CN105135366B - Wavelength conversion device and manufacturing method thereof and related light emitting device - Google Patents
Wavelength conversion device and manufacturing method thereof and related light emitting device Download PDFInfo
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- CN105135366B CN105135366B CN201510557929.9A CN201510557929A CN105135366B CN 105135366 B CN105135366 B CN 105135366B CN 201510557929 A CN201510557929 A CN 201510557929A CN 105135366 B CN105135366 B CN 105135366B
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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
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C20/00—Chemical coating by decomposition of either solid compounds or suspensions of the coating forming compounds, without leaving reaction products of surface material in the coating
- C23C20/06—Coating with inorganic material, other than metallic material
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Abstract
The embodiment of the invention discloses a wavelength conversion device and a manufacturing method thereof and a related light emitting device. The method comprises the steps that a white porous ceramic substrate is placed in a container; at least one of soluble salt solutions of barium, aluminum, calcium and strontium, at least one of potassium silicate solutions and sodium silicate solutions and functional powder are added, the functional powder is prepared from fluorescent powder, then insoluble silicate is generated, and the concentration of silicate ions ranges from 0.06 mol/L to 0.94 mol/L after a reaction is performed; the container is stood until the functional powder and the insoluble silicate are completely precipitated, and a fluorescent powder layer is formed; the redundant solutions in the container are taken out until the white porous ceramic substrate with the fluorescent powder layer is left; the white porous ceramic substrate with the fluorescent powder layer is heated to form a formed fluorescent powder sheet. According to wavelength conversion device and the manufacturing method thereof and the related light emitting device, the wavelength conversion device has the stronger binding force with the substrate.
Description
The application is the Application No. 201310092396.2 that applicant was submitted on March 21st, 2013, entitled "
A kind of divisional application of Wavelength converter and preparation method thereof, related lighting fixtures ".
Technical field
The present invention relates to illuminate and display technology field, more particularly to a kind of Wavelength converter and preparation method thereof,
Related lighting fixtures.
Background technology
Using the light source activation such as laser or LED fluorescent material to obtain predetermined monochromatic light or polychromatic light, it is a kind of extensive
It is applied to the technical scheme in the fields such as lighting source, Projection Display.This technical scheme is often using laser or LED outgoing
Light is incided on fluorescent powder color wheel, to realize good radiating.
Often using silica gel packaging phosphor sheet, it is by fluorescent material and a certain proportion of silicon to existing fluorescent powder color wheel
After glue mix homogeneously, be heating and curing molding.The chemical property of silica gel is more stable, has a higher mechanical strength, but silicon at present
Glue only can the long-term work at 200 DEG C, can only work the short time at 250 to 300 DEG C, be otherwise possible to decompose.And with
The raising of the power of excitation source, the temperature of phosphor sheet, can exceed in the temperature of phosphor sheet, particularly transmission-type colour wheel
250 DEG C and cause phosphor sheet stability decline, it is possible to cause the cracking of phosphor sheet.
In order to improve the resistance to elevated temperatures of phosphor sheet, a kind of current trend be using resistant to elevated temperatures inorganic adhesive come
Replace silica gel, such as waterglass (potassium silicate or sodium silicate).In prior art, by the use of waterglass as the fluorescent material of bonding agent
A kind of manufacture method step of piece is：(1) the addition barium acetate solution in the glass beaker for be placed with substrate.(2) and then in glass
Fluorescent material, the mixed solution of waterglass are added in glass beaker.At this moment silicic acid precipitated barium (3) can be generated in solution and stands glass beaker
Until fluorescent material is all precipitated.Now barium silicate can also be deposited in the bottom of glass beaker.(4) shape is sunk to the bottom by movement/rotation
Uniformly phosphor powder layer, the phosphor powder layer include waterglass, fluorescent material and barium silicate.(5) phosphor powder layer is dried, to be consolidated
State phosphor sheet.With it, also including during the phosphor sheet of waterglass bonding, and the phosphor sheet can be obtained a small amount of
Barium silicate.
But the problem of said method is, the substrate for being used at present depositing fluorescent material is substantially all as smooth metal plate,
To form the reflective colour wheel of higher reflectance.And smooth metal plate is smaller with the bonding force of phosphor sheet, it is easier
Come off, this becomes the main cause of the application of the phosphor sheet for limiting waterglass bonding.
The content of the invention
The embodiment of the present invention is mainly solving the technical problems that there is provided a kind of and substrate with the wavelength compared with high-bond
The manufacture method of conversion equipment and the Wavelength converter, related lighting fixtures.
