CN115893987A - Glass fluorescent ceramic, preparation method thereof and wavelength conversion device - Google Patents
Glass fluorescent ceramic, preparation method thereof and wavelength conversion device Download PDFInfo
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- CN115893987A CN115893987A CN202211571128.4A CN202211571128A CN115893987A CN 115893987 A CN115893987 A CN 115893987A CN 202211571128 A CN202211571128 A CN 202211571128A CN 115893987 A CN115893987 A CN 115893987A
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Images
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
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- Luminescent Compositions (AREA)
Abstract
The invention discloses glass fluorescent ceramic, a preparation method thereof and a wavelength conversion device, wherein the glass fluorescent ceramic comprises a phosphor, a glass packaging body and air holes, the proportion of the air holes in the glass fluorescent ceramic is 20-40 vt%, the pore diameter of the air holes is 0.6-2 mu m, the proportion of the phosphor in the glass fluorescent ceramic is 40-50 vt%, and the proportion of the glass packaging body is 10-40 vt%. According to the invention, the specific air holes are formed in the glass fluorescent ceramic, so that the light scattering capacity can be improved, the mixing uniformity of excited light and excited light after being excited is improved, the problem of yellow aperture when a laser light source realizes an illumination function is effectively solved, the uniformity of light spots obtained when the glass fluorescent ceramic is used for carrying out wavelength conversion on laser is good, and the luminous flux and the illumination intensity are high.
Description
Technical Field
The invention relates to the technical field of fluorescent materials, in particular to glass fluorescent ceramic and a preparation method and a wavelength conversion device thereof.
Background
Laser Light (LD) is an emerging light source that has continued the LED light source for the 20 th century. Exciting light of the LED light source is in Lambert distribution, exciting light energy is distributed more uniformly in a light spot size range, and therefore the uniformity of excited fluorescent light spots is better. And the exciting light emitted by the LD laser light source has Gaussian distribution property: the laser energy of the irradiation area of the right center of the facula is high; the energy is low in the area away from the center of the spot. The low energy of the edge area is caused by the Gaussian distribution characteristics of the laser, so that the energy of the blue light is low, and on the other hand, the scattering attenuation of the laser in the direction perpendicular to the incident direction occurs in the wavelength conversion material, so that the energy loss of the laser also occurs, and finally, the central position excited by the laser in the wavelength conversion material has more exciting light and less blue light deviating from the central position, so that the phenomena of white light in the middle/blue light and yellow light around the fluorescent light spot, namely the phenomenon of Huang Guangjuan, occur, and the uniformity of the light spot is greatly influenced. In particular, in a high laser power light source, the phenomenon of the spot "Huang Guangjuan" is more remarkable.
Aiming at the problem of 'yellow circle' of a light spot in a laser light source, the prior art adopts a method of reducing the size of a wavelength conversion material to reduce the size of the wavelength conversion material to be close to the size of the laser light spot, so that blue laser only generates longitudinal excitation, and lateral excitation is greatly weakened, and the 'yellow circle' of the light spot is restrained. However, when the wavelength conversion material is reduced, the heat conduction and dissipation performance of the material are deteriorated, so that the use reliability of the wavelength conversion material is remarkably reduced. In addition, the coaxiality of the small-size wavelength conversion material and the laser spot in the light source is difficult to control, and the spot still has the phenomenon of uneven color.
Disclosure of Invention
The invention aims to overcome at least one defect of the prior art, and provides glass fluorescent ceramic which is used for solving the problem that a yellow aperture exists when a laser light source realizes an illumination function.
The invention also aims to provide a preparation method of the glass fluorescent ceramic.
It is still another object of the present invention to provide a wavelength conversion device.
The technical scheme adopted by the invention is as follows:
the glass fluorescent ceramic comprises a fluorescent body, a glass packaging body and air holes, wherein the proportion of the air holes in the glass fluorescent ceramic is 20-40 vt%, the pore diameter of the air holes is 0.6-2 mu m, the proportion of the fluorescent body in the glass fluorescent ceramic is 40-50 vt%, and the proportion of the glass packaging body in mass is 10-40 vt%.
Further, the phosphor is yellow or green phosphor of yttrium aluminum garnet YAG, luAG system, nitride LSN system, alpha and beta sialon system.
Further, the particle size of the phosphor is 2 to 5 μm.
Furthermore, the glass packaging body is glass powder with the softening point temperature of 550-1250 ℃, and the main component of the glass powder is one or a combination of more of aluminum oxide, silicon oxide, boron oxide, zinc oxide and magnesium oxide.
Further, the particle size of the glass powder is preferably 2 to 5 μm.
As an embodiment, the method for preparing the glass fluorescent ceramic comprises the following steps:
(1) Respectively weighing 60-75 parts of phosphor, 20-30 parts of glass packaging body and 10-15 parts of pore-forming agent particles according to the mass parts, adding the phosphor, the glass packaging body and the pore-forming agent particles into a ball-milling tank or a mortar filled with 40-60 parts of organic solvent, and carrying out ball milling or grinding to obtain mixed slurry with uniformly dispersed components;
(2) Placing the mixed slurry in a drying oven at the temperature of 60 +/-5 ℃ for heating and drying for 12 +/-2 h, and removing the organic solvent to obtain dry mixed powder; placing the mixed powder into a pressure of 60 +/-5 Mpa for cold isostatic pressing and forming to obtain a glass fluorescent ceramic green body;
(3) And (3) placing the glass fluorescent ceramic green body in a sintering furnace, and preserving heat for 0.5-2 h for sintering at the temperature of 600-1300 ℃ to obtain the glass fluorescent ceramic with the air hole ratio of 20-40 vt% and the air hole diameter of 0.6-2 mu m.
