CN109896851A - Ceramic composite, preparation method and light supply apparatus with concentration gradient - Google Patents
Ceramic composite, preparation method and light supply apparatus with concentration gradient Download PDFInfo
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Abstract
The present invention discloses ceramic composite, preparation method and light supply apparatus with concentration gradient.The ceramic composite at least has upper layer body, middle layer body and lower layer body；The upper layer body is by the luminous phase composition of oxide astigmatism phase, the highly thermally conductive phase of oxide and oxide；The middle layer body is by the luminous phase composition of oxide astigmatism phase, the highly thermally conductive phase of oxide and oxide；The lower layer body is shone phase composition by the highly thermally conductive phase of oxide and oxide, or is shone phase composition by oxide astigmatism phase, the highly thermally conductive phase of oxide and oxide.The beneficial effects of the present invention are: high temperature fluorescence intensity is improved, and adjustable control is emitted fluorescence uniformity.
Description
Technical field
The present invention relates to laser lighting light source fields, in particular, ceramic composite, preparation method with concentration gradient
And light supply apparatus.
Background technique
Laser diode has the characteristics that photoelectric efficiency is high, brightness is high, collimation is high, irradiation distance is remote, size is small.With halogen
For plain lamp compared with xenon lamp, laser lighting light source has the advantages that the service life is long, efficiency is high, more low-carbon.Compared with LED light source, laser
Lighting source is high with brightness, irradiation distance is farther, shape-designing is flexible, design freedom is high, cooling system is simpler excellent
Point.It is only applicable to middle low-light level field relative to LED light product-derived, laser light source then can be adapted for the demand of all brightness,
Especially there is unrivaled advantage in fields such as highlighted, high photosynthetic efficiency, high directivities.
In view of the limitation of red, green, blue laser luminous efficiency and operating temperature, the white light laser of mainstream currently on the market
Lighting source is to use for reference white light LEDs light distribution principle, that is, using the blue laser of 450nm or so as excitation light source, yttroalumite
Garnet and nitric oxide fluorescent powder, fluorescence ceramics or monocrystal are then preferred laser lighting fluorescent materials.Wherein, fluorescence is made pottery
Porcelain is favored due to optical property is excellent, achievable RE high-concentration dopant, packaged type are conducive to advantages such as heat dissipations by Lighting Industry.
The blue light optical power density that fluorescent material relative to white LED light source is subjected to when working is most of in 1W/mm2With
Under, maximum is no more than 5W/mm2, and (the exposed spot size of such as Nichia-4.5W is about 1.5mm* to single laser diode
Optical power density 0.5mm) is about 1.5W/mm2, laser lighting light source would generally be total using more lasers in practical applications
It is same to converge to fluorescent material surface, that is, the blue light irradiance power density of laser lighting receiving required for fluorescent material is white light
Even hundred times or more of ten times of LED illumination.This allows for laser lighting and needs to have superpower resistance to blue light irradiation with fluorescent material
Ability, excellent temperature quenching feature and superior thermal impact.And currently, the effect of fluorescent material on the market is undesirable.
Summary of the invention
The technical problem to be solved in the present invention is to provide excellent high temperature fluorescent characteristic, provide a kind of with concentration gradient
Ceramic composite.
The technical issues of present invention further solves is that astigmatism design concept is added, mixed to mitigate subsequent secondary formula
The burden of light provides a kind of ceramic composite with concentration gradient.
In order to realize the purpose, technical scheme is as follows: the ceramic composite with concentration gradient, the pottery
Porcelain complex at least has upper layer body, middle layer body and lower layer body；
The upper layer body is by the luminous phase composition of oxide astigmatism phase, the highly thermally conductive phase of oxide and oxide；
The middle layer body is by the luminous phase composition of oxide astigmatism phase, the highly thermally conductive phase of oxide and oxide；
The lower layer body is shone phase composition by the highly thermally conductive phase of oxide and oxide, or high by oxide astigmatism phase, oxide
Thermal conductivity phase and the luminous phase composition of oxide；
Oxide astigmatism phase, the volume fraction of the oxide astigmatism phase of the middle layer body of the upper layer body are gradually increased；
The highly thermally conductive phase of oxide of the upper layer body, the highly thermally conductive phase of oxide of the middle layer body, the lower layer body
The volume fraction of the highly thermally conductive phase of oxide is gradually increased；
The luminous phase of the oxide of the upper upper layer body, the oxide luminous phase, the lower layer body of the middle layer body
Oxide shine phase volume fraction be gradually reduced.
