CN110386822A - A kind of complex phase fluorescence ceramics and preparation method thereof - Google Patents
A kind of complex phase fluorescence ceramics and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of novel complex phase fluorescence ceramics and preparation method thereof.The complex phase fluorescence ceramics include: the aluminium nitride phase as matrix phase, the fluorescent powder that is evenly distributed in described matrix phase and the aluminum oxynitride phase between the aluminium nitride phase and the fluorescent powder, wherein the aluminium nitride phase is mutually separated from each other with the fluorescent powder via the aluminum oxynitride.By the present invention in that coat one layer of aluminium salt on the surface of fluorescent powder or aluminium nitride with coprecipitation, then the mixed slurry for containing fluorescent powder or aluminium nitride and aluminium nitride or fluorescent powder that surface is coated with one layer of aluminium salt is sintered to prepare complex phase fluorescence ceramics of the invention.Complex phase fluorescence ceramics according to the present invention are a kind of High Efficiency Luminescence ceramics with high thermal conductivity, high consistency and good mechanical strength, it can be by high-power exciting light source activation, such as high-power blue-light LD or blue-ray LED, the lighting source for realizing high brightness, further increases illumination or the brightness of projection light source.
Description
Technical field
The present invention relates to a kind of complex phase fluorescence ceramics with high thermal conductivity, high consistency and high luminous efficiency and
Preparation method.
Background technique
Currently, pre- to obtain using the light source activations luminescent material such as laser diode (LD) or light emitting diode (LED)
Order coloured light or heterogeneous light technology are widely used in the fields such as lighting source, Projection Display.It is wanted with to light-source brightness
Ask higher and higher, the power of blue light LD or blue-ray LED excitation light source is higher and higher, so to the performance requirement of luminescent material
It is higher and higher.On the one hand it requires the luminescent properties of luminescent material to get well, on the other hand also requires mechanical performance, the heat of luminescent material
The characteristics such as conductance are more preferable.In this case, the mode of silica gel packaging fluorescent powder or fluorescent glass is high far from meeting
The requirement of power light-sources excitation, ceramics are widely used in height since its mechanical performance and thermal conductivity are above silica gel and glass
Power light-sources excitation, especially high-power LD light source.
Blue light LD has lot of advantages as excitation light source: (1) without " efficiency rapid drawdown " phenomenon, therefore can be single by improving
A chip goes out luminous intensity to reduce cost of light source；(2) nearly monochromaticjty, can be matched according to LD output wavelength suitable fluorophor with
Realize high conversion efficiency；(3) volume is smaller, brightness is higher, is easier to design terminal working flare；(4) there is better controllability, packet
It is controllable etc. to include photochromic adjustable, time and space.Blue light LD is likely to become the best excitation light source of higher source luminance.Compared to blue light
The hot spot of LED, blue light LD light source are smaller and more powerful, and the optical power density of hot spot is bigger, thus to the machine of luminescent ceramic
Tool performance and thermal conductivity have higher requirement.
Currently, common fluorescence ceramics are generally divided into two kinds: one is pure phase luminescent ceramic (that is, single-phase luminescent ceramic),
Such as YAG:Ce or LuAG:Ce ceramics, at porcelain phase and to shine mutually be that same phase and can sinter the higher pottery of transparency into
Porcelain, but the thermal conductivity of YAG:Ce or LuAG:Ce ceramics is lower.Another kind is complex phase luminescent ceramic, such as Al2O3&YAG:Ce pottery
Porcelain or AlN&YAG:Ce ceramics etc., bonding are mutually Al2O3Or AlN etc., shining mutually is YAG:Ce fluorescent powder.Al2O3&YAG:
Ce ceramic machinery intensity is high, but thermal conductivity is lower, and the thermal conductivity of AlN&YAG:Ce ceramics is high.However, AlN&YAG:Ce makes pottery
The thermal expansion coefficient of AlN is 4.6 × 10 in porcelain-6The thermal expansion coefficient of/K, YAG:Ce are 8.0 × 10-6/ K, the two thermal expansion system
Number difference is larger, and the complex phase ceramic AlN&YAG:Ce thermal stress for causing it to be sintered is larger, thus its consistency is lower, mechanical strength
It is poor.
It would therefore be highly desirable to which the problem solved is to develop one kind both to have high thermal conductivity, it may have high consistency
With the luminescent ceramic of good mechanical strength, the luminescent ceramic can adapt to high-power blue-light LD or the luminous of LED light source is wanted
It asks.