As another embodiment, the preparation method of the glass fluorescent ceramic comprises the following steps:
(1) Respectively weighing 60-75 parts of phosphor, 20-30 parts of glass packaging body and 10-15 parts of pore-forming agent particles according to the mass parts, adding the phosphor, the glass packaging body and the pore-forming agent particles into a ball-milling tank or a mortar filled with 40-60 parts of organic carrier, and carrying out ball milling or grinding to obtain mixed slurry with uniformly dispersed components;
(2) Placing the mixed slurry in a vacuum degree environment of-0.06 to-0.1 Mpa, and carrying out vacuum stirring and bubble discharge for 1 to 10min at the rotating speed of 600 to 1000rpm/min to prepare fluorescent slurry with proper viscosity for coating, scraping, dispensing or printing; the fluorescent slurry is attached to a substrate in a coating, dispensing or printing mode, and is pre-baked for 10-30 min at the temperature of 100-120 ℃. Then placing the glass ceramic into a sintering furnace, keeping the temperature for 0.5 to 2 hours at the temperature of between 600 and 1300 ℃, and sintering the glass ceramic to obtain the glass fluorescent ceramic with the air hole accounting ratio of between 20 and 40vt percent and the air hole aperture size of between 0.6 and 2 mu m.
Further, the pore-forming agent is one or more of PMMA, PS, starch, graphite powder, wood dust powder, ammonium bicarbonate and urea. Further, the pore-forming agent preferably has a particle diameter of 0.8 to 5 μm.
A wavelength conversion device comprises glass fluorescent ceramics, a fluorescent reflector layer or an optical film which transmits laser and reflects received laser, and a heat conduction substrate, wherein the glass fluorescent ceramics are sequentially stacked.
Furthermore, the fluorescent reflector layer is a metal reflecting layer, a dielectric film total reflection layer and a diffuse reflection layer.
Further, the heat conducting substrate is a metal substrate, an aluminum nitride ceramic substrate, a silicon carbide ceramic or a sapphire substrate.
Further, the wavelength conversion device is a fluorescent color wheel, and the fluorescent color wheel further comprises a rotating motor.
Further, the fluorescent color wheel also comprises heat dissipation fins.
Compared with the prior art, the invention has the beneficial effects that: according to the invention, the specific air holes are formed in the glass fluorescent ceramic, so that the light scattering capacity can be improved, the mixing uniformity of excited light and excited light after being excited is improved, the problem of yellow aperture when a laser light source realizes an illumination function is effectively solved, the uniformity of light spots obtained when the glass fluorescent ceramic is used for carrying out wavelength conversion on laser is good, and the luminous flux and the illumination intensity are high.
Drawings
FIG. 1 is a schematic structural view of a glass fluorescent ceramic according to embodiments 1 to 3 of the present invention.
Fig. 2 is a schematic structural diagram of a fluorescent color wheel in embodiment 4 of the present invention.
Fig. 3 is a schematic structural diagram of a fluorescent color wheel in embodiment 7.
Fig. 4 is a schematic structural diagram of the fluorescent color wheel of embodiment 8.
Fig. 5 is a diagram of the spot effect obtained by irradiating the fluorescent color wheel according to embodiment 4 with laser.
Fig. 6 is a photograph of a light beam obtained by irradiating laser light onto the fluorescent color wheel according to example 4.
Fig. 7 is a diagram of the effect of the light spot obtained by irradiating the fluorescent color wheel described in comparative example 1 with laser.
Fig. 8 is a photograph of a beam of laser light applied to the fluorescent color wheel of comparative example 1.
Fig. 9 is a diagram of the effect of the light spot obtained by irradiating the laser to the fluorescent color wheel of comparative example 2.
Fig. 10 is a photograph of a beam of laser light applied to the fluorescent color wheel of comparative example 2.
Detailed Description
In order to make the application purpose, technical solution and beneficial technical effects of the present application clearer, the present application is further described in detail with reference to the following embodiments. It should be understood that the embodiments described in this specification are only for the purpose of explaining the present application and are not intended to limit the present application.
For the sake of brevity, only some numerical ranges are explicitly disclosed herein. However, any lower limit may be combined with any upper limit to form ranges not explicitly recited; and any lower limit may be combined with any other lower limit to form a range not explicitly recited, and any upper limit may be combined with any other upper limit to form a range not explicitly recited. Also, although not explicitly recited, each point or individual value between endpoints of a range is encompassed within the range. Thus, each point or individual value can form a range not explicitly recited as its own lower or upper limit in combination with any other point or individual value or in combination with other lower or upper limits.
In the description herein, it is to be noted that, unless otherwise specified, "above" and "below" are inclusive, and "a plurality" of "one or more" means two or more.
The above summary of the present application is not intended to describe each disclosed embodiment or every implementation of the present application. The following description more particularly exemplifies illustrative embodiments. At various points throughout this application, guidance is provided through lists of examples, which examples can be used in various combinations. In each instance, the list is merely a representative group and should not be construed as exhaustive.
In the research process, the inventor finds that the most difficult point of realizing laser illumination at present is the uniformity of emergent light spots, and particularly, for a transmission type wavelength conversion device, the problem of a yellow light ring is always a technical problem of a laser illumination scheme which is difficult to overcome by the industry. In order to solve the problem of the yellow aperture, the most common practice is to not use the scheme of reducing the size of the wavelength conversion material, and not use an optical element to diffuse and homogenize light. However, the scheme of reducing the size of the wavelength conversion material can cause the heat conduction and heat dissipation performance of the material to be poor, the use reliability is poor, the optical loss can be caused by adopting the optical element to homogenize light, the luminous flux and the illumination are obviously reduced, the light effect is influenced, the high-brightness illumination effect of laser is greatly influenced, and the due advantages of the laser illumination are lost.
