CN106242539B - A kind of LED nitride fluorescent crystalline ceramics preparation method - Google Patents
A kind of LED nitride fluorescent crystalline ceramics preparation method Download PDFInfo
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- CN106242539B CN106242539B CN201610603372.2A CN201610603372A CN106242539B CN 106242539 B CN106242539 B CN 106242539B CN 201610603372 A CN201610603372 A CN 201610603372A CN 106242539 B CN106242539 B CN 106242539B
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- 150000004767 nitrides Chemical class 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229910002106 crystalline ceramic Inorganic materials 0.000 title claims abstract description 11
- 239000011222 crystalline ceramic Substances 0.000 title claims abstract description 11
- 239000000919 ceramic Substances 0.000 claims abstract description 44
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000000843 powder Substances 0.000 claims abstract description 34
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000005245 sintering Methods 0.000 claims abstract description 22
- 235000015895 biscuits Nutrition 0.000 claims abstract description 17
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 17
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 238000000137 annealing Methods 0.000 claims abstract description 11
- 239000010431 corundum Substances 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 4
- 238000000227 grinding Methods 0.000 claims abstract description 3
- 238000010792 warming Methods 0.000 claims description 21
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 16
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- RSEIMSPAXMNYFJ-UHFFFAOYSA-N europium(III) oxide Inorganic materials O=[Eu]O[Eu]=O RSEIMSPAXMNYFJ-UHFFFAOYSA-N 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 229910052681 coesite Inorganic materials 0.000 claims description 7
- 229910052906 cristobalite Inorganic materials 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 229910052682 stishovite Inorganic materials 0.000 claims description 7
- 229910052905 tridymite Inorganic materials 0.000 claims description 7
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 7
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 239000004033 plastic Substances 0.000 claims description 5
- 229920003023 plastic Polymers 0.000 claims description 5
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 3
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 3
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 claims description 2
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims 3
- 229910052737 gold Inorganic materials 0.000 claims 3
- 239000010931 gold Substances 0.000 claims 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 229910052709 silver Inorganic materials 0.000 claims 1
- 239000004332 silver Substances 0.000 claims 1
- 239000000126 substance Substances 0.000 claims 1
- QHGNHLZPVBIIPX-UHFFFAOYSA-N tin(II) oxide Inorganic materials [Sn]=O QHGNHLZPVBIIPX-UHFFFAOYSA-N 0.000 claims 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 8
- 238000005520 cutting process Methods 0.000 description 6
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- 238000003825 pressing Methods 0.000 description 5
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- 239000013078 crystal Substances 0.000 description 4
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- 230000032683 aging Effects 0.000 description 2
- 235000019270 ammonium chloride Nutrition 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
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- 239000006096 absorbing agent Substances 0.000 description 1
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- 238000010276 construction Methods 0.000 description 1
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- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
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- 238000005538 encapsulation Methods 0.000 description 1
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- 229910010272 inorganic material Inorganic materials 0.000 description 1
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- 229910052573 porcelain Inorganic materials 0.000 description 1
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- -1 rare earth ion Chemical class 0.000 description 1
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- 238000011160 research Methods 0.000 description 1
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- 238000003836 solid-state method Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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Abstract
This application discloses a kind of LED preparation methods of nitride fluorescent crystalline ceramics, in the glove box of nitrogen protection, raw material are weighed, mix, is ground；The powder ground in step 1 is put into corundum crucible, and is put into vacuum pressed sintering rapid cooling furnace, is sintered, cools down；The product that step 2 is obtained carries out grinding and is crushed, crosses 120 meshes, obtains nitride phosphor；Ceramic powder and fluorescent powder are weighed in proportion, is added in mortar and is uniformly mixed to get mixture；Mixture progress compressing tablet process is obtained into green body；Green body is put into mold, is flattened to obtain biscuit with cold isostatic press；Biscuit is subjected to high temperature sintering in high temperature resistance furnace, obtains sample；The sample is made annealing treatment, obtains fluorescent transparent ceramics, nitride fluorescent ceramic system of the invention is for simple process, at low cost, high-efficient, and nitride fluorescent ceramic dense degree obtained is high, luminous efficiency is high, uniformity is good, thickness shape is controllable.
Description
Technical field
The present disclosure relates generally to solid state lighting field of material technology more particularly to a kind of transparent potteries of LED nitride fluorescent
Porcelain preparation method.
