CN104061530A - Wavelength conversion device and manufacturing method and related light-emitting device thereof - Google Patents
Wavelength conversion device and manufacturing method and related light-emitting device thereof Download PDFInfo
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- CN104061530A CN104061530A CN201310092396.2A CN201310092396A CN104061530A CN 104061530 A CN104061530 A CN 104061530A CN 201310092396 A CN201310092396 A CN 201310092396A CN 104061530 A CN104061530 A CN 104061530A
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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Abstract
The embodiment of the invention discloses a wavelength conversion device and a manufacturing method and a related light-emitting device thereof. The manufacturing method comprises the following steps: putting white porous ceramic substrate into a container; adding at least one of soluble salt solutions of barium, aluminum, calcium and strontium, at least one of a sodium silicate solution and a potassium silicate solution, and functional powder to produce insoluble silicate, wherein the functional powder comprises phosphor powder, and after reaction, the concentration of silicate ions is 0.06-0.94mol/ L; standing the container until the functional powder and the insoluble silicate precipitate completely to form a phosphor powder layer; taking out excess solution in the container and keeping the white porous ceramic substrate attached with the phosphor powder layer; heating the white porous ceramic substrate attached with the phosphor powder layer so as to shape a phosphor powder sheet. The technical problem mainly solved by the embodiment of the invention is to provide the wavelength conversion device having a relatively high binding force with the substrate, and the manufacturing method and the related light-emitting device of the wavelength conversion device.
Description
Technical field
The present invention relates to illumination and Display Technique field, particularly relate to a kind of Wavelength converter and preparation method thereof, relevant light-emitting device.
Background technology
Utilizing the light source activation fluorescent material such as laser or LED to obtain booking list coloured light or polychromatic light, is a kind of technical scheme that is widely used in the fields such as lighting source, Projection Display.This technical scheme utilizes laser or LED emergent light to incide on fluorescent powder color wheel often, to realize good heat radiation.
Existing fluorescent powder color wheel utilizes silica gel packaging phosphor sheet often, and it is that after fluorescent material is mixed with a certain proportion of silica gel, moulding is heating and curing.The chemical property of silica gel is more stable, has higher mechanical strength, but at present silica gel only can long-term work at 200 ℃, at 250 to 300 ℃, can only work the short time, otherwise just likely decompose.And along with the raising of the power of excitation source, the temperature of phosphor sheet in the temperature of phosphor sheet, particularly transmission-type colour wheel, can surpass 250 ℃ and make the stability decreases of phosphor sheet, likely cause the cracking of phosphor sheet.
In order to improve the resistance to elevated temperatures of phosphor sheet, current a kind of trend is to utilize resistant to elevated temperatures inorganic adhesive to replace silica gel, for example waterglass (potassium silicate or sodium metasilicate).In prior art, utilize waterglass as a kind of preparation method step of the phosphor sheet of bonding agent to be: (1) adds barium acetate solution in being placed with the glass beaker of substrate.(2) then in glass beaker, add the mixed solution of fluorescent material, waterglass.At this moment in solution, can generate barium silicate precipitation (3) standing glass beaker until fluorescent material all precipitates.Now barium silicate also can be deposited in the bottom of glass beaker.(4) by movement/rotation, sunk to the bottom and formed even phosphor powder layer, this phosphor powder layer comprises waterglass, fluorescent material and barium silicate.(5) dry phosphor powder layer, to obtain solid phosphor sheet.By the method, can obtain the bonding phosphor sheet of waterglass, and in this phosphor sheet, also comprise a small amount of barium silicate.
But the problem of said method is, the substrate that is used at present depositing fluorescent material is all smooth metal plate substantially, to form the reflective colour wheel of higher reflectivity.And the bonding force of smooth metal plate and phosphor sheet is smaller, than being easier to, come off, this becomes the main cause of the application of the bonding phosphor sheet of restriction waterglass.
In prior art, the phosphor sheet of waterglass encapsulation be take metal substantially as substrate, and to make reflective Wavelength converter, for example the surperficial aluminium sheet that is coated with fine silver layer is exactly a kind of the most frequently used metal substrate.And because waterglass is inorganic adhesive, the surface of inorganic adhesive and metal substrate is physical bond, so the adhesion of waterglass and metal surface is less.On the other hand, in order to improve the reflectivity of metal substrate, it is very smooth that the surface of metal substrate need to be done, and the surface of metal substrate is more smooth, and the surperficial adhesion of waterglass and metal substrate is just less.If by metallic substrate surfaces roughening being improved to the reflectivity of metal substrate, the reflectivity of metal substrate will reduce greatly.
