CN104291796A - Preparation method of transparent fluorescent ceramic for LEDs (light-emitting diodes) - Google Patents
Preparation method of transparent fluorescent ceramic for LEDs (light-emitting diodes) Download PDFInfo
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- CN104291796A CN104291796A CN201410491094.7A CN201410491094A CN104291796A CN 104291796 A CN104291796 A CN 104291796A CN 201410491094 A CN201410491094 A CN 201410491094A CN 104291796 A CN104291796 A CN 104291796A
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Abstract
The invention discloses a preparation method of transparent fluorescent ceramic for LEDs (light-emitting diodes), which comprises the following steps: proportionally mixing high-purity ceramic raw material powder, a sintering assistant and fluorescent powder; adding into a ball milling tank, adding a ball milling medium and milling balls at the same time, and carrying out ball milling on the ball mill for some time; taking out the powder, drying, grinding and screening; sequentially carrying out dry press formation and cold isostatic compaction on the screened powder; sequentially carrying out vacuum sintering and hot isostatic compaction sintering on the formed billet; and carrying out annealing treatment to obtain the high-compactness transparent fluorescent ceramic for LEDs. In the formation and sintering steps, two different processes are respectively adopted, so that the prepared transparent fluorescent ceramic has higher compactness and better uniformity, and has better light emitting effect when being used for LED devices.
Description
Technical field
The invention belongs to LED transparent fluorescent material preparing technical field, be specifically related to a kind of preparation method of LED transparent fluorescent ceramic.
Background technology
Compared with common light source, LED component has the plurality of advantages such as response is fast, current consumption is little, the life-span is long, pollution-free, has been applied to the fields such as illumination, display screen, backlight.LED illumination is called as especially " green illumination ", has great development potentiality.
In the process preparing white light LED part, the encapsulation of fluorescent material is very crucial, and this is related to the properties such as luminous efficiency, color developing, work-ing life of white light LEDs.Traditional packaging process is mixed according to certain ratio with epoxy resin or silica gel by fluorescent material, is applied to the surface of chip after stirring, and forms the coating being similar to spherical crown shape.This technique also exists obvious defect.First be the selection of packaged material, epoxy resin has water absorbability, and poor heat resistance, easily aging, this makes the performance of LED component be greatly affected, and the life-span also substantially reduces; Silica gel again, organosilyl specific refractory power and chip differ greatly, and this can affect the output of light to a great extent, and the production cost of silica gel is higher, is not suitable as the packaged material of fluorescent material.In addition, also there is serious problem in the structure of traditional technology coating, and the structure of spherical crown shape makes coated center arrive the in uneven thickness of surface, and then causes the hot spot of formation uneven.Therefore, novel fluorescent powder packaging material is studied and packaged type tool is of great significance.
In recent years, crystalline ceramics progresses into the sight line of people as novel photoelectric material.Using the material of crystalline ceramics as encapsulation fluorescent material, there is many obvious advantages:
1. crystalline ceramics has excellent radiating effect, can extend the work-ing life of chip;
2. compare with resin-phase, the specific refractory power of crystalline ceramics is higher, can improve the light emission rate of light source to a great extent;
3. crystalline ceramics has good mechanical mechanics property, long service life, and cost is low;
4. mix mutually compared to liquid resin, fluorescent material is more even with mixing of solid ceramic powder, thus makes light-out effect better;
5. packaging process can be simplified.
But the crystalline ceramics density prepared by usual way is lower, the encapsulation being applied to LED component also exists that bright dipping is uneven, radiating effect is poor and the shortcoming such as light emission rate is lower.
Summary of the invention
The object of the invention is to the deficiency overcoming the existence of above-mentioned prior art, a kind of preparation method of LED transparent fluorescent ceramic is provided, the method raw material type is few and be easy to get, obtained transparent fluorescent ceramic density is high, good uniformity, can prepare good heat dissipation effect, LED component that light emission rate is high for LED.