Background technique
Great power LED is current research emphasis, and with the increase of LED power, quantity of heat production increases, and heat concentrates on ruler
On the chip of very little very little, the temperature of chip interior is higher and higher, accelerates device aging, or even burn chip.In addition, current fluorescence
The binder multiselect resin and silica gel of powder encapsulation, but the two is resistant to high temperatures, and uvioresistant performance is poor, is exposed to hot environment for a long time
Or under ultraviolet radioactive, it may occur that aging, cracking, xanthochromia cause LED brightness decline, color temperature shift, the lost of life occur, seriously
Influence the development of large power white light LED.In view of the above-mentioned problems, traditional having with the excellent inorganic material of high temperature resistance to replace
Machine binder improves the stability of fluorescent material, is conducive to realize high-power illumination, while simplifying packaging technology, reducing color tolerance
Difference can satisfy requirement of the development to fluorescent material of LED.
YAG yellow fluorescent powder, due to lacking red light portion, obtained white light there are excitation purity, luminous efficiency is insufficient, white
The defects of light colour rendering is poor, and color is colder, and nitride phosphor can effectively supplement YAG yellow fluorescent powder feux rouges deficiency, and
And the advantages that nitride fluorescent material has excitation energy low, and emission spectrum is wide, and colour rendering index is high, and crystal structure is stablized.
Since rare earth ion is to the more demanding of crystal substrate structure in nitride phosphor preparation process, former with ceramics
When material mixing heat treatment, it is easy to cause element nitride crystal fault of construction and destruction, luminous intensity is greatly reduced, thus limit
It is applied.
Summary of the invention
In view of drawbacks described above in the prior art or deficiency, it is intended to provide a kind of simple process, at low cost, high-efficient, and
And the LED nitride that nitride fluorescent ceramic dense degree obtained is high, luminous efficiency is high, uniformity is good, thickness shape is controllable
Fluorescent transparent ceramic preparation.
The present invention provides a kind of preparation method of LED nitride fluorescent crystalline ceramics, comprising the following steps:
Step 1: in the glove box of nitrogen protection, raw material is weighed, mixed, is ground；
Step 2: the powder ground in step 1 is put into corundum crucible, and is put into vacuum pressed sintering rapid cooling
It in furnace, is sintered, cools down；
Step 3: the product that step 2 is obtained carries out grinding and is crushed, crosses 120 meshes, obtains nitride phosphor；
Step 4: ceramic powder and fluorescent powder are weighed in proportion, are added in mortar and are uniformly mixed to get mixture；
Step 5: mixture progress compressing tablet process is obtained into green body；
Step 6: green body is put into mold, is flattened to obtain biscuit with cold isostatic press；
Step 7: biscuit is subjected to high temperature sintering in high temperature resistance furnace, obtains sample；
Step 8: the sample is made annealing treatment, and obtains fluorescent transparent ceramics.
A small amount of metallic is added, in step 1 to improve reflection and the scattering property of fluorescent transparent ceramics；Metal
When the partial size of particle is between 20-200nm, it can preferably reflect and dispersion effect, metallic are preferred golden or silver-colored；
A small amount of UV absorbers or antioxidant are added, in step 1 to improve the anti-aging of fluorescent transparent ceramics
Performance；
The ceramic material powder is SiO2、Al2O3、B2O3、P2O5、Bi2O3、SnO、ZnO、ZrO2、Li2O、K2O、Na2O、
CaCO3It is one or more of；
The spread powder is CaCO3, quality is the 1-10% of ceramic raw material；
The nitride phosphor is Ca1-XAlSiN3:X Eu2+, x 0.01-0.09；Phosphor raw material is Si3N4、
Al3N4、Ca2N3、Eu2O3、NH4Cl；
The ceramic powder mass fraction is 80-95wt%, and the fluorescent powder mass fraction is 5-20wt%；
The sintering aid NH4The weight ratio of Cl and phosphor raw material is 1:100-1:20；
The vacuum-sintering condition: it is warming up to 1500-1800 DEG C with 2-6 DEG C/min, keeps the temperature 2-10 hours, nitrogen pressure
0.2-0.9MPa；
The tabletting conditions: pressure 50-200MPa, dwell time 1-15min；
The mold materials are rubber, plastics；
The cold isostatic press pressure is 100-400MPa, dwell time 1-15min；
The high temperature sintering condition: it is warming up to 1000-1400 DEG C with 8-12 DEG C/min, keeps the temperature 1-8 hours；
The annealing condition: it is warming up to 900-1200 DEG C with 6-10 DEG C/min, keeps the temperature 1-5 hours.
