CN104061530B - A kind of Wavelength converter and preparation method thereof, related lighting fixtures - Google Patents
A kind of Wavelength converter and preparation method thereof, related lighting fixtures Download PDFInfo
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- CN104061530B CN104061530B CN201310092396.2A CN201310092396A CN104061530B CN 104061530 B CN104061530 B CN 104061530B CN 201310092396 A CN201310092396 A CN 201310092396A CN 104061530 B CN104061530 B CN 104061530B
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Abstract
The embodiment of the invention discloses a kind of Wavelength converter and preparation method thereof, related lighting fixtures, the method comprises: place white porosity ceramic substrate in a reservoir; Add at least one at least one in the soluble salt solutions of barium, aluminium, calcium, strontium, potassium silicate and sodium silicate solution and function powder, function powder comprises fluorescent material, generate insoluble silicate, and make the concentration of reacting rear silicate ion be 0.06mol/L ~ 0.94mol/L; Settling vessel, until function powder and insoluble silicate all precipitate, forms phosphor powder layer; Take out the redundant solution in container, until leave the white porosity ceramic substrate of attachment phosphor powder layer; To the white porosity ceramic substrate heating being attached with phosphor powder layer, with shaping phosphor sheet.The technical problem that the embodiment of the present invention mainly solves there is provided a kind of preparation method, the related lighting fixtures with substrate with Wavelength converter compared with high-bond and this Wavelength converter.
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, related lighting fixtures.
Background technology
Utilizing the light source activation such as laser or LED fluorescent material to obtain booking list coloured light or polychromatic light, is a kind of technical scheme being widely used in the field 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, after being mixed with a certain proportion of silica gel by fluorescent material, is heating and curing shaping.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 DEG C, can only work the short time at 250 to 300 DEG C, otherwise just likely decompose.And the raising of power along with excitation source, the temperature of phosphor sheet in the temperature of phosphor sheet, particularly transmission-type colour wheel, can make the stability of phosphor sheet decline more than 250 DEG C, likely causes the cracking of phosphor sheet.
In order to improve the resistance to elevated temperatures of phosphor sheet, current a kind of trend utilizes resistant to elevated temperatures inorganic adhesive to replace silica gel, such as waterglass (potassium silicate or sodium metasilicate).In prior art, waterglass is utilized as a kind of preparation method step of the phosphor sheet of bonding agent to be: (1) adds barium acetate solution in the glass beaker being placed with substrate.(2) in glass beaker, then add the mixed solution of fluorescent material, waterglass.At this moment can generate barium silicate precipitation (3) in solution and leave standstill glass beaker until fluorescent material all precipitates.Now barium silicate also can be deposited in the bottom of glass beaker.(4) sink to the bottom the even phosphor powder layer of formation by mobile/rotation, this phosphor powder layer comprises waterglass, fluorescent material and barium silicate.(5) dry phosphor powder layer, to obtain solid phosphor sheet.By the method, the phosphor sheet that waterglass is bonding can be obtained, and also comprise a small amount of barium silicate in this phosphor sheet.
But the problem of said method is, the substrate being used for depositing fluorescent material is at present 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, come off than being easier to, 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 is substrate substantially with metal, and to make reflective Wavelength converter, such as surface is coated with the aluminium sheet of fine silver layer is exactly a kind of the most frequently used metal substrate.And due to waterglass be inorganic adhesive, the surface of inorganic adhesive and metal substrate is physical bond, and therefore 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 needs to do, and the surface of metal substrate is more smooth, and the adhesion on the surface of waterglass and metal substrate is less.If by reflectivity metallic substrate surfaces roughening being improved metal substrate, the reflectivity of metal substrate will reduce greatly.
In order to the contradiction of the substrate reflectivity and adhesion that solve Wavelength converter, the embodiment of the present invention proposes the preparation method of a kind of Wavelength converter replacing metal substrate with white porosity ceramic substrate.Be explained in detail below in conjunction with the preparation method of specific embodiment to the Wavelength converter in the embodiment of the present invention.