As the preferred embodiment of the ceramic composite with concentration gradient, the oxide astigmatism mutually selects Y2O3、La2O3
Equal lanthanide rare earth oxides, TeO2、ZrO2、TiO2、ZnO、Nb2O5、Ta2O5、HfO2One of or it is a variety of, it is further, described
The crystallite dimension of oxide astigmatism phase is less than 1000nm, further, the crystallite dimension of the oxide astigmatism phase is 50~
800nm。
As the preferred embodiment of the ceramic composite with concentration gradient, the highly thermally conductive phase of oxide selects Al2O3、
Bi2O3、Cr2O3、MnO2、Sb2O3、Co2O3、TiO2、Ag2O's is one or more, further, the highly thermally conductive phase of oxide
Crystallite dimension is less than 2000nm, and further, the crystallite dimension of the highly thermally conductive phase of oxide is 50~500nm.
As the preferred embodiment of the ceramic composite with concentration gradient, it is mutually garnet structure that the oxide, which shines,
General formula is expressed as (Y1-x-yREyCex)3(Al1-zMz)5O12, wherein one of RE Lu, Tb, Gd, La, Pr, Eu, Sm or more
Kind, one of M Ga, Cr, Si, Sr, Mn, Sc, Ti, V or a variety of, 0.0001≤x≤0.05,0≤y≤0.5,0.0001≤
z≤0.5。
As the preferred embodiment of the ceramic composite with concentration gradient, in the upper layer body, oxide shines in phase
Ce doping content is 0.05~5.0at%, and further, Ce doping content is 0.3~2.0at% in the luminous phase of oxide；It is described
In middle layer body, Ce doping content is 0.01~3.0at% in the luminous phase of oxide, and further, Ce mixes in the luminous phase of oxide
Miscellaneous content is 0.1~1.0at%.
As the preferred embodiment of the ceramic composite with concentration gradient, in the upper layer body, oxide astigmatism phase
Volume fraction 5~20%, the volume fraction 5~20% of the highly thermally conductive phase of oxide, the volume fraction 70~90% of the luminous phase of oxide,
Three adds up to 100%；In the middle layer body, the volume fraction 10~30% of oxide astigmatism phase, the highly thermally conductive phase of oxide
The volume fraction 20~70% of the luminous phase of volume fraction 20~70%, oxide, three adds up to 100%；In the lower layer body,
The volume fraction 0~10% of oxide astigmatism phase, the volume fraction 70~99.99% of the highly thermally conductive phase of oxide, oxide shine phase
Volume fraction 0.01~20%, three adds up to 100%.
The present invention also provides the preparation methods of the ceramic composite with concentration gradient to ceramic composite includes
Following steps,
Step S1 successively forms the lower layer body, the middle layer body and the upper layer body, forms ceramic body；
Step S2 is sintered the ceramic body: using vacuum sintering furnace sintering, vacuum sintering furnace and hot isostatic pressing furnace two-step sintering
Or normal pressure atmosphere sintering；Further, during vacuum sintering furnace is sintered with normal pressure atmosphere sintering, increase week reduction gas
Atmosphere, weakly reducing atmosphere H2-N2Or H2- Ar, wherein H2Content be≤4%；
Step S3, the ceramic body of annealing: under air atmosphere or weakly reducing atmosphere, annealing temperature is 1300~1600 DEG C,
Annealing soaking time is 1~50h；Further, annealing temperature is 1400~1500 DEG C, and annealing soaking time is 10~40h；With
And
Step S4, grinding are thinned the ceramic body, obtain the ceramic composite.