The object of the invention is to be achieved through the following technical solutions:
The present invention relates to a kind of preparation method of LED transparent fluorescent ceramic, described method comprises the steps:
A, ceramic material powder, sintering aid and fluorescent material by high-purity are mixed in proportion; Add in ball grinder, add ball-milling medium, abrading-ball simultaneously, the ball milling regular hour on ball mill;
B, powder taken out and dries and grind and sieve;
C, successively dry-pressing formed, cold isostatic compaction is carried out to the powder after sieving;
Base substrate shaping in D, step C carries out vacuum sintering, HIP sintering successively;
E, anneal, obtain the fine and close LED transparent fluorescent ceramic of described height.
Preferably, described ceramic material powder is selected from Al
2o
3, Y
2o
3, MgAl
2o
4, MgAlON, AlN, SiN, ZrO
2, one or more in SiC.
Preferably, described sintering aid is selected from CaO, MgO, TiO
2, SiO
2, MnO, one or more in kaolin.
Preferably, the composition of described fluorescent material is Y
3al
5o
12: Ce
3+.Described fluorescent material is yellow fluorescent powder YAG:Ce.
Preferably, in steps A, the quality proportioning of described ceramic material powder, sintering aid and fluorescent material is: ceramic material powder 75 ~ 99wt%, sintering aid 0.9 ~ 24.9wt%, fluorescent material 0.1 ~ 10wt%.Wt% refers to the mass percentage content of each component in the mixture of ceramic material powder, sintering aid and fluorescent material.
Preferably, adopt tumbling ball mill to carry out ball milling, described ball grinder material is one or more in urethane, tetrafluoroethylene, high-purity agate; Described abrading-ball is high-purity zirconia Ceramic Balls; Described ball-milling medium is deionized water.
Preferably, the rotating speed of described ball milling is 150 ~ 500r/min, and Ball-milling Time is 3 ~ 24h.
Preferably, in step B, described bake out temperature is 90 ~ 120 DEG C, and drying time is 5 ~ 10 hours; Described grinding is sieved employing 200 mesh sieve.
Preferably, in step C, described dry-pressing formed pressure is 50 ~ 180MPa, and the dwell time is 0 ~ 10 minute.
Preferably, in step C, the pressure of described cold isostatic compaction is 200 ~ 350MPa, and the dwell time is 2 ~ 15 minutes.
Preferably, in step D, the sintering temperature of described vacuum sintering is 1500 ~ 1800 DEG C, and soaking time is 5 ~ 30 hours, and vacuum tightness is 10
-1~ 10
-4pa.
Preferably, in step D, the sintering temperature of described HIP sintering is 1600 ~ 1800 DEG C, and soaking time is 1 ~ 5 hour, and pressure is 120 ~ 180MPa.
Preferably, in step e, described anneal was specially: 800 ~ 1500 DEG C of insulations 5 ~ 40 hours, then furnace cooling.
Compared with prior art, the present invention has following beneficial effect:
1, method raw material type of the present invention is few and be easy to get, and production cost is low;
2, the present invention is in shaping and sintering step, successively have employed two kinds of diverse ways respectively, makes the transparent fluorescent ceramic density that obtains high, good uniformity, for LED component, can obtain good heat dissipation effect, LED component that light emission rate is high.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.Following examples will contribute to those skilled in the art and understand the present invention further, but not limit the present invention in any form.It should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, some distortion and improvement can also be made.These all belong to protection scope of the present invention.
embodiment 1
Take the α-Al that purity is 99.99%
2o
3powder 95g, high-purity CaO powder 3.5g and yellow fluorescent powder Y
3al
5o
12: Ce
3+1.5g puts into the ball grinder of urethane, add 300g zirconium oxide balls and 80g deionized water again, rotating speed ball milling with 300r/min on tumbling ball mill obtains mixture in 15 hours, is then taken out from ball grinder by mixture, then dries 5 hours in 110 DEG C of baking ovens.Powder is taken out and grinds and cross 200 mesh sieves, obtain base substrate with 100MPa pressure dry-pressing 3min, then take out base substrate and carry out isostatic cool pressing 5min under 200MPa pressure.By the vacuum sintering at 1600 DEG C of shaping base substrate, soaking time 10 hours, vacuum tightness is 2 × 10
-3pa, then by base substrate in 1700 DEG C, HIP sintering 3 hours under the pressure of 130MPa.The base substrate sintered is annealed 1300 DEG C of insulations for 12 hours, then furnace cooling.Polish, obtain the ceramic plate that thickness is about 1mm after polishing, carry out performance test.Obtained ceramic plate relative density > 99.95%; After in LED component, by test, the color coordinates distribution obtained is concentrated, and dominant wavelength ranges distribution is little, uniform in light emission; By test pin temperature computation junction temperature, the packaged material that the thermal diffusivity of transparent fluorescent ceramic mixes with silica gel significantly better than fluorescent material.