A kind of manufacture method of Wavelength converter is embodiments provided, the manufacture method is comprised the following steps：
A, in a reservoir placement white porosity ceramic substrate；
At least one, potassium silicate and sodium silicate in B, in a reservoir addition barium, aluminum, calcium, the soluble salt solutions of strontium is molten
At least one and function powder in liquid, function powder includes fluorescent material, and generates insoluble silicate, and holds after causing reaction
The concentration of the silicate ion in device is located between 0.06mol/L and 0.94mol/L；
C, settling vessel are until function powder and insoluble silicate whole precipitation, formation phosphor powder layer, the phosphor powder layer are attached
On white porosity ceramic substrate；
D, the redundant solution taken out in container, until leaving the white porosity ceramic substrate of attachment phosphor powder layer；
E, the white porosity ceramic substrate to being attached with phosphor powder layer are heated, with molding phosphor sheet.
Preferably, after step D, and before step E, also include：
F, the white porosity ceramic substrate of fluorescent material lamella will be attached with heat in the temperature less than or equal to 100 DEG C, until
Remove the moisture in phosphor powder layer.
Preferably, step E is：The white porosity ceramic substrate for being attached with phosphor sheet is heated at 300 DEG C to 500 DEG C,
With molding phosphor sheet.
Preferably, step E is：The white porosity ceramic substrate for being attached with phosphor sheet is heated at 300 DEG C to 500 DEG C,
With molding phosphor sheet.
Preferably, step B includes：
B1, at least one for being added in barium, aluminum, calcium, the soluble salt solutions of strontium in a reservoir；
B2, the mixed solution for adding function powder, potassium silicate and/or sodium silicate in a reservoir, generate insoluble silicate, and
So that the concentration of the silicate ion after reaction in container is located between 0.06mol/L and 0.94mol/L.
Preferably, function powder also includes glass dust.
The embodiment of the present invention additionally provides a kind of Wavelength converter, and the Wavelength converter includes：
White porosity ceramic substrate and phosphor sheet；
Phosphor sheet includes sodium silicate and/or potassium silicate, insoluble silicate and function powder, and function powder includes fluorescence
Powder, insoluble silicate at least include in barium silicate, aluminium silicate, calcium silicates, strontium silicate, sodium silicate and/or potassium silicate
For by insoluble silicate with function powder bonding into an entirety, and phosphor sheet is bonded in into white porosity ceramic substrate
On.
Preferably, insoluble silicate and the volume ratio of fluorescent material are 0.27% to 0.68%.
The embodiment of the present invention additionally provides a kind of light-emitting device, it is characterised in that including above-mentioned Wavelength converter, this
, also including an excitation source for being used for outgoing exciting light, Wavelength converter is used to receive the exciting light and outgoing is excited for electro-optical device
The mixed light of light or Stimulated Light and exciting light.
Compared with prior art, the embodiment of the present invention has the advantages that：
In the embodiment of the present invention, Wavelength converter using substrate be white porosity ceramic substrate, due to white porosity
The porosity of ceramic substrate and fluorescent powder grain particle diameter are same magnitudes, and fluorescent material can infilter the pore of white porosity ceramic substrate
In, therefore after molding, phosphor sheet is interpenetrated with white porosity ceramic substrate, phosphor sheet is in white porosity ceramic substrate table
The adhesive force in face is better than the adhesive force in smooth metallic substrate surfaces.
Description of the drawings
Structural representations of the Fig. 1 for one embodiment of the Wavelength converter manufacture method of the embodiment of the present invention；
Fig. 2 is the structural representation of the Wavelength converter that preparation method shown in Fig. 1 is obtained；
Fig. 3 is the schematic flow sheet of another embodiment of the preparation method of the Wavelength converter of the present invention；
Fig. 4 is the volume ratio of the relative luminous intensity with barium silicate/fluorescent material of Wavelength converter manufactured in the present embodiment
Relation schematic diagram；
Silicic acid after the relative luminous intensity of the Wavelength converter that Fig. 5 is made for the embodiment of the present invention and reaction in solution
The relation schematic diagram of potassium concn；
Fig. 6 is the schematic flow sheet of another embodiment of the manufacture method of the 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.
Specific embodiment
In prior art, the phosphor sheet of waterglass encapsulation is turned with making reflective wavelength substantially with metal as substrate
It is exactly a kind of the most frequently used metal basal board that changing device, such as surface are coated with the aluminium sheet of fine silver layer.And as waterglass is inorganic viscous
Agent is connect, inorganic adhesive is physical bond with the surface of metal basal board, therefore the adhesion of waterglass and metal surface is less.Separately
On the one hand, in order to improve the reflectance of metal basal board, it is very smooth that the surface of metal basal board needs to do, and the table of metal basal board
Face is more smooth, and waterglass is less with the adhesion on the surface of metal basal board.If by by metallic substrate surfaces be roughened come
The reflectance of metal basal board is improved, the reflectance of metal basal board will be substantially reduced.
In order to solve the substrate reflectivity of Wavelength converter and the contradiction of adhesion, the embodiment of the present invention is proposed with white
The manufacture method that color porous ceramic substrate replaces a kind of Wavelength converter of metal basal board.With reference to specific embodiment to this
The manufacture method of the Wavelength converter in inventive embodiments is explained in detail.
