～1750 ℃ of insulations 20 hours, obtain required crystalline ceramics.
Embodiment 14: what implementing process and the foregoing description one were inequality is x=0.06, y=0.06, z=0, n=0.75.Wherein at least a among the optional Sc of M, Ti, V, Cr and the Mn 1650～1750 ℃ of insulations 15～20 hours, obtains required crystalline ceramics.
Embodiment 15: what implementing process and the foregoing description one were inequality is x=0.06, y=0.06, z=0.75, n=0.Wherein at least a among the optional La of R, Pr, Sm, Gd, Tb and the Dy 1400～1750 ℃ of insulations 5～20 hours, obtains required crystalline ceramics.
Embodiment 16: what implementing process and the foregoing description one were inequality is x=0.06, y=0.06, z=0.75, n=0.75.At least a among the optional La of R, Pr, Sm, Gd, Tb and the Dy wherein, at least a among the optional Sc of M, Ti, V, Cr and the Mn 1400～1750 ℃ of insulations 5～20 hours, obtains required crystalline ceramics.
Embodiment 17: what implementing process and the foregoing description one were inequality is x=0.01, y=0.01, z=0.3, n=0.3.At least a among the optional La of R, Pr, Sm, Gd, Tb and the Dy wherein, at least a among the optional Sc of M, Ti, V, Cr and the Mn 1500～1750 ℃ of insulations 5～20 hours, obtains required crystalline ceramics.
Embodiment 18: what implementing process and the foregoing description one were inequality is x=0.01, y=0.01, z=0.3, n=0.6.At least a among the optional La of R, Pr, Sm, Gd, Tb and the Dy wherein, at least a among the optional Sc of M, Ti, V, Cr and the Mn 1500～1750 ℃ of insulations 5～20 hours, obtains required crystalline ceramics.
Embodiment 19: what implementing process and the foregoing description one were inequality is x=0.01, y=0.01, z=0.6, n=0.3.At least a among the optional La of R, Pr, Sm, Gd, Tb and the Dy wherein, at least a among the optional Sc of M, Ti, V, Cr and the Mn 1450～1750 ℃ of insulations 5～20 hours, obtains required crystalline ceramics.
Embodiment 20: what implementing process and the foregoing description one were inequality is x=0.01, y=0.01, z=0.6, n=0.6.At least a among the optional La of R, Pr, Sm, Gd, Tb and the Dy wherein, at least a among the optional Sc of M, Ti, V, Cr and the Mn 1450～1750 ℃ of insulations 5～20 hours, obtains required crystalline ceramics.
Embodiment 21: what implementing process and the foregoing description one were inequality is x=0.01, y=0.04, z=0.3, n=0.3.At least a among the optional La of R, Pr, Sm, Gd, Tb and the Dy wherein, at least a among the optional Sc of M, Ti, V, Cr and the Mn 1500～1750 ℃ of insulations 5～20 hours, obtains required crystalline ceramics.
Embodiment 22: what implementing process and the foregoing description one were inequality is x=0.01, y=0.04, z=0.3, n=0.6.At least a among the optional La of R, Pr, Sm, Gd, Tb and the Dy wherein, at least a among the optional Sc of M, Ti, V, Cr and the Mn 1500～1750 ℃ of insulations 5～20 hours, obtains required crystalline ceramics.
Embodiment 23: what implementing process and the foregoing description one were inequality is x=0.01, y=0.04, z=0.6, n=0.3.At least a among the optional La of R, Pr, Sm, Gd, Tb and the Dy wherein, at least a among the optional Sc of M, Ti, V, Cr and the Mn 1450～1750 ℃ of insulations 5～20 hours, obtains required crystalline ceramics.
Embodiment 24: what implementing process and the foregoing description one were inequality is x=0.01, y=0.04, z=0.6, n=0.6.At least a among the optional La of R, Pr, Sm, Gd, Tb and the Dy wherein, at least a among the optional Sc of M, Ti, V, Cr and the Mn 1450～1750 ℃ of insulations 5～20 hours, obtains required crystalline ceramics.
