CN110294627A - Luminescent ceramic and preparation method thereof - Google Patents
Luminescent ceramic and preparation method thereof Download PDFInfo
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- CN110294627A CN110294627A CN201810235684.1A CN201810235684A CN110294627A CN 110294627 A CN110294627 A CN 110294627A CN 201810235684 A CN201810235684 A CN 201810235684A CN 110294627 A CN110294627 A CN 110294627A
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Abstract
A kind of luminescent ceramic, the luminescent ceramic include MgOnAl2O3Matrix (210) and it is evenly distributed on MgOnAl2O3The Nd:YAG centre of luminescence (220) in matrix, wherein MgOnAl2O3Matrix is one-component ceramic, Al2O3Molar ratio with MgO is 1:n, n 0.7-2.The present invention prepares Nd:YAG precursor powder by urea coprecipitation method, prepares MgOnAl by solid reaction process2O3Precursor powder is prepared into Nd:YAG-MgOnAl finally by hot pressing sintering method2O3Luminescent ceramic；Using Nd:YAG as infraluminescence center, with high quantum efficiency；And MgOnAl2O3Prepared crystalline ceramics is higher in infrared band transmitance, and has more excellent thermal conductivity；When it collectively constitutes composite ceramics with Nd:YAG, infrared light scattering caused by Nd:YAG can be come out well, and simultaneously by 808nm laser excitation when generated heat carry out conduction and distribute, have many advantages, such as that high brightness, dim light decline.
Description
Technical field
The present invention relates to a kind of luminescent ceramics and preparation method thereof, belong to solid luminescent material manufacturing technology field.
Background technique
In recent years, increasing to the demand of night monitoring, skill is imaged from low-illuminance cameras to active infrared now
Art is for solving this demand.Wherein active infrared photography technology can be very good to realize round-the-clock, timeless
Monitoring.Thermal camera in active infrared photography technology is the video camera for having installed infrared filter and infrared light supply additional.As red
There are mainly three types of the infrared light supplies of outer video camera important component: first is that by installing visible light on halogen lamp or xenon lamp
Filter and obtain infrared light, there is very big deficiency in this infrared light supply that is excited in a manner of heat radiation, be such as easy comprising visible
Light has red sudden and violent phenomenon, and service life is short, and heat production is serious etc., at present replaced other infrared light supplies；Second is that by infrared
LED or infrared LED-Array generates infrared light, and infrared LED compares halogen lamp as a kind of injection electroluminescence device
Or for xenon lamp, there is that small in size, the service life is long, low in energy consumption, high reliability, it is made to be used widely, but exists and shine
The deficiencies of prescribed distance is short, brightness of illumination is low and light decay is serious；Third is that infrared light supply is used as using infra-red laser diode (LD),
Infrared LD light source although there is the features such as high brightness, there is at high cost, beam angle is small, speckle, energy concentrate the problems such as.
It can be seen from the above, the demand ten of the infrared light supply to decline on the market for high brightness, high uniformity, long-life, dim light
Divide urgent.
Summary of the invention
Technical problem to be solved by the present invention lies in view of the deficiencies of the prior art, provide a kind of luminescent ceramic and its system
Preparation Method prepares Nd:YAG precursor powder by urea coprecipitation method, prepares MgOnAl by solid reaction process2O3Front axle shell
Body is prepared into Nd:YAG-MgOnAl finally by hot pressing sintering method2O3Luminescent ceramic；Using Nd:YAG as in infraluminescence
The heart, with high quantum efficiency；And MgOnAl2O3Prepared crystalline ceramics is higher in infrared band transmitance, and has
There is more excellent thermal conductivity；It, can be well by infrared light caused by Nd:YAG when it collectively constitutes composite ceramics with Nd:YAG
Scatter out, and simultaneously by 808nm laser excitation when generated heat carry out conduction and distribute, there is high brightness, dim light to decline
Advantage.