Embodiment one
Fig. 1 is referred to, Fig. 1 shows for the structure of one embodiment of the Wavelength converter manufacture method of the embodiment of the present invention
It is intended to, as shown in figure 1, the present embodiment is comprised the following steps：
S11, in a reservoir placement white porosity ceramic substrate.
Porous ceramicss have the advantages that chemical stability is good, density is low, intensity is high, nontoxic, corrosion-resistant, high temperature resistant, can be with
Multiple fields are applied to, for example, can be used for catalyst carrier, food and medicine filtration, burner, sound-absorbing material, aeronautical material
Deng.And white porosity ceramics also have the characteristic of not extinction, while the porosity characteristic of porous ceramicss can be brought dissipate to light again
Penetrate and reflect, therefore white porosity ceramics can be used as reflecting material.White porosity ceramics include aluminium oxide, aluminium nitride,
The materials such as silicon oxide, silicon nitride, carborundum.Jing experiments are measured, when the thickness of white porosity ceramics is sufficiently thick, white porosity pottery
The reflectance of porcelain can be up to 99%.
Here container can be the devices such as glass beaker, its role is to as follow-up chemical reaction and phosphor powder layer
Formation provide place.
S12, in a reservoir addition barium nitrate, potassium silicate solution and function powder, and silicic acid precipitated barium is generated, and cause anti-
The concentration of the potassium silicate after answering in container is 0.06mol/L.
Potassium silicate solution, is commonly called as waterglass, is a kind of colourless viscous liquid, and Jing is frequently as inorganic adhesive use.
For phosphor powder layer molding in subsequent step, the effect of potassium silicate is primarily as bonding agent, and is for silicon in this step
Sour precipitated barium provides silicate ion, therefore potassium silicate can be with the mixed solution of sodium silicate or sodium silicate and potassium silicate come generation
Replace, it is also possible to obtain same effect.But, sodium silicate is for potassium silicate, it is easier to hydrolysis occurs, weatherability is slightly
Difference.
Here function powder refers to fluorescent material, and fluorescent material can absorb exciting light and be excited to produce different from excitation wavelength
Light, such as YAG (yttrium-aluminium-garnet) fluorescent material, YAG fluorescent powder can absorb blue light, ultraviolet light etc. and produce yellow and be excited
Light.Additionally, fluorescent material can also be red light fluorescent powder, green light fluorescent powder etc..In the 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 silicic acid precipitated barium in container reaction, until all of barium nitrate quilt
Consume completely, and remaining potassium silicate concentration in the solution is 0.06mol/L after causing reaction.Here why may require that surplus
The concentration of remaining potassium silicate solution is 0.06mol/L, is in order at the consideration to the molding of phosphor powder layer in subsequent step, and this will be rear
Explain in detail in continuous step.
As the purpose of this step is to generate insoluble silicate precipitation, therefore the barium nitrate in this step can be replaced
Into other barium, aluminum, calcium, strontium soluble salt solutions, such as barium chloride, aluminum nitrate etc. can also be replaced by two or more
The mixed liquor of above-mentioned soluble salt solutions, they can generate insoluble silicate, such as barium silicate, silicic acid with potassium silicate
Aluminum, calcium silicates, strontium silicate.
Here barium nitrate, potassium silicate solution and fluorescent material addition sequence be not restricted, can sequentially add, also may be used
Added with all disposable, all can generate the surface for precipitating and depositing to white porosity ceramic substrate quickly.
S13, settling vessel are until function powder and barium silicate whole precipitation, form phosphor powder layer；
Barium silicate can form layer of fluorescent powder layer with fluorescent material with fluorescent material coprecipitation, the barium silicate after precipitation,
The phosphor powder layer can be attached on white porosity ceramic substrate, and covers the surface of white porosity ceramic substrate.Due to just generation
Silicic acid precipitated barium apparent activation energy it is very high, they can be distributed in the gap of fluorescent powder grain and be attached to fluorescent powder grain
On surface, and with the carrying out of reaction, silicic acid crystal of barium can be in the surface continued growth of fluorescent powder grain, and different barium silicate
Crystal can be connected together, and produce coating function to fluorescent powder grain so that several fluorescent powder grains are connected as an entirety,
So that phosphor powder layer becomes a fine and close film layer.
Further, since the particle diameter of the particle diameter of fluorescent powder grain and white porosity ceramic substrate is on the same order of magnitude, fluorescence
Powder particles can be infiltered in the pore of porous ceramic substrate.
