CN110386820A - A kind of fluorescence ceramics and preparation method thereof of aluminum oxynitride matrix - Google Patents
A kind of fluorescence ceramics and preparation method thereof of aluminum oxynitride matrix Download PDFInfo
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Abstract
The present invention provides a kind of complex phase fluorescence ceramics, the complex phase fluorescence ceramics include the aluminum oxynitride phase as matrix phase, the fluorescent powder that is evenly distributed in described matrix phase and mix aluminium oxide phase together with the fluorescent powder and the aluminum oxynitride.The preparation method of the complex phase fluorescence ceramics by make the surface of fluorescent powder or aluminum oxynitride coat one layer of aluminium oxide, then with aluminum oxynitride or fluorescent powder are complex sintered forms the complex phase fluorescence ceramics；Or the complex phase fluorescence ceramics are formed by making aluminum oxynitride, aluminium oxide and the uniform mixing and ball milling of fluorescent powder, being then sintered together.Complex phase fluorescence ceramics according to the present invention be it is a kind of with high luminous efficiency, high thermal conductivity, excellent resistance to heat shocks energy and excellent mechanical strength fluorescence ceramics, it can be by high-power exciting light source activation, realize the semiconductor light source of high brightness, such as high-power white light LED light source, blue laser light source.
Description
Technical field
The present invention relates to a kind of fluorescence ceramics and preparation method thereof of aluminum oxynitride matrix.
Background technique
Currently, the implementation of high-power white light LED light source is mainly include the following types: a kind of mode is by transparent ceramics
It is covered in LED semiconductor core on piece.Suitable colour temperature in order to obtain, under normal circumstances, the thickness of the material of transparent light compared with
It is body Xiang Faguang that the problem of thick (150um or more), the program is primarily present, which is that crystalline ceramics shines, and body is mutually different from powder phase
It is that illuminator material shines, light, which is easy the collection efficiency for causing to receive optical lens from side-emitted, to be reduced with liquid phase.In order to improve
Light efficiency is received, the second way is the translucent fluorescent ceramics being thinned using thickness, for high color temperature product, is needed half
Transparent fluorescent ceramic thickness is thinned to 100um or less.However, when being thinned to a thickness of 100um or less, translucent fluorescent ceramics
Mechanical strength it is poor, ceramics it is frangible, yield is lower, and mass production encapsulation difficulty is larger.
On the other hand, for use blue laser light source excite fluorescence ceramics luminous mode for, since blue light swashs
The switch response of the high brightness characteristic of light, semiconductor light source is nanosecond order, and this response characteristic being exceedingly fast is to fluorescence ceramics
Thermal shock it is very big, therefore thermal conductivity for fluorescence ceramics and resistance to heat shocks can be more demanding.Further, for remotely revolving
Turn for laser fluorescence light source technology, has higher requirement to the mechanical strength of the large-sized fluorescence ceramics wheel of high speed rotation.
Thus, the development for high-brightness semiconductor light source, it is desirable that the high-luminous-efficiency and high fever of translucent fluorescent ceramics
While conductance, resistance to heat shocks can be also required to very excellent with mechanical strength.
It should be noted that there are two types of the main implementations of translucent luminescent ceramic: a kind of mode is shone in single-phase
Stomata is added in ceramics；The second way is by the way of complex phase ceramic, as shown in Figure 1, including complex phase ceramic matrix
Phase 1-1, fluorescent powder phase 1-2.Current main complex phase ceramic has aluminium oxide (Al2O3) matrix fluorescence ceramics (such as patent
) and the fluorescence ceramics (such as patent CN107200587A) of aluminium nitride (AlN) matrix CN107285745A.For it is ultra-thin (with a thickness of
100um or less) fluorescence ceramics application for, although the thermal conductivity of the fluorescence ceramics of these two types of matrix is higher, all there is
Mechanical strength is low, the problem that resistance to heat shocks can be poor.
Therefore, up for providing a kind of complex phase ceramic, with high luminous efficiency, high thermal conductivity, excellent heat-resisting
Shock stability and excellent mechanical strength.
Summary of the invention
In view of this, the present invention is intended to provide a kind of novel complex phase fluorescence ceramics, wherein in YAG:Ce3+/ AlON complex phase pottery
Increase aluminium oxide (Al between porcelain2O3) phase, to realize a kind of novel YAG:Ce3+/Al2O3The complex phase fluorescence of/AlON structure is made pottery
Porcelain.Meanwhile the present invention is also directed to a kind of preparation method of complex phase fluorescence ceramics to prepare this novel complex phase fluorescence pottery
Porcelain.
According to an aspect of the present invention, a kind of complex phase fluorescence ceramics are provided, the complex phase fluorescence ceramics include being used as base
The aluminum oxynitride phase of body phase, the fluorescent powder being evenly distributed in described matrix phase and with the fluorescent powder and the aluminum oxynitride
Mix aluminium oxide phase together.
Further, the fluorescent powder and the aluminum oxynitride are mutually mutually separated from each other via the aluminium oxide.
Further, the aluminium oxide is mutually coated on the surface of the fluorescent powder or the aluminum oxynitride phase.
Further, the fluorescent powder is YAG:Ce fluorescent powder or LuAG:Ce fluorescent powder.
Further, the aluminium oxide phase with a thickness of 0.05~5um.
Further, the fluorescent powder accounts for the 20~80% of the complex phase fluorescence ceramics total volume.