Summary of the invention
Technical problem
In view of this, to solve the above-mentioned problems, the present invention is intended to provide a kind of novel complex phase fluorescence ceramics, described multiple
Phase fluorescence ceramics are that both have high thermal conductivity, it may have the High Efficiency Luminescence ceramics of high consistency and good mechanical strength.
Meanwhile the present invention is also directed to a kind of preparation method of this novel complex phase fluorescence ceramics to prepare with above-mentioned performance
Complex phase fluorescence ceramics.
Technical solution
According to an aspect of the present invention, a kind of complex phase fluorescence ceramics are provided, the complex phase fluorescence ceramics include: as base
The aluminium nitride phase of body phase, the fluorescent powder being evenly distributed in described matrix phase and be located at the aluminium nitride phase and the fluorescent powder
Between aluminum oxynitride phase, wherein the aluminium nitride phase is mutually separated from each other with the fluorescent powder via the aluminum oxynitride.
Further, the aluminum oxynitride is mutually coated on the surface of the fluorescent powder and/or the aluminium nitride phase.
Further, the aluminum oxynitride is mutually described by being coated in the sintering process of the complex phase fluorescence ceramics
What the aluminium salt of fluorescent powder or the aluminium nitride phase surface and the aluminium nitride phase reaction generated.
Further, the fluorescent powder is YAG:Ce fluorescent powder or LuAG:Ce fluorescent powder.
Further, the aluminum oxynitride phase with a thickness of 0.05~1um.
Further, the fluorescent powder accounts for the 20~80% of the complex phase fluorescence ceramics total volume.
Further, the particle size of the fluorescent powder is 1~30um.
Further, the particle size of the aluminium nitride phase is 0.2~10um.
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 salt on the surface of fluorescent powder or aluminium nitride powder, and the particle size of the fluorescent powder is 1~
The particle size of 30um and the aluminium nitride powder is 0.05~1um；S2: by after the cladding being prepared in S1 product with
Aluminium nitride powder or fluorescent powder grain, auxiliary agent and the uniform mixing and ball milling of solvent are 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 biscuit, and it is right
The biscuit carries out ungrease treatment to obtain ceramic body；S4: place is sintered to the ceramic body being prepared in S3
Reason is to obtain the complex phase fluorescence ceramics comprising fluorescent powder, aluminum oxynitride phase and aluminium nitride phase.
Further, after step s4 further include step S5: to the complex phase fluorescence ceramics being prepared in S4 into
Row post-processing, the post-processing include reduction processing and polishing treatment.
Further, in S1, coating one layer of aluminium salt on the surface of fluorescent powder or aluminium nitride powder is by such as lower section
What method was realized: being wrapped on the surface of fluorescent powder or aluminium nitride powder using the method for co-precipitation using aluminum contained compound and precipitating reagent
Cover one layer of aluminium salt.
Beneficial effect
In the present invention, the preparation of complex phase fluorescence ceramics according to the present invention and complex phase fluorescence ceramics according to the present invention
The complex phase fluorescence ceramics of method preparation are a kind of efficient hairs with high thermal conductivity, high consistency and good mechanical strength
Light ceramic can be excited by high-power blue-light LD or blue-ray LED, realize the lighting source of high brightness, further increase illumination or
The brightness of projection light source.
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 the present invention.
Fig. 2 is the flow chart of the preparation method of according to embodiments of the present invention 1 complex phase fluorescence ceramics.
Fig. 3 is the flow chart of another preparation method of according to embodiments of the present invention 3 complex phase fluorescence ceramics.