The preferred embodiment of preparation method as the ceramic composite with concentration gradient, in step S2,
Vacuum sintering furnace sintering: sintered heat insulating temperature is 1680~1820 DEG C, and the sintered heat insulating time is 1~30h；Further,
Sintered heat insulating temperature is 1720~1780 DEG C, and the sintered heat insulating time is 5~15h；
Vacuum sintering furnace and hot isostatic pressing furnace two-step sintering: the first step is first sintered in vacuum sintering furnace, vacuum degree 10-2~10- 4Pa, sintered heat insulating temperature are 1700~1800 DEG C, and the sintered heat insulating time is 1~10h, and further, sintered heat insulating temperature is
1720~1760 DEG C, the sintered heat insulating time is 3~6h；Ceramic block obtained by the first step is put into hot isostatic pressing furnace by second step to be burnt
Knot, pressure are 150~200MPa, and sintered heat insulating temperature is 1600~1700 DEG C, and the sintered heat insulating time is 1~10h, further
Ground, sintered heat insulating temperature are 1620~1680 DEG C, and the sintered heat insulating time is 3~6h；
Normal pressure atmosphere sintering: sintered heat insulating temperature is 1650~1800 DEG C, and the sintered heat insulating time is 1~20h；Further, it burns
Tying holding temperature is 1750~1780 DEG C, and the sintered heat insulating time is 3~6h.
The preferred embodiment of preparation method as the ceramic composite with concentration gradient, step S1 include,
Step S11, weigh each layer of corresponding raw material of body: starting material can be oxide, be also possible to shine phase (Y,
Ce)3Al5O12The material powder of chemical coprecipitation technique synthesis also can be used in fluorescent powder and other oxides；
Step S12 weighs each layer of corresponding sintering aid of body: Li+, Ca2+/Mg2+/Ba2+, La3+/Y3+, TEOS/SiO2, gold
Belonging to ion can be the salt in the form of oxide, carbonate, fluoride etc.；
Raw material, sintering aid and decentralized medium needed for each layer of body are made into slurry with dehydrated alcohol respectively by step S13,
It is put into Al2O35~20h of ball milling in ball grinder, wherein the mass ratio of raw material, abrading-ball and decentralized medium is 1:3:0.5；
Step S14, by the good slurry of ball milling through tape casting, drying, lamination, then tabletting and cold isostatic compaction；Alternatively, first
By the good slurry drying and screening of ball milling, it is then sequentially placed into the layer-by-layer dry-pressing of mold, then apply 100~250Mpa cold isostatic compaction
Biscuit is made；And
Biscuit is put into 600~800 DEG C of pre-burning in Muffle furnace, keeps the temperature 2~4h, obtain the ceramic body by step S15.
The present invention also provides light supply apparatus, include,
Blue light excitation light source；And
Blue light anti-reflection film is plated in the top surface of foregoing ceramic complex, the ceramic composite, and the bottom surface of the ceramic composite is silver-plated,
The bottom surface of the ceramic composite is welded on copper cooling base；
The blue light excitation light source is collimated, focus after be irradiated to the top surface of the ceramic composite and be converted to yellow light, it is remaining blue
Light is mixed with the yellow light of transmitting obtains equal white light.
Compared with prior art, beneficial effects of the present invention at least that: it is mutually equal due to fluorescing in ceramic composite
Even distribution simultaneously contains scattering particles, available uniform yellow fluorescence.Due to being ceramic composite and containing high heat conductance phase,
With excellent heat resistance.In addition, since its own is block, so It is not necessary to addition tree in the composition of white light emitting device
Rouge can control fluorescence intensity and mixed quality white light according to luminous phase content and Ce doping content and ceramic thickness.Therefore, contain
There is the white light emitting device uniform in light emission of the composite ceramic body, and is particularly suitable for high output.
In addition to it is described above present invention solves the technical problem that, constitute technical solution technical characteristic and by these
Except beneficial effect brought by the technical characteristic of technical solution, other technologies problem, technical solution that the present invention can solve
In include other technical characteristics and these technical characteristic bring beneficial effects, will be made in conjunction with attached drawing further details of
Explanation.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of ceramic composite of the invention.
Fig. 2 is high temperature fluorescence characteristic of the invention.