It further, can also include active ions Mn in the aluminum oxynitride phase2+。
According to another aspect of the present invention, provide a kind of preparation method of complex phase fluorescence ceramics, the method includes with
Lower step: S1: coating one layer of aluminium oxide on the surface of fluorescent powder or aluminum oxynitride powder, and the particle size of the fluorescent powder is
The particle size of 5~30um and the aluminum oxynitride powder is 0.05~1um；S2: after the cladding being prepared in S1
Product and aluminum oxynitride powder or fluorescent powder, auxiliary agent and the uniform mixing and ball milling of solvent are to be made the mixing slurry comprising these raw materials
Material；S3: the mixed slurry being prepared in S2 is dry and dry-pressing formed, then by etc. static pressure suppressions obtain element
Base, and ungrease treatment is carried out to obtain ceramic body to the biscuit；S4: the ceramic body being prepared in S3 is carried out
Sintering processes are to obtain the complex phase fluorescence ceramics comprising fluorescent powder, aluminium oxide phase and aluminum oxynitride phase.
Further, the preparation method of complex phase fluorescence ceramics according to the present invention, further includes step S5 after step s4:
The complex phase fluorescence ceramics being prepared in S4 are post-processed, the post-processing includes reduction processing and polishing treatment.
Further, in S1, coating one layer of aluminium oxide on the surface of fluorescent powder or aluminum oxynitride powder is by such as
What lower method was realized: the method using co-precipitation is in coating one layer of aluminium salt on the surface of fluorescent powder or aluminum oxynitride powder, then
Make the fluorescent powder for being coated with one layer of aluminium salt or aluminum oxynitride powder through Overheating Treatment, is coated with one layer of aluminium oxide to obtain to surface
Fluorescent powder or aluminum oxynitride powder.
Beneficial effect
It is prepared in the preparation method of complex phase fluorescence ceramics according to the present invention and complex phase fluorescence ceramics according to the present invention
Complex phase fluorescence ceramics in, due to aluminium oxide (Al2O3) and fluorescent powder (YAG:Ce3+) and all have with aluminum oxynitride (AlON)
Preferable compatibility, so Al2O3Addition significantly improve YAG:Ce3+The sintered density of/AlON complex phase fluorescence ceramics,
Al simultaneously2O3Refractive index be 1.72, hence it is evident that the refractive index 1.80 of refractive index 1.83 and AlON lower than YAG utilizes refringence
The reflectivity between different phase interfaces is improved, the light transmittance of fluorescence ceramics is reduced, improves light efficiency.In addition, YAG:Ce3+/
Al2O3The translucent fluorescent ceramics of/AlON structure have high thermal conductivity, and when being machined to a thickness of 100um or less still
Light efficiency, higher mechanical strength and higher resistance to heat shocks energy with higher.Therefore, complex phase fluorescence ceramics of the invention can
High power stimulated luminescence is issued, realizes higher processing yield and easier mass production encapsulation, it can be by high-power exciting light
Source (such as blue laser, blue-ray LED equal excitation light source) excitation, realizes the semiconductor light source of high brightness, such as high power white LED light
Source, blue laser light source etc..
Detailed description of the invention
Attached drawing indicates non-restrictive illustrative embodiment as described herein.Those skilled in the art will be appreciated that, attached
Component in figure is not drawn necessarily to scale, but for stressing the principle of the present invention.In the accompanying drawings:
Fig. 1 is the schematic diagram of complex phase fluorescence ceramics according to prior art.
Fig. 2 is the schematic diagram of complex phase fluorescence ceramics according to the present invention.
Fig. 3 is the flow chart of the preparation method of according to embodiments of the present invention 1 complex phase fluorescence ceramics.
Fig. 4 is the flow chart of the preparation method of according to embodiments of the present invention 2 complex phase fluorescence ceramics.
Fig. 5 is the flow chart of the preparation method of according to embodiments of the present invention 3 complex phase fluorescence ceramics.
Reference signs list
1-1: complex phase ceramic discrete phase
1-2:YAG:Ce or LuAG:Ce fluorescent powder
1: fluorescent powder
2: aluminium oxide phase
3: aluminum oxynitride phase
Specific embodiment
Hereinafter, illustrating one or more exemplary embodiments of the invention, in the accompanying drawings, ability more fully with reference to the ac-companying drawings
Field technique personnel can be readily determined one or more exemplary embodiments of the invention.As those skilled in the art should recognize
It arrives, as long as it does not depart from the spirit of the invention or range, can carry out in a variety of ways to the exemplary embodiment
Modification, the spirit or scope of the present invention are not limited to exemplary embodiment as described herein.
The embodiment of the present invention is described in detail referring now to attached drawing.
The present invention provides a kind of translucent complex phase fluorescence ceramics of high intensity, as shown in Fig. 2, the complex phase fluorescence ceramics include
Fluorescent powder 1, aluminium oxide phase 2 and aluminum oxynitride phase 3.Aluminum oxynitride phase 3 is matrix phase, and fluorescent powder 1 is evenly distributed in matrix phase.