The technical problem to be solved by the present invention is to what is be achieved through the following technical solutions:
The present invention provides a kind of luminescent ceramic, and the luminescent ceramic includes MgOnAl2O3It matrix and is evenly distributed on
MgO·nAl2O3The Nd:YAG centre of luminescence in matrix, wherein MgOnAl2O3Matrix is one-component ceramic, Al2O3With rubbing for MgO
You are than being 1:n, n 0.7-2.
Preferably, the n is 0.9-1.3.
Preferably, the MgOnAl2O3Size of microcrystal be 0.5 μm -10 μm, the size of microcrystal of the Nd:YAG is 1 μ
m-20μm.Further, the MgOnAl2O3Size of microcrystal be 1 μm -5 μm, the size of microcrystal of the Nd:YAG is 5 μm -
10μm。
Preferably, the Nd:YAG centre of luminescence accounts for 30wt%~80wt% of the luminescent ceramic gross mass.
The present invention also provides a kind of preparation method of luminescent ceramic, the preparation method includes:
S1: preparation Nd:YAG precursor powder；
S2: preparation MgOnAl2O3Precursor powder；
S3: mixing Nd:YAG precursor powder and MgOnAl2O3Precursor powder obtains luminescent ceramic powder；
S4: being molding biscuit by luminescent ceramic pressed by powder；
S5: being sintered and makes annealing treatment the biscuit, obtains luminescent ceramic.
Preferably, in S1, stoichiometrically: Al3+Y (NO is weighed for 3:53)3·6H2O and Nd (NO3)3·6H2O,
It is added in aluminum nitrate solution, pH value of solution is adjusted to 2-3 after stirring and filtering, solution is heated after mixing evenly, makes gold
Belong to ion precipitation, will be calcined after gained precipitating drying, obtain Nd:YAG precursor powder.Wherein, the Nd3+Additive amount account for Nd3+
And Y3+The 0.2at%-2at% of total amount of adding.
Preferably, in S2, by Al2O3Powder, MgO powder are calcined after mixing in proportion, by calcined powder and ball milling
Medium carries out ball milling, finally obtains MgOnAl by drying2O3Precursor powder.
Preferably, the Al2O3The average grain diameter of powder and MgO powder is 0.05 μm -1 μm, the Al2O3Powder and MgO
The molar ratio of powder is 1:n, n 0.7-2, the MgOnAl2O3Precursor powder average grain diameter is 0.1 μm -10 μm.
Preferably, in S3, by Nd:YAG precursor powder, MgOnAl2O3Precursor powder is done after mixing with sintering aid
It is dry, it is ground up, sieved processing later and obtains luminescent ceramic powder.
Preferably, the sintering aid is one of lithium fluoride, calcirm-fluoride, tetraethyl orthosilicate or a variety of, is averaged
Partial size is 0.05 μm -1 μm, accounts for the 0.01wt%-1wt% of luminescent ceramic powder gross mass.
Preferably, bonding agent can be also added in S3 to be mixed, the binder is the ethyl alcohol of polyvinyl butyral
Solution.
Preferably, the quality of the Nd:YAG precursor powder accounts for the 30wt%-80wt% of luminescent ceramic powder gross mass.
In conclusion the present invention prepares Nd:YAG precursor powder by urea coprecipitation method, prepared by solid reaction process
MgO·nAl2O3Precursor powder is prepared into Nd:YAG-MgOnAl finally by hot pressing sintering method2O3Luminescent ceramic；Utilize Nd:
YAG is as infraluminescence center, with high quantum efficiency；And MgOnAl2O3Prepared crystalline ceramics is in infrared waves
Section transmitance is higher, and has more excellent thermal conductivity；It, can be well by Nd when it collectively constitutes composite ceramics with Nd:YAG:
Infrared light scattering caused by YAG comes out, and simultaneously by 808nm laser excitation when generated heat carry out conduction and distribute, have
Have the advantages that high brightness, dim light decline.