S14, the redundant solution taken out in container, until leaving the white porosity ceramic substrate of attachment phosphor powder layer；
After phosphor powder layer is formed, phosphor powder layer is weaker to the adhesive force of porous ceramic substrate, in order to avoid in container
Phosphor powder layer be destroyed, it is impossible to by substrate directly from solution take out, and should by around substrate aqueous solution remove.It is preferred that
Ground, can be suctioned out using suction pipe, and its impact to phosphor powder layer is less.
After fluorescent powder grain and silicic acid precipitated barium, the fluorescent powder grain in solution can be molten by the potassium silicate in surrounding medium
Liquid adsorbs in space.When the redundant solution in container is removed, in redundant solution, potassium silicate can equally be removed, and fluorescent material
In space between granule, potassium silicate solution can be attached in the gap of fluorescent powder grain as its viscosity is higher so that fluorescent material
Layer is kept by wet face state, while barium silicate can be also dispersed in the gap of fluorescent powder grain, so as to barium silicate and fluorescent material
Grain is by potassium silicate solution bonding into an entirety.And after working as solution mixing, the concentration of potassium silicate is less than 0.06mol/L, its flowing
Property it is too strong, during redundant solution is taken away, the potassium silicate solution in phosphor powder layer can with solution flow and flow away so that
Seldom, the bonding force between fluorescent powder grain is not enough, and phosphor sheet does not allow easy-formation for the amount of the potassium silicate under residual.Therefore, it is molten
After liquid mixing, the concentration of potassium silicate should be in more than 0.06mol/L.
In the case of only fluorescent material, fluorescent powder grain can be easy to move with the taking-up of solution so that fluorescence
Bisque is difficult to molding.And in the present embodiment, silicic acid precipitated barium in phosphor powder layer, is had, and silicic acid precipitated barium can cause fluorescent material
Grain between produce connection so that take out container in redundant solution when, fluorescent powder grain is not easily moveable, so that fluorescence
Bisque is not easy to be destroyed, and the molding of phosphor sheet is easier.
S15, the white porosity ceramic substrate to being attached with phosphor powder layer are heated, with molding phosphor sheet.
In this step, the moisture in phosphor powder layer can be removed, and the phosphor sheet adhesion after heated molding compared with
Become an entirety by force.
By said method, can obtain including the Wavelength converter of white porosity ceramic substrate, Fig. 2 is shown in Fig. 1
The structural representation of the Wavelength converter that preparation method is obtained, as shown in Fig. 2 Wavelength converter includes phosphor sheet 110
With white porosity ceramic substrate 120.Phosphor sheet 110 includes fluorescent material 111, barium silicate 112 and potassium silicate 113.Potassium silicate
Barium silicate 112 is formed phosphor sheet 110 into an entirety with 111 bonding of fluorescent material by 113.Potassium silicate 113 will also be glimmering simultaneously
Light powder piece 110 is bonded on white porosity ceramic substrate 120.
In order to improve the bonding force of phosphor sheet and substrate, the embodiment of the present invention utilizes 120 generation of white porosity ceramic substrate
Traditional metal basal board is replaced.Different from metal basal board, the surface of white porosity ceramic substrate has many pores, and white is more
The porosity of hole ceramic substrate and fluorescent powder grain particle diameter are same magnitudes, in the forming process of phosphor sheet, fluorescent material
Grain can be infiltered in the pore of white porosity ceramic substrate, therefore after molding, phosphor sheet is oozed with white porosity ceramic substrate mutually
Thoroughly, phosphor sheet in the adhesive force of white porosity ceramic base plate surface better than the adhesive force in smooth metallic substrate surfaces.
Embodiment two
Fig. 3 is the schematic flow sheet of another embodiment of the preparation method of the Wavelength converter of the present invention, such as Fig. 3 institutes
Show, the present embodiment includes：
S21, in a reservoir placement white porosity ceramic substrate.
The explanation of step S21 refers to the explanation to step S11.
S22, in a reservoir addition barium nitrate solution.
Here different from step S12 in embodiment illustrated in fig. 1, the present embodiment places white porosity ceramic base in a reservoir
After plate, a kind of material has been initially charged here in a reservoir：Barium nitrate solution.
S23, the mixed solution for adding fluorescent material and potassium silicate in a reservoir, and silicic acid precipitated barium is generated, and cause reaction
The concentration of the potassium silicate in container is 0.94mol/L afterwards.
After step s 22, this step adds the mixed solution of fluorescent material and potassium silicate again in a reservoir.Here glimmering
Light powder is function powder.As fluorescent material is particulate powder, if being directly added in aqueous solution, fluorescent material is easily precipitated and is caused
Solution split-phase.And potassium silicate solution has certain viscosity, fluorescent material can be caused to be dispersed in silicic acid by modes such as stirrings
In potassium solution, without precipitating.
After adding the mixed solution of potassium silicate and fluorescent material in a reservoir, silicic acid precipitated barium, and silicic acid can be generated at once
Barium can adhere to the surface of nigh fluorescent material.Thus after fluorescent material and silicic acid precipitated barium, barium silicate can it is scattered more
Uniformly.
