CN106866132A - It is a kind of for fluorescence ceramics for illuminating or showing and preparation method thereof - Google Patents
It is a kind of for fluorescence ceramics for illuminating or showing and preparation method thereof Download PDFInfo
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- CN106866132A CN106866132A CN201710033395.9A CN201710033395A CN106866132A CN 106866132 A CN106866132 A CN 106866132A CN 201710033395 A CN201710033395 A CN 201710033395A CN 106866132 A CN106866132 A CN 106866132A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000000498 ball milling Methods 0.000 claims abstract description 57
- 239000000843 powder Substances 0.000 claims abstract description 38
- 229910000323 aluminium silicate Inorganic materials 0.000 claims abstract description 29
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000001354 calcination Methods 0.000 claims abstract description 26
- 238000003825 pressing Methods 0.000 claims abstract description 25
- 238000005245 sintering Methods 0.000 claims abstract description 17
- 239000000126 substance Substances 0.000 claims abstract description 14
- 229910010293 ceramic material Inorganic materials 0.000 claims abstract description 13
- 238000005056 compaction Methods 0.000 claims abstract description 8
- 238000003837 high-temperature calcination Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims description 49
- 239000002994 raw material Substances 0.000 claims description 20
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 17
- 229910052681 coesite Inorganic materials 0.000 claims description 9
- 229910052906 cristobalite Inorganic materials 0.000 claims description 9
- 239000000377 silicon dioxide Substances 0.000 claims description 9
- 229910052682 stishovite Inorganic materials 0.000 claims description 9
- 229910052905 tridymite Inorganic materials 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 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
- 229910052593 corundum Inorganic materials 0.000 claims description 7
- RSEIMSPAXMNYFJ-UHFFFAOYSA-N europium(III) oxide Inorganic materials O=[Eu]O[Eu]=O RSEIMSPAXMNYFJ-UHFFFAOYSA-N 0.000 claims description 7
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 7
- 238000000695 excitation spectrum Methods 0.000 claims description 4
- 238000000295 emission spectrum Methods 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 2
- 229910026161 MgAl2O4 Inorganic materials 0.000 claims description 2
- 229910052596 spinel Inorganic materials 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000012752 auxiliary agent Substances 0.000 claims 1
- 238000000137 annealing Methods 0.000 abstract description 7
- 238000013019 agitation Methods 0.000 abstract description 4
- 238000005286 illumination Methods 0.000 abstract description 4
- 230000006641 stabilisation Effects 0.000 abstract description 4
- 238000011105 stabilization Methods 0.000 abstract description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 10
- 229910000019 calcium carbonate Inorganic materials 0.000 description 5
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 3
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 229910000018 strontium carbonate Inorganic materials 0.000 description 2
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(III) oxide Inorganic materials O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- -1 organic siliconresin Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
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Abstract
The invention discloses a kind of for fluorescence ceramics for illuminating or showing and preparation method thereof, described fluorescence ceramics include ceramic material powder, sintering aid and aluminosilicate fluorescent powder.The aluminosilicate fluorescent powder chemical formula is (Ca1‑xMx)1‑y‑zAl2Si2O8：yEu2+, zR, element M is Mg, Sr, and the one kind in Ba, R is Ce3+, Mn4+, Dy3+, Tb3+In one kind, wherein x, y, z are mole coefficient, the ＜ x ＜ 1 of scope 0.01,0.2≤y≤0.7,0≤z≤0.6, y+z ＜ 1, prepare fluorescence ceramics mainly by high-temperature calcination technique, and specific steps include：Ball milling, after ball milling terminates, carries out dry-pressing formed, cold isostatic compaction, vacuum calcining, high temperature insostatic pressing (HIP) calcining and makes annealing treatment.Fluorescence ceramics prepared by the present invention, excite and emission effciency with high, physico-chemical property stabilization, are adapted to high-energy-density light continuous agitation and use, and have preferable application prospect in illumination or display field.
Description
Technical field
The present invention relates to a kind of fluorescence ceramics for illuminating or showing, and there is provided the preparation method of the fluorescence ceramics,
Belong to field of light emitting materials.