Aluminium oxide phase 2 can be mixed with fluorescent powder 1 and aluminum oxynitride phase 3.Specifically, aluminium oxide phase 2 can be coated on fluorescence
On the surface of powder 1.Selectively, aluminium oxide phase 2 can also be coated on the surface of aluminum oxynitride phase 3.In other words, fluorescent powder
1 and aluminum oxynitride phase 3 can be separated from each other via aluminium oxide phase 2.That is, aluminium oxide phase 2 can be distinguished at phase interface
It contacts and is combined together with fluorescent powder 1 and aluminum oxynitride phase 3.Selectively, fluorescent powder can be such as YAG:Ce or LuAG:Ce
Fluorescent powder, and the partial size of fluorescent powder can be 5~30um.Fluorescent powder passes through surface alumina oxide phase and the mutually compound burning of aluminum oxynitride
It ties and forms the complex phase fluorescence ceramics comprising aluminum oxynitride phase, aluminium oxide phase and fluorescent powder, wherein the aluminium oxide of phosphor surface
The thickness of phase can be 0.05~5um sufficiently to be coated to fluorescent powder and have good light transmission rate, and in order to make
Obtained complex phase fluorescence ceramics have good luminous efficiency, fluorescent powder can account for complex phase fluorescence ceramics total volume 20~
80%.Using YAG:Ce or LuAG:Ce as fluorescent powder of the invention, the knot of complex phase fluorescence ceramics of the invention
Structure is YAG:Ce/Al2O3/ AlON or LuAG:Ce/Al2O3/ AlON, shining mutually is YAG:Ce or LuAG:Ce, and matrix is mutually
Al2O3And AlON.
In complex phase fluorescence ceramics of the invention, aluminium oxide (Al2O3) addition so that complex phase fluorescence in the prior art make pottery
Phase interface in porcelain between the bad fluorescent powder of reciprocal compatibility (YAG:Ce) and aluminum oxynitride (AlON) is partially or completely eliminated,
But replace with Al2O3Phase interface and Al between YAG:Ce2O3Phase interface between AlON.Due to Al2O3With YAG:
Ce and all there is preferable compatibility between AlON, so the sintering at phase interface in complex phase fluorescence ceramics of the invention
Consistency is greatly improved compared with complex phase fluorescence ceramics in the prior art.That is, complex phase of the invention is glimmering
The mechanical strength of light ceramic is greatly improved compared with complex phase fluorescence ceramics in the prior art.In addition, Al2O3Folding
Penetrating rate is 1.72, hence it is evident that difference can be improved using refringence in the refractive index 1.80 of refractive index 1.83 and AlON lower than YAG
Reflectivity between phase interface reduces the light transmittance of fluorescence ceramics, improves light efficiency, therefore complex phase fluorescence pottery of the invention can be improved
The luminous efficiency of porcelain.Meanwhile Al2O3Thermal conductivity it is also higher, so Al2O3Addition also improve complex phase fluorescence of the invention
The heating conduction of ceramics.Further, it is present such that complex phase fluorescence ceramics of the invention have high machine due to AlON
Tool intensity and resistance to heat shocks energy.
Compared with prior art, complex phase fluorescence ceramics of the invention have high thermal conductivity and when be machined to a thickness of
Light efficiency, higher mechanical strength and higher resistance to heat shocks energy still with higher when 100um or less, can be by high-power blue-light light
Source excitation realizes the semiconductor light source of high brightness, such as high-power white light LED light source, blue laser light source.
In addition, the above-mentioned complex phase fluorescence ceramics in the present invention can be prepared by the preparation method included the following steps.
S1: one layer of aluminium oxide, the particle size of the fluorescent powder are coated on the surface of fluorescent powder or aluminum oxynitride powder
Particle size for 5~30um and the aluminum oxynitride powder is 0.05~1um.Specifically, using the method for co-precipitation in
One layer of aluminium salt is coated on the surface of fluorescent powder or aluminum oxynitride powder and is obtained after the heat treatment to surface is coated with one layer of oxygen
Change the fluorescent powder or aluminum oxynitride of aluminium.
S2: by after the cladding being prepared in S1 product and aluminum oxynitride powder or fluorescent powder, auxiliary agent and solvent it is uniform
Mixing and ball milling is to be made the mixed slurry comprising these raw materials.Specifically, the surface being prepared in S1 is coated with one layer of oxygen
Fluorescent powder (or aluminum oxynitride) and aluminum oxynitride (or fluorescent powder), auxiliary agent and the uniform mixing and ball milling of solvent for changing aluminium include with obtained
It is coated with the fluorescent powder (or aluminum oxynitride) of one layer of aluminium oxide, the mixing slurry of aluminum oxynitride (or fluorescent powder) and auxiliary agent and solvent
Material, wherein auxiliary agent may include sintering aid and dispersing agent etc., and sintering aid can be Y2O3Or MgO, the partial size of sintering aid
It can be 0.02~1um, and sintering aid accounts for fluorescent powder (or aluminum oxynitride), the aluminum oxynitride for being coated with one layer of aluminium oxide
The 0.01~4% of the gross mass of (or fluorescent powder) and sintering aid, to help to reach good sintering effect.
S3: the mixed slurry being prepared in S2 is dry and dry-pressing formed, then by etc. static pressure suppressions obtain
Biscuit is obtained, and ungrease treatment is carried out to obtain ceramic body to the biscuit.Specifically, it will be prepared in S2 comprising cladding
The mixed slurry of fluorescent powder (or aluminum oxynitride), aluminum oxynitride (or fluorescent powder) and the auxiliary agent and solvent that have one layer of aluminium oxide is set
It is dry in baking oven, keep its dry-pressing formed under the dry-pressing pressure of 10~20MPa, then in the equal static pressure pressure of 200~300MPa
Under power by etc. static pressure suppressions obtain biscuit, and ungrease treatment carried out to obtain ceramic body to the biscuit, wherein biscuit
Skimming temp can be 500~1000 DEG C, and degreasing time can be 2~6h.