In order to solve the substrate reflectivity of Wavelength converter and the contradiction of adhesion, the embodiment of the present invention has proposed to replace with white porous ceramic substrate the preparation method of a kind of Wavelength converter of metal substrate.Below in conjunction with specific embodiment, the preparation method of the Wavelength converter in the embodiment of the present invention is explained in detail.
Summary of the invention
The technical problem that the embodiment of the present invention mainly solves has been to provide a kind ofly to be had compared with the preparation method of the Wavelength converter of high-bond and this Wavelength converter, relevant light-emitting device to substrate.
The embodiment of the present invention provides a kind of preparation method of Wavelength converter, and this preparation method comprises the following steps:
A, in container, place white porous ceramic substrate;
B, in container, add at least one in the soluble-salt solution of barium, aluminium, calcium, strontium, at least one and the function powder in potassium silicate and sodium silicate solution, function powder comprises fluorescent material, and generate insoluble silicate, and make the concentration of reacting the silicate ion in rear container between 0.06mol/L and 0.94mol/L;
C, standing container, until function powder and insoluble silicate all precipitate, form phosphor powder layer, and this phosphor powder layer is attached on white porous ceramic substrate;
Redundant solution in D, taking-up container, until leave the white porous ceramic substrate that adheres to phosphor powder layer;
E, to being attached with the white porous ceramic substrate heating of phosphor powder layer, with moulding phosphor sheet.
Preferably, after step D, and before step e, also comprise:
F, by the white porous ceramic substrate that is attached with fluorescent material lamella in the temperature heating that is less than or equal to 100 ℃, until remove the moisture in phosphor powder layer.
Preferably, step e is: by the white porous ceramic substrate that is attached with phosphor sheet 300 ℃ to 500 ℃ heating, with moulding phosphor sheet.
Preferably, step e is: by the white porous ceramic substrate that is attached with phosphor sheet 300 ℃ to 500 ℃ heating, with moulding phosphor sheet.
Preferably, step B comprises:
B1, in container, add at least one in the soluble-salt solution of barium, aluminium, calcium, strontium;
B2, in container, add the mixed solution of function powder, potassium silicate and/or sodium metasilicate, generate insoluble silicate, and make the concentration of reacting the silicate ion in rear container between 0.06mol/L and 0.94mol/L.
Preferably, function powder also comprises glass dust.
The embodiment of the present invention also provides a kind of Wavelength converter, and this Wavelength converter comprises:
White porous ceramic substrate and phosphor sheet;
Phosphor sheet comprises sodium metasilicate and/or potassium silicate, insoluble silicate and function powder, function powder comprises fluorescent material, insoluble silicate at least comprises in barium silicate, alumina silicate, calcium silicates, strontium silicate, sodium metasilicate and/or potassium silicate be for becoming an integral body by insoluble silicate and function powder are bonding, and phosphor sheet is bonded on white porous ceramic substrate.
Preferably, the volume ratio of insoluble silicate and fluorescent material is 0.27% to 0.68%.
The embodiment of the present invention also provides a kind of light-emitting device, it is characterized in that, comprise above-mentioned Wavelength converter, this light-emitting device also comprises an excitation source for outgoing exciting light, and Wavelength converter is for receiving the mixed light of this exciting light outgoing Stimulated Light or Stimulated Light and exciting light.
Compared with prior art, the embodiment of the present invention has following beneficial effect:
In the embodiment of the present invention, the substrate that Wavelength converter is used is white porous ceramic substrate, because porosity and the fluorescent powder grain particle diameter of white porous ceramic substrate is same magnitude, fluorescent material can infilter in the pore of white porous ceramic substrate, therefore after moulding, phosphor sheet and white porous ceramic substrate interpenetrate, and phosphor sheet is better than the adhesive force in smooth metallic substrate surfaces at the adhesive force on white porous ceramic substrate surface.
Accompanying drawing explanation
Fig. 1 is the structural representation of an embodiment of the Wavelength converter preparation method of the embodiment of the present invention;
Fig. 2 is the structural representation of the Wavelength converter that shown in Fig. 1, preparation method obtains;
Fig. 3 is the preparation method's of the Wavelength converter of the present invention schematic flow sheet of another embodiment;
Fig. 4 is the schematic diagram that is related to of the relative luminous intensity of Wavelength converter prepared of the present embodiment and the volume ratio of barium silicate/fluorescent material;
Fig. 5 is the relative luminous intensity and the schematic diagram that is related to that reacts concentration of potassium silicate in solution afterwards of the Wavelength converter made of the embodiment of the present invention;
Fig. 6 is the schematic flow sheet of another embodiment of the preparation method of Wavelength converter of the present invention;
Fig. 7 is the preparation method's of the Wavelength converter of the present invention schematic flow sheet of another embodiment.