In the following with reference to the drawings and specific embodiments, technical solution of the present invention is described in detail.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of luminescent ceramic of the present invention；
Fig. 2 is launching light spectrogram of the luminescent ceramic of the present invention under 808nm laser excitation.
Specific embodiment
Fig. 1 is the structural schematic diagram of luminescent ceramic of the present invention.As shown in Figure 1, the present invention provides a kind of luminescent ceramic, it is described
Luminescent ceramic includes MgOnAl2O3Matrix 210 and it is evenly distributed on MgOnAl2O3Nd:YAG in matrix 210
(Neodymium-doped Yttrium Aluminium Garnet) centre of luminescence 220.Wherein, MgOnAl2O3Matrix 210
Middle Al2O3Molar ratio with MgO is 1:n, n 0.7-2, preferably 0.9-1.3.
Wherein, the MgOnAl2O3Size of microcrystal be 0.5 μm -10 μm, the size of microcrystal of the Nd:YAG is 1 μm -
20μm.Preferably, the MgOnAl2O3Size of microcrystal be 1 μm -5 μm, the size of microcrystal of the Nd:YAG is 5 μm -10 μm.
White continuous phase in Fig. 1 is MgOnAl2O3Matrix 210, black particle are the Nd:YAG centre of luminescence 220.Fig. 2
For launching light spectrogram of the luminescent ceramic of the present invention under 808nm laser excitation.As shown in Fig. 2, the luminescent ceramic is in wavelength
When 808nm laser diode makees excitation light source, the infrared light of 850nm-1350nm wavelength can be inspired, wherein with 1050nm-
1080nm wavelength excitation peak is most strong.
Current existing Nd:YAG ceramics either single-crystal ceramic or polycrystalline ceramics are excited in the light of 808nm wavelength
When, only ceramic surface portion crystal is excited, because of the influence of the Multiple factors such as its material and crystal structure attribute, so that
For the Nd:YAG of pure phase ceramics, exciting light by crystal boundary can be directed through and it is less reflect so that exciting light is in ceramics
The middle chance reflected is less to which light path is short, and then excites the light quantity of Nd:YAG few, and the light efficiency of exciting light is not high, generates simultaneously
Stimulated light it is also few.Meanwhile the thermal conductivity of Nd:YAG is not high, the Nd:YAG ceramics of pure phase are excited and the generated heat that shines
It cannot conduct and distribute in time, will lead to ceramic temperature and rise, the heat for easily causing Nd:YAG ceramics declines and reduces light conversion
Efficiency.
The present invention uses the centre of luminescence of the Nd:YAG ceramic particle as luminescent ceramic, it is made to be evenly distributed on MgO
nAl2O3In crystalline ceramics, MgOnAl is utilized2O3The excellent optical property of crystalline ceramics (80% or more transmitance) and thermal conductivity
Can (17W/mk-20W/mk), in the case where will not influence light propagation, exciting light can be conducted to inside luminescent ceramic with
More Nd:YAG ceramic particles are excited, while can also be transferred heat away from well；On the other hand, MgOnAl2O3It is transparent
The refractive index of ceramics, close to (about 1.7-1.8), will not influence the light extraction efficiency of Nd:YAG ceramic particle with Nd:YAG ceramics；
MgOnAl simultaneously2O3The similar thermal expansion coefficient of crystalline ceramics and Nd:YAG ceramics, at (6.7-8) × 10-6/ DEG C range
Interior, luminescent ceramic is not easy to cause ceramic cracking because of temperature difference.By MgOnAl in the present invention2O3Matrix 210 and uniformly point
Cloth is in MgOnAl2O3The luminescent ceramic that the Nd:YAG centre of luminescence 220 in matrix 210 forms, Nd:YAG are dispersed in
MgO·nAl2O3In, phase interface is increased, exciting light can reflected and/or reflected to generation between interface；Meanwhile MgO
nAl2O3Lattice structure and its material property but also in MgOnAl2O3Crystal boundary on can also occur more reflection and/or
Refraction, is excited so that incident light is repeatedly oriented to different Nd:YAG.Therefore compared to pure phase ceramics, incident light is at this
Light path in kind luminescent ceramic is longer, also more abundant to the absorption of incident exciting light.