The present application has been made based on the discovery and study of the above-mentioned problems.
One aspect of the present application provides a glass fluorescent ceramic, including a phosphor, a glass package body and an air hole, wherein the proportion of the air hole in the glass fluorescent ceramic is 20-40 vt%, the pore size of the air hole is 0.6-2 μm, the proportion of the phosphor in the glass fluorescent ceramic is 40-50 vt%, and the proportion of the glass package body is 10-40 vt% (the proportion of the air hole, the glass fluorescent ceramic and the phosphor in the present application refers to the volume ratio).
According to the technical scheme, the proper pore phase is arranged in the glass fluorescent ceramic, the scattering capacity of light is enhanced, for example, the laser is blue laser, the refractive index of the blue light in the fluorescent body is about 1.7, the refractive index at the pore phase is about 1, the scattering of light in the glass fluorescent ceramic is enhanced by the difference of the refractive indexes of the blue light and the fluorescent body, the interaction between the blue light and the fluorescent material is enhanced by the proper scattering effect, more blue light is absorbed, part of the received laser light exceeding the critical angle can be reflected back, compared with a system without pores, the large-angle yellow light is reduced, the side light guiding is weakened, the overall emergent light spot is smaller, the yellow light ring is weakened or even disappears, and the uniformity of the emergent fluorescent light spot is improved. The laser light source adopting the scheme can solve the problem of uniformity of light spots such as 'yellow light ring' without reducing the size of the wavelength conversion material, and the degradation of the heat conduction and heat dissipation capacity of the wavelength conversion material can not be caused.
More specifically, the application takes the air holes with the volume ratio of 20-40 vt% and the pore size of 0.6-2 μm as the air hole phase, and the existence of the proper air holes enhances the scattering of light in the glass fluorescent ceramic, increases the interaction between the blue light and the fluorescent material, and leads to more blue light to be absorbed by the fluorescent material. When the content of the air holes is lower than 20vt%, the blue light absorbed by the fluorescent material is insufficient, the blue light is saturated, and the fluorescent material cannot realize the output of higher brightness; when the air hole content is higher than 40vt%, the blue light is too strongly scattered by the air holes, the scattering loss of the blue light is increased, the blue light is reduced, the fluorescent material is unsaturated, and the fluorescent material cannot realize the output of higher brightness. In addition, the scattering effect of the pores on blue light is related to pore size. The pore diameter satisfying the better scattering effect for visible light is in the range of about 2 times of wavelength, and the scattering effect of the pore diameter exceeding the range is deteriorated. The visible light wavelength is in the range of 400-800nm, so the pore diameter of the pores with better scattering effect is in the range of 0.8-1.6um, and the pore diameter of the internal pores is difficult to control in such a narrow range in the ceramic preparation process, so the pore diameter of the pores is in the range of 0.6-2um through formula and process control.
This application is through the size and the volume ratio of gas pocket in glass fluorescence pottery that rationally set up the gas pocket, can promote the scattering ability of this application glass fluorescence pottery to the exciting light, improve excited back exciting light and the mixing homogeneity that receives the laser, and then avoided the facula to appear middle white edge yellow "Huang Guangjuan" phenomenon, and because the gas pocket scattering has only changed the blue light scattering route in the present case, do not lead to the too much scattering loss of blue light, therefore holistic illuminance of facula and luminous flux are not influenced, the light efficiency of having guaranteed laser lighting when solving "yellow light circle" problem is unchangeable, very big promotion laser lighting's effect.
More preferably, the ratio of the pores in the glass fluorescent ceramic is 25 to 35vt%, the ratio of the phosphor in the glass fluorescent ceramic is 43 to 48vt%, and the ratio of the glass sealing body is 15 to 35vt%.
In any embodiment, the phosphor is a yellow or green phosphor of yttrium aluminum garnet YAG, luAG system, nitride LSN system, alpha and beta sialon system.
In any of the examples, the particle size of the phosphor is 2 to 5 μm. The pore diameter of the pores in the glass fluorescent ceramic is 0.6-2um, and the pore sources have two aspects, namely, the pore-forming agent is decomposed and the residual position is formed into a cavity, fluorescent powder particles are bridged, and the fluorescent powder particles with the particle diameter of 2-5um are bridged to well form the pores with the pore diameter of 0.6-2 um.
In any embodiment, the glass packaging body is glass powder with the softening point temperature of 450-1250 ℃, and the main component of the glass powder is one or a combination of more of aluminum oxide, silicon oxide, boron oxide, zinc oxide and magnesium oxide. More preferably, the glass package is glass frit having a softening point temperature of 550 to 1250 ℃, specifically glass frit containing silicon oxide, boron oxide, and zinc oxide. Because the complete decomposition temperature of the pore-forming agent particles in the glass fluorescent ceramic is about 600 ℃, the glass powder with the softening point above 550 ℃ is selected, and the sintering temperature is usually above 600 ℃, the complete residue-free decomposition of the pore-forming agent particles can be ensured, and the luminous efficiency of the glass fluorescent ceramic is not influenced. In addition, some rare earth doping elements are usually added in the phosphor, and functional rare earth elements are easy to oxidize, decompose and volatilize at the temperature of over 1300 ℃, so that the light efficiency of the glass fluorescent ceramic is weakened, the sintering temperature of the glass fluorescent ceramic cannot exceed the temperature, and the softening temperature of glass powder does not exceed 1250 ℃.