The specific embodiment
Embodiment mono-
Refer to Fig. 1, the structural representation of an embodiment of the Wavelength converter preparation method that Fig. 1 is the embodiment of the present invention, as shown in Figure 1, the present embodiment comprises the following steps:
S11, in container, place white porous ceramic substrate.
Porous ceramics has the advantages such as chemical stability is good, density is low, intensity is high, nontoxic, corrosion-resistant, high temperature resistant, can be applied to a plurality of fields, such as can be for catalyst carrier, food and medicine filtration, burner, sound-absorbing material, aeronautical material etc.And white porous ceramics also has the not characteristic of extinction, the porosity characteristic of porous ceramics can be brought again scattering of light and reflection simultaneously, and therefore white porous ceramics can be used as reflecting material use.White porous ceramics comprises the materials such as aluminium oxide, aluminium nitride, silica, silicon nitride, carborundum.Through experiment, record, when the thickness of white porous ceramics is enough thick, the reflectivity of white porous ceramics can be up to 99%.
The container here can be the devices such as glass beaker, and its role is to provides place for the formation of follow-up chemical reaction and phosphor powder layer.
S12, in container, add barium nitrate, potassium silicate solution and function powder, and generate barium silicate precipitation, and the concentration that makes to react the potassium silicate in rear container is 0.06mol/L.
Potassium silicate solution, is commonly called as waterglass, is a kind of colourless viscous liquid, often as inorganic adhesive, uses.For phosphor powder layer moulding in subsequent step, the effect of potassium silicate is mainly as bonding agent, and in this step, be to provide silicate ion for barium silicate precipitation, so potassium silicate can replace with the mixed solution of sodium metasilicate or sodium metasilicate and potassium silicate, also can obtain same effect.But sodium metasilicate, with respect to potassium silicate, is more easily hydrolyzed, weatherability is slightly poor.
The function powder here refers to fluorescent material, and fluorescent material can absorb exciting light and be excited to produce the light that is different from excitation wavelength, for example YAG(yttrium-aluminium-garnet) fluorescent material, YAG fluorescent material can absorb blue light, ultraviolet light etc. and produce yellow Stimulated Light.In addition, fluorescent material can also be red light fluorescent powder, green light fluorescent powder etc.In other embodiment of the embodiment of the present invention, function powder can also refer to fluorescent material and glass dust.
In this step, potassium silicate and barium nitrate generate barium silicate precipitation in container reaction, until all barium nitrates are consumed completely, and to make the concentration of potassium silicate remaining after reaction in solution be 0.06mol/L.The concentration that why can require to remain potassium silicate solution is here 0.06mol/L, is for the consideration to the moulding of phosphor powder layer in subsequent step, and this will explain in detail in subsequent step.
Because the object of this step is to generate insoluble silicate precipitation, therefore the barium nitrate in this step can be replaced by other barium, aluminium, calcium, the soluble-salt solution of strontium, such as barium chloride, aluminum nitrate etc., can also be replaced by the mixed liquor of two or more above-mentioned soluble-salt solution, they can generate insoluble silicate with potassium silicate, for example barium silicate, alumina silicate, calcium silicates, strontium silicate.
The barium nitrate here, potassium silicate solution and fluorescent material addition sequence be restriction not, can add successively, also whole disposable adding, all can generate very soon the surface of precipitating and depositing to white porous ceramic substrate.
S13, standing container, until function powder and barium silicate all precipitate, form phosphor powder layer;
Barium silicate can be along with fluorescent material coprecipitation, and the barium silicate after precipitation and fluorescent material can form layer of fluorescent powder layer, and this phosphor powder layer can be attached on white porous ceramic substrate, and covers the surface of white porous ceramic substrate.Because the apparent activation energy of the barium silicate precipitation of harsh one-tenth is very high, they can be distributed in the gap of fluorescent powder grain and be attached on the surface of fluorescent powder grain, and the carrying out along with reaction, barium silicate crystal can be in the surperficial continued growth of fluorescent powder grain, and different silicic acid crystal of barium can connect together, fluorescent powder grain is produced to coating function, several fluorescent powder grains are connected as a whole, thereby make phosphor powder layer become a fine and close rete.
In addition, because the particle diameter of fluorescent powder grain and the particle diameter of white porous ceramic substrate are on the same order of magnitude, fluorescent powder grain can infilter in the pore of porous ceramic substrate.