Summary of the invention
The technical problem that the embodiment of the present invention mainly solves there is provided a kind of preparation method, the related lighting fixtures with substrate with Wavelength converter compared with high-bond and this Wavelength converter.
Embodiments provide a kind of preparation method of Wavelength converter, this preparation method comprises the following steps:
A, in a reservoir placement white porosity ceramic substrate;
B, add in the soluble salt solutions of barium, aluminium, calcium, strontium at least one, potassium silicate and sodium silicate solution in a reservoir at least one and function powder, function powder comprises fluorescent material, and generate insoluble silicate, and make the concentration of the silicate ion reacted in rear container between 0.06mol/L and 0.94mol/L;
C, settling vessel are until function powder and insoluble silicate all precipitate, and form phosphor powder layer, this phosphor powder layer is attached on white porosity ceramic substrate;
D, the redundant solution of taking out in container, until leave the white porosity ceramic substrate of attachment phosphor powder layer;
E, to be attached with phosphor powder layer white porosity ceramic substrate heating, with shaping phosphor sheet.
Preferably, after step D, and before step e, also comprise:
F, will the white porosity ceramic substrate of fluorescent material lamella be attached with at the heating temperatures being less than or equal to 100 DEG C, until the moisture in removing phosphor powder layer.
Preferably, step e is: by being attached with the white porosity ceramic substrate of phosphor sheet 300 DEG C to 500 DEG C heating, with shaping phosphor sheet.
Preferably, step e is: by being attached with the white porosity ceramic substrate of phosphor sheet 300 DEG C to 500 DEG C heating, with shaping phosphor sheet.
Preferably, step B comprises:
B1, at least one added in a reservoir in the soluble salt solutions of barium, aluminium, calcium, strontium;
B2, add the mixed solution of function powder, potassium silicate and/or sodium metasilicate in a reservoir, generate insoluble silicate, and make the concentration of the silicate ion reacted in rear container between 0.06mol/L and 0.94mol/L.
Preferably, function powder also comprises glass dust.
The embodiment of the present invention additionally provides a kind of Wavelength converter, and this Wavelength converter comprises:
White porosity 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 one in barium silicate, alumina silicate, calcium silicates, strontium silicate, sodium metasilicate and/or potassium silicate be used for by bonding to insoluble silicate and function powder become an entirety, and phosphor sheet to be bonded on white porosity ceramic substrate.
Preferably, the volume ratio of insoluble silicate and fluorescent material is 0.27% to 0.68%.
The embodiment of the present invention additionally provides a kind of light-emitting device, it is characterized in that, comprise above-mentioned Wavelength converter, this light-emitting device also comprises one for the excitation source of outgoing exciting light, and Wavelength converter is for receiving this exciting light and the mixed light of 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 uses is white porosity ceramic substrate, because the porosity of white porosity ceramic substrate and fluorescent powder grain particle diameter are same magnitudes, fluorescent material can infilter in the pore of white porosity ceramic substrate, therefore after shaping, phosphor sheet and white porosity ceramic substrate interpenetrate, and phosphor sheet is better than the adhesive force in smooth metallic substrate surfaces at the adhesive force of white porosity ceramic base plate 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;
The structural representation of the Wavelength converter that Fig. 2 obtains for preparation method shown in Fig. 1;
Fig. 3 is the schematic flow sheet of another embodiment of the preparation method of Wavelength converter of the present invention;
Fig. 4 is the relation schematic diagram of the relative luminous intensity of Wavelength converter prepared by the present embodiment and the volume ratio of barium silicate/fluorescent material;
Fig. 5 is the relative luminous intensity of the Wavelength converter that the embodiment of the present invention makes and the relation schematic diagram of the concentration of potassium silicate in the rear solution of reaction;
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 schematic flow sheet of another embodiment of the preparation method of Wavelength converter of the present invention.