Embodiment 25: with purity greater than 99.9% Y
2O
3, Al
2O
3, CeO
2, Li
2CO
3, R
2O
3And the oxide powder of M is raw material, by molecular formula (Y
3-x-y-zCe
xLi
yR
z) (Al
5-nM
n) O
12Weighing and burden, x=0.003 wherein, y=0.003, z=0, n=0, be dissolved in the nitric acid of respective amount, be diluted to 0.025mol/L concentration, add the urea of 50～100 times of nitrate molar weights with appropriate amount of deionized water, 1 times ammonium sulfate, dissolving also mixes, and gained solution is placed 90 ℃ of water-bath reactions 2 hours, takes out and leaves standstill 1 hour, filter the collecting precipitation thing and successively use deionized water and absolute ethanol washing three times, with drying precipitate, the precursor powder that obtains after the drying and grinding was in 900 ℃ of calcinings 3 hours, and single shaft is molded then, the 210MPa isostatic cool pressing, green sheet is placed vacuum oven, rise to 1700～1750 ℃ of insulations 20 hours, obtain required crystalline ceramics.
Embodiment 26: what implementing process and the foregoing description 25 were inequality is x=0.003, y=0.003, z=0, n=0.75.Wherein at least a among the optional Sc of M, Ti, V, Cr and the Mn 1700～1800 ℃ of insulations 15～30 hours, obtains required crystalline ceramics.
Embodiment 27: what implementing process and the foregoing description 25 were inequality is x=0.003, y=0.003, z=0.75, n=0.Wherein at least a among the optional La of R, Pr, Sm, Gd, Tb and the Dy 1400～1750 ℃ of insulations 5～30 hours, obtains required crystalline ceramics.
Embodiment 28: what implementing process and the foregoing description 25 were inequality is x=0.003, y=0.003, z=0.75, n=0.75.At least a among the optional La of R, Pr, Sm, Gd, Tb and the Dy wherein, at least a among the optional Sc of M, Ti, V, Cr and the Mn 1400～1800 ℃ of insulations 5～30 hours, obtains required crystalline ceramics.
Embodiment 29: what implementing process and the foregoing description 25 were inequality is x=0.003, y=0.06, z=0, n=0.1650～1750 ℃ of insulations 20 hours, obtain required crystalline ceramics.
Embodiment 30: what implementing process and the foregoing description 25 were inequality is x=0.003, y=0.06, z=0, n=0.75.Wherein at least a among the optional Sc of M, Ti, V, Cr and the Mn 1650～1750 ℃ of insulations 15～20 hours, obtains required crystalline ceramics.
The embodiment hentriaconta-: what implementing process and the foregoing description 25 were inequality is x=0.003, y=0.06, z=0.75, n=0.Wherein at least a among the optional La of R, Pr, Sm, Gd, Tb and the Dy 1400～1750 ℃ of insulations 5～20 hours, obtains required crystalline ceramics.
Embodiment 32: what implementing process and the foregoing description 25 were inequality is x=0.003, y=0.06, z=0.75, n=0.75.At least a among the optional La of R, Pr, Sm, Gd, Tb and the Dy wherein, at least a among the optional Sc of M, Ti, V, Cr and the Mn 1400～1750 ℃ of insulations 5～20 hours, obtains required crystalline ceramics.
Embodiment 33: what implementing process and the foregoing description 25 were inequality is x=0.06, y=0.003, z=0, n=0.1700～1750 ℃ of insulations 20 hours, obtain required crystalline ceramics.
Embodiment 34: what implementing process and the foregoing description 25 were inequality is x=0.06, y=0.003, z=0, n=0.75.Wherein at least a among the optional Sc of M, Ti, V, Cr and the Mn 1700～1800 ℃ of insulations 15～30 hours, obtains required crystalline ceramics.
Embodiment 35: what implementing process and the foregoing description 25 were inequality is x=0.06, y=0.003, z=0.75, n=0.75.Wherein at least a among the optional La of R, Pr, Sm, Gd, Tb and the Dy 1400～1750 ℃ of insulations 5～30 hours, obtains required crystalline ceramics.
Embodiment 36: what implementing process and the foregoing description 25 were inequality is x=0.06, y=0.003, z=0.75, n=0.75.At least a among the optional La of R, Pr, Sm, Gd, Tb and the Dy wherein, at least a among the optional Sc of M, Ti, V, Cr and the Mn 1400～1800 ℃ of insulations 5～30 hours, obtains required crystalline ceramics.
Embodiment 37: what implementing process and the foregoing description 25 were inequality is x=0.06, y=0.06, z=0, n=0.1650～1750 ℃ of insulations 20 hours, obtain required crystalline ceramics.
Embodiment 38: what implementing process and the foregoing description 25 were inequality is x=0.06, y=0.06, z=0, n=0.75.Wherein at least a among the optional Sc of M, Ti, V, Cr and the Mn 1650～1750 ℃ of insulations 15～20 hours, obtains required crystalline ceramics.
