CN110927844B - Diffuse reflection device, preparation method thereof and wavelength conversion device - Google Patents
Diffuse reflection device, preparation method thereof and wavelength conversion device Download PDFInfo
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- CN110927844B CN110927844B CN201811099651.5A CN201811099651A CN110927844B CN 110927844 B CN110927844 B CN 110927844B CN 201811099651 A CN201811099651 A CN 201811099651A CN 110927844 B CN110927844 B CN 110927844B
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/02—Diffusing elements; Afocal elements
- G02B5/0205—Diffusing elements; Afocal elements characterised by the diffusing properties
- G02B5/021—Diffusing elements; Afocal elements characterised by the diffusing properties the diffusion taking place at the element's surface, e.g. by means of surface roughening or microprismatic structures
- G02B5/0226—Diffusing elements; Afocal elements characterised by the diffusing properties the diffusion taking place at the element's surface, e.g. by means of surface roughening or microprismatic structures having particles on the surface
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F21—LIGHTING
- F21V—FUNCTIONAL FEATURES OR DETAILS OF LIGHTING DEVICES OR SYSTEMS THEREOF; STRUCTURAL COMBINATIONS OF LIGHTING DEVICES WITH OTHER ARTICLES, NOT OTHERWISE PROVIDED FOR
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F21—LIGHTING
- F21V—FUNCTIONAL FEATURES OR DETAILS OF LIGHTING DEVICES OR SYSTEMS THEREOF; STRUCTURAL COMBINATIONS OF LIGHTING DEVICES WITH OTHER ARTICLES, NOT OTHERWISE PROVIDED FOR
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- F21V9/40—Elements for modifying spectral properties, polarisation or intensity of the light emitted, e.g. filters with provision for controlling spectral properties, e.g. colour, or intensity
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- G02B5/00—Optical elements other than lenses
- G02B5/02—Diffusing elements; Afocal elements
- G02B5/0205—Diffusing elements; Afocal elements characterised by the diffusing properties
- G02B5/0236—Diffusing elements; Afocal elements characterised by the diffusing properties the diffusion taking place within the volume of the element
- G02B5/0242—Diffusing elements; Afocal elements characterised by the diffusing properties the diffusion taking place within the volume of the element by means of dispersed particles
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- G02B5/12—Reflex reflectors
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03B—APPARATUS OR ARRANGEMENTS FOR TAKING PHOTOGRAPHS OR FOR PROJECTING OR VIEWING THEM; APPARATUS OR ARRANGEMENTS EMPLOYING ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ACCESSORIES THEREFOR
- G03B21/00—Projectors or projection-type viewers; Accessories therefor
- G03B21/14—Details
- G03B21/20—Lamp housings
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03B—APPARATUS OR ARRANGEMENTS FOR TAKING PHOTOGRAPHS OR FOR PROJECTING OR VIEWING THEM; APPARATUS OR ARRANGEMENTS EMPLOYING ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ACCESSORIES THEREFOR
- G03B21/00—Projectors or projection-type viewers; Accessories therefor
- G03B21/14—Details
- G03B21/20—Lamp housings
- G03B21/2006—Lamp housings characterised by the light source
- G03B21/2033—LED or laser light sources
- G03B21/204—LED or laser light sources using secondary light emission, e.g. luminescence or fluorescence
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Abstract
The invention discloses a diffuse reflection device which comprises a substrate and a diffuse reflection layer which are superposed, wherein the diffuse reflection layer comprises ceramic microspheres, diffuse reflection particles and adhesives, and the diffuse reflection particles and the adhesives are coated on the surfaces of the ceramic microspheres and/or are filled in gaps among the ceramic microspheres; wherein the grain diameter of the ceramic microspheres is 0.1 mm-0.5 mm; the particle size of the diffuse reflection particles is 20 nm-200 nm. According to the invention, micron-sized ceramic microspheres are introduced into the diffuse reflection layer, and other finer diffuse reflection particles coat the surfaces of the ceramic microspheres and/or are filled into gaps of the alumina spheres; the network structure main body is formed by relatively compact ceramic microspheres, the pores formed among the ceramic microspheres are uniform, the pore diameter is relatively smaller, and the pore structure of the diffuse reflection layer can be refined, so that the shielding effect of diffuse reflection particles in the diffuse reflection layer on the surfaces of pores and glass phases can be effectively improved, and the reflectivity of the diffuse reflection device is further improved.