Above-mentioned luminescent ceramic provided by the invention can form a kind of completely new infrared light supply with 808nm laser semiconductor.
You need to add is that the MgOnAl in the present invention as matrix2O3Crystalline ceramics and existing Al2O3Ceramics are
Two kinds of ceramics are not in Al2O3Disperse MgO particle in ceramics to be formed, Al2O3Ceramics belong to trigonal system, and MgOnAl2O3
The ceramic crystal form and MgAl of crystalline ceramics2O4It is identical, it is cubic system, there was only a kind of object phase in two kinds of ceramics.Also, it adopts
Use MgOnAl2O3As matrix, relative to Al2O3As matrix, due to the introducing of MgO, during sinter molding, have
Conducive to inhibition Al2O3Grain growth is too much, and controls Al2O3The size of crystal grain can provide more exciting lights in this pottery that shines
Refraction in porcelain, to improve luminous efficiency.
Wherein the Nd:YAG centre of luminescence 220 accounts for 30wt%~80wt% of luminescent ceramic gross mass.In Nd:YAG shines
When heart content is too low, the centre of luminescence is very little, inefficient；When Nd:YAG centre of luminescence too high levels, matrix is bonded phase MgO
nAl2O3Content is very little, and sintering is difficult, it is difficult to form fine and close ceramics.Preferably, in the present invention, the Nd:YAG centre of luminescence 220
Quality accounting be 40%~60%, centre of luminescence moderate number, discrete phase are also easy to be sintered at this time, luminescent ceramic it is relatively close
Degree easily reaches highest, therefore luminous efficiency, heating conduction, mechanical property are optimal.
The present invention also provides a kind of preparation method of above-mentioned luminescent ceramic, the preparation method includes:
S1: preparation Nd:YAG precursor powder；
S2: preparation MgOnAl2O3Precursor powder；
S3: mixing Nd:YAG precursor powder and MgOnAl2O3Precursor powder obtains luminescent ceramic powder；
S4: being molding biscuit by luminescent ceramic pressed by powder；
S5: being sintered and makes annealing treatment the biscuit, obtains luminescent ceramic.
Specifically, in S1, stoichiometrically (Nd3++Y3+): Al3+Y (NO is weighed for 3:53)3·6H2O and Nd
(NO3)3·6H2O is added in aluminum nitrate solution, and pH value of solution is adjusted to 2-3 after stirring and filtering, after mixing evenly to solution into
Row heating, makes precipitation by metallic ion, will calcine after gained precipitating drying, obtains Nd:YAG precursor powder.Wherein, the aluminum nitrate
Solution can be by weighing a certain amount of Al (NO3)3·9H2O and deionized water are stirred and are obtained after filtering.Nd3+Additive amount
Account for Nd3+And Y3+The 0.2at%-2at% of total amount of adding.The adjusting of pH value of solution can by weigh it is a certain amount of (urea with metal from
Sub- molar ratio be 10:1-20:1) urea in mixing salt solution, while add a certain amount of ammonium sulfate be dispersing agent, be used in combination
PH value of solution is adjusted to 2-3 by ammonium hydroxide.It stirs until carrying out heating water bath to 90 DEG C of guarantors to solution immediately after solution clarification
Warm 4h-8h, so as to precipitation by metallic ion.Gained precipitating is carried out repeatedly washing and alcohol to wash, is then dried at sieving
Reason.Powder calcination after sieving is finally obtained into Nd:YAG precursor powder.Preferably, calcination temperature is 900 DEG C -1300 DEG C, heat preservation
Time is 1h-4h, it should be noted that the present invention is not defined the specific process parameter of above-mentioned production procedure, ability
Field technique personnel can be adjusted according to the actual situation.