Background technology
White light LEDs due to having the advantages that light efficiency high, long lifespan, energy-conserving and environment-protective, safe and reliable, at present in illumination, display
Deng field gradually occuping market share.The principal mode for realizing white light LEDs is semiconductor chip excitated fluorescent powder material, tool
The technique of body is spot printing after phosphor material powder is mixed into deaeration with organic resin material (such as organic siliconresin, epoxy resin)
To the surface of semiconductor chip, then by after curing molding, you can white light LEDs are obtained.This form process is simple, low cost,
But many problems that can not be solved are there is also, with the increase of semiconductor chip power energy density, unit area emergent light
When energy rising, such as lasing of laser, the optical attenuation of the fluorescent material in traditional this form is very serious, while organic resin material
Used as a kind of macromolecular material, strand depolymerization to material will occur under long-term high-energy, hot environment, produce yellow to show
As causing the decline of luminous efficiency, therefore prepare physico-chemical property stabilization, the fluorescence that the light of resistance to high-energy-density continuous agitation is used
Material, is the key link for realizing super high power White-light LED illumination or display.
The content of the invention
In order to solve the above technical problems, the present invention provides a kind of fluorescence ceramics for illuminating or showing, the fluorescence ceramics
It is prepared from by high-sintering process by ceramic material powder, sintering aid and aluminosilicate fluorescent powder；The fluorescence pottery of preparation
Porcelain, excites and emission effciency with high, physico-chemical property stabilization, be adapted to high-energy-density light continuous agitation use, illumination or
Display field has preferable application prospect.
Described aluminosilicate fluorescent powder chemical formula is (Ca1-xMx)1-y-zAl2Si2O8：yEu2+, zR, element M is Mg, Sr,
One kind in Ba, R is Ce3+, Mn4+, Dy3+, Tb3+In one kind, wherein x, y, z are mole coefficient, the ＜ x ＜ 1,0.2 of scope 0.01
≤ y≤0.7,0≤z≤0.6, y+z ＜ 1, excitation spectrum scope 250-480nm, emission spectrum scope 400-700nm；
Described ceramic material powder is MgAl2O4、Y2O3, at least one in MgAlON and AlN；
Described sintering aid is MgO, SiO2、TiO2With at least one in CaO；
The quality proportioning difference of ceramic material powder, sintering aid and aluminosilicate fluorescent powder in described fluorescence ceramics
For：70-90%, 0.5-8% and 2-29.5%；
The present invention also provides the preparation method of above-mentioned fluorescence ceramics, concretely comprises the following steps：
A. the preparation of alumino-silicate fluorescent material：According to chemical formula (Ca1-xMx)1-y-zAl2Si2O8：yEu2+, each element in zR
Ratio, weighs carbonate, the CaCO of element M3、Al2O3、SiO2、Eu2O3With the oxide of element R as raw material, the original that will be weighed
Material is well mixed, carries out ball milling, and Ball-milling Time is 3-4 hours, 100-130 revs/min of ball milling speed；After ball milling terminates, by original
Material is fitted into crucible, and high-temperature calcination is carried out in high temperature solid-state stove reducing atmosphere, and temperature is 1050-1450 DEG C, and the time is 8-12
Hour, after calcining terminates, when high temperature solid-state furnace temperature is down into room temperature, burner hearth is opened, material is taken out, pulverize and sieve, you can system
Aluminosilicate fluorescent powder needed for standby；
B. the preparation of fluorescence ceramics：According to the ceramic material powder in fluorescence ceramics, sintering aid and aluminosilicate fluorescence
The quality proportioning of powder weighs material respectively, and ball milling is carried out in addition ball grinder, and Ball-milling Time is 5-20 hours, ball milling speed 200-
300 revs/min, after ball milling terminates, material is carried out dry-pressing formed, pressure is 80-150MPa, dwell time 5-15 minutes, is done
Pressure carries out cold isostatic compaction after terminating, pressure is 200-400MPa, dwell time 5-10 minutes, after isostatic cool pressing terminates, is incited somebody to action
Material carries out vacuum calcining, and temperature is 1500-1750 DEG C, and the time is 7-13 hours, vacuum 10-1-10-4Pa, vacuum calcining knot
High temperature insostatic pressing (HIP) calcining is carried out after beam, temperature is 1600-1700 DEG C, and the time is 2-8 hours, and pressure is 150-200MPa, most laggard
Row annealing, temperature is 700-1000 DEG C, and the time is 8-12 hours, is then cooled to room temperature, you can the fluorescence needed for preparing
Ceramics；
In the above-mentioned methods, described reducing atmosphere is by activated carbon or N2/H2There is provided.
Beneficial effect：
1st, there is fluorescence ceramics of the present invention wide range to excite and transmitting, excitation spectrum scope 250-480nm, launching light
Spectral limit 400-700nm；
2nd, fluorescence ceramics physico-chemical property stabilization of the present invention, is adapted to high-energy-density light continuous agitation and uses.