In any embodiment, the particle size of the glass powder is preferably 2 to 5 μm. In the glass fluorescent ceramic, the glass powder plays a role in connecting phosphor particles to provide strength. Under high-temperature sintering, the glass powder particles are melted to bond the fluorescent particles with each other and fill the holes formed by bridging the fluorescent particles, if the particle size of the glass powder particles is less than 2um, the particles fill part of the bridging holes of the fluorescent particles, and the porosity of the glass fluorescent ceramic is reduced. The particle size of the glass powder exceeds 5 mu m, the glass powder can be incompletely melted and bridged to form holes, and the size of the holes can be out of the range of the inner holes of the glass fluorescent ceramic, so that the luminous performance of the glass fluorescent ceramic is influenced.
The invention also provides a preparation method of the glass fluorescent ceramic, which comprises the following steps:
(1) Respectively weighing 60-75 parts of phosphor, 20-30 parts of glass packaging body and 10-15 parts of pore-forming agent particles according to the mass parts, adding the phosphor, the glass packaging body and the pore-forming agent particles into a ball-milling tank or a mortar filled with 40-60 parts of organic solvent, and carrying out ball milling or grinding to obtain mixed slurry with uniformly dispersed components;
(2) Placing the mixed slurry in a drying oven at the temperature of 60 +/-5 ℃ for heating and drying for 12 +/-2 h, removing the organic solvent in a ball milling tank or a mortar, and carrying out ball milling or grinding to obtain mixed slurry with uniformly dispersed components, thereby obtaining dry mixed powder; placing the mixed powder into a pressure of 60 +/-5 Mpa for cold isostatic pressing and forming to obtain a glass fluorescent ceramic green body;
(3) And placing the glass fluorescent ceramic green body in a sintering furnace, and preserving heat for 0.5-2 h for sintering at the temperature of 600-1300 ℃ to obtain the glass fluorescent ceramic with the volume ratio of 10-40% of pores and the pore diameter of 0.6-2 mu m.
In any embodiment, the organic solvent is one or two of absolute ethyl alcohol and isopropyl alcohol.
Preferably, the glass fluorescent ceramic green body is placed in a sintering furnace and is sintered for 0.5 to 2 hours at the temperature of 650 to 750 ℃.
Preferably, the phosphor is used in an amount of 60 to 65 parts.
The invention also provides another preparation method of the glass fluorescent ceramic, which comprises the following steps:
(1) Respectively weighing 60-75 parts of phosphor, 20-30 parts of glass packaging body and 10-15 parts of pore-forming agent particles according to the mass parts, adding the phosphor, the glass packaging body and the pore-forming agent particles into a ball-milling tank or a mortar filled with 40-60 parts of organic carrier, and carrying out ball milling or grinding to obtain mixed slurry with uniformly dispersed components;
(2) Placing the mixed slurry in a vacuum degree environment of-0.06-0.1 Mpa, and stirring and discharging the mixed slurry in vacuum at the rotating speed of 600-1000 rpm/min for 1-10 min to prepare fluorescent slurry with proper viscosity for coating, dispensing or printing; the fluorescent slurry is attached to a substrate in a coating, dispensing or printing mode, and is pre-baked for 10-30 min at the temperature of 100-120 ℃. Then placing the glass ceramic into a sintering furnace, keeping the temperature for 0.5 to 2 hours at the temperature of between 600 and 1300 ℃, and sintering the glass ceramic to obtain the glass fluorescent ceramic with the air hole accounting ratio of between 20 and 40vt percent and the air hole aperture size of between 0.6 and 2 mu m.
The pores in the glass fluorescent ceramic have two major forming ways, one of which contributes to gaps among bridging of phosphor particles; the other is provided by the residual positions of the particles after the pore-forming agent particles added in the preparation of the glass fluorescent material are burnt out.
In any embodiment, the pore-forming agent particles are preferably high-temperature easy-to-burn particles such as PMMA, PS, starch, graphite powder, wood dust powder, ammonium bicarbonate, urea and the like, and the particle size is preferably 0.8 to 5 μm.
This application on the other hand still provides a wavelength conversion device, including the glass fluorescence pottery, the optical film that the fluorescence reflector layer or transmission laser reflection received the laser and the heat conduction base plate that stack gradually the setting, the glass fluorescence pottery is foretell glass fluorescence pottery.
In any embodiment, the fluorescent reflector layer is a metal reflective layer, a dielectric film total reflective layer, or a diffuse reflective layer.
In any embodiment, the heat conductive substrate is a metal substrate, an aluminum nitride ceramic substrate, a silicon carbide ceramic, or a sapphire substrate.
In any embodiment, the wavelength conversion device is a fluorescent color wheel, and the fluorescent color wheel further comprises a rotation motor.
In any embodiment, the fluorescent color wheel further includes heat dissipation fins.
Examples
The present disclosure is more particularly described in the following examples that are intended as illustrative only, since various modifications and changes within the scope of the present disclosure will be apparent to those skilled in the art. Unless otherwise stated, all parts, percentages, and ratios reported in the following examples are on a mass basis, and all materials used in the examples are commercially available or synthesized according to conventional methods, as otherwise specified, and can be used directly without further treatment, and the instruments used in the examples are commercially available.