Nitride fluorescent ceramics are made using high temperature solid state reaction in the present invention, by adding spread powder in ceramic raw material
CaCO3, when so that ceramic raw material mixing heat treatment with nitride phosphor, reduce to element nitride crystal structural damage, together
When make ceramic raw material with nitride phosphor when mixing, certain spatial joint clearance is formed, so that the light of nitride fluorescent ceramics
Son scattering enhancing, improves transmitance；And CaCO3Pyrolytic is CaO, can be used as ceramic composition, improves nitride fluorescent
The consistency of ceramics.Nitride fluorescent ceramic system of the invention is for simple process, at low cost, high-efficient, and nitridation obtained
Object fluorescence ceramics consistency is high, luminous efficiency is high, uniformity is good, thickness shape is controllable.
The present invention is described in detail combined with specific embodiments below.On those skilled in the art is according to the present invention
It states content and makes some nonessential modifications and adaptations and belong to protection content of the invention.
The present invention is using the saturating fluorescent transparent ceramics of high temperature solid-state method preparation LED nitride.More specifically as an example, originally
Invention may comprise steps of:
(1) it in the glove box of nitrogen protection, weighed fluorescent powder is raw materials used, is mixed, is ground, the nitride
Fluorescent powder is Ca1-XAlSiN3:XEu2+, X is in 0.01-0.09；Phosphor raw material is Si3N4、Al3N4、Ca2N3、Eu2O3,NH4Cl；
The weight ratio of the sintering aid NH4Cl and phosphor raw material is 1:100-1:20；
(2) ground powder is placed in corundum crucible, is immediately placed in vacuum pressed sintering rapid cooling, is burnt
Knot, cooling；The vacuum-sintering condition: it is warming up to 1500-1800 DEG C with 2-6 DEG C/min, keeps the temperature 2-10 hours, nitrogen pressure
0.2-0.9MPa；
(3) obtained product grind and be crushed, cross 120 meshes, obtain nitride phosphor；
(4) high-purity ceramic material powder, fluorescent powder obtained are weighed in proportion, is added in mortar and uniformly mixes, institute
Stating ceramic powder mass fraction is 80-95wt%, and the fluorescent powder mass fraction is 5-20wt%；The spread powder is CaCO3,
Quality is the 1-10% of ceramic raw material；
(5) mixture progress compressing tablet process is obtained into green body, the tabletting conditions: pressure 50-200MPa, dwell time
1-15min；
(6) green body is put into mold, flattens to obtain biscuit with cold isostatic press, the mold materials be rubber,
Plastics；The cold isostatic press pressure is 100-400MPa, dwell time 1-15min；
(7) biscuit is carried out to high temperature sintering, the high temperature sintering condition: in high temperature resistance furnace with 8-12 DEG C/min liter
Temperature arrives 1000-1400 DEG C, keeps the temperature 1-8 hours；
(8) gained sample is made annealing treatment, obtains fluorescent transparent ceramics, the annealing condition: with 6-10
DEG C/min is warming up to 900-1200 DEG C, keep the temperature 1-5 hours；
(9) the fluorescent transparent ceramics of high quality are obtained by cutting and polishing.
Specific embodiment
The application is described in further detail below with reference to embodiment.It is understood that tool described herein
Body embodiment is used only for explaining related invention, rather than the restriction to the invention.
It should be noted that in the absence of conflict, the features in the embodiments and the embodiments of the present application can phase
Mutually combination.The application is described in detail below with reference to embodiment.
Embodiment 1
In the glove box of nitrogen protection, Si is weighed respectively3N45.65g、Al3N45.53g、Ca2N37.09g、
Eu2O30.85g、NH4Cl 0.76g progress ground and mixed is uniform, is transferred in corundum pot, is immediately placed in vacuum sintering furnace,
1700 DEG C are warming up to 2 DEG C/min, keeps the temperature 3 hours, nitrogen pressure 0.65MPa, it is cooling to furnace, take out sample ground 120
Mesh obtains nitride phosphor；Weigh SiO231.8g、Al2O37.5g、Bi2O322.6g、B2O3 15.9g、ZnO 9.7g、
CaCO36.8g, a small amount of metallic are uniformly mixed with 8g nitride phosphor, then by mixture with 100MPa pressure dry-pressing
5min obtains green body, and it is that pressure maintaining 5min obtains biscuit in 200MPa cold isostatic press that green body, which is put into rubber mold in pressure,
Biscuit is warming up to 1200 DEG C in high temperature resistance furnace with 8 DEG C/min, 2 hours is kept the temperature, is then warming up to 1000 DEG C with 6 DEG C/min
Made annealing treatment, keep the temperature 2 hours, furnace cooling, finally by ceramic sheet carry out cutting and polishing processing, be made thickness 600um,
The fluorescent transparent ceramics of transmitance 51%.