Reference signs list
1: fluorescent powder
2: aluminum oxynitride phase
3: aluminium nitride 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 complex phase fluorescence ceramics, as shown in Figure 1, the complex phase fluorescence ceramics include fluorescent powder 1, nitrogen oxygen
Change aluminium phase 2 and aluminium nitride phase 3.Aluminium nitride phase 3 is matrix phase, and fluorescent powder 1 is evenly distributed in matrix phase.Aluminum oxynitride phase 2
Between fluorescent powder 1 and aluminium nitride phase 3.Specifically, aluminum oxynitride phase 2 can be coated on the outer surface of fluorescent powder 1.It is optional
Ground is selected, aluminum oxynitride phase 2 can also be coated on the surface of aluminium nitride phase 3.In other words, fluorescent powder 1 and aluminium nitride phase 3 can be with
It is separated from each other via aluminum oxynitride phase 2.That is, aluminum oxynitride phase 2 can at phase interface respectively with fluorescent powder 1 and nitridation
The contact of aluminium phase 3 is combined together, and fluorescent powder 1 and aluminium nitride phase 3 are not directly contacted with, that is, between fluorescent powder 1 and aluminium nitride phase 3
There is no phase interfaces.As described above, complex phase fluorescence ceramics of the invention include matrix phase and luminous phase two-phase, wherein matrix phase
(that is, at porcelain phase) is aluminium nitride and aluminum oxynitride phase, and shining mutually is fluorescent powder phase.Selectively, fluorescent powder can be for such as YAG:
Ce fluorescent powder or LuAG:Ce fluorescent powder etc., and the partial size of fluorescent powder can be 1~30um.Fluorescent powder passes through surface coated
Aluminium salt is complex sintered with aluminium nitride and forms the complex phase fluorescence ceramics comprising aluminium nitride phase, aluminum oxynitride phase and fluorescent powder,
The aluminum oxynitride phase of middle phosphor surface with a thickness of 0.05~1um to avoid thickness is too thin and leads to that fluorescence cannot be coated completely
Larger difficulty on grain and manufacture craft, while it is too thick and lead to the reduction of light transmittance and influence fluorescent powder to also avoid thickness
The light extraction efficiency of particle.In addition, in order to make obtained complex phase fluorescence ceramics have good luminous efficiency, fluorescent powder can be accounted for
The 20~80% of complex phase fluorescence ceramics total volume.Using YAG:Ce or LuAG:Ce as fluorescent powder of the invention,
The structure of complex phase fluorescence ceramics of the invention is YAG:Ce-AlON-AlN or LuAG:Ce-AlON-AlN, and shining mutually is YAG:
Ce or LuAG:Ce, matrix are mutually AlN and AlON.
In complex phase fluorescence ceramics of the invention, due to aluminum oxynitride phase (AlON) be located at fluorescent powder (YAG:Ce or LuAG:
Ce it) is not directly contacted between aluminium nitride phase (AlN) and between fluorescent powder and aluminium nitride phase (between the two without phase interface),
So only existing the phase interface between aluminum oxynitride phase and fluorescent powder and the phase interface between aluminum oxynitride phase and aluminium nitride phase.
On the one hand, aluminum oxynitride is mutually that aluminium salt and aluminium nitride Binder Phase by coating on the surface of fluorescent powder or aluminium nitride powder exist
Reaction is formed in sintering process, which ensure that enough adhesion strengths between aluminum oxynitride phase and aluminium nitride phase, simultaneously because
The compatibility of aluminum oxynitride and both aluminium nitride is preferable, so can burn at the phase interface between aluminum oxynitride phase and aluminium nitride phase
Knot is fine and close.On the other hand, since the thermal expansion coefficient of aluminum oxynitride is 7.9 × 10-6The thermal expansion coefficient of/K, YAG fluorescent powder is
8.0×10-6/ K, the two is about the same, so not having thermal stress between aluminum oxynitride phase and fluorescent powder during the sintering process, is sintered
Consistency is higher, and mechanical strength is preferable, therefore solves AlN and the interface YAG:Ce in AlN&YAG:Ce ceramics in the prior art
In conjunction with poor problem.In addition, it should be noted that, aluminum oxynitride is mutually cubic system, exists and will not influence the saturating of ceramics
Lightness and luminous efficiency.In addition, complex phase fluorescence ceramics of the invention also have high thermal conductivity due to the presence of AlN.Therefore,
The present invention provides a kind of fluorescence with high thermal conductivity, high consistency, good mechanical strength and high luminous efficiency
Ceramics, the luminescent ceramic High Efficiency Luminescence and can be realized when being irradiated by the high powers excitation light source such as blue light LD or blue-ray LED
The lighting source of high brightness to further increase illumination and the brightness of projection light source, therefore can adapt to high-power blue-light LD
Or the lighting requirements of the high powers excitation light source such as LED 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: coating one layer of aluminium salt on the surface of fluorescent powder (or aluminium nitride powder), and the particle size of the fluorescent powder is 1
The particle size of~30um and the aluminium nitride powder is 0.05~1um.Specifically, it is used using the method for co-precipitation and contains aluminium
Compound and precipitating reagent coat one layer of aluminium salt on the surface of fluorescent powder or aluminium nitride powder.