Fig. 3 is the luminous device structure schematic diagram (transmission-type) of laser lighting of the invention.
Fig. 4 is the luminous device structure schematic diagram (reflective) of laser lighting of the invention.
Specific embodiment
Below by specific embodiment combination attached drawing, invention is further described in detail.It needs to illustrate herein
It is the explanation of these embodiments to be used to help to understand the present invention, but do not constitute a limitation of the invention.In addition, below
Involved technical characteristic as long as they do not conflict with each other can phase in the described each embodiment of the present invention
Mutually combination.
Comparative example 1:
Using high-purity yttrium oxide (Y2O3), aluminium oxide (Al2O3), cerium oxide (CeO2) it is raw material, with magnesia (MgO) and positive silicon
Acetoacetic ester (TEOS) is used as sintering aid.Magnesia (MgO) additive amount is mass fraction 0.1%, and ethyl orthosilicate (TEOS) adds
Dosage is mass fraction 0.6%.According to (Y0.995Ce0.005)3Al5O12Stoichiometric ratio has configured powder material, then with anhydrous second
Alcohol be ball-milling medium and be put into alumina balls grinding jar carry out wet ball grinding prepare ceramic powder, powder is through drying, sieving, tabletting；
200MPa isostatic cool pressing is imposed to it again and forms green body, ceramic body is put into vacuum sintering furnace after 700 DEG C of heat preservation 4h pre-burnings
In in 1750 DEG C of vacuum degrees 10-3It is sintered under the conditions of Pa 8 hours, is finally obtained in Muffle furnace through 1450 DEG C of annealing 20h
(Y0.995Ce0.005)3Al5O12Fluorescence ceramics carry out obtained ceramic material to cut throwing working process, and obtaining diameter is 12mm
With a thickness of the white-light illuminating complex phase fluorescence ceramics of 0.5mm.
Embodiment 1:
Upper layer body (that is, light-emitting surface) contains (Y0.995Ce0.005)3Al5O12Volume fraction 80%, Y2O3Volume fraction 10%, Al2O3Body
Fraction 10%, diameter 12mm, with a thickness of 1mm.Middle layer body contains (Y0.99Ce0.01)3Al5O12Volume fraction 50%, Y2O3Volume
Score 15%, Al2O3Volume fraction 35%, diameter 12mm, with a thickness of 0.3mm.Lower layer body contains (Y0.99Ce0.01)3Al5O12Volume
Score 10%, Al2O3Volume fraction 90%, diameter 12mm, with a thickness of 1mm.Corresponding stratiform is weighed respectively according to above-mentioned concentration gradient
Starting oxides and sintering aid needed for structure (with comparative example 1) are respectively that medium will slurry after ball mill mixing with dehydrated alcohol
Expect drying and screening, every layer of raw material is sequentially placed into the layer-by-layer dry-pressing of mold, then apply 200Mpa cold isostatic compaction and biscuit is made, pressed
Ceramic body is made according to the ceramic sintering process in comparative example 1, then same thickness is thinned in two-sided grind respectively of ceramic body
Obtaining diameter is 12mm, with a thickness of the complex phase fluorescence ceramics of 0.5mm.
Embodiment 2:
Upper layer body (that is, light-emitting surface) contains (Y0.995Ce0.005)3Al5O12Volume fraction 80%, Y2O3Volume fraction 10%, Al2O3Body
Fraction 10%, diameter 12mm, with a thickness of 0.5mm.Middle layer body contains (Y0.99Ce0.01)3Al5O12Volume fraction 50%, Y2O3Body
Fraction 15%, Al2O3Volume fraction 35%, diameter 12mm, with a thickness of 0.1mm.Lower layer body contains (Y0.99Ce0.01)3Al5O12Body
Fraction 10%, Al2O3Volume fraction 90%, diameter 12mm, with a thickness of 0.5mm.It is weighed respectively accordingly according to above-mentioned concentration gradient
Starting oxides and sintering aid needed for layer structure (with comparative example 1) and bridging agent, plasticizer, dispersing agent, dehydrated alcohol
Slurry is made through ball mill mixing in equal additives, is implanted sequentially in casting machine after froth in vacuum and carries out tape casting, by the stream
Prolong piece and biscuit is made through drying, lamination, dry-pressing formed, isostatic cool pressing.Ceramic body is put into true after 800 DEG C of heat preservation 4h pre-burnings
In 1800 DEG C of vacuum degrees 10 in empty sintering furnace-3It is sintered 2 hours under the conditions of Pa, is cooled to 1720 DEG C and keeps the temperature 10 hours, then in horse
Not through 1450 DEG C of annealing 20h in furnace.Finally the two-sided grinding respectively of ceramic body is thinned same thickness to obtain diameter is 12mm,
With a thickness of the complex phase fluorescence ceramics of 0.5mm.