embodiment 2
Take the α-Al that purity is 99.99%
2o
3powder 92.5g, high-purity CaO powder 7g and yellow fluorescent powder Y
3al
5o
12: Ce
3+o.5g the ball grinder of urethane is put into, add 300g zirconium oxide balls and 80g deionized water again, rotating speed ball milling with 300r/min on tumbling ball mill obtains mixture in 15 hours, is then taken out from ball grinder by mixture, then dries 5 hours in 110 DEG C of baking ovens.Powder is taken out and grinds and cross 200 mesh sieves, with 100MPa pressure dry-pressing 3min, then take out base substrate and carry out isostatic cool pressing 5min under 200MPa pressure.By the vacuum sintering at 1580 DEG C of shaping biscuit, soaking time 10 hours, vacuum tightness is 2 × 10
-3pa, then by base substrate in 1650 DEG C, HIP sintering 3 hours under the pressure of 130MPa.The base substrate sintered is annealed 1250 DEG C of insulations for 12 hours, then furnace cooling.Polish, obtain the ceramic plate that thickness is about 1mm after polishing, carry out performance test.Obtained ceramic plate relative density > 99.95%; After in LED component, by test, the color coordinates distribution obtained is concentrated, and dominant wavelength ranges distribution is little, uniform in light emission; By test pin temperature computation junction temperature, the packaged material that the thermal diffusivity of transparent fluorescent ceramic mixes with silica gel significantly better than fluorescent material.
embodiment 3
Take the α-Al that purity is 99.99%
2o
3powder 96.5g, high-purity CaO powder 3g and yellow fluorescent powder Y
3al
5o
12: Ce
3+0.5g puts into the ball grinder of urethane, add 300g zirconium oxide balls and 80g deionized water again, rotating speed ball milling with 300r/min on tumbling ball mill obtains mixture in 15 hours, is then taken out from ball grinder by mixture, then dries 5 hours in 110 DEG C of baking ovens.Powder is taken out and grinds and cross 200 mesh sieves, obtain base substrate with 100MPa pressure dry-pressing 3min, then take out base substrate and carry out isostatic cool pressing 5min under 200MPa pressure.By the vacuum sintering at 1500 DEG C of shaping base substrate, soaking time 10 hours, vacuum tightness is 2 × 10
-3pa, then by base substrate in 1650 DEG C, HIP sintering 3 hours under the pressure of 130MPa.The base substrate sintered is annealed 1250 DEG C of insulations for 12 hours, then furnace cooling.Polish, obtain the ceramic plate that thickness is about 1mm after polishing, carry out performance test.Obtained ceramic plate relative density > 99.95%; After in LED component, by test, the color coordinates distribution obtained is concentrated, and dominant wavelength ranges distribution is little, uniform in light emission; By test pin temperature computation junction temperature, the packaged material that the thermal diffusivity of transparent fluorescent ceramic mixes with silica gel significantly better than fluorescent material.