Description
Technical Field
The invention relates to the field of illumination and projection display, in particular to a diffuse reflection device, a preparation method thereof and a wavelength conversion device.
Background
Currently, laser light source technology is focused on the illumination field due to its high brightness and high electro-optical efficiency. In the technical route of the laser light source, a wavelength conversion scheme has the advantages of efficiency and cost, and becomes one of the mainstream technical routes; among them, the diffuse reflection device or the wavelength conversion device is an important component in the laser light source, which is one of important components directly determining the performance of the laser light source. In the prior art, a diffuse reflection device generally comprises a diffuse reflection layer, the diffuse reflection layer is a functional layer with low thermal conductivity, the diffuse reflection layer is mainly formed by bonding fine white diffuse reflection particles (titanium oxide, aluminum oxide and the like) through a bonding phase (silica gel, glass and the like), wherein the thermal conductivity of the fine white diffuse reflection particles (titanium oxide and the like) and the bonding phase is poor, the excitation power is difficult to improve, and the brightness or the luminous efficiency cannot be improved; thus, for a diffuse reflective layer, it requires not only a higher reflectivity but also a better thermal conductivity.
At present, the reflectivity of the reflecting layer is mainly improved by increasing the content of the diffuse reflection particles or increasing the thickness of the reflecting layer. The increase of the content of the diffuse reflection particles in the diffuse reflection layer inevitably needs more binding phase to wet and coat the surfaces of the particles to form a continuous and compact reflection layer; however, the content of diffuse reflection particles in the diffuse reflection layer is increased, the content of a binding phase is bound to be reduced, so that more pores and the like are formed in the formed reflection layer, the loose reflection layer is not favorable for being well attached to the heat dissipation substrate, and meanwhile, the loose structure is not favorable for improving the heat conduction performance; on the other hand, increasing the thickness of the diffuse reflection layer will increase the reflectivity, but at the same time the thermal conductivity will decrease. This is not advantageous for improving the efficiency and brightness of the diffuse reflection device or the wavelength conversion device. Therefore, it is necessary to provide a diffuse reflection device having a high reflectance while having a high thermal conductivity.
Disclosure of Invention
The invention mainly aims to provide a diffuse reflection device, and aims to solve the technical problem of low reflectivity in the prior art.
The invention provides a diffuse reflection device which is characterized by comprising a substrate and a diffuse reflection layer which are superposed, wherein the diffuse reflection layer comprises ceramic microspheres, diffuse reflection particles and adhesives, and the diffuse reflection particles and the adhesives are coated on the surfaces of the ceramic microspheres and/or filled between gaps of the ceramic microspheres;
wherein the grain diameter of the ceramic microspheres is 0.1 mm-0.5 mm; the particle size of the diffuse reflection particles is 20-200 nm, and the mass ratio of the diffuse reflection particles to the ceramic microspheres to the adhesive is (0.6-10) to (0.3-8): (1-5).
Preferably, the ceramic microspheres are at least one of alumina, magnesia, or boron nitride.
Preferably, the diffuse reflection particles are at least one of barium sulfate, aluminum oxide, magnesium oxide, titanium oxide, or zirconium oxide.
Preferably, the adhesive is one of glass, water glass, silica gel or resin.
Preferably, the substrate is a metal substrate or a ceramic substrate.
Preferably, the ceramic microspheres are in a single-layer tiled arrangement in the diffuse reflective layer.
Preferably, the ceramic microspheres are laid flat in a single layer close-packed manner in the diffuse reflection layer.
Preferably, the thickness of the diffuse reflection layer is 0.1mm to 0.5 mm.
The second aspect of the present invention further provides a light emitting device, including any one of the diffuse reflection devices described above, further including a fluorescent layer disposed on the diffuse reflection layer, wherein the fluorescent layer is capable of emitting excited light under excitation of the excited light.