Detailed description of the invention
Embodiment one
Refer to Fig. 1, Fig. 1 is the structural representation of an embodiment of the Wavelength converter preparation method of the embodiment of the present invention, and as shown in Figure 1, the present embodiment comprises the following steps:
S11, in a reservoir placement white porosity 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 multiple field, such as, may be used for catalyst carrier, food and medicine filtration, burner, sound-absorbing material, aeronautical material etc.And white porosity pottery also has the characteristic of not extinction, the porosity characteristic of porous ceramics can bring again scattering to light and reflection simultaneously, and therefore white porosity pottery can use as reflecting material.White porosity pottery comprises the materials such as aluminium oxide, aluminium nitride, silica, silicon nitride, carborundum.Record through experiment, when the thickness of white porosity pottery is enough thick, the reflectivity of white porosity pottery can up to 99%.
Here container can be the devices such as glass beaker, and the formation that its role is to as follow-up chemical reaction and phosphor powder layer provides place.
S12, add barium nitrate, potassium silicate solution and function powder in a reservoir, and generate barium silicate precipitation, and make the concentration of the potassium silicate reacted in rear container be 0.06mol/L.
Potassium silicate solution, is commonly called as waterglass, is a kind of colourless viscous liquid, often uses as inorganic adhesive.Shaping for phosphor powder layer in subsequent step, the effect of potassium silicate is mainly as bonding agent, and be provide silicate ion for barium silicate precipitation in this step, therefore 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, relative to potassium silicate, is more easily hydrolyzed, weatherability is slightly poor.
Here function powder refers to fluorescent material, and fluorescent material can absorb exciting light and be excited to produce the light being different from excitation wavelength, such as YAG(yttrium-aluminium-garnet) fluorescent material, YAG fluorescent powder 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 totally consumed, and after making reaction, remaining potassium silicate concentration is in the solution 0.06mol/L.Here why can require that the concentration remaining potassium silicate solution is 0.06mol/L, be that this will explain in detail in subsequent step for the shaping consideration to phosphor powder layer in subsequent step.
Object due to this step generates insoluble silicate precipitation, therefore the barium nitrate in this step can be replaced by other barium, aluminium, calcium, strontium soluble salt solutions, such as barium chloride, aluminum nitrate etc., the mixed liquor of two or more above-mentioned soluble salt solutions can also be replaced by, they can generate insoluble silicate with potassium silicate, such as barium silicate, alumina silicate, calcium silicates, strontium silicate.
Here barium nitrate, potassium silicate solution and fluorescent material addition sequence be restriction not, can add successively, also can all disposablely add, and all can generate very soon and precipitates and deposit to the surface of white porosity ceramic substrate.
S13, settling vessel, until function powder and barium silicate all precipitate, form phosphor powder layer;
Barium silicate can 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 porosity ceramic substrate, and cover the surface of white porosity ceramic substrate.The apparent activation energy precipitated due to the barium silicate 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 along with the carrying out of reaction, barium silicate crystal can in the surperficial continued growth of fluorescent powder grain, and different silicic acid crystal of barium can connect together, coating function is produced to fluorescent powder grain, several fluorescent powder grains is connected as a whole, thus 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 porosity ceramic substrate are on the same order of magnitude, fluorescent powder grain can infilter in the pore of porous ceramic substrate.
S14, the redundant solution of taking out in container, until leave the white porosity ceramic substrate of attachment phosphor powder layer;
After phosphor powder layer is formed, the adhesive force of phosphor powder layer to porous ceramic substrate is more weak, in order to avoid the phosphor powder layer in container is destroyed, substrate directly can not be taken out from solution, and the aqueous solution around substrate should be removed.Preferably, can adopt suction pipe sucking-off, it is less on the impact of phosphor powder layer.