In the present embodiment, after the fluorescent material for adding in a reservoir and the mixed solution of potassium silicate and potassium nitrate solution reaction,
The concentration of the potassium silicate in container is 0.94mol/L.The molding for being advantageously selected for phosphor sheet of the concentration, this subsequently will enter
Row is described in detail.
S24, settling vessel are until fluorescent material and barium silicate whole precipitation, form phosphor powder layer.
The explanation of step S24 refers to the explanation to step S13.
S25, the redundant solution taken out in container, until leaving the white porosity ceramic substrate of attachment phosphor powder layer.
The explanation of step S25 refers to the explanation to step S14.
S26, the white porosity ceramic substrate to being attached with phosphor powder layer are heated, with molding 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, will be to glimmering as long as producing barium silicate in phosphor powder layer
Light powder particles have certain interconnection function so that the phosphor powder layer after precipitation becomes fine and close, is conducive to molding.And Jing experiments find,
When the volume ratio between barium silicate and fluorescent powder grain reaches more than 2.7%, the compactness of phosphor powder layer is preferable so that fluorescence
The molding of powder piece is relatively easy.Certainly, the barium silicate of generation is more, and barium silicate is become apparent to the coating function of fluorescent powder grain,
Phosphor powder layer after precipitation is finer and close, easier molding.But barium silicate is white solid, scattering can be produced to light and is rolled over
Penetrate, although therefore the generation of barium silicate is conducive to the molding of phosphor sheet, the presence of barium silicate affect phosphor sheet
Luminous efficiency.
Fig. 4 is the volume ratio of the relative luminous intensity with barium silicate/fluorescent material of Wavelength converter manufactured in the present embodiment
Relation schematic diagram, as shown in figure 4, when the volume ratio between barium silicate and fluorescent powder grain is more than 2.7%, with silicon
The increase of the ratio of sour barium and fluorescent material volume ratio, the relative luminous intensity of Wavelength converter are reduced, and when barium silicate with
When fluorescent material volume ratio increases to 6.8%, when relative luminous intensity is relative to 2.7%, 10% is have dropped.Therefore, it is glimmering in order to ensure
The luminous efficiency of mating plate does not have larger decline, it is preferable that barium silicate in phosphor sheet and fluorescent material volume ratio be 2.7% to
6.8%.
The Wavelength converter higher with substrate adhesion can be prepared by the method for the present embodiment.With shown in Fig. 1
The Wavelength converter that embodiment is prepared is compared, the potassium silicate of the phosphor sheet of Wavelength converter manufactured in the present embodiment
Ratio is different, and tests discovery, and the ratio regular meeting of potassium silicate slightly affects the luminous efficiency of phosphor sheet.
And as the potassium silicate in the phosphor sheet after final molding is by the silicic acid being attached in fluorescent powder grain space
Obtain after potassium solution drying, therefore the amount of the potassium silicate in phosphor sheet is added to the mixed solution of fluorescent material and potassium silicate
After barium nitrate solution reaction, the concentration of the potassium silicate in container is relevant.The concentration of the potassium silicate is higher, the phosphor sheet after molding
In potassium silicate ratio it is higher.
Refer to Fig. 5, Fig. 5 be the relative luminous intensity of the Wavelength converter that the embodiment of the present invention makes with react after it is molten
The relation schematic diagram of the concentration of potassium silicate in liquid, as shown in figure 5, between 0.06mol/L to 0.94mol/L, after reaction
The rising of the concentration of potassium silicate in solution, the ratio regular meeting of potassium silicate in the phosphor sheet after molding are raised, and the wavelength produced
The luminous efficiency of conversion equipment first can be reduced, and tend towards stability after 0.5mol/L.Potassium silicate after the reaction in solution is dense
Spend for 0.5mol/L when, the luminous efficiency of Wavelength converter is minimum, and when being 0.06mol/L, the 98% of relative luminous intensity is left
It is right, it is seen that impact of the concentration of potassium silicate to light efficiency is simultaneously little.
And the bonding force passed through to phosphor sheet in the Wavelength converter produced with porous ceramic substrate is tested,
Experiment finds, between 0.06mol/L to 0.94mol/L, with the rising of the concentration of potassium silicate in solution after reaction, i.e. molding
The ratio of the potassium silicate in phosphor sheet afterwards is raised, and bonding force becomes larger.
But, concentration of potassium silicate after reaction in solution is more than 0.94mol/L, and the phosphor sheet after molding occurs out
Split phenomenon.This is that, as the potassium silicate ratio in phosphor sheet is excessive, during phosphor sheet is dried, potassium silicate is hardened simultaneously
Fluorescent powder grain is wrapped up into very thick one layer, when internal vapor air pressure is excessive, outside potassium silicate can be washed open and be caused glimmering
Light powder piece ftractures, and concentration of potassium silicate after reaction in solution is less than 0.94mol/L, and potassium silicate is not enough during drying
Very thin to wrap up potassium silicate or integument, vapor is easy to constantly vapor away, and destroys phosphor sheet without gathering.