embodiment 4
Take the α-Al that purity is 99.99%
2o
3powder 88g, high-purity CaO powder 10.8g and yellow fluorescent powder Y
3al
5o
12: Ce
3+1.2g puts into the ball grinder of urethane, add 300g zirconium oxide balls and 80g deionized water again, rotating speed ball milling with 300r/min on tumbling ball mill obtains mixture in 15 hours, is then taken out from ball grinder by mixture, then dries 5 hours in 110 DEG C of baking ovens.Powder is taken out and grinds and cross 200 mesh sieves, obtain base substrate with 100MPa pressure dry-pressing 3min, then take out base substrate and carry out isostatic cool pressing 5min under 200MPa pressure.By the vacuum sintering at 1700 DEG C of shaping base substrate, soaking time 10 hours, vacuum tightness is 2 × 10
-3pa, then by base substrate in 1750 DEG C, HIP sintering 3 hours under the pressure of 130MPa.The biscuit sintered is annealed 1300 DEG C of insulations for 12 hours, then furnace cooling.Polish, obtain the ceramic plate that thickness is about 1mm after polishing, carry out performance test.Obtained ceramic plate relative density > 99.95%; After in LED component, by test, the color coordinates distribution obtained is concentrated, and dominant wavelength ranges distribution is little, uniform in light emission; By test pin temperature computation junction temperature, the packaged material that the thermal diffusivity of transparent fluorescent ceramic mixes with silica gel significantly better than fluorescent material.
embodiment 5
Take the α-Al that purity is 99.99%
2o
3powder 85g, high-purity CaO powder 12.5g and yellow fluorescent powder Y
3al
5o
12: Ce
3+2.5g puts into the ball grinder of urethane, add 300g zirconium oxide balls and 80g deionized water again, rotating speed ball milling with 300r/min on tumbling ball mill obtains mixture in 15 hours, is then taken out from ball grinder by mixture, then dries 5 hours in 110 DEG C of baking ovens.Powder is taken out and grinds and cross 200 mesh sieves, obtain base substrate with 100MPa pressure dry-pressing 3min, then take out base substrate and carry out isostatic cool pressing 5min under 200MPa pressure.By the vacuum sintering at 1600 DEG C of shaping base substrate, soaking time 10 hours, vacuum tightness is 2 × 10
-3pa, then by base substrate in 1680 DEG C, HIP sintering 3 hours under the pressure of 130MPa.The biscuit sintered is annealed 1100 DEG C of insulations for 12 hours, then furnace cooling.Polish, obtain the ceramic plate that thickness is about 1mm after polishing, carry out performance test.Obtained ceramic plate relative density > 99.95%; After in LED component, by test, the color coordinates distribution obtained is concentrated, and dominant wavelength ranges distribution is little, uniform in light emission; By test pin temperature computation junction temperature, the packaged material that the thermal diffusivity of transparent fluorescent ceramic mixes with silica gel significantly better than fluorescent material.
embodiment 6
Take SiC powder 85g, high-purity Ti O that purity is 99.99%
2powder 5g and yellow fluorescent powder Y
3al
5o
12: Ce
3+10g puts into the ball grinder of tetrafluoroethylene, add 300g zirconium oxide balls and 80g deionized water again, rotating speed ball milling with 500r/min on tumbling ball mill obtains mixture in 3 hours, is then taken out from ball grinder by mixture, then dries 10 hours in 90 DEG C of baking ovens.Powder is taken out and grinds and cross 200 mesh sieves, obtain base substrate with 50MPa pressure dry-pressing 10min, then take out base substrate and carry out isostatic cool pressing 15min under 300MPa pressure.By shaping biscuit body vacuum sintering at 1800 DEG C, soaking time 5 hours, vacuum tightness is 1 × 10
-1pa, then by base substrate in 1600 DEG C, HIP sintering 1 hour under the pressure of 180MPa.The base substrate sintered is annealed 1500 DEG C of insulations for 5 hours, then furnace cooling.Polish, obtain the ceramic plate that thickness is about 1mm after polishing, carry out performance test.Obtained ceramic plate relative density > 99.95%; After in LED component, by test, the color coordinates distribution obtained is concentrated, and dominant wavelength ranges distribution is little, uniform in light emission; By test pin temperature computation junction temperature, the packaged material that the thermal diffusivity of transparent fluorescent ceramic mixes with silica gel significantly better than fluorescent material.