Redundant solution in S14, taking-up container, until leave the white porous ceramic substrate that adheres to phosphor powder layer;
After phosphor powder layer forms, phosphor powder layer to the adhesive force of porous ceramic substrate a little less than, the phosphor powder layer in container is destroyed, substrate directly can not be taken out from solution, and the substrate aqueous solution around should be removed.Preferably, can adopt suction pipe sucking-off, its impact on phosphor powder layer is less.
After fluorescent powder grain and barium silicate precipitation, the fluorescent powder grain in solution can be adsorbed on the potassium silicate solution in solution around in space.Redundant solution in container is removed, redundant solution mesosilicic acid potassium can be removed equally, and space mesosilicic acid potassium solution between fluorescent powder grain is because the higher meeting of its viscosity is attached in the gap of fluorescent powder grain, phosphor powder layer is kept by wet face state, simultaneously barium silicate also can be dispersed in the gap of fluorescent powder grain, thereby barium silicate and fluorescent powder grain are become an integral body by potassium silicate solution is bonding.And after solution mixes, the concentration of potassium silicate is less than 0.06mol/L, its mobility is too strong, in taking the process of redundant solution away, potassium silicate solution in phosphor powder layer can flow away along with flow of solution, make the amount of the potassium silicate under residual seldom, the bonding force between fluorescent powder grain is not enough, and phosphor sheet is not easy moulding.Therefore,, after solution mixes, the concentration of potassium silicate should be more than 0.06mol/L.
In the situation that only having fluorescent material, fluorescent powder grain can be easy to move along with the taking-up of solution, makes phosphor powder layer be difficult to moulding.And in the present embodiment, in phosphor powder layer, have barium silicate precipitation, and barium silicate precipitation can make to produce and connect between fluorescent powder grain, while making the redundant solution in taking out container, fluorescent powder grain is not easy mobile, thereby it is destroyed that phosphor powder layer is not easy, the moulding of phosphor sheet is easier.
S15, to being attached with the white porous ceramic substrate heating of phosphor powder layer, with moulding phosphor sheet.
In this step, the moisture in phosphor powder layer can be removed, and the phosphor sheet adhesion after hot briquetting forms more by force as a whole.
Pass through said method, can obtain comprising the Wavelength converter of white porous ceramic substrate, Fig. 2 is the structural representation of the Wavelength converter that shown in Fig. 1, preparation method obtains, and as shown in Figure 2, Wavelength converter comprises phosphor sheet 110 and white porous ceramic substrate 120.Phosphor sheet 110 comprises fluorescent material 111, barium silicate 112 and potassium silicate 113.Potassium silicate 113 becomes an integral body and forms phosphor sheet 110 barium silicate 112 and fluorescent material 111 are bonding.Potassium silicate 113 is also bonded in phosphor sheet 110 on white porous ceramic substrate 120 simultaneously.
In order to improve the bonding force of phosphor sheet and substrate, the embodiment of the present invention utilizes white porous ceramic substrate 120 to replace traditional metal substrate.Different from metal substrate; the surface of white porous ceramic substrate has a lot of pores; and the porosity of white porous ceramic substrate and fluorescent powder grain particle diameter are same magnitudes; in the forming process of phosphor sheet; fluorescent powder grain can infilter in the pore of white porous ceramic substrate; therefore after moulding, phosphor sheet and white porous ceramic substrate interpenetrate, and phosphor sheet is better than the adhesive force in smooth metallic substrate surfaces at the adhesive force on white porous ceramic substrate surface.
Embodiment bis-
Fig. 3 is the preparation method's of the Wavelength converter of the present invention schematic flow sheet of another embodiment, and as shown in Figure 3, the present embodiment comprises:
S21, in container, place white porous ceramic substrate.
The explanation of step S21 refers to the explanation to step S11.
S22, in container, add barium nitrate solution.
Here from embodiment illustrated in fig. 1 in step S12 different, after the present embodiment is placed white porous ceramic substrate in container, in container, first added a kind of material here: barium nitrate solution.
S23, in container, add the mixed solution of fluorescent material and potassium silicate, and generate barium silicate precipitation, and the concentration that makes to react the potassium silicate in rear container is 0.94mol/L.
After step S22, this step has added again the mixed solution of fluorescent material and potassium silicate in container.The fluorescent material is here function powder.Because fluorescent material is granulated powders, if directly add in the aqueous solution, fluorescent material easily precipitates and makes solution phase-splitting.And potassium silicate solution has certain viscosity, can fluorescent material be dispersed in potassium silicate solution by modes such as stirrings, and can not precipitate.