Embodiment three
Fig. 6 is the schematic flow sheet of another embodiment of the manufacture method of the Wavelength converter of the present invention, such as Fig. 6 institutes
Show, the present embodiment includes：
S31, in a reservoir placement white porosity ceramic substrate.
Step S31 refers to the explanation of step S21.
S32, in a reservoir addition barium nitrate solution.
Step S32 refers to the explanation of step S22.
S33, the mixed solution for adding fluorescent material and potassium silicate in a reservoir, and silicic acid precipitated barium is generated, and cause reaction
The concentration of the potassium silicate in container is 0.19mol/L afterwards.
In step S33, the concentration of the potassium silicate after reaction in container is 0.19mol/L, and this is to take into account luminous efficiency and glimmering
A kind of selection of the adhesion between light powder piece and substrate.
S34, ultrasonic disperse is carried out to solution.
The present embodiment increased step S34 after by fluorescent material, potassium silicate solution, the mixing of barium nitrate solution：Solution is entered
Row ultrasonic disperse.
As, during fluorescent material and potassium silicate mixed solution is added, fluorescent material and potassium silicate may dispersedly not
Uniformly so that the barium silicate that reaction is produced compares concentration.By ultrasonic disperse, barium silicate can it is dispersed in the solution, and
It is uniformly dispersed in the space of fluorescent powder grain during precipitation, and gradually in the superficial growth of fluorescent powder grain so that
Phosphor powder layer is more fine and close.What deserves to be explained is, can carry out after the completion of S33 steps the step of ultrasonic disperse here,
Can be with step S33 while carrying out.It is easily understood that ultrasonic disperse can also obtain dispersed phase with mechanical agitation etc.
Other methods replace, can equally reach effect homodisperse to barium silicate, certainly, ultrasonic disperse relative to it is other
For even dispersing mode, ultrasonic disperse it is more uniform.
S35, settling vessel are until fluorescent material whole precipitation, forms phosphor powder layer.
Step S35 refers to the explanation of step S24.
S36, the redundant solution taken out in container, until leaving the white porosity ceramic substrate of attachment phosphor powder layer.
Step S36 refers to the explanation of step S25.
S37, the white porosity ceramic substrate of phosphor powder layer will 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 increased before phosphor sheet molding：Will be attached
The white porosity ceramic substrate of phosphor powder layer in 50 DEG C of dryings 1 hour.
Jing experiments find, if be directly heated into white porosity ceramic substrate to phosphor powder layer at relatively high temperatures
Type, the phosphor sheet after molding occur a large amount of pores.This is the moisture in phosphor powder layer due to heating at higher than 100 DEG C
Can quickly be volatilized by boiling and produce pore.It is preferred that by phosphor powder layer and white porosity ceramic substrate 100 DEG C with
Lower drying, until removing the moisture in phosphor powder layer.Certainly, temperature is too low, and it is long to result in heat time heating time, therefore temperature is more excellent
Selection of land is proper at 50 DEG C～100 DEG C.For example, in the present embodiment, after heating 1 hour at 50 DEG C, in phosphor sheet
Moisture can be removed substantially.
S38, the white porosity ceramic substrate of phosphor powder layer will be attached with heat 1 hour at 400 DEG C.
The moisture evaporation in phosphor powder layer is not enough to into molding phosphor sheet only, now the inadequate cause of phosphor sheet
It is close, excessively loosely.For the potassium silicate that allows in phosphor powder layer and the growth of barium silicate crystal structure so that the cause that phosphor powder layer becomes
Close, adhesion is uprised, in addition it is also necessary to heated phosphor powder layer with white porosity ceramic substrate more than higher temperature, with molding fluorescence
Powder piece, it is generally desirable to more than 150 DEG C.
Easily aoxidized in view of fluorescent material at high temperature and reduce light efficiency, preferably lower than 500 DEG C of heating-up temperature.The opposing party
Face, when temperature is higher, such as more than 300 DEG C, fluorescent material can produce chemical reaction with white porosity ceramics and improve the two knot
With joint efforts, it is preferred that the temperature setting of molding phosphor sheet is at 300 DEG C～500 DEG C, such as 400 in the present embodiment DEG C add
Heat 1 hour, can obtain the Wavelength converter compared with high-bond.Certainly, if heated in reducing atmosphere or not
Consider the problem of oxidation of fluorescent material, heating-up temperature is also an option that more than 500 DEG C of higher temperature.