S2: by after the cladding being prepared in S1 product and aluminium nitride 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 aluminium
Fluorescent powder (or aluminium nitride powder) and aluminium nitride powder (or fluorescent powder), the auxiliary agent and the uniform mixing and ball milling of solvent of salt are wrapped with being made
It is mixed containing fluorescent powder (or aluminium nitride powder), aluminium nitride powder (or fluorescent powder) and the auxiliary agent and solvent for being coated with one layer of aluminium salt
Slurry is closed, wherein auxiliary agent may include sintering aid and dispersing agent etc., and sintering aid can be Y2O3Or MgO, sintering aid
Partial size can be 0.02~1um, and sintering aid accounts for fluorescent powder (or aluminium nitride powder), the aluminium nitride for being coated with one layer of aluminium salt
The 0.01~4 of powder (or fluorescent powder) and sintering aid gross mass.
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
There is the mixed slurry of the fluorescent powder (or aluminium nitride powder) of one layer of aluminium salt, aluminium nitride powder (or fluorescent powder) and auxiliary agent and solvent
It is placed in baking oven dry, keeps its dry-pressing formed under the dry-pressing pressure of 10~20MPa, then in the equal static pressure of 200~300MPa
Under pressure by etc. static pressure suppressions obtain biscuit, wherein the skimming temp of biscuit can be 800~1000 DEG C, and degreasing time can
Think 2~6h.
S4: the ceramic body being prepared in S3 is sintered to obtain comprising fluorescent powder, aluminum oxynitride
The complex phase fluorescence ceramics of phase and aluminium nitride phase.Specifically, the ceramic bad body being prepared in S3 is put into sintering furnace and is burnt
Knot, cooling obtains the complex phase fluorescence ceramics comprising fluorescent powder, aluminum oxynitride phase and aluminium nitride 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, one layer of aluminium then will be coated with by coating one layer of aluminium salt on the surface of fluorescent powder (or aluminium nitride powder)
The fluorescent powder (or aluminium nitride powder) of salt is mixed and is sintered with aluminium nitride powder (or fluorescent powder), can be by during the sintering process
So that aluminium salt, which is first reacted, forms aluminium oxide, nitrogen oxidation then is formed between fluorescent powder and aluminium nitride phase with reactive aluminum is nitrogenized again
Aluminium phase, it is hereby ensured that aluminum oxynitride mutually between fluorescent powder and aluminium nitride phase and fluorescent powder and aluminium nitride mutually each other it
Between be not directly contacted with.That is, fluorescent powder is mutually combined together by aluminum oxynitride with aluminium nitride.In other words, it is burning
During knot, only there are phase interfaces between aluminum oxynitride phase and fluorescent powder and between aluminum oxynitride phase and aluminium nitride phase, and
Phase interface is not present between fluorescent powder and aluminium nitride phase.Due to having good compatibility between aluminum oxynitride and aluminium nitride,
So sintered density is high at phase interface between aluminum oxynitride phase and aluminium nitride phase, and since aluminum oxynitride is mutually to pass through aluminium
What salt and aluminium nitride phase reaction generated, so the adhesion strength between aluminum oxynitride phase and aluminium nitride phase is also bigger.In addition, by
It is essentially identical in the thermal expansion coefficient of aluminum oxynitride and fluorescent powder, therefore there is no thermal stress between aluminum oxynitride and fluorescent powder, it can
With densified sintering product, the relatively high complex phase ceramic of mechanical strength is obtained.In other words, the present invention solves the thermal expansion system of aluminium nitride
The complex phase ceramic AlN&YAG:Ce heat of aluminium nitride and fluorescent powder is answered caused by number differs larger with the thermal expansion coefficient of fluorescent powder
The problem that power is larger, consistency is lower, mechanical strength is poor.In addition, as described above, the complex phase fluorescence ceramics of AlN&YAG:Ce have
There is high thermal conductivity, therefore, the present invention has prepared a kind of luminescent ceramic with high thermal conductivity and good mechanical strength,
The luminescent ceramic High Efficiency Luminescence and can realize high brightness when being irradiated by the high powers excitation light source such as blue light LD or blue-ray LED
Lighting source, to further increase illumination and the brightness of projection light source, therefore can adapt to high-power blue-light LD or LED light
The lighting requirements in source.
Referring to specific embodiment, the present invention is described in detail.
Embodiment 1
Fig. 2 shows the flow charts of the preparation method of according to embodiments of the present invention 1 complex phase fluorescence ceramics.In the present embodiment
In, use the aluminium nitride, commercialization YAG:Ce fluorescent powder and aluminum nitrate of high-purity to prepare complex phase fluorescence ceramics for raw material, wherein selecting
Use polyvinyl butyral (PVB) as bonding agent, and dispersing agent, sintering aid can be elected additional member etc..Specific preparation method is such as
Under.