embodiment 7
Take the MgAl that purity is 99.99%
2o
4powder 75g, high-purity MnO powder 24.0g and yellow fluorescent powder Y
3al
5o
12: Ce
3+1.0g puts into the ball grinder of high-purity agate, add 300g zirconium oxide balls and 80g deionized water again, rotating speed ball milling with 150r/min on tumbling ball mill obtains mixture in 24 hours, is then taken out from ball grinder by mixture, then dries 6 hours in 120 DEG C of baking ovens.Powder is taken out and grinds and cross 200 mesh sieves, obtain base substrate with 180MPa pressure dry-pressing 0.5min, then take out base substrate and carry out isostatic cool pressing 2min under 350MPa pressure.By the vacuum sintering at 1650 DEG C of shaping base substrate, soaking time 30 hours, vacuum tightness is 1 × 10
-4pa, then by base substrate in 1800 DEG C, HIP sintering 5 hours under the pressure of 120MPa.The base substrate sintered is annealed 800 DEG C of insulations for 40 hours, then furnace cooling.Polish, obtain the ceramic plate that thickness is about 1mm after polishing, carry out performance test.Obtained ceramic plate relative density > 99.95%; After in LED component, by test, the color coordinates distribution obtained is concentrated, and dominant wavelength ranges distribution is little, uniform in light emission; By test pin temperature computation junction temperature, the packaged material that the thermal diffusivity of transparent fluorescent ceramic mixes with silica gel significantly better than fluorescent material.
embodiment 8
Take the Y that purity is 99.99%
2o
3powder 99g, high-purity MgO powder 0.9g and yellow fluorescent powder Y
3al
5o
12: Ce
3+0.1g puts into the ball grinder of urethane, add 300g zirconium oxide balls and 80g deionized water again, rotating speed ball milling with 300r/min on tumbling ball mill obtains mixture in 12 hours, is then taken out from ball grinder by mixture, then dries 8 hours in 105 DEG C of baking ovens.Powder is taken out and grinds and cross 200 mesh sieves, obtain base substrate with 110MPa pressure dry-pressing 5min, then take out base substrate and carry out isostatic cool pressing 10min under 250MPa pressure.By the vacuum sintering at 1600 DEG C of shaping base substrate, soaking time 8 hours, vacuum tightness is 5 × 10
-3pa, then by base substrate in 1700 DEG C, HIP sintering 3 hours under the pressure of 130MPa.The base substrate sintered is annealed 1300 DEG C of insulations for 12 hours, then furnace cooling.Polish, obtain the ceramic plate that thickness is about 1mm after polishing, carry out performance test.Obtained ceramic plate relative density > 99.95%; After in LED component, by test, the color coordinates distribution obtained is concentrated, and dominant wavelength ranges distribution is little, uniform in light emission; By test pin temperature computation junction temperature, the packaged material that the thermal diffusivity of transparent fluorescent ceramic mixes with silica gel significantly better than fluorescent material.
comparative example 1
Take the α-Al that purity is 99.99%
2o
3powder 95g, high-purity CaO powder 3.5g and yellow fluorescent powder Y
3al
5o
12: Ce
3+1.5g puts into the ball grinder of urethane, add 300g zirconium oxide balls and 80g deionized water again, rotating speed ball milling with 300r/min on tumbling ball mill obtains mixture in 15 hours, is then taken out from ball grinder by mixture, then dries 5 hours in 110 DEG C of baking ovens.Powder is taken out and grinds and cross 200 mesh sieves, obtain base substrate with 100MPa pressure dry-pressing 3min, then take out base substrate and carry out isostatic cool pressing 5min under 200MPa pressure.By the vacuum sintering at 1600 DEG C of shaping base substrate, soaking time 10 hours, vacuum tightness is 2 × 10
-3pa.The base substrate sintered is annealed 1300 DEG C of insulations for 12 hours, then furnace cooling.Polish, obtain the ceramic plate that thickness is about 1mm after polishing, carry out performance test.Obtained ceramic plate relative density is 87.50%; After in LED component, by test, uniform in light emission effect comparatively embodiment 1-8 is poor, and pin probe temperature is than the pin probe temperature height 3-5 DEG C in embodiment 1-8, and thermal diffusivity is slightly poor.As can be seen here, all in sintering step, vacuum sintering and HIP sintering is adopted in embodiment 1-8, the relative density of the ceramic plate that comparative example of comparing 1 adopts merely vacuum sintering to obtain is higher, the ceramic plate of therefore high densification for LED component in after can reach that light-emitting uniformity is better, radiating effect better and the higher effect of light emission rate.