Example IV
Find in an experiment, phosphor powder layer and the whiteware substrate of the Wavelength converter that above-described embodiment is prepared
Adhesion improves a lot relative to the adhesion with metal basal board.But, due to heating-up temperature during phosphor sheet molding it is remote
Less than the fusing point of potassium silicate, the combination between potassium silicate and white porosity ceramic substrate is substantially physical bond, even if heating
Temperature is higher, and the chemical bond produced between potassium silicate and white porosity ceramic substrate is also relatively weak.Although therefore wavelength turns
Changing device can meet use requirement, but the adhesion of phosphor sheet and white porosity ceramic substrate is not very high.
For this purpose, present embodiments providing a kind of improved plan to improve the knot of phosphor sheet and white porosity ceramic substrate
With joint efforts：Using fluorescent material and glass dust as function powder.Fig. 7 is referred to, Fig. 7 is the preparation method of Wavelength converter of the present invention
Another embodiment schematic flow sheet, as shown in fig. 7, the present embodiment includes：
S41, in a reservoir placement white porosity ceramic substrate.
The explanation of step S41 refers to the explanation to step S11.
S42, in a reservoir addition barium nitrate solution, potassium silicate solution, fluorescent material, glass dust, and silicic acid precipitated barium is generated,
And the concentration of the potassium silicate after causing reaction in container is 0.06mol/L.
Unlike step S12, in this step, function powder is fluorescent material and glass dust.Glass dust is a kind of amorphous
Granular glass isotropic body, its transparency height and stable chemical nature.Here glass dust can't be to the chemistry in container
Reaction has any impact, and it can be precipitated down as fluorescent material.Here barium silicate solution, potassium silicate solution, fluorescent material, glass
The not certain order of the addition of glass powder, it is preferable that first adding barium silicate solution then adds potassium silicate solution, fluorescence
The mixed solution of powder, glass dust, is beneficial to silicic acid precipitated barium and is uniformly dispersed.
S43, settling vessel are until fluorescent material, barium silicate, glass dust whole precipitation, form phosphor powder layer, the phosphor powder layer
It is attached on white porosity ceramic substrate.
From unlike step S13, the glass dust that container is added can also be precipitated, therefore, phosphor powder layer includes glass dust.
S44, the redundant solution taken out in container, until leaving the white porosity ceramic substrate of attachment phosphor powder layer.
The explanation of step S44 refers to the explanation to step S14.
S45, the white porosity ceramic substrate to being attached with phosphor powder layer are heated, with molding phosphor sheet.
From unlike step S15, due to adding glass dust in fluorescent material, for molding phosphor sheet, heating-up temperature will
More than the softening temperature of glass dust (temperature is still far below the fusing point of potassium silicate).Now, after hot briquetting, glass
Powder can produce chemical bond with white porosity ceramic substrate, substantially increase the adhesion of glass dust and white porosity ceramics.
In addition, in order to reduce pore of the fluorescent material in forming process, step S45 can also be divided into the heating of two steps, i.e.,
First in the temperature less than 100 DEG C, the moisture in phosphor sheet is removed；Then molding is carried out to phosphor powder layer at high temperature.
By the manufacture method of the present embodiment, a Wavelength converter can be prepared, the Wavelength converter includes white
Color porous ceramic substrate and phosphor sheet, and phosphor sheet includes potassium silicate, barium silicate, fluorescent material and glass dust.Here
Potassium silicate and glass dust for by fluorescent material with barium silicate bonding into an entirety, while phosphor sheet is bonded in white porosity
On ceramic substrate.As the adhesion between glass dust and white porosity ceramic substrate is greater than potassium silicate with white porosity ceramics
Adhesion between substrate, the adhesion of phosphor sheet here and white porosity ceramic substrate can be than embodiment illustrated in fig. 1 more
It is high.
Similarly, in order to improve the luminous efficiency of phosphor sheet, it is preferable that the barium silicate in phosphor sheet and fluorescent material
Volume ratio is 2.7% to 6.8%.
What deserves to be explained is, in fact, the method in the present embodiment is not limited in using whiteware substrate, using saturating
The Wavelength converter of the preparations such as bright ceramic substrate also has higher adhesion.
The embodiment of the present invention also provides a kind of light-emitting device, including Wavelength converter, and the Wavelength converter can have
The structure having in the various embodiments described above and function.Light-emitting device is also including an excitation source for being used for outgoing exciting light, above-mentioned ripple
Long conversion equipment is used to receive the exciting light and the mixed light of outgoing Stimulated Light or Stimulated Light and exciting light.
Embodiments of the present invention are the foregoing is only, the scope of the claims of the present invention is not thereby limited, it is every using this
Equivalent structure or equivalent flow conversion that description of the invention and accompanying drawing content are made, or directly or indirectly it is used in other correlations
Technical field, is included within the scope of the present invention.