First step S1 is first carried out, YAG:Ce phosphor surface is made to coat one layer of aluminium salt: the method using co-precipitation exists
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.Tool
Body, the commercial YAG:Ce fluorescent powder and aluminum nitrate (AlNO for being 1~30um by suitable particle size3) it is dissolved in aqueous solution
In, precipitating reagent is added while stirring, precipitating reagent can be ammonium hydroxide or ammonium salt (such as ammonium hydrogen carbonate), sufficiently obtain surface after reaction
It is coated with the suspension of the YAG:Ce fluorescent powder of one layer of aluminium salt (that is, aluminium hydroxide)；The YAG:Ce for being coated with one layer of aluminium salt is glimmering
It is neutral and drying that the suspension of light powder, which is cleaned with deionized water to PH, obtains to surface and is coated with the YAG:Ce fluorescence of one layer of aluminium salt
Powder particles.It should be noted that, although using aluminum nitrate (AlNO here3) as raw material and using ammonium hydroxide or ammonium salt conduct
Precipitating reagent to coat one layer of aluminium salt on the surface in YAG:Ce fluorescent powder, and but the invention is not restricted to this, those skilled in the art
Any appropriate aluminum contained compound be can choose as raw material, and selected according to the type of selected aluminum contained compound raw material
Suitable deposition agent coats the purpose of one layer of aluminium salt to realize on the surface of YAG:Ce fluorescent powder.Illustratively, other one
In a little embodiments, sodium metaaluminate (NaAlO can be selected2) it is used as raw material, while dilute hydrochloric acid (HCl) being selected to come as precipitating reagent
One layer of aluminium salt (that is, aluminium hydroxide) is coated on the surface of YAG:Ce fluorescent powder.In addition, it is necessary to explanation, although using here
Coprecipitation has coated one layer of aluminium salt on the surface of YAG:Ce fluorescent powder, and but the invention is not restricted to this, can be in YAG:
Any means that one layer of aluminium salt is coated on the surface of Ce fluorescent powder can use, such as spray drying process etc..It is understood that
It is that aluminium salt here is broadest aluminum contained compound, for example including aluminium hydroxide (Al (OH)3), aluminum nitrate (AlNO3), sulfuric acid
Aluminium (Al2(SO4)3) and such as sodium metaaluminate (NaAlO2) and potassium metaaluminate (KAlO2) etc. meta-aluminates etc..
Then second step S2 is executed, mixing is carried out: being the aluminium nitride powder of 0.05~1um, in S1 by particle size
To surface be coated with one layer of aluminium salt YAG:Ce fluorescent powder, solvent and particle size be 0.02~1um sintering aid Y2O3Or
The uniform mixing and ball milling of person MgO for a period of time, such as 6~for 24 hours, aluminium nitride is made and above-mentioned surface is coated with the YAG of one layer of aluminium salt:
The mixed slurry of Ce fluorescent powder, wherein sintering aid accounts for aluminium nitride, is coated with the YAG:Ce fluorescent powder of one layer of aluminium salt 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
Ceramic powder obtained above is dry-pressing formed, then under the hydrostatic pressure of 200~300MPa by etc. static pressure suppressions come
Biscuit is obtained, and ungrease treatment is carried out to obtain ceramic body to the biscuit, wherein the skimming temp of biscuit is 800~1000
DEG C, degreasing time is 2~6h.
Then execute four steps S4, carry out ceramic post sintering: by ceramic body obtained in S3 in vacuum atmosphere oven
It is sintered under 1600~1800 DEG C of sintering temperature, which is nitrogen, and sintering time is 6~12h, is obtained after cooling
The complex phase fluorescence ceramics comprising fluorescent powder, aluminum oxynitride phase and aluminium nitride phase with structure as shown in Figure 1.