Embodiment 3:
Upper layer body (that is, light-emitting surface) contains (Y0.99Ce0.01)3Al5O12Volume fraction 85%, La2O3Volume fraction 10%, Al2O3Body
Fraction 5%, diameter are 12mm with a thickness of 0.6mm.Middle layer body contains (Y0.99Ce0.01)3Al5O12Volume fraction 40%, La2O3Volume
Score 20%, Al2O3Volume fraction 40%, diameter are 12mm with a thickness of 0.1mm.Lower layer body contains (Y0.99Ce0.01)3Al5O12Volume
Score 5%, Al2O3Volume fraction 95%, diameter 12mm, with a thickness of 0.4mm.Equivalent layer is weighed respectively according to above-mentioned concentration gradient
Starting oxides needed for shape structure and sintering aid (with comparative example 1) and bridging agent, plasticizer, dispersing agent, dehydrated alcohol etc.
Slurry is made through ball mill mixing in additive, is implanted sequentially in casting machine after froth in vacuum and carries out tape casting, by the curtain coating
Biscuit is made through drying, lamination, dry-pressing formed, isostatic cool pressing in piece.Ceramic body is put into vacuum after 800 DEG C of heat preservation 4h pre-burnings
In 1750 DEG C of vacuum degrees 10 in sintering furnace-3Be sintered 5 hours under the conditions of Pa, be then placed in hot isostatic pressing furnace through 1650 DEG C and
It is sintered 5 hours under the conditions of 200MPa, then gained ceramic body is put into Muffle furnace through 1450 DEG C of annealing 20h.It finally will be ceramic
It is 12mm that the two-sided grinding respectively of green body, which is thinned same thickness to obtain diameter, with a thickness of the complex phase fluorescence ceramics of 0.5mm.
As seen from Figure 2, embodiment 1, embodiment 2 and embodiment 3 are better than comparative example, and high temperature fluorescent characteristic obtains obviously
It is promoted.And embodiment 3 is substantially better than embodiment 1 and embodiment 2.
Light supply apparatus schematic diagram containing the ceramic composite refers to Fig. 3 to 4, can be by transmission-type or reflective
Optical path realizes white-light illuminating.Using single or more lasers 1 as excitation light source, filled through the collimation of lens 2, pack and even light
Set and expose to the 4 upper layer body of ceramic composite after 3 even light, the ceramic composite by excitation light source wavelength 6 be converted to yellow light or
Orange light, remaining blue light mix with potsherd transmitting light and obtain equal white light 7 of high brightness.The bottom surface of lower layer body is silver-plated and welds
In copper cooling base 5.The ceramic composite has excellent thermal shock resistance and even light ability, particularly suitable for big function
Rate laser lighting.
Embodiments of the present invention are only expressed above, and the description thereof is more specific and detailed, but and cannot therefore understand
For the limitation to patent of invention range.It should be pointed out that for those of ordinary skill in the art, not departing from this hair
Under the premise of bright design, various modifications and improvements can be made, and these are all within the scope of protection of the present invention.Therefore, this hair
The scope of protection shall be subject to the appended claims for bright patent.