Brief description of the drawings
Fig. 1 is the excitation and emission spectra of the fluorescence ceramics sample of preparation in specific embodiment 1
Specific embodiment
The present invention is described in further details with reference to case study on implementation, but the scope of the present invention is not limited to the content.
Embodiment 1：
A. the preparation of alumino-silicate fluorescent material：According to chemical formula (Ca0.3Mg0.7)0.8Al2Si2O8：0.2Eu2+Middle each element
Ratio, weighs MgCO3、CaCO3、Al2O3、SiO2And Eu2O3Used as raw material, the raw material that will be weighed is well mixed, and carries out ball milling, ball
It is 3 hours to consume time, 120 revs/min of ball milling speed；After ball milling terminates, raw material is fitted into crucible, in high temperature solid-state stove activity
High-temperature calcination is carried out in the reducing atmosphere that charcoal is formed, temperature is 1250 DEG C, and the time is 8.5 hours, after calcining terminates, by high temperature
When solid phase furnace temperature is down to room temperature, burner hearth is opened, take out material, pulverized and sieved, you can the aluminosilicate fluorescent powder needed for preparing；
B. the preparation of fluorescence ceramics：According to the ceramic material powder in fluorescence ceramics, sintering aid and aluminosilicate fluorescence
The quality proportioning of powder is respectively 75%, 3% and 22% weighs material, and ball milling is carried out in addition ball grinder, and Ball-milling Time is 13 small
When, 240 revs/min of ball milling speed after ball milling terminates, material is carried out dry-pressing formed, and pressure is 100MPa, 10 points of dwell time
Clock, dry-pressing carries out cold isostatic compaction after terminating, pressure is 270MPa, 8 minutes dwell times, after isostatic cool pressing terminates, by material
Material carries out vacuum calcining, and temperature is 1600 DEG C, and the time is 8 hours, vacuum 10-3Pa, it is quiet that vacuum calcining carries out heat etc. after terminating
Pressure calcining, temperature is 1690 DEG C, and the time is 3 hours, and pressure is 180MPa, is finally made annealing treatment, and temperature is 850 DEG C, when
Between be 9 hours, be then cooled to room temperature, you can prepare needed for fluorescence ceramics；
Embodiment 2：
A. the preparation of alumino-silicate fluorescent material：According to chemical formula (Ca0.4Sr0.6)0.5Al2Si2O8：0.4Eu2+, 0.1Ce3+In
The ratio of each element, weighs SrCO3、CaCO3、Al2O3、SiO2、Eu2O3And CeO2Used as raw material, the raw material mixing that will be weighed is equal
It is even, ball milling is carried out, Ball-milling Time is 3.5 hours, 120 revs/min of ball milling speed；After ball milling terminates, raw material is fitted into crucible,
High-temperature calcination is carried out in the reducing atmosphere that high temperature solid-state stove activated carbon is formed, temperature is 1150 DEG C, and the time is 9.5 hours,
After calcining terminates, when high temperature solid-state furnace temperature is down into room temperature, burner hearth is opened, take out material, pulverized and sieved, you can needed for preparing
Aluminosilicate fluorescent powder；
B. the preparation of fluorescence ceramics：According to the ceramic material powder in fluorescence ceramics, sintering aid and aluminosilicate fluorescence
The quality proportioning of powder is respectively 80%, 2% and 18% weighs material, and ball milling is carried out in addition ball grinder, and Ball-milling Time is 12 small
When, 245 revs/min of ball milling speed after ball milling terminates, material is carried out dry-pressing formed, and pressure is 110MPa, 6 points of dwell time
Clock, dry-pressing carries out cold isostatic compaction after terminating, pressure is 300MPa, 8 minutes dwell times, after isostatic cool pressing terminates, by material
Material carries out vacuum calcining, and temperature is 1650 DEG C, and the time is 8.5 hours, vacuum 10-1Pa, vacuum calcining carries out heat etc. after terminating
Static pressure is calcined, and temperature is 1650 DEG C, and the time is 5 hours, and pressure is 150MPa, is finally made annealing treatment, and temperature is 7900 DEG C,
Time is 10 hours, is then cooled to room temperature, you can the fluorescence ceramics needed for preparing；
Embodiment 3：
A. the preparation of alumino-silicate fluorescent material：According to chemical formula (Ca0.9Sr0.1)0.3Al2Si2O8：0.25Eu2+, 0.45Ce3+
The ratio of middle each element, weighs SrCO3、CaCO3、Al2O3、SiO2、Eu2O3And CeO2Used as raw material, the raw material mixing that will be weighed is equal
It is even, ball milling is carried out, Ball-milling Time is 3.5 hours, 120 revs/min of ball milling speed；After ball milling terminates, raw material is fitted into crucible,
In high temperature solid-state stove stove N2/H2High-temperature calcination is carried out in the reducing atmosphere for being formed, temperature is 1350 DEG C, and the time is 8 hours, is forged
After sintering beam, when high temperature solid-state furnace temperature is down into room temperature, burner hearth is opened, take out material, pulverized and sieved, you can needed for preparing