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 aluminum oxynitride phase of obtained phosphor surface cladding with a thickness of 0.05um~1um, 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 aluminum oxynitride
Spend it is relatively thin in the case where, aluminum oxynitride may not be able to mutually realize complete cladding to fluorescent powder, it is possible to occur aluminium nitride phase with
The case where fluorescent powder directly contacts causes the sintered density of prepared complex phase fluorescence ceramics not good enough.It also will be understood that
It is that in the case that the thickness of aluminum oxynitride is thicker, light transmission rate can be reduced, influences the light extraction efficiency of fluorescent powder.Therefore, it prepares
The aluminum oxynitride of suitable thickness is mutually important for the present invention out.It should be noted that the nitrogen oxidation of phosphor surface cladding
The thickness of aluminium phase can by adjusting precipitation solution concentration or repeat precipitation process (that is, aluminium salt cladding process) in S1
The modes such as multiple are carried out to control.Illustratively, first step S1 can be executed by following procedure to obtain the nitrogen of required thickness
Aluminium oxide phase disperses commercial YAG:Ce fluorescent powder and aluminum nitrate that suitable particle size is 1~30um in aqueous solution, side
It stirs side and precipitating reagent is added, precipitating reagent can be ammonium hydroxide or ammonium salt (such as ammonium hydrogen carbonate), and surface cladding is sufficiently obtained after reaction
There is the suspension of the YAG:Ce fluorescent powder of one layer of aluminium salt (that is, aluminium hydroxide)；The YAG:Ce fluorescent powder of one layer of aluminium salt will be coated with
Suspension cleaned with deionized water to PH be it is neutral and dry, obtain to surface and be coated with the YAG:Ce fluorescent powder of one layer of aluminium salt
Grain；Then, it disperses the YAG:Ce fluorescent powder for being coated with one layer of aluminium salt in aqueous solution with aluminum nitrate again, is added while stirring
Precipitating reagent sufficiently coats one layer of aluminium salt (that is, aluminium hydroxide) after reaction again on the basis of the aluminium salt layer of YAG:Ce fluorescent powder,
And the fluorescent powder grain that more aluminium salts are coated with to surface is obtained after washing and drying.Although being pointed out that here
It is repeated an aluminium salt cladding process process by way of example, but according to the difference of used precipitant concentration,
It can also repeat multiple this aluminium salt cladding process process, so that the aluminium salt of required thickness is obtained, to obtain required thickness
The aluminum oxynitride phase of degree.
In the present embodiment, by the surface of YAG:Ce fluorescent powder coat one layer of aluminium salt, then with aluminium nitride powder one
It rising and mixes and be sintered, the YAG:Ce fluorescent powder that can differ bigger to avoid thermal expansion coefficient is contacted with the direct of aluminium nitride, and
It is mediate by aluminium salt.During the sintering process, aluminium salt first pass through chemical reaction generate aluminium oxide, then again with nitridation reactive aluminum
Generate aluminum oxynitride, aluminum oxynitride generated can with YAG:Ce fluorescent powder densified sintering product, overcome YAG:Ce fluorescent powder with
The problem of aluminium nitride sintered density difference, to obtain the complex phase fluorescence ceramics that mechanical strength is improved.
Embodiment 2
Compared with Example 1, the sintering processing of ceramics is changed in the present embodiment, other aspects are same as Example 1.
In the present embodiment, selection carries out discharge plasma sintering, that is, ceramic powder is fitted into graphite jig, 5~40MPa's
It is sintered under pressure and 1600~1800 DEG C of sintering temperature.The main advantage of discharge plasma sintering mode is can be with
It reduces sintering temperature and shortens sintering time, prevent grain growth excessive and reduce ceramic mechanical strength, but pass through the burning
The ceramics that knot mode obtains need to be made annealing treatment in nitrogen atmosphere in the later period.The present embodiment is suitable for the machinery to ceramics
The relatively high occasion of intensity requirement, therefore for the present invention provides alternative dispensing means.
Embodiment 3
Fig. 3 shows the flow chart of another preparation method of according to embodiments of the present invention 3 complex phase fluorescence ceramics.At this
In embodiment, with Examples 1 and 2, use the aluminium nitride, commercialization YAG:Ce fluorescent powder and aluminum nitrate of high-purity for raw material
Complex phase fluorescence ceramics are prepared, wherein select PVB as bonding agent, and can elect dispersing agent, sintering aid additional member etc..Specific system
Preparation Method is as follows.