Claims (10)
1. the ceramic composite with concentration gradient, which is characterized in that the ceramic composite at least has upper layer body, centre
Layer body and lower layer body；
The upper layer body is by the luminous phase composition of oxide astigmatism phase, the highly thermally conductive phase of oxide and oxide；
The middle layer body is by the luminous phase composition of oxide astigmatism phase, the highly thermally conductive phase of oxide and oxide；
The lower layer body is shone phase composition by the highly thermally conductive phase of oxide and oxide, or high by oxide astigmatism phase, oxide
Thermal conductivity phase and the luminous phase composition of oxide；
Oxide astigmatism phase, the volume fraction of the oxide astigmatism phase of the middle layer body of the upper layer body are gradually increased；
The highly thermally conductive phase of oxide of the upper layer body, the highly thermally conductive phase of oxide of the middle layer body, the lower layer body
The volume fraction of the highly thermally conductive phase of oxide is gradually increased；
The luminous phase of the oxide of the upper upper layer body, the oxide luminous phase, the lower layer body of the middle layer body
Oxide shine phase volume fraction be gradually reduced.
2. the ceramic composite according to claim 1 with concentration gradient, which is characterized in that the oxide astigmatism phase
Select Y2O3、La2O3Equal lanthanide rare earth oxides, TeO2、ZrO2、TiO2、ZnO、Nb2O5、Ta2O5、HfO2One of or it is a variety of,
Further, the crystallite dimension of the oxide astigmatism phase is less than 1000nm, further, the crystalline substance of the oxide astigmatism phase
Particle size is 50~800nm.
3. the ceramic composite according to claim 1 with concentration gradient, which is characterized in that the oxide is highly thermally conductive
Mutually select Al2O3、Bi2O3、Cr2O3、MnO2、Sb2O3、Co2O3、TiO2、Ag2O's is one or more, further, the oxidation
The crystallite dimension of the highly thermally conductive phase of object is less than 2000nm, further, the crystallite dimension of the highly thermally conductive phase of oxide is 50~
500nm。
4. the ceramic composite according to claim 1 with concentration gradient, which is characterized in that the oxide shines phase
For garnet structure, general formula is expressed as (Y1-x-yREyCex)3(Al1-zMz)5O12, wherein RE Lu, Tb, Gd, La, Pr, Eu, Sm
One of or a variety of, one of M Ga, Cr, Si, Sr, Mn, Sc, Ti, V or a variety of, 0.0001≤x≤0.05,0≤y≤
0.5,0.0001≤z≤0.5.
5. the ceramic composite according to claim 4 with concentration gradient, which is characterized in that in the upper layer body,
Ce doping content is 0.05~5.0at% in the luminous phase of oxide, and further, Ce doping content is 0.3 in the luminous phase of oxide
~2.0at%；In the middle layer body, Ce doping content is 0.01~3.0at% in the luminous phase of oxide, further, oxidation
Ce doping content is 0.1~1.0at% in the luminous phase of object.
6. the ceramic composite as claimed in any of claims 1 to 5 with concentration gradient, which is characterized in that institute
It states in upper layer body, the volume fraction 5~20% of oxide astigmatism phase, the volume fraction 5~20% of the highly thermally conductive phase of oxide, aoxidizes
The volume fraction 70~90% of the luminous phase of object；In the middle layer body, the volume fraction 10~30% of oxide astigmatism phase, oxide
The volume fraction 20~70% of the luminous phase of the volume fraction 20~70% of highly thermally conductive phase, oxide；In the lower layer body, oxide
The volume fraction 0~10% of astigmatism phase, the volume fraction 70~99.99% of the highly thermally conductive phase of oxide, the volume of the luminous phase of oxide
Score 0.01~20%.
7. the preparation method of the ceramic composite with concentration gradient, to prepare described in any one of claim 1 to 6
Ceramic composite, which is characterized in that it include following steps,
Step S1 successively forms the lower layer body, the middle layer body and the upper layer body, forms ceramic body；
Step S2 is sintered the ceramic body: being burnt using vacuum sintering furnace sintering, vacuum sintering furnace and two step of hot isostatic pressing furnace
Knot or normal pressure atmosphere sintering；Further, during vacuum sintering furnace is sintered with normal pressure atmosphere sintering, increase week reduction
Atmosphere, weakly reducing atmosphere H2-N2Or H2- Ar, wherein H2Content be≤4%；
Step S3, the ceramic body of annealing: under air atmosphere or weakly reducing atmosphere, annealing temperature is 1300~1600 DEG C,
Annealing soaking time is 1~50h；Further, annealing temperature is 1400~1500 DEG C, and annealing soaking time is 10~40h；With
And
Step S4, grinding are thinned the ceramic body, obtain the ceramic composite.