It should be noted that preparation Nd:YAG precursor powder can also be using solid other than it can use above-mentioned coprecipitation
Xiang Fa.
In S2, by Al2O3Powder, MgO powder are calcined after mixing in proportion, by calcined powder and ball-milling medium into
Row ball milling finally obtains MgOnAl by drying2O3Precursor powder.
Specifically, by the high-purity Al of a certain amount of business2O3Powder, the same abrasive media of MgO powder (dehydrated alcohol) carry out ball milling
Mix certain time；Wherein, Al2O3The average grain diameter of powder and MgO powder is 0.05 μm -1 μm, Al2O3Powder and MgO powder
Molar ratio be 1:n, n value difference be affected to Ceramic optical performance, different n values, ceramic transmitance is also different, if oxygen
Change magnesium or aluminium oxide is excessive, two kinds of object phases can be presented in ceramics, i.e. second of object is mutually magnesia or aluminium oxide, these second
It meets the scattering phase become in crystalline ceramics and reduces the transparency of crystalline ceramics or even opaque.Therefore, process is repeatedly real
It tests, inventor obtains when n is 0.7-2, further preferably 0.9-1.3, can obtain the higher MgOnAl of transparency2O3Pottery
Porcelain.
Powder after ball milling is dried, is ground up, sieved processing.It is carried out in Muffle furnace with the powder after will being sieved
Calcined powder and ball-milling medium dehydrated alcohol are carried out high-energy ball milling, finally handle to obtain by drying, sieving by calcining
MgO·nAl2O3Precursor powder, it is preferable that calcination temperature is 1000 DEG C -1300 DEG C, soaking time 1h-8h, after ball milling
MgO·nAl2O3Precursor powder average grain diameter is 0.1 μm -10 μm.
In S3, the Nd:YAG precursor powder, the MgOnAl that will prepare2O3Precursor powder is done after mixing with sintering aid
It is dry, it is ground up, sieved processing later and obtains luminescent ceramic powder.Specifically, sintering aid is lithium fluoride, calcirm-fluoride, positive silicic acid four
One of ethyl ester is a variety of, and average grain diameter is 0.05 μm -1 μm, accounts for the 0.01wt%- of luminescent ceramic powder gross mass
1wt%.Mixing is preferably ball milling mixing, and Ball-milling Time is preferably 6h-8h.Dry temperature is 50 DEG C -80 DEG C, preferably in vacuum
It is dried under atmosphere.Wherein, the quality of the Nd:YAG precursor powder accounts for the 30wt%- of luminescent ceramic powder gross mass
80wt%.Preferably, bonding agent can be also added in S3 to be mixed, the binder is polyvinyl butyral (PVB)
Ethanol solution.
In step S2, S3, the present invention is first to be sintered Al2O3Powder and MgO is powder sintered obtains MgOnAl2O3Forerunner
It is sintered again with Nd:YAG precursor powder after powder, i.e., by the way of two-step sintering, and indirect uses Al2O3Powder, MgO powder
The mode that end, the common step of Nd:YAG precursor powder three are sintered, this is because in MgO and Al2O3Synthesize MgOnAl2O3Pottery
There can be the volume expansion of 5-8% when porcelain, if three's direct sintering, the MgO of Nd:YAG ceramic particle and synthesis
It can be easily formed stomata/gap between nAl2O3 ceramics, be unfavorable for the heat transfer of ceramics.And by the way of two-step sintering, MgO
nAl2O3Ceramics first molding finish, i.e. volume expansion is also completed, then with Nd:YAG be sintered when avoid because of volume change
Caused by stomata or gap.