Example 1
As shown in fig. 1, a glass fluorescent ceramic comprises a fluorescent body 12, a glass package 11 and air holes 13, wherein the volume ratio of the air holes 13 in the glass fluorescent ceramic is 33vt%, the pore diameter size of the air holes is 0.6-2 μm, the ratio of the fluorescent body 12 in the glass fluorescent ceramic is 44vt%, and the ratio of the glass package 11 is 23vt%, wherein:
the phosphor is yttrium aluminum garnet YAG yellow fluorescent powder, and the particle size of the phosphor is 2-5 mu m.
The main components of the glass packaging body are glass powder of silicon oxide, boron oxide and zinc oxide, the softening point temperature is 650 ℃, and the particle size is 2-5 mu m.
The glass fluorescent ceramic is prepared by the following preparation method:
(1) Respectively weighing 64 parts of phosphor, 24 parts of glass packaging body and 12 parts of pore-forming agent particles according to mass parts, adding the phosphor, the glass packaging body and the pore-forming agent particles into a ball-milling tank filled with 52 parts of absolute ethyl alcohol, ball-milling and mixing alumina or zirconia grinding balls for 12-24 hours according to the ball-material ratio of 2:1, and taking the ball-milling tank down to obtain mixed slurry with uniformly dispersed components;
(2) Placing the mixed slurry in a drying oven at the temperature of 60 +/-5 ℃ for heating and drying for 12 +/-2 h, and removing absolute ethyl alcohol to obtain dry mixed powder; placing the mixed powder into a pressure of 60 +/-5 Mpa for cold isostatic pressing and forming to obtain a glass fluorescent ceramic green body;
(3) And (3) placing the glass fluorescent ceramic green body in a sintering furnace, and preserving heat for 0.5-2 h at the temperature of 680-720 ℃ for sintering to obtain the glass fluorescent ceramic with the volume ratio of the pores of 33vt% and the pore diameter of 0.6-2 mu m.
Example 2
As shown in fig. 1, a glass fluorescent ceramic comprises a phosphor 12, a glass package 11 and pores 13, wherein the volume proportion of the pores 13 in the glass fluorescent ceramic is 25%, the pore diameter size of the pores is 0.6 to 2 μm, the proportion of the phosphor 12 in the glass fluorescent ceramic is 43vt%, and the proportion of the glass package 11 in the glass fluorescent ceramic is 32vt%, wherein:
the phosphor is yttrium aluminum garnet YAG yellow fluorescent powder, and the particle size of the phosphor is 2-5 mu m.
The glass package is glass powder with silicon oxide, boron oxide and zinc oxide as main components and has softening point temperature of 650 deg.c and grain size of 2-5 microns.
The glass fluorescent ceramic is prepared by the following preparation method:
(1) Respectively weighing 62 parts of a phosphor, 28 parts of a glass packaging body and 10 parts of pore-forming agent particles according to mass parts, adding the phosphor, the glass packaging body and the pore-forming agent particles into a ball-milling tank filled with 50 parts of absolute ethyl alcohol, ball-milling and mixing alumina or zirconia grinding balls for 12-24 hours according to a ball-to-material ratio of 2:1, and taking the ball-milling tank down to obtain mixed slurry with uniformly dispersed components;
(2) Placing the mixed slurry in a drying oven at the temperature of 60 +/-5 ℃ for heating and drying for 12 +/-2 h, and removing absolute ethyl alcohol to obtain dry mixed powder; placing the mixed powder into a pressure of 60 +/-5 Mpa for cold isostatic pressing and forming to obtain a glass fluorescent ceramic green body;
(3) And (3) placing the glass fluorescent ceramic green body in a sintering furnace, and preserving heat for 0.5-2 h at the temperature of 680-720 ℃ for sintering to obtain the glass fluorescent ceramic with the volume ratio of air holes of 25vt% and the pore diameter of 0.6-2 mu m.
Example 3
As shown in fig. 1, a glass fluorescent ceramic includes a phosphor, a glass package and pores, the volume ratio of the pores in the glass fluorescent ceramic is 35vt%, the pore size of the pores is 0.6 to 2 μm, the ratio of the phosphor in the glass fluorescent ceramic is 48vt%, and the ratio of the glass package is 17vt%, wherein:
the fluorophor is yttrium aluminum garnet YAG yellow fluorescent powder, and the grain size of the fluorophor is 2-5 mu m.
The glass package is glass powder with silicon oxide, boron oxide and zinc oxide as main components and has softening point temperature of 650 deg.c and grain size of 2-5 microns. .
The glass fluorescent ceramic is prepared by the following preparation method:
(1) Weighing 65 parts of phosphor, 21 parts of glass packaging body and 14 parts of pore-forming agent particles according to mass parts, respectively, adding the phosphor, the glass packaging body and the pore-forming agent particles into a ball-milling tank filled with 55 parts of absolute ethyl alcohol, ball-milling and mixing alumina or zirconia grinding balls for 12-24 hours according to a ball-material ratio of 2:1, and taking the ball-milling tank down to obtain mixed slurry with uniformly dispersed components;
(2) Placing the mixed slurry in a drying oven at the temperature of 60 +/-5 ℃ for heating and drying for 12 +/-2 h, and removing absolute ethyl alcohol to obtain dry mixed powder; placing the mixed powder into a pressure of 60 +/-5 Mpa for cold isostatic pressing and forming to obtain a glass fluorescent ceramic green body;
(3) And (3) placing the glass fluorescent ceramic green body in a sintering furnace, and preserving heat for 0.5-2 h at the temperature of 680-720 ℃ for sintering to obtain the glass fluorescent ceramic with the volume ratio of the pores of 35vt% and the pore diameter of 0.6-2 mu m.