After fluorescent powder grain and barium silicate precipitation, the potassium silicate solution in surrounding medium can be adsorbed in space by the fluorescent powder grain in solution.When the 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 attached in the gap of fluorescent powder grain due to the higher meeting of its viscosity, phosphor powder layer is kept by wet face state, simultaneously barium silicate also can be dispersed in the gap of fluorescent powder grain, thus barium silicate and fluorescent powder grain by potassium silicate solution bonding become an entirety.And when after solution mixing, the concentration of potassium silicate is less than 0.06mol/L, its mobility is too strong, in the process taking redundant solution away, potassium silicate solution in phosphor powder layer can flow away along with solution flowing, make the amount of the potassium silicate under remaining little, the bonding force between fluorescent powder grain is not enough, and phosphor sheet is not easy shaping.Therefore, after solution mixing, the concentration of potassium silicate should at more than 0.06mol/L.
When only having fluorescent material, fluorescent powder grain can be easy to move along with the taking-up of solution, phosphor powder layer is difficult to shaping.And in the present embodiment, barium silicate precipitation is had in phosphor powder layer, and barium silicate precipitation can make to produce between fluorescent powder grain to connect, make when taking out the redundant solution in container, fluorescent powder grain is not easy mobile, thus make phosphor powder layer be not easy to be destroyed, phosphor sheet shaping easier.
S15, to be attached with phosphor powder layer white porosity ceramic substrate heating, with shaping 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, the Wavelength converter comprising white porosity ceramic substrate can be obtained, the structural representation of the Wavelength converter that Fig. 2 obtains for preparation method shown in Fig. 1, as shown in Figure 2, Wavelength converter comprises phosphor sheet 110 and white porosity ceramic substrate 120.Phosphor sheet 110 comprises fluorescent material 111, barium silicate 112 and potassium silicate 113.Potassium silicate 113 by bonding to barium silicate 112 and fluorescent material 111 become an entirety and form phosphor sheet 110.Phosphor sheet 110 is also bonded on white porosity ceramic substrate 120 by potassium silicate 113 simultaneously.
In order to improve the bonding force of phosphor sheet and substrate, the embodiment of the present invention utilizes white porosity ceramic substrate 120 to instead of traditional metal substrate.Different from metal substrate; the surface of white porosity ceramic substrate has a lot of pore; and the porosity of white porosity 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 porosity ceramic substrate; therefore, after shaping, phosphor sheet and white porosity ceramic substrate interpenetrate, and phosphor sheet is better than the adhesive force in smooth metallic substrate surfaces at the adhesive force of white porosity ceramic base plate surface.
Embodiment two
Fig. 3 is the schematic flow sheet of another embodiment of the preparation method of Wavelength converter of the present invention, and as shown in Figure 3, the present embodiment comprises:
S21, in a reservoir placement white porosity ceramic substrate.
The explanation of step S21 refers to the explanation to step S11.
S22, add barium nitrate solution in a reservoir.
Here from embodiment illustrated in fig. 1 in step S12 different, after the present embodiment places white porosity ceramic substrate in a reservoir, first add a kind of material in a reservoir here: barium nitrate solution.
S23, add the mixed solution of fluorescent material and potassium silicate in a reservoir, and generate barium silicate precipitation, and make the concentration of the potassium silicate reacted in rear container be 0.94mol/L.
After step s 22, this step adds again the mixed solution of fluorescent material and potassium silicate in a reservoir.Here fluorescent material is function powder.Because fluorescent material is particulate powder, if directly add in the aqueous solution, fluorescent material easily precipitates and makes solution phase-splitting.And potassium silicate solution has certain viscosity, fluorescent material can be made to be dispersed in potassium silicate solution by modes such as stirrings, and can not precipitate.
After adding the mixed solution of potassium silicate and fluorescent material in a reservoir, barium silicate precipitation can be generated at once, and barium silicate can adhere to the surface of nigh fluorescent material.Thus, after fluorescent material and barium silicate precipitation, it is more even that barium silicate can disperse.