S4: the ceramic body being prepared in S3 is sintered to obtain comprising fluorescent powder, aluminium oxide phase
With the complex phase fluorescence ceramics of aluminum oxynitride phase.Specifically, the ceramic body being prepared in S3 is put into sintering furnace and is burnt
Knot, cooling obtains the complex phase fluorescence ceramics comprising fluorescent powder, aluminium oxide phase and aluminum oxynitride phase after the completion of sintering, wherein being sintered
Mode can be hot pressing, air pressure, vacuum, hot isostatic pressing or plasma discharging etc..
S5: post-processing the complex phase fluorescence ceramics being prepared in S4, and the post-processing includes reduction processing
And polishing treatment.
In this way, aluminium oxide then will be coated with by coating one layer of aluminium oxide on the surface of fluorescent powder (or aluminum oxynitride)
Fluorescent powder (or aluminum oxynitride) mix and be sintered with aluminum oxynitride (or fluorescent powder), it can be ensured that aluminium oxide mutually between fluorescent powder
Between aluminum oxynitride phase and fluorescent powder is not directly contacted with each other with aluminum oxynitride phase.That is, fluorescent powder and nitrogen
Aluminium oxide communicates peroxidating aluminium and is combined together.In other words, during the sintering process, only between aluminium oxide phase and fluorescent powder
And there are phase interfaces between aluminium oxide phase and aluminum oxynitride phase, and phase boundary is not present between fluorescent powder and aluminum oxynitride phase
Face.All there is good compatibility due to aluminium oxide and fluorescent powder and between aluminum oxynitride, can be obtained with densified sintering product
The complex phase ceramic relatively high to mechanical strength.In other words, solve that aluminum oxynitride is poor with fluorescent powder compatibility, is difficult to be sintered
Fine and close problem.In addition, as described above, the refractive index of aluminium oxide and the refractive index of fluorescent powder and aluminum oxynitride are dramatically different,
Therefore aluminium oxide and fluorescent powder and the reflectivity with the phase interface of aluminum oxynitride can be improved, reduces the light transmission of fluorescence ceramics
Rate improves luminous light efficiency.Meanwhile the thermal conductivity of aluminium oxide is also higher, therefore the addition of aluminium oxide also improve it is of the invention
The heating conduction of complex phase fluorescence ceramics.In addition, the mechanical strength and resistance to heat shocks of aluminum oxynitride can be all very high, it is ensured that super
The good mechanical strength of thin fluorescence ceramics and good resistance to heat shocks energy.Therefore, prepared it is a kind of with high luminous efficiency,
The luminescent ceramic of high thermal conductivity, excellent resistance to heat shocks energy and excellent mechanical strength, the luminescent ceramic have high sintering
Consistency and high phototransformation efficiency can be used for LED encapsulation, solve poor reliability, light efficiency existing for existing LED stage lamp light source
The problems such as low and processing yield is low.
Referring to specific embodiment, the present invention is described in detail.
Embodiment 1
Fig. 3 shows the flow chart of the preparation method of according to embodiments of the present invention 1 complex phase fluorescence ceramics.In the present embodiment
In, it selects the aluminum oxynitride of high-purity as matrix phase raw material, selects commercialization YAG:Ce fluorescent powder as the phase raw material that shines, select
Polyvinyl butyral (PVB) is used as bonding agent, and dispersing agent, sintering aid can be elected additional member etc., to prepare complex phase fluorescence
Ceramics.Specific preparation method is as follows.
First step S1 is first carried out, YAG:Ce phosphor surface is made to coat one layer of aluminium oxide: using the method for co-precipitation
One layer of aluminium salt is coated on the surface of commercial YAG:Ce fluorescent powder to obtain to surface the YAG:Ce fluorescent powder for being coated with one layer of aluminium salt.
Specifically, the commercial YAG:Ce fluorescent powder and aluminum nitrate (AlNO for being 5~30um by suitable particle size3) it is scattered in solution
In (preferably dehydrated alcohol), precipitating reagent is added while stirring, precipitating reagent can be ammonium hydroxide or ammonium salt (such as ammonium hydrogen carbonate), sufficiently
The suspension that the YAG:Ce fluorescent powder of one layer of aluminium salt (that is, aluminium hydroxide) is coated with to surface is obtained after reaction；One layer will be coated with
It is neutral and drying that the suspension of the YAG:Ce fluorescent powder of aluminium salt, which is cleaned with deionized water to PH, in the heat by 300~600 DEG C
The YAG:Ce fluorescent powder grain that one layer of aluminium oxide is coated with to surface is obtained after processing.Although it should be pointed out that using here
Aluminum nitrate (AlNO3) wrapped on the surface of YAG:Ce fluorescent powder as raw material and using ammonium hydroxide or ammonium salt as precipitating reagent
One layer of aluminium salt is covered, but the invention is not restricted to this, and those skilled in the art can choose any appropriate aluminum contained compound conduct
Raw material, and select suitable deposition agent to realize in YAG:Ce fluorescent powder according to the type of selected aluminum contained compound raw material
Surface on coat one layer of aluminium salt purpose.Illustratively, in some other embodiment, sodium metaaluminate can be selected
(NaAlO2) it is used as raw material, while dilute hydrochloric acid (HCl) is selected as precipitating reagent to coat one on the surface of YAG:Ce fluorescent powder
Layer aluminium salt (that is, aluminium hydroxide).In addition, it is necessary to explanation, although coprecipitation is employed herein in YAG:Ce fluorescent powder
One layer of aluminium salt is coated on surface, but the invention is not restricted to this, and one layer of aluminium can be coated on the surface of YAG:Ce fluorescent powder
Any means of salt can use, such as spray drying process etc..It is understood that aluminium salt here is broadest containing aluminium
Compound, for example including aluminium hydroxide (Al (OH)3), aluminum nitrate (AlNO3), aluminum sulfate (Al2(SO4)3) and such as meta-aluminic acid
Sodium (NaAlO2) and potassium metaaluminate (KAlO2) etc. meta-aluminates etc..