In container, add after the mixed solution of potassium silicate and fluorescent material, can generate at once barium silicate precipitation, and barium silicate can adhere to the surface of nigh fluorescent material.Thereby after fluorescent material and barium silicate precipitation, it is more even that barium silicate can disperse.
In the present embodiment, after the fluorescent material adding in container and the mixed solution of potassium silicate react with potassium nitrate solution, the concentration of the potassium silicate in container is 0.94mol/L.The selection of this concentration is conducive to the moulding of phosphor sheet, and this will be elaborated follow-up.
S24, standing container, until fluorescent material and barium silicate all precipitate, form phosphor powder layer.
The explanation of step S24 refers to the explanation to step S13.
Redundant solution in S25, taking-up container, until leave the white porous ceramic substrate that adheres to phosphor powder layer.
The explanation of step S25 refers to the explanation to step S14.
S26, to being attached with the white porous ceramic substrate heating of phosphor powder layer, with moulding phosphor sheet.
The explanation of step S26 refers to the explanation to step S15.
In addition, what deserves to be explained is, in the method for the present embodiment, in phosphor powder layer, as long as produce barium silicate, will have certain connection function to fluorescent powder grain, make the phosphor powder layer after precipitation become fine and close, be conducive to moulding.And find through experiment, the volume ratio between barium silicate and fluorescent powder grain reaches more than 2.7%, and the compactness of phosphor powder layer is better, makes the moulding of phosphor sheet relatively easy.Certainly, the barium silicate of generation is more, and barium silicate is more obvious to the coating function of fluorescent powder grain, and the phosphor powder layer after precipitation is finer and close, easier moulding.But barium silicate is white solid, can produce scattering and refraction to light, therefore, although the generation of barium silicate is conducive to the moulding of phosphor sheet, the existence of barium silicate can affect the luminous efficiency of phosphor sheet.
Fig. 4 is the schematic diagram that is related to of the relative luminous intensity of Wavelength converter prepared of the present embodiment and the volume ratio of barium silicate/fluorescent material, as shown in Figure 4, in the volume ratio between barium silicate and fluorescent powder grain 2.7% when above, along with the increase of barium silicate with the ratio of fluorescent material volume ratio, the relative luminous intensity of Wavelength converter reduces, and when barium silicate increases to 6.8% with fluorescent material volume ratio, relative luminous intensity has declined 10% with respect to 2.7% time.Therefore,, in order to guarantee that the luminous efficiency of flourescent sheet does not have larger decline, preferably, the barium silicate in phosphor sheet is 2.7% to 6.8% with fluorescent material volume ratio.
By the method for the present embodiment, can prepare and the substrate junction higher Wavelength converter of making a concerted effort.Compare with the Wavelength converter of preparing embodiment illustrated in fig. 1, the ratio of the potassium silicate of the phosphor sheet of Wavelength converter prepared by the present embodiment is different, and experiment discovery, and the ratio regular meeting of potassium silicate affects the luminous efficiency of phosphor sheet slightly.
And because the potassium silicate in the phosphor sheet after final molding is to obtain after dry by being attached to potassium silicate solution in fluorescent powder grain space, therefore the amount of potassium silicate and the mixed solution of fluorescent material and potassium silicate in phosphor sheet joins after barium nitrate solution reaction, and the concentration of the potassium silicate in container is relevant.The concentration of this potassium silicate is higher, and the ratio of the potassium silicate in the phosphor sheet after moulding is higher.
Refer to Fig. 5, Fig. 5 is the relative luminous intensity and the schematic diagram that is related to that reacts concentration of potassium silicate in solution afterwards of the Wavelength converter made of the embodiment of the present invention, as shown in Figure 5, between 0.06mol/L to 0.94mol/L, rising along with the concentration of potassium silicate in solution after reaction, the ratio regular meeting of the phosphor sheet mesosilicic acid potassium after moulding raises, and the luminous efficiency of the Wavelength converter of producing can first reduce, and tends towards stability after 0.5mol/L.When the concentration of potassium silicate after reaction in solution is 0.5mol/L, the luminous efficiency of Wavelength converter is minimum, 98% left and right of relative luminous intensity during for 0.06mol/L, and the concentration of visible potassium silicate is on the impact of light efficiency little.
And by the bonding force of phosphor sheet and porous ceramic substrate in the Wavelength converter of producing is tested, experiment is found, between 0.06mol/L to 0.94mol/L, rising along with the concentration of potassium silicate in solution after reaction, the ratio that is the potassium silicate in the phosphor sheet after moulding raises, and it is large that bonding force becomes gradually.