In the present embodiment, after the fluorescent material added in a reservoir and the mixed solution of potassium silicate and potassium nitrate solution react, the concentration of the potassium silicate in container is 0.94mol/L.The selection of this concentration is conducive to the shaping of phosphor sheet, and this will be described in detail follow-up.
S24, settling vessel, until fluorescent material and barium silicate all precipitate, form phosphor powder layer.
The explanation of step S24 refers to the explanation to step S13.
S25, the redundant solution of taking out in container, until leave the white porosity ceramic substrate of attachment phosphor powder layer.
The explanation of step S25 refers to the explanation to step S14.
S26, to be attached with phosphor powder layer white porosity ceramic substrate heating, with shaping 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, as long as produce barium silicate in phosphor powder layer will have certain connection function to fluorescent powder grain, make the phosphor powder layer after precipitating become fine and close, be conducive to shaping.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 relatively easily shaping of phosphor sheet.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, more shaping.But barium silicate is white solid, can produce scattering and refraction to light, although therefore the generation of barium silicate is conducive to the shaping of phosphor sheet, the existence of barium silicate can affect the luminous efficiency of phosphor sheet.
Fig. 4 is the relation schematic diagram of the relative luminous intensity of Wavelength converter prepared by the present embodiment and the volume ratio of barium silicate/fluorescent material, as shown in Figure 4, when volume ratio between barium silicate and fluorescent powder grain is more than 2.7%, along with the increase of the ratio of barium silicate and fluorescent material volume ratio, the relative luminous intensity of Wavelength converter reduces, and when barium silicate and fluorescent material volume ratio increase to 6.8%, when relative luminous intensity is relative to 2.7%, have dropped 10%.Therefore, in order to ensure that the luminous efficiency of flourescent sheet does not have larger decline, preferably, the barium silicate in phosphor sheet and fluorescent material volume ratio are 2.7% to 6.8%.
The Wavelength converter higher with joint efforts with substrate junction can be prepared by the method for the present embodiment.Compared with the Wavelength converter prepared 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 finds, the ratio regular meeting of potassium silicate affects the luminous efficiency of phosphor sheet slightly.
And due to the potassium silicate in the phosphor sheet after final molding be by obtaining after the potassium silicate solution drying be attached in fluorescent powder grain space, after the mixed solution of the amount of the potassium silicate therefore in phosphor sheet and fluorescent material and potassium silicate joins barium nitrate solution reaction, 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 shaping is higher.
Refer to Fig. 5, Fig. 5 is the relative luminous intensity of the Wavelength converter that the embodiment of the present invention makes and the relation schematic diagram of the concentration of potassium silicate in the rear solution of reaction, as shown in Figure 5, between 0.06mol/L to 0.94mol/L, along with the rising of the concentration of potassium silicate in solution after reaction, the ratio regular meeting of the phosphor sheet mesosilicic acid potassium after shaping raises, and the luminous efficiency of the Wavelength converter produced can first reduce, and tends towards stability after 0.5mol/L.When concentration of potassium silicate after the reaction in solution is 0.5mol/L, the luminous efficiency of Wavelength converter is minimum, is about 98% of relative luminous intensity during 0.06mol/L, and the concentration of visible potassium silicate is also little on the impact of light efficiency.
And by testing the bonding force of phosphor sheet and porous ceramic substrate in the Wavelength converter produced, experiment finds, between 0.06mol/L to 0.94mol/L, along with the rising of the concentration of potassium silicate in solution after reaction, the ratio of the potassium silicate in the phosphor sheet after namely shaping raises, and bonding force becomes large gradually.