Embodiment 2
In the glove box of nitrogen protection, Si is weighed respectively3N45.65g、Al3N45.53g、Ca2N36.79g、
Eu2O30.91g、NH4Cl 0.94g progress ground and mixed is uniform, is transferred in corundum pot, is immediately placed in vacuum sintering furnace,
1600 DEG C are warming up to 3 DEG C/min, keeps the temperature 4 hours, nitrogen pressure 0.45MPa, it is cooling to furnace, take out sample ground 120
Mesh obtains nitride phosphor；Weigh SiO232.7g、Al2O36.2g、Bi2O323.6g、B2O3 16.7g、ZnO 7.7g、
CaCO34.3g, a small amount of metallic are uniformly mixed with 10g nitride phosphor, then by mixture with 100MPa pressure dry-pressing
10min obtains green body, and it is that pressure maintaining 10min obtains element in 200MPa cold isostatic press that green body, which is put into plastic mould in pressure,
Biscuit is warming up to 1000 DEG C in high temperature resistance furnace with 10 DEG C/min, keeps the temperature 2 hours, be then warming up to 7 DEG C/min by base
1100 DEG C are made annealing treatment, and keep the temperature 1 hour, and ceramic sheet is finally carried out cutting and polishing processing by furnace cooling, and thickness is made
The fluorescent transparent ceramics of 800um, transmitance 47%.
Embodiment 3
In the glove box of nitrogen protection, Si is weighed respectively3N45.65g、Al3N45.53g、Ca2N38.12g、
Eu2O30.65g、NH4Cl 0.4g progress ground and mixed is uniform, is transferred in corundum pot, is immediately placed in vacuum sintering furnace, with
2 DEG C/min is warming up to 1800 DEG C, keeps the temperature 3 hours, nitrogen pressure 0.5MPa, cooling to furnace, takes out ground 120 mesh of sample
Obtain nitride phosphor；Weigh SiO226.4g、Al2O33.6g、P2O521.8g、B2O3 12.9g、ZnO 4.8g、
CaCO32.8g, a small amount of metallic are uniformly mixed with 5g nitride phosphor, then by mixture with 150MPa pressure dry-pressing
5min obtains green body, and it is that pressure maintaining 10min obtains biscuit in 150MPa cold isostatic press that green body, which is put into plastic mould in pressure,
Biscuit is warming up to 1100 DEG C in high temperature resistance furnace with 9 DEG C/min, 2 hours is kept the temperature, is then warming up to 1000 DEG C with 8 DEG C/min
Made annealing treatment, keep the temperature 2 hours, furnace cooling, finally by ceramic sheet carry out cutting and polishing processing, be made thickness 500um,
The fluorescent transparent ceramics of transmitance 53%.
Embodiment 4
In the glove box of nitrogen protection, Si is weighed respectively3N45.65g、Al3N45.53g、Ca2N36.88g、
Eu2O30.81g、NH4Cl 1.13g progress ground and mixed is uniform, is transferred in corundum pot, is immediately placed in vacuum sintering furnace,
1600 DEG C are warming up to 4 DEG C/min, keeps the temperature 5 hours, nitrogen pressure 0.75MPa, it is cooling to furnace, take out sample ground 120
Mesh obtains nitride phosphor；Weigh SiO234.3g、Al2O34.5g、Li2O8.9g、K2O 15.6g、Na2O 11.1g、
CaCO31.5g is uniformly mixed with 10g nitride phosphor, and mixture is then obtained green body with 100MPa pressure dry-pressing 10min,
It is that pressure maintaining 10min obtains biscuit in 200MPa cold isostatic press that green body, which is put into rubber mold in pressure, by biscuit in high temperature
1100 DEG C are warming up to 9 DEG C/min in resistance furnace, 3 hours is kept the temperature, is then warming up to 1100 DEG C with 6 DEG C/min and carries out at annealing
Reason keeps the temperature 3 hours, and ceramic sheet is finally carried out cutting and polishing processing by furnace cooling, and thickness 700um, transmitance 49% is made
Fluorescent transparent ceramics.