The third aspect of the present invention also provides a method for manufacturing a diffuse reflection apparatus, comprising the steps of:
A. mixing and dispersing raw materials;
B. b, printing by adopting a silk screen or a steel screen mesh plate, and coating the slurry obtained in the step A on a substrate;
C. sintering or curing to obtain the diffuse reflection device.
Has the advantages that: according to the invention, micron-sized ceramic microspheres are introduced into the diffuse reflection layer, and other finer nanoscale diffuse reflection particles coat the surfaces of the ceramic microspheres and/or are filled into gaps of the ceramic microspheres; the network structure main body is formed by relatively compact ceramic microspheres, the pores formed among the ceramic microspheres are uniform and relatively smaller, and the pore structure in the diffuse reflection layer can be refined, so that the shielding effect of diffuse reflection particles in the diffuse reflection layer on the surfaces of the pores and the glass phase can be effectively improved, and the reflectivity of the diffuse reflection device is further improved.
Drawings
FIG. 1 is a schematic diagram of the construction of one embodiment of the diffuse reflection apparatus of the present invention;
FIG. 2 is a schematic structural diagram of another embodiment of the diffuse reflection apparatus of the present invention;
FIG. 3 is a schematic structural diagram of an embodiment of the diffuse reflection apparatus of the present invention;
FIG. 4 is a schematic structural view of one embodiment of a tiling of ceramic microspheres according to the present invention;
FIG. 5 is a schematic structural diagram of one embodiment of the close-packed and flat-laid arrangement of ceramic microspheres in the present invention;
FIG. 6 is a schematic structural diagram of another embodiment of the close-packed and flat-laid ceramic microspheres of the present invention;
FIG. 7 is a schematic structural diagram of another embodiment of the close-packed and flat-laid ceramic microspheres of the present invention;
FIG. 8 is a schematic structural diagram of a light-emitting device according to the present invention;
FIG. 9 is a graph showing the reflectance of an embodiment of the diffuse reflection apparatus according to the present invention;
FIG. 10 is a graph showing the measurement of the luminous intensity of the light-emitting device according to the embodiment of the present invention.
The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
It should be understood that the detailed description and specific examples, while indicating the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
As shown in fig. 1 to 7, a diffuse reflection apparatus 100 according to the present invention includes a substrate 110 and a diffuse reflection layer 120 stacked on each other; the diffuse reflection layer 120 comprises ceramic microspheres 121, and diffuse reflection particles 122 and a binder (not shown in the figure) coated on the surfaces of the ceramic microspheres and/or filling the gaps between the ceramic microspheres; wherein the grain diameter of the ceramic microspheres is 0.1 mm-0.5 mm; the grain diameter of the diffuse reflection particles is 20 nm-200 nm.
The adhesive mainly functions as an adhesive and a sealing. And since the adhesive cannot be completely uniformly dispersed, a certain amount of glass phase is formed in the case where the adhesive is aggregated; the glass phase herein refers to a portion of amorphous solid, which exists between particles and serves as a binder; typically, it consists primarily of adhesive components. The glass phase is generally in a transparent state, and light can directly penetrate through the glass phase, so that the reflectivity of the reflecting layer is reduced. Therefore, in order to increase the reflectance of the reflective layer, it is necessary to shield the glass phase in the reflective layer as much as possible. According to the invention, micron-sized ceramic microspheres are introduced into the diffuse reflection layer, and other finer nanoscale diffuse reflection particles coat the surfaces of the ceramic microspheres and/or are filled into gaps of the alumina spheres; the network structure main body is formed by relatively compact ceramic microspheres, relatively uniform pores are formed among the ceramic microspheres, the pore size can be controlled to be relatively smaller, and the pore structure of the diffuse reflection layer can be refined, so that the shielding effect of diffuse reflection particles in the diffuse reflection layer on the surfaces of pores and glass phases can be effectively improved, and the reflectivity of the diffuse reflection device is further improved. Furthermore, in the prior art, the size and shape of the diffuse reflection particles are different, and when the diffuse reflection particles are mixed with a binder (silica gel, glass, or the like) to form a slurry, the slurry viscosity is easily increased, the diffuse reflection particles are difficult to form a close-packed structure, and voids with different sizes are easily generated among the particles when the particles are packed. The micron-sized ceramic microspheres can easily form a uniform network structure main body, relatively uniform pore structures are formed among the ceramic microspheres, and the nano-sized diffuse reflection particles are coated and/or filled among pores, so that a more dense stacking structure can be formed, and the shielding effect on a glass phase is improved; thereby increasing the reflectivity of the diffuse reflective layer.