But when the concentration of potassium silicate in solution after reaction is greater than 0.94mol/L, the phosphor sheet after shaping there will be cracking phenomena.This is because the potassium silicate ratio in phosphor sheet is excessive, in the process of phosphor sheet drying, fluorescent powder grain is also wrapped up very thick one deck by potassium silicate sclerosis, when the steam air pressure of inside is excessive, the potassium silicate of outside can be washed open causes phosphor sheet ftracture, and when the concentration of potassium silicate in solution after reacting is less than 0.94mol/L, potassium silicate be not enough to wrap up potassium silicate in the process of drying or integument very thin, steam is easy to constantly vapor away, and can not gather and destroy phosphor sheet.
Embodiment three
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 a reservoir placement white porosity ceramic substrate.
Step S31 refers to the explanation of step S21.
S32, add barium nitrate solution in a reservoir.
Step S32 refers to the explanation of step S22.
S33, add the mixed solution of fluorescent material and potassium silicate in a reservoir, and generate barium silicate precipitation, and make the concentration of the potassium silicate reacted in rear container be 0.19mol/L.
In step S33, the concentration of the potassium silicate after reaction in container is 0.19mol/L, and this is that the one taking into account luminous efficiency and the adhesion between phosphor sheet and substrate is selected.
S34, ultrasonic disperse is carried out to solution.
The present embodiment, after fluorescent material, potassium silicate solution, barium nitrate solution being mixed, adds step S34: carry out ultrasonic disperse to solution.
Due in the process adding fluorescent material and potassium silicate mixed solution, fluorescent material and potassium silicate may dispersedly and uneven, make to react the barium silicate produced more concentrated.By ultrasonic disperse, barium silicate can be in the solution dispersed, and be dispersed in the space of fluorescent powder grain uniformly in the process of precipitation, and gradually in the superficial growth of fluorescent powder grain, make phosphor powder layer more fine and close.What deserves to be explained is, the step of ultrasonic disperse here can be carried out after S33 step completes, and also can be carry out with step S33 simultaneously.It is easily understood that, ultrasonic disperse can also obtain other method replacement of dispersed phase by mechanical agitation etc., can reach the homodisperse effect of barium silicate equally, certainly, ultrasonic disperse relative to other dispersed mode, ultrasonic disperse more even.
S35, settling vessel, until fluorescent material all precipitates, form phosphor powder layer.
Step S35 refers to the explanation of step S24.
S36, the redundant solution of taking out in container, until leave the white porosity ceramic substrate of attachment phosphor powder layer.
Step S36 refers to the explanation of step S25.
S37, will the white porosity ceramic substrate of phosphor powder layer be attached with 50 DEG C of dryings 1 hour.
Relative to embodiment illustrated in fig. 3, in the present embodiment, step S36 will be added before phosphor sheet is shaping: will the white porosity ceramic substrate of phosphor powder layer be attached with 50 DEG C of dryings 1 hour.
Find through experiment, if directly carry out hot briquetting to phosphor powder layer and white porosity ceramic substrate at relatively high temperatures, the phosphor sheet after shaping there will be a large amount of pore.This is that the moisture in phosphor powder layer can be volatilized fast by seething with excitement and produce pore owing to heating at higher than 100 DEG C.Therefore preferably, the drying below 100 DEG C by phosphor powder layer and white porosity ceramic substrate, until the moisture in removing phosphor powder layer.Certainly, temperature is too low, just causes the heat time long, and therefore temperature is more preferably proper at 50 DEG C ~ 100 DEG C.Such as, in the present embodiment, heat after 1 hour at 50 DEG C, the moisture in phosphor sheet can be removed substantially.
S38, will phosphor powder layer be attached with white porosity ceramic substrate 400 DEG C of heating 1 hour.
Only the moisture evaporation in phosphor powder layer is not enough to shaping phosphor sheet, now phosphor sheet is fine and close, too loose not.In order to allow potassium silicate in phosphor powder layer and the growth of barium silicate crystal structure, make the densification that phosphor powder layer becomes, adhesion uprises, phosphor powder layer and white porosity ceramic substrate is also needed to heat more than higher temperature, with shaping phosphor sheet, in general, need more than 150 DEG C.