In S4, a certain amount of luminescent ceramic pressed by powder is weighed into the biscuit of certain shapes, it is preferable that briquetting pressure is
50MPa-100MPa.By biscuit dumping after molding processing, it is preferable that binder removal is to keep the temperature 1h-4h at 400 DEG C -600 DEG C,
800 DEG C of -1300 DEG C of heat preservation 1-6h later.Biscuit after dumping is subjected to isostatic cool pressing at 150MPa-300MPa, with further
Improve its relative volume density.
In S5, by after isostatic cool pressing biscuit carry out hot pressed sintering, it is preferable that hot pressed sintering temperature be 1400 DEG C-
1700 DEG C, soaking time 1h-4h, pressure 20MPa-150MPa.High annealing is carried out after sintering, to remove hot pressed sintering mistake
Residual carbon in journey, it is preferable that annealing temperature is 1200 DEG C -1400 DEG C, and annealing soaking time is 5h-20h.
You need to add is that the present invention is not intended to limit above-mentioned technological parameter (temperature, pressure, time etc.), art technology
Personnel can according to actual needs be adjusted above-mentioned technological parameter.
Embodiment one
Weigh a certain amount of Al (NO3)3·9H2O and deionized water stir and obtain aluminum nitrate solution after filtering, while right
Al3+Ion concentration is demarcated.Stoichiometrically (Nd3++Y3+): Al3+A certain amount of Y (NO is weighed for 3:53)3·6H2O with
And Nd (NO3)3·6H2O is added in above-mentioned aluminum nitrate solution, is stirred and is obtained mixing salt solution after filtering, wherein Nd3+'s
Additive amount accounts for Nd3+And Y3+The 1at% of total amount of adding.A certain amount of urea is weighed in mixing salt solution, while being added a certain amount of
Ammonium sulfate be dispersing agent, and pH value of solution is adjusted to 2-3 with ammonium hydroxide, stirred until solution is clarified.Immediately to solution
Heating water bath is carried out to 90 DEG C of heat preservation 4h-8h, so as to precipitation by metallic ion.Gained precipitating is carried out repeatedly washing and alcohol to wash, with
Sieving processing is dried afterwards.Finally powder after sieving is calcined into 2h at 1100 DEG C and obtains Nd:YAG precursor powder.
By the high-purity Al of a certain amount of business2O3Powder, MgO powder carry out one timing of ball milling mixing with abrasive media dehydrated alcohol
Between；Wherein, Al2O3The average grain diameter of powder and MgO powder is 0.05 μm -1 μm, Al2O3The molar ratio of powder and MgO powder is
Powder after ball milling is dried, is ground up, sieved processing by 1:1, with the powder after will being sieved in Muffle furnace at 1200 DEG C
4h is calcined, is obtained after calcined powder is finally carried out high-energy ball milling, drying, sieving processing with ball-milling medium dehydrated alcohol
MgO·Al2O3Precursor powder.
Nd:YAG precursor powder, the MgOAl that will have been prepared2O3Precursor powder and sintering aid lithium fluoride and binder
Ball milling mixing is carried out, wherein the average grain diameter of sintering aid is 0.05 μm -1 μm, accounts for luminescent ceramic powder gross mass
0.05wt%, binder is the ethanol solution of polyvinyl butyral (PVB), finally by slurry after ball milling at 50 DEG C -80 DEG C
It is dried in vacuo, and carries out being ground up, sieved processing and obtain luminescent ceramic powder.
A certain amount of luminescent ceramic pressed by powder is weighed at the biscuit of certain shapes, by biscuit after molding at 500 DEG C
Dumping handles 2h, and in 1000 DEG C of heat preservation 3h.Biscuit after dumping is subjected to isostatic cool pressing at 200MPa, to further increase
Its relative volume density.
By the biscuit after isostatic cool pressing at 1700 DEG C, 60MPa hot pressed sintering 2h.Anneal at 1300 DEG C 8h after sintering,
To remove the residual carbon during hot pressed sintering, finally ceramics are roughly ground, fine grinding and polishing treatment obtain Nd:YAG-
MgO·Al2O3Luminescent ceramic.