Embodiment 39: what implementing process and the foregoing description 25 were inequality is x=0.06, y=0.06, z=0.75, n=0.Wherein at least a among the optional La of R, Pr, Sm, Gd, Tb and the Dy 1400～1750 ℃ of insulations 5～20 hours, obtains required crystalline ceramics.
Embodiment 40: what implementing process and the foregoing description 25 were inequality is x=0.06, y=0.06, z=0.75, n=0.75.At least a among the optional La of R, Pr, Sm, Gd, Tb and the Dy wherein, at least a among the optional Sc of M, Ti, V, Cr and the Mn 1400～1750 ℃ of insulations 5～20 hours, obtains required crystalline ceramics.
Embodiment 41: what implementing process and the foregoing description 25 were inequality is x=0.01, y=0.01, z=0.3, n=0.3.At least a among the optional La of R, Pr, Sm, Gd, Tb and the Dy wherein, at least a among the optional Sc of M, Ti, V, Cr and the Mn 1500～1750 ℃ of insulations 5～20 hours, obtains required crystalline ceramics.
Embodiment 42: what implementing process and the foregoing description 25 were inequality is x=0.01, y=0.01, z=0.3, n=0.6.At least a among the optional La of R, Pr, Sm, Gd, Tb and the Dy wherein, at least a among the optional Sc of M, Ti, V, Cr and the Mn 1500～1750 ℃ of insulations 5～20 hours, obtains required crystalline ceramics.
Embodiment 43: what implementing process and the foregoing description 25 were inequality is x=0.01, y=0.01, z=0.6, n=0.3.At least a among the optional La of R, Pr, Sm, Gd, Tb and the Dy wherein, at least a among the optional Sc of M, Ti, V, Cr and the Mn 1450～1750 ℃ of insulations 5～20 hours, obtains required crystalline ceramics.
Embodiment 44: what implementing process and the foregoing description 25 were inequality is x=0.01, y=0.01, z=0.6, n=0.6.At least a among the optional La of R, Pr, Sm, Gd, Tb and the Dy wherein, at least a among the optional Sc of M, Ti, V, Cr and the Mn 1450～1750 ℃ of insulations 5～20 hours, obtains required crystalline ceramics.
Embodiment 45: what implementing process and the foregoing description 25 were inequality is x=0.01, y=0.04, z=0.3, n=0.3.At least a among the optional La of R, Pr, Sm, Gd, Tb and the Dy wherein, at least a among the optional Sc of M, Ti, V, Cr and the Mn 1500～1750 ℃ of insulations 5～20 hours, obtains required crystalline ceramics.
Embodiment 46: what implementing process and the foregoing description 25 were inequality is x=0.01, y=0.04, z=0.3, n=0.6.At least a among the optional La of R, Pr, Sm, Gd, Tb and the Dy wherein, at least a among the optional Sc of M, Ti, V, Cr and the Mn 1500～1750 ℃ of insulations 5～20 hours, obtains required crystalline ceramics.
Embodiment 47: what implementing process and the foregoing description 25 were inequality is x=0.01, y=0.04, z=0.6, n=0.3.At least a among the optional La of R, Pr, Sm, Gd, Tb and the Dy wherein, at least a among the optional Sc of M, Ti, V, Cr and the Mn 1450～1750 ℃ of insulations 5～20 hours, obtains required crystalline ceramics.
Embodiment 48: what implementing process and the foregoing description 25 were inequality is x=0.01, y=0.04, z=0.6, n=0.6.At least a among the optional La of R, Pr, Sm, Gd, Tb and the Dy wherein, at least a among the optional Sc of M, Ti, V, Cr and the Mn 1450～1750 ℃ of insulations 5～20 hours, obtains required crystalline ceramics.
Fig. 1 mixes YAG crystalline ceramics and fluorescence intensity contrast (identical experiment condition) fluorescent spectrum curve of singly mixing the Ce crystalline ceramics altogether for Ce, Li in the embodiment of the invention 25, as seen from the figure, Ce of the present invention, Li mix the YAG crystalline ceramics altogether and have higher fluorescence spectrum, and other embodiment have similar result.Illustrate that the present invention is with Ce
3+Be main active ions, Li
+Crystalline ceramics for the co-activation ion makes can improve degree of crystallinity, improves Ce
3+The ionic luminous intensity, the even grain size of the crystalline ceramics that obtains, void content is extremely low; And doping La
3+, Pr
3+, Sm
3+, Gd
3+, Tb
3+, Dy
3+Or Sc
3+, Ti
3+, V
3+, Cr
3+, Mn
3+In one or more increase lattice distortion, make Ce
3+The red shift of ionic light emitting region, this crystalline ceramics is by blue-ray LED fluorescence excitation efficiency of conversion height, and the white light colour temperature that obtains is low, the colour rendering index height, and thermal conductivity and Heat stability is good, the material for transformation of wave length and the package casing that therefore can be used as high-brightness white-light LED use.