Then second step S2 is executed, mixing is carried out: being the aluminum oxynitride powder of 0.05~5um, in S1 by particle size
Obtained surface is coated with the sintering aid that the YAG:Ce fluorescent powder, solvent and particle size of one layer of aluminium oxide are 0.02~1um
Y2O3Or the uniform mixing and ball milling of MgO 6~for 24 hours, be made aluminum oxynitride and above-mentioned surface be coated with one layer of aluminium oxide YAG:Ce it is glimmering
The mixed slurry of light powder, wherein sintering aid accounts for aluminum oxynitride, is coated with the YAG:Ce fluorescent powder of one layer of aluminium oxide and sintering helps
The 0.01~4% of the gross mass of agent.
Then third step S3 is executed, forming of green body is carried out: mixed slurry obtained in S2 being placed in drying in baking oven, so
After be ground up, sieved to avoid powder reuniting and adverse effect generated to ceramic post sintering, later under the dry-pressing pressure of 10~20MPa
Keep its dry-pressing formed, then under the hydrostatic pressure of 200~300MPa by etc. static pressure suppressions obtain biscuit, and to the element
Base carries out ungrease treatment to obtain ceramic body, and wherein the skimming temp of biscuit is 500~1000 DEG C, and degreasing time is 2~5h.
Then execute four steps S4, carry out ceramic post sintering: by hot pressed sintering mode 20~80MPa sintering pressure
And be sintered ceramic body obtained in S3 under about 1600~2000 DEG C of sintering temperature, then by sintered ceramics
Being made annealing treatment in nitrogen atmosphere with obtain having structure as shown in Figure 2 includes fluorescent powder, aluminium oxide phase and nitrogen oxygen
Change the complex phase fluorescence ceramics of aluminium phase.
The 5th step S5 is finally executed, ceramic post-processing is carried out: complex phase fluorescence ceramics obtained in S4 is carried out including subtracting
The post-processing such as thin and polishing treatment.
In the present embodiment, the aluminium oxide of obtained YAG:Ce phosphor surface cladding with a thickness of 0.05~5um, with
It can be realized the complete cladding to fluorescent powder and there is good light transmission rate.It is understood that working as the thickness of aluminium oxide
In the case where relatively thin, aluminium oxide may not be able to mutually realize complete cladding to fluorescent powder, it is possible to occur aluminum oxynitride phase with it is glimmering
The case where light powder directly contacts causes the sintered density of prepared complex phase fluorescence ceramics not good enough.It will also be appreciated that
In the case that the thickness of aluminium oxide is thicker, light transmission rate can be reduced, and influence the light extraction efficiency of fluorescent powder.Therefore, conjunction is prepared
The aluminium oxide of suitable thickness is mutually important for the present invention.It should be noted that the thickness of the aluminium oxide phase of phosphor surface cladding
Degree can by adjusting precipitation solution concentration or repeat precipitating in S1, sintering process (that is, alumina-coated technique)
The modes such as multiple are carried out to control.Illustratively, first step S1 can be executed by following procedure to obtain the oxygen of required thickness
Change aluminium phase, it is (preferably anhydrous to disperse solution for commercial YAG:Ce fluorescent powder and aluminum nitrate that suitable particle size is 5~30um
Ethyl alcohol) in, precipitating reagent is added while stirring, precipitating reagent can be ammonium hydroxide or ammonium salt (such as ammonium hydrogen carbonate), sufficiently after reaction
The suspension of the YAG:Ce fluorescent powder of one layer of aluminium salt (that is, aluminium hydroxide) is coated with to surface；One layer of aluminium salt will be coated with
The suspension of YAG:Ce fluorescent powder cleaned with deionized water to PH be it is neutral and dry, the heat treatments by 300~600 DEG C it
The YAG:Ce fluorescent powder that one layer of aluminium oxide is coated with to surface is obtained afterwards；Then, the YAG:Ce fluorescence of one layer of aluminium oxide will be coated with
Powder is scattered in solution (preferably dehydrated alcohol) again with aluminum nitrate, and precipitating reagent is added while stirring, sufficiently in YAG after reaction:
One layer of aluminium salt (that is, aluminium hydroxide) is coated on the basis of the alumina layer of Ce fluorescent powder again, and again passes by 300~600
DEG C heat treatment after the YAG:Ce fluorescent powders of more aluminium oxide is coated with to surface.Although be pointed out that here with
Example way is repeated once oxidation aluminium cladding process process, but according to the difference of used precipitant concentration,
It can also repeat multiple this alumina-coated technical process, to obtain the aluminium oxide phase of required thickness.