Embodiment 5
In the glove box of nitrogen protection, Si is weighed respectively3N45.65g、Al3N45.53g、Ca2N311.24g、
Eu2O30.45g、NH4Cl 0.69g progress ground and mixed is uniform, is transferred in corundum pot, is immediately placed in vacuum sintering furnace,
1800 DEG C are warming up to 3 DEG C/min, keeps the temperature 3 hours, nitrogen pressure 0.65MPa, it is cooling to furnace, take out sample ground 120
Mesh obtains nitride phosphor；Weigh SiO228.8g、Al2O36.8g、P2O524.3g、B2O3 16.5g、ZrO29.9g、
CaCO33.2g is uniformly mixed with 12g nitride phosphor, and mixture is then obtained green body with 150MPa pressure dry-pressing 5min,
It is that pressure maintaining 10min obtains biscuit in 250MPa cold isostatic press that green body, which is put into rubber mold in pressure, by biscuit in high temperature
1100 DEG C are warming up to 8 DEG C/min in resistance furnace, 2 hours is kept the temperature, is then warming up to 1200 DEG C with 10 DEG C/min and carries out at annealing
Reason keeps the temperature 2 hours, and ceramic sheet is finally carried out cutting and polishing processing by furnace cooling, and thickness 900um, transmitance 45% is made
Fluorescent transparent ceramics.
Above description is only the preferred embodiment of the application and the explanation to institute's application technology principle.Those skilled in the art
Member is it should be appreciated that invention scope involved in the application, however it is not limited to technology made of the specific combination of above-mentioned technical characteristic
Scheme, while should also cover in the case where not departing from the inventive concept, it is carried out by above-mentioned technical characteristic or its equivalent feature
Any combination and the other technical solutions formed.Such as features described above has similar function with (but being not limited to) disclosed herein
Can technical characteristic replaced mutually and the technical solution that is formed.
Claims (7)
1. a kind of LED preparation method of nitride fluorescent crystalline ceramics, which comprises the following steps:
Step 1: in the glove box of nitrogen protection, raw material is weighed, mixed, is ground；
Step 2: the powder that the step 1 obtains is put into corundum crucible, and is put into vacuum pressed sintering rapid cooling furnace
In, it is sintered, cools down；
Step 3: the product that the step 2 is obtained carries out grinding and is crushed, crosses 120 meshes, obtains nitride phosphor；
Step 4: ceramic powder and nitride phosphor are weighed in proportion, are added in mortar and are uniformly mixed to get mixture；
Step 5: mixture progress compressing tablet process is obtained into green body；
Step 6: the green body is put into mold, is flattened to obtain biscuit with cold isostatic press；
Step 7: the biscuit is subjected to high temperature sintering in high temperature resistance furnace, obtains sample；
Step 8: the sample is made annealing treatment, and obtains fluorescent transparent ceramics；
Wherein, the chemical formula of the nitride phosphor is Ca1-XAlSiN3:XEu2+, the X is 0.01-0.09, the raw material
For Si3N4、Al3N4、Ca2N3And Eu2O3One or more of, sintering aid is NH in the step 24Cl, the sintering help
The weight ratio of agent and phosphor raw material is 1:100-1:20；
The ceramic powder is SiO2、Al2O3、B2O3、P2O5、Bi2O3、SnO、ZnO、ZrO2、Li2O、K2O、Na2O and CaCO3In
The ratio of one or more, the ceramic powder and the fluorescent powder is that the ceramic powder mass fraction is 80-95wt%,
The fluorescent powder mass fraction is 5-20wt%, and the ceramic powder includes spread powder, and the spread powder is CaCO3, the expansion
The mass fraction of loose powder is the 1-10% of ceramic powder.
2. the LED according to claim 1 preparation method of nitride fluorescent crystalline ceramics, which is characterized in that the step
Metallic is added in rapid one.
3. the LED according to claim 2 preparation method of nitride fluorescent crystalline ceramics, which is characterized in that the gold
The partial size for belonging to particle is 20-200nm.
4. the LED according to claim 2 preparation method of nitride fluorescent crystalline ceramics, which is characterized in that the gold
Belonging to particle is gold particle or silver particles.
5. the LED according to claim 1-4 preparation method of nitride fluorescent crystalline ceramics, feature exist
In being warming up to 1500-1800 DEG C with 2-6 DEG C/min, keep the temperature 2-10 hours, nitrogen pressure in the step 2 vacuum-sintering
0.2-0.9Mpa。
6. the LED according to claim 1-4 preparation method of nitride fluorescent crystalline ceramics, feature exist
In the pressure of the tabletting is 50-200MPa, dwell time 1-15min.
7. the LED according to claim 1-4 preparation method of nitride fluorescent crystalline ceramics, feature exist
In the mold materials are rubber or plastics.
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