But the concentration of potassium silicate after reaction in solution is greater than 0.94mol/L, the phosphor sheet after moulding there will be cracking phenomena.This is because the potassium silicate ratio in phosphor sheet is excessive, in the dry process of phosphor sheet, potassium silicate sclerosis is also wrapped up very thick one deck by fluorescent powder grain, when inner steam air pressure excessive, outside potassium silicate can be washed open and caused phosphor sheet cracking, and the concentration of potassium silicate in solution is less than 0.94mol/L after reacting, potassium silicate in dry process, be not enough to wrap up potassium silicate or integument very thin, steam is easy to constantly vapor away, and can not gather and destroy phosphor sheet.
Embodiment tri-
Fig. 6 is the schematic flow sheet of another embodiment of the preparation method of Wavelength converter of the present invention, and as shown in Figure 6, the present embodiment comprises:
S31, in container, place white porous ceramic substrate.
Step S31 refers to the explanation of step S21.
S32, in container, add barium nitrate solution.
Step S32 refers to the explanation of step S22.
S33, in container, add the mixed solution of fluorescent material and potassium silicate, and generate barium silicate precipitation, and the concentration that makes to react the potassium silicate in rear container is 0.19mol/L.
In step S33, the concentration of the potassium silicate after reaction in container is 0.19mol/L, and this is a kind of selection that takes into account the adhesion between luminous efficiency and phosphor sheet and substrate.
S34, solution is carried out to ultrasonic dispersion.
The present embodiment, after fluorescent material, potassium silicate solution, barium nitrate solution are mixed, has increased step S34: solution is carried out to ultrasonic dispersion.
Due in adding the process of fluorescent material and potassium silicate mixed solution, fluorescent material and potassium silicate may be also inhomogeneous dispersedly, and the barium silicate that reaction is produced is more concentrated.By ultrasonic dispersion, barium silicate can be dispersed in solution, and is dispersed in uniformly in the space of fluorescent powder grain in the process of precipitation, and gradually in the superficial growth of fluorescent powder grain, makes phosphor powder layer more fine and close.What deserves to be explained is, the step of the ultrasonic dispersion here can be carried out after S33 step completes, and can be also to carry out with step S33 simultaneously.Hold and be intelligiblely, ultrasonic dispersion can also replace by other method of the dispersed phases of acquisition such as mechanical agitation, can reach equally the homodisperse effect of barium silicate, certainly, ultrasonic decentralized photo is for other dispersed mode, ultrasonic dispersion more even.
S35, standing container, until fluorescent material all precipitates, form phosphor powder layer.
Step S35 refers to the explanation of step S24.
Redundant solution in S36, taking-up container, until leave the white porous ceramic substrate that adheres to phosphor powder layer.
Step S36 refers to the explanation of step S25.
S37, by the white porous ceramic substrate that is attached with phosphor powder layer 50 ℃ dry 1 hour.
With respect to embodiment illustrated in fig. 3, in the present embodiment, will before phosphor sheet moulding, increase step S36: the white porous ceramic substrate that is attached with phosphor powder layer is dried to 1 hour at 50 ℃.
Through experiment, find, if directly phosphor powder layer and white porous ceramic substrate are carried out to hot briquetting under higher temperature, the phosphor sheet after moulding there will be a large amount of pores.This is due to heating at higher than 100 ℃, and the moisture in phosphor powder layer can be seethed with excitement and volatilize fast and produce pore.Therefore preferably, phosphor powder layer and white porous ceramic substrate are dried below at 100 ℃, until remove the moisture in phosphor powder layer.Certainly, temperature is too low, just causes the heat time long, so temperature is more preferably proper at 50 ℃～100 ℃.For example, in the present embodiment, heat after 1 hour at 50 ℃, the moisture in phosphor sheet can be removed substantially.
S38, by the white porous ceramic substrate that is attached with phosphor powder layer 400 ℃ of heating 1 hour.
Only the moisture evaporation in phosphor powder layer is not enough to moulding phosphor sheet, now phosphor sheet is fine and close, too loose not.For potassium silicate and the growth of barium silicate crystal structure allowing in phosphor powder layer, the densification that phosphor powder layer is become, adhesion uprises, also need phosphor powder layer and white porous ceramic substrate to heat more than higher temperature, with moulding phosphor sheet, in general, need to be more than 150 ℃.
Consider fluorescent material to be at high temperature easily oxidized and reduce light efficiency, heating-up temperature is preferably lower than 500 ℃.On the other hand, when temperature is higher, for example, more than 300 ℃, fluorescent material meeting and white porous ceramics produce chemical reaction and improve the two adhesion, therefore preferably, the temperature of moulding phosphor sheet is arranged on 300 ℃～500 ℃, and for example the heating of 400 ℃ in the present embodiment is 1 hour, can obtain the Wavelength converter compared with high-bond.Certainly, if heat or do not consider the problem of oxidation of fluorescent material in reducing atmosphere, heating-up temperature can also be selected 500 ℃ of above higher temperatures.