Further, in some embodiments, the ceramic microspheres 121 are uniform in particle size. The term "uniform particle size" as used herein means that the ceramic microspheres are selected to have the same particle size within the particle size range, and the ceramic microspheres in the same embodiment have the same particle size. Specifically, for example, ceramic microspheres having a particle size of any one of 0.1mm, 0.2mm, 0.3mm, 0.4mm, and 0.5mm are used. It will be appreciated that relatively consistent particle size allows for easier process control during the manufacturing process; the consistency of the product is relatively good.
Further, in other embodiments, the ceramic microspheres 121 have non-uniform particle sizes. The term "particle size is not uniform" as used herein means that the ceramic microspheres are selected from different particle sizes within the particle size range, and the particle sizes of the ceramic microspheres in the same embodiment are not uniform. Specifically, ceramic microspheres with the particle diameters of 0.1mm, 0.2mm, 0.3mm, 0.4mm and 0.5mm are adopted in a certain proportion by weight respectively and then are mixed for use; the ceramic microspheres in the diffuse reflection layer contain 5 ceramic microspheres with different particle sizes within the particle size range of 0.1-0.5 mm. It can be understood that the ceramic microspheres with different particle sizes and smaller particle sizes can mutually fill the pores between the ceramic microspheres with larger particle sizes, so that the density of the main body of the network structure formed by the ceramic microspheres is higher, the pores between the ceramic microspheres are smaller and more uniform, and the diffuse reflection particles 122 can be conveniently and uniformly coated on the surfaces of the ceramic microspheres and/or filled between the pores of the ceramic microspheres; the reflectivity and thermal conductivity of the diffuse reflective layer can be further improved.
Preferably, the ceramic microspheres 121 are one or more of alumina, magnesia, or boron nitride. In some embodiments, the ceramic microspheres are alumina. It is understood that alumina has higher thermal conductivity and thermal stability than other ceramic materials, and is a desirable material for the main body of the network skeleton structure. Of course, other ceramic materials or high temperature resistant glass materials can also implement the present invention, and those skilled in the art can select them according to the actual needs, and will not be described herein again.
Preferably, the diffuse reflective particles 122 are at least one of barium sulfate, aluminum oxide, magnesium oxide, titanium oxide, or zirconium oxide. It will be appreciated that the diffusely reflecting particles are mainly white particles, enabling scattering or reflection of light.
Preferably, the adhesive is one of glass, water glass, silica gel or resin. In some embodiments, to improve the thermal stability and thermal conductivity of the reflective layer, inorganic materials such as glass or water glass are preferred. The glass has higher thermal stability and thermal conductivity, and the chemical property and the physical property of the glass are very stable, so that the glass can be conveniently matched with other materials in a mutual cooperation manner; for example, when the glass is contacted with the fluorescent powder, the luminous performance of the fluorescent powder is not influenced, and excellent bonding and packaging effects can be provided.
Preferably, the substrate 110 is a metal substrate or a ceramic substrate. Specifically, the metal substrate may be aluminum-basedPure metal substrates such as plates and copper substrates; the substrate may be an alloy metal substrate such as an aluminum alloy, a copper alloy, and a nickel alloy. The ceramic substrate may be Al2O3AlN, SiC, SiN, sapphire, or the like. It can be understood that the substrate mainly plays a role in bearing and radiating, on one hand, the substrate can play a role in bearing in the preparation process, so that the substrate is required to have certain thermal stability and higher melting point, and is not damaged or melted in the preparation process and under the high-temperature condition in the use process; on the other hand, in order to achieve a good heat dissipation effect, the substrate should also have a high thermal conductivity. Further, the thickness of the substrate can be selected according to actual needs. Specifically, the thickness of the substrate is 0.5mm to 200 mm.