The pore volume ratio of the glass fluorescent ceramic described in the above example was measured by the following method: and testing the pore volume of the glass fluorescent ceramic by adopting an Archimedes drainage method. Testing the mass M dry of the ceramic in the air, and after absorbing water, the mass M wet in the air, wherein the mass M wet-M dry is the water absorption volume and is also the pore volume; testingThe mass M of the ceramic in water, (Mdry-Mwater) is the volume of water to be drained and is also the volume of the ceramic; and (M wet-M dry)/(M dry-M water) is the porosity of the glass fluorescent ceramic. The pore size of the pores of the glass fluorescent ceramic described in the above example is measured by the following method: testing the pore diameter of the glass fluorescent ceramic by adopting a mercury pressing method:
in the formula: r-pore diameter; σ -surface tension-constant of mercury, θ -wetting angle-constant of porous material and mercury measured, ρ -pressure of mercury intrusion, N/m 2 . The pore size distribution of the ceramic can be obtained by testing the pressure rho of the pressed mercury.
Example 4
As shown in fig. 2, the fluorescent color wheel includes a glass fluorescent ceramic 1, a metal reflective layer 2, and an aluminum substrate 3, which are sequentially stacked, where the glass fluorescent ceramic 1 is the glass fluorescent ceramic described in embodiment 1. In particular, the fluorescent color wheel also comprises a rotation motor 4. The assembly scheme of the fluorescent color wheel of the embodiment is as follows: the glass fluorescent ceramic is adhered to an aluminum circular ring plated with a metal reflective silver layer through a high-transparency organic silicon adhesive, the aluminum circular ring is baked for 0.5 to 4 hours at the temperature of 120 to 180 ℃, cured at high temperature, cooled and then provided with a rotating motor, and the fluorescent color wheel is manufactured.
Example 5
A fluorescent color wheel, the structure and assembly scheme of which are substantially the same as those of embodiment 4, except that the glass fluorescent ceramic used in embodiment 5 is the glass fluorescent ceramic described in embodiment 2.
Example 6
A fluorescent color wheel having substantially the same structure and assembly scheme as in example 4, except that the glass fluorescent ceramic used in example 6 is the glass fluorescent ceramic described in example 3.
Example 7
As shown in fig. 3, a fluorescent color wheel includes a glass fluorescent ceramic 1, a diffuse reflection layer 4, and a high thermal conductivity aluminum nitride ceramic substrate 6, which are sequentially stacked, where the glass fluorescent ceramic is the glass fluorescent ceramic described in embodiment 1. The diffuse reflection layer 5 is made of glass powder to encapsulate white particles such as alumina and magnesia. In particular, the fluorescent color wheel also comprises a rotation motor 4. The assembly scheme of the fluorescent color wheel of the embodiment is as follows: co-firing the glass fluorescent ceramic and the aluminum nitride ceramic ring coated with the diffuse reflection slurry on the surface at a high temperature of 600-650 ℃, preserving the temperature for 30-120min, and assembling a rotating motor after sintering to obtain the fluorescent color wheel.
Example 8
The utility model provides a fluorescence colour wheel, includes the glass fluorescence pottery 1, the anti-membrane of turning yellow 7 and the sapphire ring 8 of passing through the blue light that stack gradually the setting, still includes rotation motor 4. The fluorescent color wheel is prepared and assembled by the following scheme:
respectively weighing 64 parts of a phosphor, 24 parts of a glass packaging body and 12 parts of pore-forming agent particles according to parts by mass, adding the phosphor, the glass packaging body and the pore-forming agent particles into a mortar made of agate material, and dropwise adding an organic carrier prepared from 40 parts of terpineol and 1.6 parts of ethyl cellulose; grinding and dispersing for 5-20 min, then pouring out the fluorescent slurry, stirring and discharging the fluorescent slurry in a planetary vacuum manner for 2-5 min under the vacuum degree of-0.1 Mpa and the rotating speed of 600-1000 rpm/min to prepare the fluorescent slurry with moderate viscosity and suitable for coating, scraping, dispensing and printing; the fluorescent slurry is attached to the surface of a transparent sapphire substrate with a blue light-transmitting and yellow-reflecting film attached to the surface in a coating, dispensing or printing mode, and is pre-baked at the temperature of 100-120 ℃ for 10-30 min; and after the fluorescent layer is dried, placing the sapphire transparent substrate attached with the fluorescent layer in a sintering furnace for heat preservation at the temperature of 500-1300 ℃.
Comparative example 1
A fluorescent color wheel comprises glass fluorescent ceramics, a metal reflecting layer and an aluminum substrate which are sequentially stacked, and the preparation method of the fluorescent color wheel is substantially the same as that of embodiment 4, the difference is that the glass fluorescent ceramics in comparative example 1 are different, the volume proportion of pores of the glass fluorescent in the glass fluorescent ceramics in the comparative example 1 is 8vt%, and the fluorescent color wheel is obtained by the following scheme:
(1) Respectively weighing 56 parts of phosphor, 42 parts of glass packaging body and 2 parts of pore-forming agent particles according to mass parts, adding the phosphor, the glass packaging body and the pore-forming agent particles into a ball-milling tank filled with 48 parts of absolute ethyl alcohol, ball-milling and mixing alumina or zirconia grinding balls for 12-24 hours according to a ball-material ratio of 2:1, and taking the ball-milling tank down to obtain mixed slurry with uniformly dispersed components;
(2) Placing the mixed slurry in a drying oven at the temperature of 60 +/-5 ℃ for heating and drying for 12 +/-2 h, and removing absolute ethyl alcohol to obtain dry mixed powder; placing the mixed powder into a pressure of 60 +/-5 Mpa for cold isostatic pressing and forming to obtain a glass fluorescent ceramic green body;
(3) And (3) placing the glass fluorescent ceramic green body in a sintering furnace, and sintering at 680-720 ℃ for 2h to obtain the glass fluorescent ceramic with the volume of air holes accounting for 8vt% and the pore diameter of the air holes being 0.6-2 mu m.