Above specific embodiments of the invention are described.It is to be appreciated that the present invention is not limited to above-mentioned particular implementation, those skilled in the art can make various distortion or amendment within the scope of the claims, and this does not affect flesh and blood of the present invention.
Claims (10)
1. a preparation method for LED transparent fluorescent ceramic, is characterized in that, described method comprises the steps:
A, ceramic material powder, sintering aid and fluorescent material to be mixed in proportion; Add in ball grinder, add ball-milling medium, abrading-ball simultaneously, on ball mill, the ball milling regular hour obtains mixture;
B, mixture taken out and dries and grind and sieve;
C, successively dry-pressing formed, cold isostatic compaction is carried out to the powder after sieving and obtain base substrate;
Base substrate shaping in D, step C carries out vacuum sintering, HIP sintering successively;
E, anneal, obtain the fine and close LED transparent fluorescent ceramic of described height.
2. the preparation method of LED transparent fluorescent ceramic according to claim 1, is characterized in that, described ceramic material powder is selected from Al
2o
3, Y
2o
3, MgAl
2o
4, MgAlON, AlN, SiN, ZrO
2, one or more in SiC; Described sintering aid is selected from CaO, MgO, TiO
2, SiO
2, MnO, one or more in kaolin; The composition of described fluorescent material is Y
3al
5o
12: Ce
3+.
3. the preparation method of LED transparent fluorescent ceramic according to claim 1, it is characterized in that, in steps A, the quality proportioning of described ceramic material powder, sintering aid and fluorescent material is: ceramic material powder 75 ~ 99wt%, sintering aid 0.9 ~ 24.9wt%, fluorescent material 0.1 ~ 10wt%.
4. the preparation method of LED transparent fluorescent ceramic according to claim 1, is characterized in that, adopt tumbling ball mill to carry out ball milling, described ball grinder material is the one in urethane, tetrafluoroethylene, high-purity agate; Described abrading-ball is high-purity zirconia Ceramic Balls; Described ball-milling medium is deionized water; The rotating speed of described ball milling is 150 ~ 500r/min, and Ball-milling Time is 3 ~ 24h.
5. the preparation method of LED transparent fluorescent ceramic according to claim 1, is characterized in that, in step B, described bake out temperature is 90 ~ 120 DEG C, and drying time is 5 ~ 10 hours; Described grinding is sieved employing 200 mesh sieve.
6. the preparation method of LED transparent fluorescent ceramic according to claim 1, is characterized in that, in step C, described dry-pressing formed pressure is 50 ~ 180MPa, and the dwell time is 0 ~ 10 minute.
7. the preparation method of LED transparent fluorescent ceramic according to claim 1, is characterized in that, in step C, the pressure of described cold isostatic compaction is 200 ~ 350MPa, and the dwell time is 2 ~ 15 minutes.
8. the preparation method of LED transparent fluorescent ceramic according to claim 1, is characterized in that, in step D, the sintering temperature of described vacuum sintering is 1500 ~ 1800 DEG C, and soaking time is 5 ~ 30 hours, and vacuum tightness is 10
-1~ 10
-4pa.
9. the preparation method of LED transparent fluorescent ceramic according to claim 1, is characterized in that, in step D, the sintering temperature of described HIP sintering is 1600 ~ 1800 DEG C, and soaking time is 1 ~ 5 hour, and pressure is 120 ~ 180MPa.
10. the preparation method of LED transparent fluorescent ceramic according to claim 1, is characterized in that, in step e, described anneal is specially: 800 ~ 1500 DEG C of insulations 5 ~ 40 hours, then furnace cooling.
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| CN115947604A (en) * | 2022-12-14 | 2023-04-11 | 福建臻璟新材料科技有限公司 | Aluminum nitride matrix fluorescent ceramic and preparation method thereof |
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