Claims (5)
1. crystalline ceramics that is used for the high-brightness white-light photodiode and preparation method thereof is characterized in that its chemical formula is: (Y
3-x-y-zCe
xLi
yR
z) (Al
5-nM
n) O
12,
Wherein: R is at least a among La, Pr, Sm, Gd, Tb and the Dy,
M is at least a among Sc, Ti, V, Cr and the Mn,
The span of x, y, z and n is 0.003≤x≤0.06,0.003≤y≤0.06 ,≤z≤0.75,0≤n≤0.75.
2. crystalline ceramics that is used for the high-brightness white-light photodiode as claimed in claim 1 and preparation method thereof is characterized in that with Ce
3+Be main active ions, with Li
+Be the co-activation ion, and doping La
3+, Pr
3+, Sm
3+, Gd
3+, Tb
3+, Dy
3+Or Sc
3+, Ti
3+, V
3+, Cr
3+, Mn
3+In one or more regulate colour rendering index with the white light emitting diode of this crystalline ceramics encapsulation.
3. the described preparation method who is used for the crystalline ceramics of high-brightness white-light photodiode of claim 1 is characterized in that this method comprises the steps:
1. selected chemical formula (Y
3-x-y-zCe
xLi
yR
z) (Al
5-nM
n) O
12Element that middle R and M refer to and the value of x, y, z and n;
2. by the selected required powder raw material of the accurate weighing of chemical formula, adopt the solid phase ball milled or the urea precipitator method to make the superfine powder raw material;
3. moulding: described superfine powder raw material single shaft is molded, obtain having the green sheet of certain intensity again with 200MPa or above pressure isostatic cool pressing;
4. sintering: described green sheet is put into vacuum oven in 1400～1800 ℃ of following sintering 5～30 hours, and its vacuum tightness is not less than 3 * 10
-3Pa, thus required chemical formula (Y obtained
3-x-y-zCe
xLi
yR
z) (Al
5-nM
n) O
12Crystalline ceramics.
4. the preparation method who is used for the crystalline ceramics of high-brightness white-light photodiode according to claim 3 is characterized in that the solid phase ball milled of described superfine powder raw material is as follows:
By the selected required high-purity Y of the accurate weighing of chemical formula
2O
3, Al
2O
3, CeO
2, Li
2CO
3, R
2O
3And the oxide powder of M, its purity is not less than 99.9%, is ball-milling medium then with the dehydrated alcohol, and the high purity aluminium oxide ball is an abrading-ball, and positive tetraethyl orthosilicate is a sintering aid, and poly(oxyethylene glycol) 400 is a dispersion agent, in planetary ball mill high speed ball milling.Ball milling finishes after drying, grinds, and sieves, obtain the high-purity powder of submicron order, this powder forms corresponding oxide compound 700～800 ℃ of calcinings 3 hours to remove remaining organism and decomposing carbonate, sieve once more after the calcining, obtain the high-purity superfine powder raw material of submicron order.
5. the preparation method who is used for the crystalline ceramics of high-brightness white-light photodiode according to claim 3 is characterized in that the urea precipitator method of described superfine powder raw material are as follows:
By the selected required high-purity Y of the accurate weighing of chemical formula
2O
3, Al
2O
3, CeO
2, Li
2CO
3, R
2O
3And the oxide powder of M, its purity is not less than 99.9%, be dissolved in the respective amount nitric acid and be made into nitrate solution, this nitrate solution and urea soln, ammoniumsulphate soln are mixed, wherein, urea content is 50～100 times of nitrate concentration, and the molar weight of ammonium sulfate and the molar weight of nitrate are equal to, and adding deionized water at last is 0.001～0.03mol/L with the concentration that mixing solutions is diluted to nitrate; Place 80～99 ℃ of isoperibols to react 2～5 hours mixing solutions, leave standstill after taking out then, filter the collecting precipitation thing, washing, drying, the precursor powder that obtains after the grinding obtains the submicron-grade superfine powder raw material in 800～1100 ℃ of high-temperature calcinations 2～5 hours.
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