Light efficiency test is carried out to luminescent ceramic prepared in the present embodiment, the light efficiency in the present invention refers in particular to every watt of 808nm
The 1000nm-1100nm infrared light that laser is excited, light efficiency reach 60lm/W.
Embodiment two
Weigh a certain amount of Al (NO3)3·9H2O and deionized water stir and obtain aluminum nitrate solution after filtering, while right
Al3+Ion concentration is demarcated.Stoichiometrically (Nd3++Y3+):
Al3+A certain amount of Y (NO is weighed for 3:53)3·6H2O and Nd (NO3)3·6H2It is molten to be added to above-mentioned aluminum nitrate by O
In liquid, stirs and obtain mixing salt solution after filtering, wherein Nd3+Additive amount account for Nd3+And Y3+The 0.5at% of total amount of adding.
A certain amount of urea is weighed in mixing salt solution, while adding a certain amount of ammonium sulfate is dispersing agent, and with ammonium hydroxide by solution
PH is adjusted to 2-3, stirs until solution is clarified.Heating water bath is carried out to 90 DEG C of heat preservation 4h-8h to solution immediately, so as to
Precipitation by metallic ion.Gained precipitating is carried out repeatedly washing and alcohol to wash, sieving processing is then dried.It finally will sieving
Powder calcines 3h at 1000 DEG C and obtains Nd:YAG precursor powder afterwards.
By the high-purity Al of a certain amount of business2O3Powder, MgO powder carry out one timing of ball milling mixing with abrasive media dehydrated alcohol
Between；Wherein, Al2O3The average grain diameter of powder and MgO powder is 0.05 μm -1 μm, Al2O3The molar ratio of powder and MgO powder is
Powder after ball milling is dried, is ground up, sieved processing by 1:1.3, with the powder after will being sieved 1100 DEG C in Muffle furnace
Lower calcining 6h is obtained after calcined powder is finally carried out high-energy ball milling, drying, sieving processing with ball-milling medium dehydrated alcohol
MgO·1.3Al2O3Precursor powder.
Nd:YAG precursor powder, the MgO1.3Al that will have been prepared2O3Precursor powder and sintering aid tetraethyl orthosilicate with
And binder carries out ball milling mixing, wherein the average grain diameter of sintering aid is 0.05 μm -1 μm, accounts for luminescent ceramic powder gross mass
0.5wt%, binder be polyvinyl butyral (PVB) ethanol solution, finally by slurry after ball milling at 50 DEG C -80 DEG C
It is dried in vacuo, and carries out being ground up, sieved processing and obtain luminescent ceramic powder.
A certain amount of luminescent ceramic pressed by powder is weighed at the biscuit of certain shapes, by biscuit after molding at 450 DEG C
Dumping handles 4h, and in 900 DEG C of heat preservation 5h.Biscuit after dumping is subjected to isostatic cool pressing at 250MPa, to further increase
Its relative volume density.
By the biscuit after isostatic cool pressing at 1600 DEG C, 80MPa hot pressed sintering 3h.Anneal at 1250 DEG C 10h after sintering,
To remove the residual carbon during hot pressed sintering, finally it is roughly ground, fine grinding and polishing treatment obtain Nd:YAG-
MgO·1.3Al2O3Luminescent ceramic.
Light efficiency test is carried out to luminescent ceramic prepared in the present embodiment, light efficiency reaches 65lm/W.
In conclusion the present invention prepares Nd:YAG precursor powder by urea coprecipitation method, prepared by solid reaction process
MgO·nAl2O3Precursor powder is prepared into Nd:YAG-MgOnAl finally by hot pressing sintering method2O3Luminescent ceramic；Utilize Nd:
YAG is as infraluminescence center, with high quantum efficiency；And MgOnAl2O3Prepared crystalline ceramics is in infrared waves
Section transmitance is higher, and has more excellent thermal conductivity；It, can be well by Nd when it collectively constitutes composite ceramics with Nd:YAG:
Infrared light scattering caused by YAG comes out, and simultaneously by 808nm laser excitation when generated heat carry out conduction and distribute, have
Have the advantages that high brightness, dim light decline.