Embodiment tetra-
In experiment, find, the adhesion of the phosphor powder layer of the Wavelength converter that above-described embodiment is prepared and whiteware substrate is with respect to improving a lot with the adhesion of metal substrate.But, heating-up temperature during due to phosphor sheet moulding is far below the fusing point of potassium silicate, combination between potassium silicate and white porous ceramic substrate is physical bond substantially, even if heating-up temperature is higher, the chemical bond producing between potassium silicate and white porous ceramic substrate also relatively a little less than.Although therefore Wavelength converter can meet instructions for use, the adhesion of phosphor sheet and white porous ceramic substrate is not very high.
For this reason, the present embodiment provides the adhesion that a kind of improved plan is usingd raising phosphor sheet and white porous ceramic substrate: use fluorescent material and glass dust as function powder.Refer to Fig. 7, the schematic flow sheet of another embodiment of the preparation method that Fig. 7 is Wavelength converter of the present invention, as shown in Figure 7, the present embodiment comprises:
S41, in container, place white porous ceramic substrate.
The explanation of step S41 refers to the explanation to step S11.
S42, in container, add barium nitrate solution, potassium silicate solution, fluorescent material, glass dust, and generate barium silicate precipitation, and the concentration that makes to react the potassium silicate in rear container is 0.06mol/L.
From different in step S12, in this step, function powder is fluorescent material and glass dust.Glass dust is a kind of glass isotropic body of amorphous granular shape, the high and stable chemical nature of its transparency.The glass dust here can't have on the chemical reaction in container any impact, its can precipitate down the same with fluorescent material.The barium silicate solution here, potassium silicate solution, fluorescent material, adding of glass dust do not have a definite sequence, but preferably, first add the mixed solution that barium silicate solution then adds potassium silicate solution, fluorescent material, glass dust, be beneficial to barium silicate precipitation and be uniformly dispersed.
S43, standing container, until fluorescent material, barium silicate, glass dust all precipitate, form phosphor powder layer, and this phosphor powder layer is attached on white porous ceramic substrate.
S13 is different from step, and the glass dust that container adds also can precipitate, and therefore, phosphor powder layer comprises glass dust.
Redundant solution in S44, taking-up container, until leave the white porous ceramic substrate that adheres to phosphor powder layer.
The explanation of step S44 refers to the explanation to step S14.
S45, to being attached with the white porous ceramic substrate heating of phosphor powder layer, with moulding phosphor sheet.
S15 is different from step, and owing to adding glass dust in fluorescent material, for moulding phosphor sheet, heating-up temperature will be more than the softening temperature of glass dust (this temperature is still far below the fusing point of potassium silicate).Now, after hot briquetting, glass dust can produce chemical bond with white porous ceramic substrate, has greatly improved the adhesion of glass dust and white porous ceramics.
In addition, in order to reduce the pore of fluorescent material in forming process, step S45 is divided into two steps heating, first in the temperature lower than 100 ℃, removes the moisture in phosphor sheet; Then at high temperature phosphor powder layer is carried out to moulding.
By the preparation method of the present embodiment, can prepare a Wavelength converter, this Wavelength converter comprises white porous ceramic substrate and phosphor sheet, and phosphor sheet comprises potassium silicate, barium silicate, fluorescent material and glass dust.The potassium silicate here and glass dust, for becoming an integral body by fluorescent material and barium silicate are bonding, are bonded in phosphor sheet on white porous ceramic substrate simultaneously.Because the adhesion between glass dust and white porous ceramic substrate is greater than the adhesion between potassium silicate and white porous ceramic substrate, the phosphor sheet here can be higher than embodiment illustrated in fig. 1 with the adhesion of white porous ceramic substrate.
Similarly, in order to improve the luminous efficiency of phosphor sheet, preferably, the barium silicate in phosphor sheet and the volume ratio of fluorescent material are 2.7% to 6.8%.
What deserves to be explained is, in fact, the method in the present embodiment is not limited in uses whiteware substrate, uses the Wavelength converter of the preparations such as crystalline ceramics substrate also to have higher adhesion.
The embodiment of the present invention also provides a kind of light-emitting device, comprises Wavelength converter, and this Wavelength converter can have structure and the function in the various embodiments described above.Light-emitting device also comprises an excitation source for outgoing exciting light, and above-mentioned Wavelength converter is for receiving the mixed light of this exciting light outgoing Stimulated Light or Stimulated Light and exciting light.