In the present embodiment, by the surface of YAG:Ce fluorescent powder coat one layer of aluminium oxide, then with aluminum oxynitride
Powder is mixed together and is sintered, and can contact to avoid the poor YAG:Ce fluorescent powder of compatibility with the direct of aluminum oxynitride, and
It is mediate by aluminium oxide, and overcomes YAG:Ce fluorescent powder and nitrogen respectively with alumina sintering densification during the sintering process
The problem of alumina sintering low density, to obtain the complex phase fluorescence ceramics that mechanical strength is improved.
Embodiment 2
Fig. 4 shows the flow chart of the preparation method of according to embodiments of the present invention 2 complex phase fluorescence ceramics.In the present embodiment
In, as in Example 1, selects the aluminum oxynitride of high-purity as matrix phase raw material, commercialization YAG:Ce fluorescent powder is selected to make
For the phase raw material that shines, polyvinyl butyral (PVB) is selected to be used as bonding agent, and dispersing agent, sintering aid can be elected additional member etc.,
To prepare complex phase fluorescence ceramics.Specific preparation method is as follows.
First step S1 is first carried out, coats one layer of aluminium oxide difference with the surface of YAG:Ce fluorescent powder is made in embodiment 1,
Be that the surface of aluminum oxynitride powder is made to coat one layer of aluminium oxide in the present embodiment: the same method using co-precipitation is in nitrogen oxidation
Coated on the surface of aluminium powder body one layer of aluminium salt be coated with to surface the aluminum oxynitride powder of one layer of aluminium salt, coprecipitation method and
Embodiment 1 is identical.Specifically, the aluminum oxynitride powder and aluminum nitrate (AlNO for being 0.05~1um by suitable particle size3) point
It dissipates in solution (preferably dehydrated alcohol), precipitating reagent is added while stirring, precipitating reagent can be ammonium hydroxide or ammonium salt (such as bicarbonate
Ammonium), sufficiently the suspension that the aluminum oxynitride powder of one layer of aluminium salt (that is, aluminium hydroxide) is coated with to surface is obtained after reaction；It will packet
It is neutral and dry for being covered with the suspension of the aluminum oxynitride powder of one layer of aluminium salt and being cleaned with deionized water to PH, by 300~
The aluminum oxynitride powder that one layer of aluminium oxide is coated with to surface is obtained after 600 DEG C of heat treatment, wherein the grain of aluminum oxynitride powder
Diameter size be 0.05~1um, smaller than 5~30um of partial size of commercial fluorescent powder, specific surface area is bigger, thus in embodiment 1
It is compared in phosphor surface coated aluminum oxide, it is higher in the feasibility that the surface of aluminum oxynitride powder coats one layer of aluminium oxide.With
It is identical in embodiment 1, in the present embodiment, it also can choose any appropriate aluminum contained compound as raw material, and according to institute
The type of the aluminum contained compound raw material of selection selects suitable deposition agent and coats one on the surface of aluminum oxynitride powder to realize
The purpose of layer aluminium salt.Equally, in the same manner as in Example 1, the energy other than coprecipitation also can be used in the present embodiment
Any means of one layer of aluminium salt are coated on the surface of aluminum oxynitride powder enough to coat one on the surface of aluminum oxynitride powder
Layer aluminium salt, such as spray drying process etc..
Then second step S2 is executed, mixing is carried out: surface obtained in S1 is coated with to the nitrogen oxidation of one layer of aluminium oxide
The sintering that commercial YAG:Ce fluorescent powder, solvent and the particle size that aluminium powder body, particle size are 5~30um are 0.02~1um helps
Agent Y2O3Or the uniform mixing and ball milling of MgO 6~for 24 hours, aluminum oxynitride and YAG:Ce that above-mentioned surface is coated with one layer of aluminium oxide is made
The mixed slurry of fluorescent powder, wherein sintering aid account for surface be coated with the aluminum oxynitride of one layer of aluminium oxide, YAG:Ce fluorescent powder with
The 0.01~4% of the gross mass of sintering aid.
Then third step S3 is executed, forming of green body is carried out: mixed slurry obtained in S2 being placed in drying in baking oven, so
After be ground up, sieved to avoid powder reuniting and adverse effect generated to ceramic post sintering, later under the dry-pressing pressure of 10~20MPa
Keep its dry-pressing formed, then under the hydrostatic pressure of 200~300MPa by etc. static pressure suppressions obtain biscuit, and to the element
Base carries out ungrease treatment to obtain ceramic body, and wherein the skimming temp of biscuit is 500~1000 DEG C, and degreasing time is 2~5h.
Then execute four steps S4, carry out ceramic post sintering: by hot pressed sintering mode 20~80MPa sintering pressure
And be sintered ceramic body obtained in S3 under about 1600~2000 DEG C of sintering temperature, then by sintered ceramics
Made annealing treatment in nitrogen atmosphere with obtain equally with structure as shown in Figure 2 comprising fluorescent powder, aluminium oxide phase and
The complex phase fluorescence ceramics of aluminum oxynitride phase.