Claims (13)
1. a kind of luminescent ceramic, which is characterized in that the luminescent ceramic includes MgOnAl2O3It matrix (210) and is uniformly distributed
In MgOnAl2O3The Nd:YAG centre of luminescence (220) in matrix, wherein MgOnAl2O3Matrix is one-component ceramic, Al2O3With
The molar ratio of MgO is 1:n, n 0.7-2.
2. luminescent ceramic as described in claim 1, which is characterized in that the n is 0.9-1.3.
3. luminescent ceramic as described in claim 1, which is characterized in that the MgOnAl2O3Size of microcrystal be 0.5 μm -10
μm, the size of microcrystal of the Nd:YAG is 1 μm -20 μm；Preferably, the MgOnAl2O3Size of microcrystal be 1 μm -5 μm, institute
The size of microcrystal for stating Nd:YAG is 5 μm -10 μm.
4. luminescent ceramic as described in claim 1, which is characterized in that the Nd:YAG centre of luminescence (220) accounts for described shine
30wt%~80wt% of ceramic gross mass.
5. a kind of preparation method of luminescent ceramic, which is characterized in that the preparation method includes:
S1: preparation Nd:YAG precursor powder；
S2: preparation MgOnAl2O3Precursor powder；
S3: mixing Nd:YAG precursor powder and MgOnAl2O3Precursor powder obtains luminescent ceramic powder；
S4: being molding biscuit by luminescent ceramic pressed by powder；
S5: being sintered and makes annealing treatment the biscuit, obtains luminescent ceramic.
6. preparation method as claimed in claim 5, which is characterized in that in S1, stoichiometrically (Nd3++Y3+): Al3+For
3:5 weighs Y (NO3)3·6H2O and Nd (NO3)3·6H2O is added in aluminum nitrate solution, by pH value of solution after stirring and filtering
It is adjusted to 2-3, solution is heated after mixing evenly, makes precipitation by metallic ion, will be calcined after gained precipitating drying, obtain Nd:
YAG precursor powder.
7. preparation method as claimed in claim 6, which is characterized in that the Nd3+Additive amount account for Nd3+And Y3+Total amount of adding
0.2at%-2at%.
8. preparation method as claimed in claim 5, which is characterized in that in S2, by Al2O3Powder, MgO powder mix in proportion
It is calcined after conjunction, calcined powder and ball-milling medium is subjected to ball milling, finally obtain MgOnAl by drying2O3Precursor powder.
9. preparation method as claimed in claim 8, which is characterized in that the Al2O3The average grain diameter of powder and MgO powder is
0.05 μm -1 μm, the Al2O3The molar ratio of powder and MgO powder is 1:n, n 0.7-2, the MgOnAl2O3Front axle shell
Body average grain diameter is 0.1 μm -10 μm.
10. preparation method as claimed in claim 5, which is characterized in that in S3, by Nd:YAG precursor powder, MgO
nAl2O3Precursor powder is dry after mixing with sintering aid, is ground up, sieved processing later and obtains luminescent ceramic powder.
11. preparation method as claimed in claim 10, which is characterized in that the sintering aid is lithium fluoride, calcirm-fluoride, positive silicon
One of sour tetra-ethyl ester is a variety of, and average grain diameter is 0.05 μm -1 μm, accounts for the 0.01wt%- of luminescent ceramic powder gross mass
1wt%.
12. preparation method as claimed in claim 10, which is characterized in that bonding agent, which can be also added, in S3 is mixed, institute
State the ethanol solution that binder is polyvinyl butyral.
13. preparation method as claimed in claim 10, which is characterized in that the quality of the Nd:YAG precursor powder accounts for luminous pottery
The 30wt%-80wt% of porcelain powder gross mass.
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