Consider that fluorescent material is at high temperature easily oxidized and reduces light efficiency, heating-up temperature is preferably lower than 500 DEG C.On the other hand, when temperature is higher, such as more than 300 DEG C, fluorescent material meeting and white porosity pottery produce chemical reaction and improve the two adhesion, therefore preferably, the temperature of shaping phosphor sheet is arranged on 300 DEG C ~ 500 DEG C, and such as, 400 DEG C of heating in the present embodiment 1 hour, can obtain the Wavelength converter compared with high-bond.Certainly, if carry out the problem of oxidation heating or do not consider fluorescent material in reducing atmosphere, heating-up temperature can also select the higher temperature of more than 500 DEG C.
Embodiment four
Find in an experiment, the phosphor powder layer of the Wavelength converter that above-described embodiment is prepared and the adhesion of whiteware substrate improve a lot relative to the adhesion with metal substrate.But, due to phosphor sheet shaping time heating-up temperature far below the fusing point of potassium silicate, combination between potassium silicate and white porosity ceramic substrate is physical bond substantially, even if heating-up temperature is higher, the chemical bond produced between potassium silicate and white porosity ceramic substrate is also relatively weak.Although therefore Wavelength converter can meet instructions for use, the adhesion of phosphor sheet and white porosity ceramic substrate is not very high.
For this reason, a kind of improved plan is present embodiments provided to improve the adhesion of phosphor sheet and white porosity ceramic substrate: use fluorescent material and glass dust as function powder.Refer to Fig. 7, Fig. 7 is the schematic flow sheet of another embodiment of the preparation method of Wavelength converter of the present invention, and as shown in Figure 7, the present embodiment comprises:
S41, in a reservoir placement white porosity ceramic substrate.
The explanation of step S41 refers to the explanation to step S11.
S42, add barium nitrate solution, potassium silicate solution, fluorescent material, glass dust in a reservoir, and generate barium silicate precipitation, and make the concentration of the potassium silicate reacted in rear container be 0.06mol/L.
With in step S12 unlike, 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.Here glass dust can't have any impact on the chemical reaction in container, it is the same with fluorescent material can precipitate down.Here adding of barium silicate solution, potassium silicate solution, fluorescent material, glass dust does 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, settling vessel are until fluorescent material, barium silicate, glass dust all precipitate, and form phosphor powder layer, this phosphor powder layer is attached on white porosity ceramic substrate.
With step S13 unlike, the glass dust that container adds also can precipitate, and therefore, phosphor powder layer comprises glass dust.
S44, the redundant solution of taking out in container, until leave the white porosity ceramic substrate of attachment phosphor powder layer.
The explanation of step S44 refers to the explanation to step S14.
S45, to be attached with phosphor powder layer white porosity ceramic substrate heating, with shaping phosphor sheet.
With step S15 unlike, owing to adding glass dust in fluorescent material, in order to shaping phosphor sheet, heating-up temperature will 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 porosity ceramic substrate, substantially increases the adhesion of glass dust and white porosity pottery.
In addition, in order to reduce the pore of fluorescent material in forming process, step S45 is divided into two step heating, namely first lower than in the temperature of 100 DEG C, removes the moisture in phosphor sheet; Then at high temperature carry out shaping to phosphor powder layer.
By the preparation method of the present embodiment, can prepare a Wavelength converter, this Wavelength converter comprises white porosity ceramic substrate and phosphor sheet, and phosphor sheet comprises potassium silicate, barium silicate, fluorescent material and glass dust.Here potassium silicate and glass dust be used for by bonding to fluorescent material and barium silicate become an entirety, phosphor sheet is bonded on white porosity ceramic substrate simultaneously.Because the adhesion between glass dust and white porosity ceramic substrate is greater than the adhesion between potassium silicate and white porosity ceramic substrate, phosphor sheet here can be higher than embodiment illustrated in fig. 1 with the adhesion of white porosity 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 and uses whiteware substrate, uses the Wavelength converter of the preparations such as transparent ceramic base 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 the structure and fuction in the various embodiments described above.Light-emitting device also comprises one for the excitation source of outgoing exciting light, and above-mentioned Wavelength converter is for receiving this exciting light and the mixed light of outgoing Stimulated Light or Stimulated Light and exciting light.