The 5th step S5 is finally executed, ceramic post-processing is carried out: complex phase fluorescence ceramics obtained in S4 is post-processed,
Including thinned and polishing treatment.
Equally, in the present embodiment, the aluminium oxide of obtained aluminum oxynitride powder surface cladding with a thickness of 0.05~
5um, can be realized the complete cladding to aluminum oxynitride powder and there is good light transmission rate.As in Example 1,
Can by adjusting precipitation solution concentration or make precipitating in S1, sintering process (that is, alumina-coated technique) repeat into
The modes such as multiple go to control the thickness of the aluminium oxide phase of aluminum oxynitride powder surface cladding.
In the present embodiment, by the surface of aluminum oxynitride powder coat one layer of aluminium oxide, then with YAG:Ce fluorescence
Powder is mixed together and is sintered, and can equally contact to avoid the poor YAG:Ce fluorescent powder of compatibility with the direct of aluminum oxynitride,
But it is mediate by aluminium oxide, and YAG:Ce fluorescence is equally overcome respectively with alumina sintering densification during the sintering process
The problem of powder and aluminum oxynitride sintered density difference, to obtain the complex phase fluorescence ceramics that mechanical strength is improved.
Embodiment 3
Fig. 5 shows the flow chart of the preparation method of according to embodiments of the present invention 3 complex phase fluorescence ceramics.The present embodiment with
Embodiment 1 and embodiment 2 are different.In the first step S1 of the present embodiment, not in fluorescent powder or the table of aluminum oxynitride powder
Face coated aluminum oxide, but alumina powder, aluminum oxynitride powder, commercialization YAG:Ce fluorescent powder, solvent and sintering aid is straight
Uniform mixing and ball milling 6~for 24 hours is connect, the mixed slurry comprising alumina powder, aluminum oxynitride powder and YAG:Ce fluorescent powder is made.
Then second step S2 is executed, forming of green body is carried out: mixed slurry obtained in S1 being placed in drying in baking oven, so
After be ground up, sieved to avoid powder reuniting and adverse effect generated to ceramic post sintering, later under the dry-pressing pressure of 10~20MPa
Keep its dry-pressing formed, then under the hydrostatic pressure of 200~300MPa by etc. static pressure suppressions obtain biscuit, and to the element
Base carries out ungrease treatment to obtain ceramic body, and wherein the skimming temp of biscuit is 500~1000 DEG C, and degreasing time is 2~5h.
Then execute third step S3, carry out high temperature sintering: by hot pressed sintering mode 20~80MPa sintering pressure
And be sintered ceramic body obtained in S2 under about 1600~2000 DEG C of sintering temperature, then by sintered ceramics
It is made annealing treatment in nitrogen atmosphere to obtain the complex phase fluorescence ceramics comprising fluorescent powder, aluminium oxide phase and aluminum oxynitride phase.
Four steps S4 is finally executed, ceramic post-processing is carried out: complex phase fluorescence ceramics obtained in S3 is carried out including subtracting
The post-processing such as thin and polishing treatment.
In the present embodiment, in embodiment 1 and embodiment 2 in YAG:Ce fluorescent powder or aluminum oxynitride powder surface packet
Cover one layer of aluminium oxide, then it is different from aluminum oxynitride powder or the complex sintered formation complex phase fluorescence ceramics of YAG:Ce fluorescent powder again,
Without carrying out this cladding processing in the present embodiment, but by YAG:Ce fluorescent powder, alumina powder and aluminum oxynitride powder this
Three-phase is uniformly mixed and is sintered.The ceramics of this method production cannot avoid YAG:Ce fluorescent powder and nitrogen oxygen completely in the present embodiment
Change the direct contact between aluminium phase, therefore intensity is slightly lower compared with the structure of ceramics prepared in embodiment 1 and embodiment 2,
But to a certain extent, therefore the addition of aluminium oxide can still be reduced the phase interface between YAG:Ce fluorescent powder and aluminum oxynitride phase
Still very big improvement, while the standby side of this ceramic system have been carried out to the sintered density of YAG:Ce/AlON complex phase fluorescence ceramics
Method is also fairly simple compared with embodiment 1 and embodiment 2, and can add more aluminium oxide in a simple manner, in oxygen
In the increased situation of content for changing aluminium, the thermal conductivity of obtained complex phase fluorescence ceramics can also be higher.
Embodiment 4
In the present embodiment, compared with embodiment 1, embodiment 2 and embodiment 3, increase in used Binder Phase AlON
Active ions Mn is added2+, rest part is identical as in embodiment 1, embodiment 2 and embodiment 3, to prepare comprising Υ-
AlON:Mn2+Another complex phase fluorescence ceramics of green light ceramics.The advantages of complex phase fluorescence ceramics prepared in the present embodiment, is energy
Enough supplement YAG:Ce3+Green light it is insufficient, promote the colour rendering index of green light band.