The foregoing is only embodiments of the present invention; not thereby limit the scope of the claims of the present invention; every equivalent structure or conversion of equivalent flow process that utilizes description of the present invention and accompanying drawing content to do; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (11)
1. a preparation method for Wavelength converter, is characterized in that, this preparation method comprises the following steps:
A, in container, place white porous ceramic substrate;
B, in described container, add at least one in the soluble-salt solution of barium, aluminium, calcium, strontium, at least one and the function powder in potassium silicate and sodium silicate solution, function powder comprises fluorescent material, and generate insoluble silicate, and make the concentration of the silicate ion in the rear described container of reaction between 0.06mol/L and 0.94mol/L;
C, standing described container, until described function powder and insoluble silicate all precipitate, form phosphor powder layer, and this phosphor powder layer is attached on described white porous ceramic substrate;
D, take out the redundant solution in described container, until leave the white porous ceramic substrate that adheres to described phosphor powder layer;
E, to the described white porous ceramic substrate heating that is attached with phosphor powder layer, with moulding phosphor sheet.
2. the preparation method of Wavelength converter according to claim 1, is characterized in that, after step D, and before step e, also comprises:
F, by the described white porous ceramic substrate that is attached with fluorescent material lamella in the temperature heating that is less than or equal to 100 ℃, until remove the moisture in phosphor powder layer.
3. the preparation method of Wavelength converter according to claim 2, is characterized in that,
Described step e is: by the described white porous ceramic substrate that is attached with phosphor sheet 300 ℃ to 500 ℃ heating, with moulding phosphor sheet.
4. the preparation method of Wavelength converter according to claim 1, is characterized in that,
Described step e is: by the described white porous ceramic substrate that is attached with phosphor sheet 300 ℃ to 500 ℃ heating, with moulding phosphor sheet.
5. the preparation method of Wavelength converter according to claim 1, is characterized in that, described step B comprises:
B1, in described container, add at least one in the soluble-salt solution of barium, aluminium, calcium, strontium;
B2, in described container, add the mixed solution of function powder, potassium silicate and/or sodium metasilicate, generate insoluble silicate, and make the concentration of the silicate ion in described container after reaction between 0.06mol/L and 0.94mol/L.
6. according to the preparation method of the Wavelength converter described in any one in claim 1 to 4, it is characterized in that, described step B comprises:
B1, in described container, add at least one in the soluble-salt solution of barium, aluminium, calcium, strontium;
B2, in described container, add the mixed solution of function powder, potassium silicate and/or sodium metasilicate, generate insoluble silicate, and make the concentration of the silicate ion in described container after reaction between 0.06mol/L and 0.94mol/L.
7. according to the preparation method of the Wavelength converter described in any one in claim 1 to 6, it is characterized in that, described function powder also comprises glass dust.
8. a Wavelength converter, is characterized in that, this Wavelength converter comprises:
White porous ceramic substrate and phosphor sheet;
Described phosphor sheet comprises sodium metasilicate and/or potassium silicate, insoluble silicate and function powder, described function powder comprises fluorescent material, described insoluble silicate at least comprises in barium silicate, alumina silicate, calcium silicates, strontium silicate, described sodium metasilicate and/or potassium silicate be for becoming an integral body by described insoluble silicate and function powder are bonding, and described phosphor sheet is bonded on described white porous ceramic substrate.
9. Wavelength converter according to claim 8, is characterized in that, described function powder also comprises glass dust.
10. Wavelength converter according to claim 8 or claim 9, is characterized in that, the volume ratio of described insoluble silicate and fluorescent material is 0.27% to 0.68%.
11. 1 kinds of light-emitting devices, it is characterized in that, comprise the Wavelength converter as described in claim 8 to 10 any one, this light-emitting device also comprises an excitation source for outgoing exciting light, and described Wavelength converter is for receiving the mixed light of this exciting light outgoing Stimulated Light or Stimulated Light and exciting light.
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| CN201510557929.9A CN105135366B (en) | 2013-03-21 | 2013-03-21 | Wavelength conversion device and manufacturing method thereof and related light emitting device |
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| CN105135366B (en) * | 2013-03-21 | 2017-04-12 | 深圳市绎立锐光科技开发有限公司 | Wavelength conversion device and manufacturing method thereof and related light emitting device |
| CN112578551A (en) | 2019-09-30 | 2021-03-30 | 台达电子工业股份有限公司 | Wavelength conversion device |
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| CN105135366B (en) | 2017-04-12 |
| CN104061530B (en) | 2015-09-09 |
| CN105135366A (en) | 2015-12-09 |
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