Aluminosilicate fluorescent powder；
B. the preparation of fluorescence ceramics：According to the ceramic material powder in fluorescence ceramics, sintering aid and aluminosilicate fluorescence
The quality proportioning of powder is respectively 90%, 0.5% and 9.5% weighs material, and ball milling is carried out in addition ball grinder, and Ball-milling Time is 5
Hour, 300 revs/min of ball milling speed after ball milling terminates, material is carried out dry-pressing formed, and pressure is 80MPa, dwell time 13
Minute, dry-pressing carries out cold isostatic compaction after terminating, pressure is 280MPa, 7 minutes dwell times, after isostatic cool pressing terminates, is incited somebody to action
Material carries out vacuum calcining, and temperature is 1700 DEG C, and the time is 8 hours, vacuum 10-4Pa, vacuum calcining carries out heat etc. after terminating
Static pressure is calcined, and temperature is 1680 DEG C, and the time is 3 hours, and pressure is 180MPa, is finally made annealing treatment, and temperature is 900 DEG C,
Time is 10 hours, is then cooled to room temperature, you can the fluorescence ceramics needed for preparing；
Embodiment 4：
A. the preparation of alumino-silicate fluorescent material：According to chemical formula (Ca0.6Ba0.4)0.1Al2Si2O8：0.6Eu2+, 0.3Dy3+)
The ratio of middle each element, weighs BaCO3、CaCO3、Al2O3、SiO2、Eu2O3And Dy2O3As raw material, the raw material mixing that will be weighed
Uniformly, ball milling is carried out, Ball-milling Time is 4 hours, 120 revs/min of ball milling speed；After ball milling terminates, raw material is fitted into crucible,
High-temperature calcination is carried out in the reducing atmosphere that high temperature solid-state stove activated carbon is formed, temperature is 1400 DEG C, and the time is 11 hours, is forged
After sintering beam, when high temperature solid-state furnace temperature is down into room temperature, burner hearth is opened, take out material, pulverized and sieved, you can needed for preparing
Aluminosilicate fluorescent powder；
B. the preparation of fluorescence ceramics：According to the ceramic material powder in fluorescence ceramics, sintering aid and aluminosilicate fluorescence
The quality proportioning of powder is respectively 70%, 1% and 29% weighs material, and ball milling is carried out in addition ball grinder, and Ball-milling Time is 9 small
When, 300 revs/min of ball milling speed after ball milling terminates, material is carried out dry-pressing formed, and pressure is 120MPa, 13 points of dwell time
Clock, dry-pressing carries out cold isostatic compaction after terminating, pressure is 300MPa, 8 minutes dwell times, after isostatic cool pressing terminates, by material
Material carries out vacuum calcining, and temperature is 1500 DEG C, and the time is 13 hours, vacuum 10-4Pa, it is quiet that vacuum calcining carries out heat etc. after terminating
Pressure calcining, temperature is 1650 DEG C, and the time is 5 hours, and pressure is 150MPa, is finally made annealing treatment, and temperature is 950 DEG C, when
Between be 11 hours, be then cooled to room temperature, you can prepare needed for fluorescence ceramics；
Embodiment 5：
A. the preparation of alumino-silicate fluorescent material：According to chemical formula (Ca0.5Ba0.5)0.3Al2Si2O8：0.5Eu2+, 0.2Tb3+)
The ratio of middle each element, weighs BaCO3、CaCO3、Al2O3、SiO2、Eu2O3And Tb2O3As raw material, the raw material mixing that will be weighed
Uniformly, ball milling is carried out, Ball-milling Time is 3.5 hours, 120 revs/min of ball milling speed；After ball milling terminates, raw material is loaded into crucible
In, in high temperature solid-state stove N2/H2High-temperature calcination is carried out in the reducing atmosphere for being formed, temperature is 1050 DEG C, and the time is 11 hours,
After calcining terminates, when high temperature solid-state furnace temperature is down into room temperature, burner hearth is opened, take out material, pulverized and sieved, you can needed for preparing
Aluminosilicate fluorescent powder；
B. the preparation of fluorescence ceramics：According to the ceramic material powder in fluorescence ceramics, sintering aid and aluminosilicate fluorescence
The quality proportioning of powder weighs material respectively, and ball milling is carried out in addition ball grinder, and Ball-milling Time is 10 hours, and 250 turns of ball milling speed/
Minute, after ball milling terminates, material is carried out dry-pressing formed, pressure is 140MPa, and 12 minutes dwell times, dry-pressing is carried out after terminating
Cold isostatic compaction, pressure is 300MPa, 6 minutes dwell times, after isostatic cool pressing terminates, material is carried out into vacuum calcining, temperature
It is 1650 DEG C to spend, and the time is 11 hours, vacuum 10-2Pa, vacuum calcining carries out high temperature insostatic pressing (HIP) calcining after terminating, temperature is 1600
DEG C, the time is 6.5 hours, and pressure is 200MPa, is finally made annealing treatment, and temperature is 950 DEG C, and the time is 8.5 hours, then
It is cooled to room temperature, you can the fluorescence ceramics needed for preparing.