Comparative example 2
A fluorescent color wheel comprises glass fluorescent ceramics, a metal reflecting layer and an aluminum substrate which are sequentially stacked, and the preparation method of the fluorescent color wheel is substantially the same as that of embodiment 4, except that the glass fluorescent ceramics in the comparative example 1 are different, the volume proportion of pores of the glass fluorescent in the comparative example 1 in the glass fluorescent ceramics is 48vt%, and the fluorescent color wheel is obtained by the following scheme:
(1) Respectively weighing 64 parts of phosphor, 18 parts of glass packaging body and 18 parts of pore-forming agent particles according to the mass parts, adding the phosphor, the glass packaging body and the pore-forming agent particles into a ball-milling tank filled with 58 parts of absolute ethyl alcohol, ball-milling and mixing alumina or zirconia grinding balls for 12-24 hours according to the ball-material ratio of 2:1, and taking the ball-milling tank down to obtain mixed slurry with uniformly dispersed components;
(2) Placing the mixed slurry in a drying oven at the temperature of 60 +/-5 ℃ for heating and drying for 12 +/-2 h, and removing absolute ethyl alcohol to obtain dry mixed powder; placing the mixed powder into a pressure of 60 +/-5 Mpa for cold isostatic pressing and forming to obtain a glass fluorescent ceramic green body;
(3) And (3) placing the glass fluorescent ceramic green body in a sintering furnace, and preserving heat for 2h for sintering at the temperature of 680-720 ℃ to obtain the glass fluorescent ceramic with the pore volume ratio of 48vt% and the pore diameter of 0.6-2 mu m.
Comparative example 3
A fluorescent color wheel comprises glass fluorescent ceramics, a metal reflecting layer and an aluminum substrate which are sequentially stacked, and the preparation method of the fluorescent color wheel is substantially the same as that of embodiment 4, the difference is that the glass fluorescent ceramics in comparative example 1 is different from that of the glass fluorescent ceramics in comparative example 1, the pore size of pores of the glass fluorescent in comparative example 1 is 4-5 μm, the volume ratio of the pores in the glass fluorescent ceramics is 34vt%, the ratio of the fluorescent body 12 in the glass fluorescent ceramics is 43vt%, and the ratio of the glass package 11 is 23vt%, and the fluorescent color wheel is obtained by the following scheme:
the phosphor is yttrium aluminum garnet YAG, and the particle size of the phosphor is 12-14 μm.
The glass packaging body mainly comprises glass powder of silicon oxide, boron oxide and zinc oxide, the softening point temperature of the glass powder is 650 ℃, and the particle size of the glass powder is 12-14 mu m.
The glass fluorescent ceramic is prepared by the following preparation method:
(1) Respectively weighing 64 parts of phosphor, 23 parts of glass packaging body and 13 parts of pore-forming agent particles according to mass parts, adding the phosphor, the glass packaging body and the pore-forming agent particles into a ball-milling tank filled with 52 parts of absolute ethyl alcohol, ball-milling and mixing alumina or zirconia grinding balls for 12-24 hours according to the ball-material ratio of 2:1, and taking the ball-milling tank down to obtain mixed slurry with uniformly dispersed components;
(2) Placing the mixed slurry in a drying oven at the temperature of 60 +/-5 ℃ for heating and drying for 12 +/-2 h, and removing absolute ethyl alcohol to obtain dry mixed powder; placing the mixed powder into a pressure of 60 +/-5 Mpa for cold isostatic pressing and forming to obtain a glass fluorescent ceramic green body;
(3) And (3) placing the glass fluorescent ceramic green body in a sintering furnace, and preserving heat for 0.5-2 h at the temperature of 680-720 ℃ for sintering to obtain the glass fluorescent ceramic with the volume ratio of the pores being 34vt% and the pore diameter of the pores being 4-5 mu m.
In order to verify the effect of the fluorescent color wheel described in the present application, the fluorescent color wheels described in examples 4 to 8, comparative example 1, comparative example 2, and comparative example 3 were subjected to a correlation performance test:
the fluorescent color wheel was irradiated with laser light of 100W in laser power, and the rotational speed of the color wheel was set at 7200rpm/min. And testing the illuminance and luminous flux of the light spots, and observing the light spot effect and the light beams. The test methods of the respective data are as follows
(1) Testing the central illumination of the light spot: the laser light source with the blue light power of 100w is adopted, the laser spot size is phi 2.5mm, and the energy is in Gaussian distribution; the central illuminance of the spot on the upper wall of the glass fluorescent color wheel is tested by using the laser light source of the glass fluorescent color wheel mounting machine in the embodiment 4 to the embodiment 8, the comparative example 1, the comparative example 2 and the comparative example 3, and under a collimating lens with the distance of 10m and the length of 130 mm.
(2) And (3) testing luminous flux: the laser light source with the blue light power of 100w is adopted, the laser spot size is phi 2.5mm, and the energy is in Gaussian distribution; the laser light source of the glass fluorescent color wheel assembly machine in the embodiment 4 to the embodiment 8, the comparative example 1, the comparative example 2 and the comparative example 3 is lightened, a light outlet of the light source is aligned to an entrance of an integrating sphere, so that light rays completely enter the integrating sphere, and the luminous flux of the glass fluorescent color wheel is tested.