First step S1 is first carried out, coats one layer of aluminium with the surface of YAG:Ce fluorescent powder is made in embodiment 1 and embodiment 2
Salt is different, and be that the surface of aluminium nitride powder is made to coat one layer of aluminium salt in the present embodiment: the same method using co-precipitation is in nitrogen
Change and coat one layer of aluminium salt on the surface of aluminium powder body, coprecipitation method is same as Example 1.Specifically, by suitable particle size
It is dissolved in aqueous solution for the aluminium nitride powder and aluminum nitrate of 0.05~1um, precipitating reagent is added while stirring, precipitating reagent can be
Ammonium hydroxide or ammonium salt (such as ammonium hydrogen carbonate) sufficiently obtain the nitridation that one layer of aluminium salt (that is, aluminium hydroxide) is coated with to surface after reaction
The suspension of aluminium powder body；By the suspension for being coated with the aluminium nitride powder of one layer of aluminium salt with deionized water clean to PH be it is neutral simultaneously
It is dry, it obtains to surface and is coated with the aluminium nitride powder of one layer of aluminium salt, wherein the particle size of aluminium nitride powder is 0.05~1um,
Smaller than 1~30um of partial size of commercial fluorescent powder, specific surface area is larger, therefore coats aluminium in phosphor surface with embodiment 1
Salt is compared, higher in the feasibility that the surface of aluminium nitride powder coats one layer of aluminium salt.It is in the same manner as in Example 1, in the present embodiment
In, it also can choose any appropriate aluminum contained compound as raw material, and according to the kind of selected aluminum contained compound raw material
Class selects suitable deposition agent to realize the purpose for coating one layer of aluminium salt on the surface of aluminium nitride powder.Equally, with embodiment 1
In it is identical, also can be used can coat one on the surface of aluminium nitride powder other than coprecipitation in the present embodiment
Any means of layer aluminium salt to coat one layer of aluminium salt, such as spray drying process etc. on the surface of aluminium nitride powder.
Then second step S2 is executed, mixing is carried out: aluminium nitride powder, the grain of one layer of aluminium salt will be coated with obtained in S1
The sintering aid Y that commercial YAG:Ce fluorescent powder, solvent and the particle size that diameter size is 1~30um are 0.02~1um2O3Or
The uniform mixing and ball milling of MgO for a period of time, such as 6~for 24 hours, the aluminium nitride powder and YAG:Ce fluorescence for being coated with one layer of aluminium salt is made
The mixed slurry of powder, wherein sintering aid accounts for the aluminium nitride powder for being coated with one layer of aluminium salt, YAG:Ce fluorescent powder and sintering aid
Gross mass 0.01~4%.
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
Ceramic powder obtained above is dry-pressing formed, then under the hydrostatic pressure of 200~300MPa by etc. static pressure suppressions come
Biscuit is obtained, and ungrease treatment is carried out to obtain ceramic body to the biscuit, wherein the skimming temp of biscuit is 800~1000
DEG C, degreasing time is 2~6h.
Then execute four steps S4, carry out ceramic post sintering: by ceramic body obtained in S3 in vacuum atmosphere oven
It is sintered under 1600~1800 DEG C of sintering temperature, which is nitrogen, and sintering time is 6~12h, is obtained after cooling
The complex phase fluorescence ceramics comprising fluorescent powder, aluminum oxynitride phase and aluminium nitride phase with structure as shown in Figure 1.
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 surface coated aluminum oxynitride phase of obtained aluminium nitride powder with a thickness of
0.05um~1um, can be realized the complete cladding to aluminium nitride powder and there is good light transmission rate.With embodiment 1
In it is the same, can by adjusting precipitation solution concentration or make the precipitation process (that is, aluminium salt cladding process) in S1 repeat into
The modes such as multiple go to control the thickness in the surface coated aluminium salt of aluminium nitride powder, to obtain the aluminum oxynitride of required thickness
Phase.
In the present embodiment, by the surface of aluminium nitride powder coat one layer of aluminium salt, then with YAG:Ce fluorescent powder one
It rises and mixes and be sintered, directly connecing for bigger YAG:Ce fluorescent powder and aluminium nitride can be equally differed to avoid thermal expansion coefficient
Touching, but it is mediate by aluminium salt.During the sintering process, aluminium salt first pass through chemical reaction generate aluminium oxide, then again with nitridation
Reactive aluminum generates aluminum oxynitride, and aluminum oxynitride generated can equally overcome YAG with YAG:Ce fluorescent powder densified sintering product:
The problem of Ce fluorescent powder and aluminium nitride sintered density difference, to obtain the complex phase fluorescence ceramics that mechanical strength is improved.
It should be pointed out that in the present embodiment, ceramic post sintering mode can also be changed into and be put described in embodiment 2
Electric plasma agglomeration prevents grain growth excessive and reduces ceramics so as to reduce sintering temperature and shorten sintering time
Mechanical strength.This is equally applicable to the occasion relatively high to the requirement of mechanical strength of ceramics.