The fluorescence ceramics prepared in above-described embodiment 1~4 are complex phase fluorescence ceramics, and bonding is mutually AlON and Al2O3, hair
Light is mutually YAG:Ce fluorescent powder, and for the complex phase fluorescence ceramics there are two types of structure, a kind of structure is the thin layer oxygen of phosphor surface cladding
Change aluminium (0.05~5um of thickness) and the compound complex phase ceramic of aluminum oxynitride, is also possible to the oxygen of aluminum oxynitride powder surface cladding
Change aluminium (0.05~5um) and the compound complex phase ceramic of fluorescent powder；Another structure is alumina powder, aluminum oxynitride powder, glimmering
The uniform compound complex phase ceramic of light powder；In addition, aluminum oxynitride ceramic is also possible to Υ-AlON:Mn2+Green light ceramics.Of the invention
Complex phase fluorescence ceramics are with high luminous efficiency, high thermal conductivity, excellent resistance to heat shocks energy and excellent mechanical strength
Luminescent ceramic, in light efficiency still with higher when being machined to 100um or less and stronger mechanical strength and resistance to heat shocks energy,
High-power white light can be issued, realizes higher processing yield and easier mass production encapsulation, it can be by high-power exciting light
Source excitation realizes the semiconductor light source of high brightness, such as high-power white light LED light source, blue laser light source.
In the above-described embodiments, the particle size of aluminum oxynitride powder is 0.05~1um, and the partial size of YAG:Ce fluorescent powder is big
Small is 5~30um, and fluorescent powder accounts for the 20~80% of the gross mass of aluminum oxynitride, fluorescent powder and sintering aid, sintering aid Y2O3
Or MgO, the partial size of sintering aid is 0.02~1um, and sintering aid accounts for the gross mass of aluminum oxynitride, fluorescent powder and sintering aid
0.01~4%.
On the other hand, the fluorescent powder in above-described embodiment also could alternatively be LuAG:Ce fluorescent powder, the complex phase so prepared
The structure of fluorescence ceramics is LuAG:Ce-Al2O3- AlON, wherein shining mutually is LuAG:Ce fluorescent powder.Height equally may be implemented in this
Sintered density and high light efficiency, in light efficiency still with higher when being machined to 100um or less and stronger mechanical strength
With resistance to heat shocks energy, while also there is high thermal conductivity, therefore high-power white light can be issued, realize higher processing yield with
And easier mass production encapsulation, the semiconductor light source of high brightness, such as high-power white can be realized by high-power blue-light light source activation
Light LED light source, blue laser light source etc..
The bound of each raw material cited by the present invention and each raw material of the present invention, the bound of technological parameter, section take
Value can realize the present invention, embodiment numerous to list herein；According to the technical essence of the invention to above embodiments institute
Any simple modification or equivalent variations made, within the scope of still falling within technical solution of the present invention.
Claims (10)
1. a kind of complex phase fluorescence ceramics, which is characterized in that the complex phase fluorescence ceramics include as matrix phase aluminum oxynitride phase,
The fluorescent powder that is evenly distributed in described matrix phase and oxygen together is mixed with the fluorescent powder and the aluminum oxynitride
Change aluminium phase.
2. complex phase fluorescence ceramics as described in claim 1, which is characterized in that
The fluorescent powder and the aluminum oxynitride are mutually mutually separated from each other via the aluminium oxide.
3. complex phase fluorescence ceramics as claimed in claim 2, which is characterized in that
The aluminium oxide is mutually coated on the surface of the fluorescent powder or the aluminum oxynitride phase.
4. complex phase fluorescence ceramics according to any one of claims 1 to 3, which is characterized in that
The fluorescent powder is YAG:Ce fluorescent powder or LuAG:Ce fluorescent powder.
5. complex phase fluorescence ceramics according to any one of claims 1 to 3, which is characterized in that
The aluminium oxide phase with a thickness of 0.05~5um.
6. complex phase fluorescence ceramics according to any one of claims 1 to 3, which is characterized in that
The fluorescent powder accounts for the 20~80% of the complex phase fluorescence ceramics total volume.
7. complex phase fluorescence ceramics according to any one of claims 1 to 3, which is characterized in that
It further include active ions Mn in the aluminum oxynitride phase2+。
8. a kind of preparation method of complex phase fluorescence ceramics, the described method comprises the following steps:
S1: coating one layer of aluminium oxide on the surface of fluorescent powder or aluminum oxynitride powder, and the particle size of the fluorescent powder is 5~
The particle size of 30um and the aluminum oxynitride powder is 0.05~1um；
S2: the product after the cladding being prepared in S1 is uniformly mixed with aluminum oxynitride powder or fluorescent powder, auxiliary agent and solvent
Ball milling is to be made the mixed slurry comprising these raw materials；
S3: the mixed slurry being prepared in S2 is dry and dry-pressing formed, then by etc. static pressure suppressions obtain element
Base, and ungrease treatment is carried out to obtain ceramic body to the biscuit；
S4: the ceramic body being prepared in S3 is sintered to obtain comprising fluorescent powder, aluminium oxide phase and nitrogen
The complex phase fluorescence ceramics of aluminium oxide phase.
9. method according to claim 8, which is characterized in that after step s4 further include step S5: to being prepared into S4
To the complex phase fluorescence ceramics post-processed, it is described post-processing include reduction processing and polishing treatment.
10. method according to claim 8, which is characterized in that
In S1, one layer of aluminium oxide is coated on the surface of fluorescent powder or aluminum oxynitride powder and is realized by the following method:
Then method using co-precipitation makes to be coated with one layer of aluminium in coating one layer of aluminium salt on the surface of fluorescent powder or aluminum oxynitride powder
The fluorescent powder or aluminum oxynitride powder of salt are through Overheating Treatment, to obtain the fluorescent powder or nitrogen oxygen for being coated with one layer of aluminium oxide to surface
Change aluminium powder body.
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