(3) Color of light spot on wall: the laser light source with the blue light power of 100w is adopted, the laser spot size is phi 2.5mm, and the energy is in Gaussian distribution; the laser light sources of the glass fluorescent color wheel mounting machine in the embodiment 4 to the embodiment 8, the comparative example 1, the comparative example 2 and the comparative example 3 are collimated by a 130mm collimating lens, fluorescent light spots are projected to a white wall, and the color uniformity of the light spots is observed.
(4) Color of light beam: the laser light source with the blue light power of 100w is adopted, the laser spot size is phi 2.5mm, and the energy is in Gaussian distribution; the laser light source of the glass fluorescent color wheel machine in the embodiment 4 to the embodiment 8, the comparative example 1, the comparative example 2 and the comparative example 3 adopts a 130mm collimating lens to collimate light and observe the color uniformity of fluorescent light beams.
The test results are shown in Table 1.
The spot effect diagram and the beam photograph diagram of example 4 are shown in fig. 5 and 6, respectively. The speckle effect pattern and the beam photograph pattern of comparative example 1 are shown in fig. 7 and 8, respectively. The spot effect diagram and the beam photograph diagram obtained in comparative example 2 are shown in fig. 9 and 10, respectively.
It should be understood that the above-mentioned embodiments of the present invention are only examples for clearly illustrating the technical solutions of the present invention, and are not intended to limit the specific embodiments of the present invention. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention claims should be included in the protection scope of the present invention claims.
Claims (10)
1. The glass fluorescent ceramic is characterized by comprising a fluorescent body, a glass packaging body and air holes, wherein the proportion of the air holes in the glass fluorescent ceramic is 20-40 vt%, the pore diameter of the air holes is 0.6-2 mu m, the proportion of the fluorescent body in the glass fluorescent ceramic is 40-50 vt%, and the proportion of the glass packaging body is 10-40 vt%.
2. The glass fluorescent ceramic of claim 1, wherein the phosphor is a yellow or green phosphor of Yttrium Aluminum Garnet (YAG), luAG system, nitride (LSN) system, alpha and beta sialon system.
3. The glass fluorescent ceramic according to claim 1, wherein the particle size of the phosphor is 2 to 5 μm.
4. The glass fluorescent ceramic of claim 1, wherein the glass package is glass powder with a softening point temperature of 450-1250 ℃, and the main component of the glass powder is one or a combination of more of aluminum oxide, silicon oxide, boron oxide, zinc oxide and magnesium oxide.
5. The glass fluorescent ceramic according to claim 4, wherein the glass frit has a particle size of 2 to 5 μm.
6. The method for preparing a glass fluorescent ceramic according to any of claims 1 to 5, characterized by comprising the steps of:
(1) Respectively weighing 60-75 parts of phosphor, 20-30 parts of glass packaging body and 10-15 parts of pore-forming agent particles according to the mass parts, adding the phosphor, the glass packaging body and the pore-forming agent particles into a ball-milling tank or a mortar filled with 40-60 parts of organic solvent, and carrying out ball milling or grinding to obtain mixed slurry with uniformly dispersed components;
(2) Placing the mixed slurry in a drying oven at the temperature of 60 +/-5 ℃ for heating and drying for 12 +/-2 h, and removing the organic solvent to obtain dry mixed powder; placing the mixed powder into a pressure of 60 +/-5 Mpa for cold isostatic pressing and forming to obtain a glass fluorescent ceramic green body;
(3) And (3) placing the glass fluorescent ceramic green body in a sintering furnace, and preserving heat for 0.5-2 h for sintering at the temperature of 600-1300 ℃ to obtain the glass fluorescent ceramic with the air hole ratio of 20-40 vt% and the air hole diameter of 0.6-2 mu m.
7. The method for preparing a glass fluorescent ceramic according to any of claims 1 to 5, characterized by comprising the steps of:
(1) Respectively weighing 60-75 parts of phosphor, 20-30 parts of glass packaging body and 10-15 parts of pore-forming agent particles according to the mass parts, adding the phosphor, the glass packaging body and the pore-forming agent particles into a ball-milling tank or a mortar filled with 40-60 parts of organic carrier, and carrying out ball milling or grinding to obtain mixed slurry with uniformly dispersed components;
(2) Placing the mixed slurry in a vacuum degree environment of-0.06 to-0.1 Mpa, and carrying out vacuum stirring and bubble discharge for 1 to 10min at the rotating speed of 600 to 1000rpm/min to prepare fluorescent slurry with proper viscosity for coating, scraping, dispensing or printing; the fluorescent slurry is attached to a substrate in a coating, scraping, dispensing or printing mode, and is pre-baked for 10-30 min at the temperature of 100-120 ℃. Then placing the glass ceramic into a sintering furnace, keeping the temperature for 0.5 to 2 hours at the temperature of between 600 and 1300 ℃, and sintering the glass ceramic to obtain the glass fluorescent ceramic with the air hole accounting ratio of between 20 and 40vt percent and the air hole aperture size of between 0.6 and 2 mu m.
8. A wavelength conversion device comprising a glass fluorescent ceramic according to any one of claims 1 to 5, a fluorescent reflector layer or an optical film which transmits laser light and reflects received laser light, and a heat conductive substrate, which are stacked in this order.
9. The wavelength conversion device according to claim 1, wherein the fluorescent reflector layer is a metallic reflective layer or a diffuse reflective layer.
10. The wavelength conversion device according to claim 1, wherein the thermally conductive substrate is a metal substrate, an aluminum nitride ceramic substrate, a silicon carbide ceramic, or a sapphire substrate.
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