The fluorescence ceramics prepared in above-described embodiment 1~3 are complex phase fluorescence ceramics, and structure can be expressed as YAG:
Ce-AlON-AlN, wherein Binder Phase is AlN, and the particle size of AlN raw material is 0.05~1um, particle size range after sintering are as follows: 0.2
~10um, and shining mutually is YAG:Ce fluorescent powder, and YAG:Ce fluorescent powder accounts for the 20~80% of ceramic total volume to reach good
Luminous efficiency.AlON is between YAG:Ce and AlN and it is with a thickness of 0.05~1um, so as to avoid YAG:Ce and AlN
Between direct contact, with overcome due to its thermal expansion coefficient difference it is larger caused by complex phase ceramic AlN&YAG:Ce thermal stress
Problem larger, consistency is lower, mechanical strength is poor.
The complex phase fluorescence ceramics prepared in above-described embodiment 1~3 are to include YAG:Ce fluorescent powder, aluminum oxynitride phase and nitrogen
The luminescent ceramic for changing aluminium phase, is a kind of with high thermal conductivity, high consistency, good mechanical strength and high luminous effect
The fluorescence ceramics of rate, the luminescent ceramic can efficiently be sent out when being irradiated by the high powers excitation light source such as blue light LD or blue-ray LED
Light and the lighting source for realizing high brightness, to further increase illumination and the brightness of projection light source, therefore can adapt to Gao Gong
The lighting requirements of rate blue light LD or LED light source.
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-AlON-AlN, wherein shining mutually is LuAG:Ce fluorescent powder.This equally may be implemented high
Thermal conductivity, high consistency, good mechanical strength and high luminous efficiency, by high powers such as blue light LD or blue-ray LEDs
Excitation light source High Efficiency Luminescence and can realize the lighting source of high brightness when irradiating, to further increase illumination and projection light source
Brightness, therefore equally can adapt to the lighting requirements of high-power blue-light LD or LED light source.
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 (11)
1. a kind of complex phase fluorescence ceramics, which is characterized in that the complex phase fluorescence ceramics include: as matrix phase aluminium nitride phase,
The fluorescent powder and the aluminum oxynitride between the aluminium nitride phase and the fluorescent powder being evenly distributed in described matrix phase
Phase, wherein the aluminium nitride phase is mutually separated from each other with the fluorescent powder via the aluminum oxynitride.
2. complex phase fluorescence ceramics as described in claim 1, which is characterized in that
The aluminum oxynitride is mutually coated on the surface of the fluorescent powder and/or the aluminium nitride phase.
3. complex phase fluorescence ceramics as described in claim 1, which is characterized in that
The aluminum oxynitride is mutually in the sintering process of the complex phase fluorescence ceramics by being coated on the fluorescent powder or described
What the aluminium salt of aluminium nitride phase surface and the aluminium nitride phase reaction generated.
4. complex phase fluorescence ceramics as described in claim 1, which is characterized in that
The fluorescent powder is YAG:Ce fluorescent powder or LuAG:Ce fluorescent powder.
5. complex phase fluorescence ceramics as described in claim 1, which is characterized in that
The aluminum oxynitride phase with a thickness of 0.05~1um.
6. complex phase fluorescence ceramics as described in claim 1, 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 as described in claim 1, which is characterized in that
The particle size of the fluorescent powder is 1~30um.
8. complex phase fluorescence ceramics as described in claim 1, which is characterized in that
The particle size of the aluminium nitride phase is 0.2~10um.
9. a kind of preparation method of complex phase fluorescence ceramics, the described method comprises the following steps:
S1: coating one layer of aluminium salt on the surface of fluorescent powder or aluminium nitride powder, and the particle size of the fluorescent powder is 1~30um
And the particle size of the aluminium nitride powder is 0.05~1um；
S2: the product after the cladding being prepared in S1 is uniformly mixed into ball with aluminium nitride powder or fluorescent powder, auxiliary agent and solvent
Mill 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 with obtain comprising fluorescent powder, aluminum oxynitride phase and
The complex phase fluorescence ceramics of aluminium nitride phase.
10. method as claimed in claim 9, 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.
11. method as claimed in claim 9, which is characterized in that
In S1, one layer of aluminium salt is coated on the surface of fluorescent powder or aluminium nitride powder and is realized by the following method: being used
The method of co-precipitation coats one layer of aluminium salt using aluminum contained compound and precipitating reagent on the surface of fluorescent powder or aluminium nitride powder.
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| CN110386822B (en) | 2021-02-26 |
| WO2019200934A1 (en) | 2019-10-24 |
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