8. the preparation method of the ceramic composite according to claim 7 with concentration gradient, which is characterized in that step S2
In,
Vacuum sintering furnace sintering: sintered heat insulating temperature is 1680~1820 DEG C, and the sintered heat insulating time is 1~30h；Further,
Sintered heat insulating temperature is 1720~1780 DEG C, and the sintered heat insulating time is 5~15h；
Vacuum sintering furnace and hot isostatic pressing furnace two-step sintering: the first step is first sintered in vacuum sintering furnace, vacuum degree 10-2~
10-4Pa, holding temperature are 1700~1800 DEG C, and the sintered heat insulating time is 1~10h, and further, sintered heat insulating temperature is 1720
~1760 DEG C, the sintered heat insulating time is 3~6h；Ceramic block obtained by the first step is put into hot isostatic pressing furnace and is sintered by second step,
Pressure is 150~200MPa, and holding temperature is 1600~1700 DEG C, and the sintered heat insulating time is 1~10h, and further, sintering is protected
Temperature is 1620~1680 DEG C, and the sintered heat insulating time is 3~6h；
Normal pressure atmosphere sintering: sintered heat insulating temperature is 1650~1800 DEG C, and the sintered heat insulating time is 1~20h；Further, it burns
Tying holding temperature is 1750~1780 DEG C, and the sintered heat insulating time is 3~6h.
9. the preparation method of the ceramic composite according to claim 7 with concentration gradient, which is characterized in that step S1
Include,
Step S11 weighs each layer of corresponding raw material of body；
Step S12 weighs each layer of corresponding sintering aid of body；
Raw material, sintering aid and decentralized medium needed for each layer of body are made into slurry with dehydrated alcohol respectively by step S13,
It is put into Al2O35~20h of ball milling in ball grinder, wherein the mass ratio of raw material, abrading-ball and decentralized medium is 1:3:0.5；
Step S14, by the good slurry of ball milling through tape casting, drying, lamination, then tabletting and cold isostatic compaction；Alternatively, first
By the good slurry drying and screening of ball milling, it is then sequentially placed into the layer-by-layer dry-pressing of mold, then apply 100~250Mpa cold isostatic compaction
Biscuit is made；And
Biscuit is put into 600~800 DEG C of pre-burning in Muffle furnace, keeps the temperature 2~4h, obtain the ceramic body by step S15.
10. light supply apparatus, which is characterized in that include,
Blue light excitation light source；And
The top surface plating blue light of ceramic composite described in any one of claim 1 to 9, the ceramic composite is anti-reflection
The bottom surface of film, the ceramic composite is silver-plated, and the bottom surface of the ceramic composite is welded on copper cooling base；
The blue light excitation light source is collimated, focus after be irradiated to the top surface of the ceramic composite and be converted to yellow light, it is remaining blue
Light is mixed with the yellow light of transmitting obtains equal white light.
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| CN112174647A (en) * | 2019-07-04 | 2021-01-05 | 上海航空电器有限公司 | Low-temperature co-fired fluorescent ceramic composite for white light illumination, preparation method and light source device |
| CN113024242A (en) * | 2019-12-09 | 2021-06-25 | 上海航空电器有限公司 | Superfine ceramic phosphor for obtaining high lumen laser illumination and preparation method thereof |
| WO2022199623A1 (en) * | 2021-03-24 | 2022-09-29 | 中国科学院福建物质结构研究所 | Enhanced single-matrix ceramic phosphor for white light led, preparation method therefor, and application thereof |
| CN115490508A (en) * | 2022-10-12 | 2022-12-20 | 中国科学院上海光学精密机械研究所 | Composite fluorescent ceramic for white light LD illumination and preparation method thereof |
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