Claims (13)
1. a kind of manufacture method of Wavelength converter, it is characterised in that the manufacture method is comprised the following steps：
A, porous ceramic substrate is placed in a reservoir, the porous ceramic substrate is that white porosity ceramic substrate or transparent porous are made pottery
Porcelain substrate；
B, generation insoluble silicate：Soluble salt solutions are added in the above-described container, in adding potassium silicate and sodium silicate solution
At least one, and add function powder, function powder includes fluorescent material so that the soluble salt solutions and the potassium silicate and
At least one reaction in sodium silicate solution generates insoluble silicate, and also have in the container after making reaction potassium silicate and
At least one in sodium silicate is for insoluble silicate described in bonding and the function powder；
C, the standing container are until the function powder and insoluble silicate whole precipitation, form phosphor powder layer, the fluorescent material
Layer is attached on the porous ceramic substrate；
D, the redundant solution taken out in the container, until leaving the ceramic substrate of attachment phosphor powder layer；
E, the ceramic substrate heating to the attachment phosphor powder layer, with molding phosphor sheet；
Soluble salt solutions described in step B are barium, aluminum, calcium, at least one in the soluble salt solutions of strontium.
2. the manufacture method of Wavelength converter according to claim 1, it is characterised in that after step D, and in step
Before rapid E, also include：
F, by it is described attachment phosphor powder layer ceramic substrate less than or equal to 100 DEG C temperature heat, until remove phosphor powder layer
In moisture.
3. the manufacture method of Wavelength converter according to claim 1, it is characterised in that step E is：Will be described
The ceramic substrate of attachment phosphor powder layer is heated at 300 DEG C to 500 DEG C, with molding phosphor sheet.
4. the manufacture method of Wavelength converter according to claim 1, it is characterised in that step B includes：
B1, add in the above-described container to generate the soluble salt solutions of insoluble silicate；
B2, the function powder and at least one mixed solution in potassium silicate and sodium silicate solution are added in the above-described container,
And react generation insoluble silicate, and also there is in the container after causing reaction silicate ion for described in bonding not
Soluble silicate and the fluorescent material.
5. the manufacture method of Wavelength converter according to claim 4, it is characterised in that step B also includes：It is right
Solution in the container carries out ultrasonic disperse.
6. the manufacture method of Wavelength converter according to claim 1, it is characterised in that the function powder also includes glass
Glass powder.
7. the manufacture method of Wavelength converter according to any one of claim 1 to 6, it is characterised in that in step B
The concentration of the silicate ion after reaction in the container is 0.06mol/L or in more than 0.06mol/L.
8. the manufacture method of Wavelength converter according to claim 7, it is characterised in that the porous ceramic substrate is
Transparent porous ceramic substrate；
The concentration of the silicate ion after reacting in step B in the container is located between 0.06mol/L and 0.94mol/L.
9. the manufacture method of Wavelength converter according to claim 7, it is characterised in that described after reacting in step B
The concentration of the silicate ion in container is 0.19mol/L.
10. a kind of Wavelength converter, it is characterised in that the Wavelength converter includes：
Porous ceramic substrate and phosphor sheet, the porous ceramic substrate are transparent porous ceramic substrate；
The phosphor sheet includes sodium silicate and/or potassium silicate, insoluble silicate and function powder, and the function powder includes glimmering
Light powder, the sodium silicate and/or potassium silicate for by the insoluble silicate with function powder bonding into an entirety, and by institute
State phosphor sheet to be bonded on the ceramic substrate；
The insoluble silicate at least includes in barium silicate, aluminium silicate, calcium silicates and strontium silicate.
11. Wavelength converters according to claim 10, it is characterised in that the function powder also includes glass dust.
12. Wavelength converters according to any one of claim 10 to 11, it is characterised in that the insoluble silicic acid
Salt is 2.7% to 6.8% with the volume ratio of fluorescent material.
13. a kind of light-emitting devices, it is characterised in that include the wavelength convert dress as any one of claim 10 to 12
Put, also including an excitation source for being used for outgoing exciting light, the Wavelength converter is excited the light-emitting device for receiving this
The mixed light of light outgoing Stimulated Light or Stimulated Light and exciting light.
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| CN104315459B (en) * | 2014-11-03 | 2016-08-31 | 天津理工大学 | A kind of high efficiency laser lighting remote fluorescence coating and application thereof |
| 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 |
| CN112578551A (en) | 2019-09-30 | 2021-03-30 | 台达电子工业股份有限公司 | Wavelength conversion device |
| CN112578552A (en) | 2019-09-30 | 2021-03-30 | 台达电子工业股份有限公司 | Wavelength conversion device |
| CN112178591A (en) * | 2020-09-18 | 2021-01-05 | 广州光联电子科技有限公司 | Preparation method of wavelength conversion device for laser and wavelength conversion device |
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| CN102782082A (en) * | 2010-07-14 | 2012-11-14 | 日本电气硝子株式会社 | Phosphor composite member, LED device and method for manufacturing phosphor composite member |
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