Claims (6)
1. a kind of fluorescence ceramics for illuminating or showing, it is characterised in that：Described fluorescence ceramics are by ceramic material powder, burning
Knot auxiliary agent and aluminosilicate fluorescent powder are prepared from by high-sintering process；Described aluminosilicate fluorescent powder chemical formula is
(Ca1-xMx)1-y-zAl2Si2O8：yEu2+, zR, element M is Mg, Sr, and the one kind in Ba, R is Ce3+, Mn4+, Dy3+, Tb3+In one
Kind, wherein x, y, z are mole coefficient, the ＜ x ＜ 1 of scope 0.01,0.2≤y≤0.7,0≤z≤0.6, y+z ＜ 1, excitation spectrum model
Enclose 250-480nm, emission spectrum scope 400-700nm.
2. fluorescence ceramics for illuminating or showing according to claim 1, it is characterised in that：Described ceramic raw material powder
Body is MgAl2O4、Y2O3, at least one in MgAlON and AlN.
3. fluorescence ceramics for illuminating or showing according to claim 1, it is characterised in that：Described sintering aid is
MgO、SiO2、TiO2With at least one in CaO.
4. fluorescence ceramics for illuminating or showing according to claim 1, it is characterised in that：In described fluorescence ceramics
The quality proportioning of ceramic material powder, sintering aid and aluminosilicate fluorescent powder be respectively：70-90%, 0.5-8% and 2-
29.5%.
5. the fluorescence ceramics for illuminating or showing according to claim 1, including implemented below step：
A. the preparation of alumino-silicate fluorescent material：According to chemical formula (Ca1-xMx)1-y-zAl2Si2O8：yEu2+, the ratio of each element in zR
Example, weighs carbonate, the CaCO of element M3、Al2O3、SiO2、Eu2O3With the oxide of element R as raw material, the raw material that will be weighed
It is well mixed, ball milling is carried out, Ball-milling Time is 3-4 hours, 100-130 revs/min of ball milling speed；After ball milling terminates, by raw material
It is fitted into crucible, high-temperature calcination is carried out in high temperature solid-state stove reducing atmosphere, temperature is 1050-1450 DEG C, and the time is that 8-12 is small
When, after calcining terminates, when high temperature solid-state furnace temperature is down into room temperature, burner hearth is opened, material is taken out, pulverize and sieve, you can prepare
Required aluminosilicate fluorescent powder；
B. the preparation of fluorescence ceramics：According to the ceramic material powder in fluorescence ceramics, sintering aid and aluminosilicate fluorescent powder
Quality proportioning weighs material respectively, and ball milling is carried out in addition ball grinder, and Ball-milling Time is 5-20 hours, ball milling speed 200-300
Rev/min, after ball milling terminates, material is carried out dry-pressing formed, pressure is 80-150MPa, dwell time 5-15 minutes, dry-pressing knot
Carry out cold isostatic compaction after beam, pressure is 200-400MPa, dwell time 5-10 minutes, after isostatic cool pressing terminates, by material
Vacuum calcining is carried out, temperature is 1500-1750 DEG C, and the time is 7-13 hours, vacuum 10-1-10-4Pa, after vacuum calcining terminates
High temperature insostatic pressing (HIP) calcining is carried out, temperature is 1600-1700 DEG C, and the time is 2-8 hours, and pressure is 150-200MPa, is finally moved back
Fire treatment, temperature is 700-1000 DEG C, and the time is 8-12 hours, is then cooled to room temperature, you can the fluorescence ceramics needed for preparing.
It is 6. according to claim 5 to realize step for the fluorescence ceramics that illuminate or show, it is characterised in that：Described
Reducing atmosphere is by activated carbon or N2/H2There is provided.
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