The foregoing is only embodiments of the present invention; not thereby the scope of the claims of the present invention is limited; every utilize description of the present invention and accompanying drawing content to do equivalent structure or equivalent flow process conversion; 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 a reservoir placement white porosity ceramic substrate;
B, add in the soluble salt solutions of barium, aluminium, calcium, strontium at least one, potassium silicate and sodium silicate solution in the above-described container at least one and function powder, function powder comprises fluorescent material, and generate insoluble silicate, and make the concentration of the silicate ion reacted in rear described container between 0.06mol/L and 0.94mol/L;
C, standing described container are until described function powder and insoluble silicate all precipitate, and form phosphor powder layer, this phosphor powder layer is attached on described white porosity ceramic substrate;
D, the redundant solution of taking out in described container, until the white porosity ceramic substrate leaving attachment phosphor powder layer;
E, the white porosity ceramic substrate of described attachment phosphor powder layer to be heated, with shaping 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 white porosity ceramic substrate of described attachment phosphor powder layer at the heating temperatures being less than or equal to 100 DEG C, until removing phosphor powder layer in moisture.
3. the preparation method of Wavelength converter according to claim 2, is characterized in that,
Described step e is: by the white porosity ceramic substrate of described attachment phosphor powder layer 300 DEG C to 500 DEG C heating, with shaping phosphor sheet.
4. the preparation method of Wavelength converter according to claim 1, is characterized in that,
Described step e is: by the white porosity ceramic substrate of described attachment phosphor powder layer 300 DEG C to 500 DEG C heating, with shaping phosphor sheet.
5. the preparation method of Wavelength converter according to any one of claim 1 to 4, is characterized in that, described step B comprises:
B1, at least one added in the above-described container in the soluble salt solutions of barium, aluminium, calcium, strontium;
B2, add the mixed solution of function powder, potassium silicate and/or sodium metasilicate in the above-described container, generate insoluble silicate, and the concentration of silicate ion after making to react in described container is between 0.06mol/L and 0.94mol/L.
6. the preparation method of Wavelength converter according to claim 5, is characterized in that, described function powder also comprises glass dust.
7. the preparation method of Wavelength converter according to any one of claim 1 to 4, is characterized in that, described function powder also comprises glass dust.
8. a Wavelength converter, is characterized in that, this Wavelength converter comprises:
White porosity 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 one in barium silicate, alumina silicate, calcium silicates, strontium silicate, described sodium metasilicate and/or potassium silicate be used for by bonding to described insoluble silicate and function powder become an entirety, and described phosphor sheet to be bonded on described white porosity 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, it 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 any one of claim 8 to 10, this light-emitting device also comprises one for the excitation source of outgoing exciting light, and described Wavelength converter is for receiving this exciting light and the mixed light of outgoing Stimulated Light or Stimulated Light and exciting light.
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| CN106933011A (en) * | 2015-12-31 | 2017-07-07 | 深圳市光峰光电技术有限公司 | Colour wheel module, light source module and optical projection system |
| JP2018013670A (en) * | 2016-07-22 | 2018-01-25 | 日本電気硝子株式会社 | Wavelength conversion member and light emitting device prepared therewith |
| CN111123629A (en) * | 2018-11-01 | 2020-05-08 | 深圳光峰科技股份有限公司 | Wavelength conversion device, manufacturing method thereof, light emitting device and projection device |
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| CN105135366B (en) | 2017-04-12 |
| CN104061530A (en) | 2014-09-24 |
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