It is further noted that, in general, the reflection efficiency of a diffuse reflection device cannot be one hundred percent, and thus the lost light will be concentrated in the form of heat in the diffuse reflection layer; meanwhile, when the diffuse reflection device is matched with a fluorescent material as a light emitting device, the fluorescent layer can generate a large amount of heat in the light emitting process; the heat accumulated on the diffuse reflection layer may damage the structure of the diffuse reflection layer and reduce the reflectivity of the diffuse reflection layer, and the extremely high temperature may affect the light emitting efficiency of the fluorescent layer, and may cause the thermal quenching phenomenon of the fluorescent layer when the temperature exceeds a certain value, so that the whole light emitting device may fail. "Thermal quenching" refers to the phenomenon that the luminous efficiency of a fluorescent material or a wavelength conversion material decreases greatly with increasing temperature.
Preferably, the mass ratio of the diffuse reflection particles, the ceramic microspheres and the adhesive is (0.6-10) to (0.3-8): (1-5). It can be understood that the adhesive with the proper proportion can meet the wetting and dispersing requirements of the powder material, and the diffuse reflection particles and the ceramic microspheres are bonded and encapsulated, and meanwhile, a large amount of glass phase is not formed, so that the reflectivity of the diffuse reflection device is reduced.
Preferably, the ceramic microspheres 121 are in a single-layer tiled arrangement in the diffusive reflective layer 120. It should be noted that the term "single-layer tiled arrangement" as used herein means that the ceramic microspheres have only one layer of ceramic microspheres in the thickness direction of the diffuse reflection layer, and are tiled and spread along the planar direction of the diffuse reflection layer. It is understood that in some embodiments, the ceramic microspheres may be laid down on the same plane; as shown in fig. 1, a single layer of ceramic microspheres 121 is laid down parallel to a plane of the diffusive reflective layer 120. In other embodiments, a certain misalignment of the monolayer ceramic microspheres in the thickness direction is allowed, i.e. the ceramic microspheres may lie in at least 2 planes; as shown in fig. 2, a portion of the ceramic microspheres 121a lie in a plane parallel to one of the diffusely reflective layers 120 and another portion of the ceramic microspheres 121b lie in a plane parallel to the other of the diffusely reflective layers 120. And, further preferably, the distance between any two different planes is less than or equal to the diameter of the ceramic microspheres. It will be appreciated that this has the advantage of enabling a single-layer tiled arrangement.
It can be understood that the ceramic microspheres 121 may have a particle size in the micron level range, specifically, 100um to 500 um; therefore, the single layer arrangement can achieve a good heat dissipation effect. As shown in fig. 3, in the actual use process, the diffuse reflection layer 120 generates a certain amount of heat, and since the particle size of the diffuse reflection particles 122 is small, the number of pores between the diffuse reflection particles 122 is large, and the thermal conductivity is low; however, in the present invention, since the ceramic microspheres 121 are directly made of micron-sized ceramic materials, the ceramic microspheres 121 have extremely high compactness and good thermal conductivity, and therefore, when the diffuse reflection particles 122 are coated on the surfaces of the ceramic microspheres 121 and/or filled in the gaps between the ceramic microspheres 121, the heat of the diffuse reflection particles 122 can be rapidly conducted to the ceramic microspheres 121, and the ceramic microspheres 121 conduct the heat to the substrate through direct thermal contact with the substrate, thereby achieving rapid heat dissipation of the heat dissipation layer. In fact, since the ceramic microspheres are much larger than the size of the diffuse reflection particles, the volume of a single ceramic microsphere is more than ten million times of the volume of a single diffuse reflection particle, and thus the ceramic microspheres play a role of heat sink. By heat sink is meant herein that its temperature does not vary with the amount of heat energy transferred to it. Therefore, the micron-sized ceramic microspheres enable the thermal stability of the diffuse reflection layer to be higher, prevent the diffuse reflection layer from being damaged at high temperature, and improve the reflectivity of the reflection layer at higher temperature.
Of course, in some other embodiments, the distance between the two different planes may be greater than the diameter of the ceramic microspheres. The ceramic microspheres in these embodiments may be considered to be in a multilayer arrangement. Particularly, in the case of using a plurality of ceramic microspheres having different particle sizes, the ceramic microspheres having a smaller particle size are filled in the pores formed between the ceramic microspheres having a larger particle size to some extent. In fact, these embodiments form a multi-layered arrangement of ceramic microspheres.
In some embodiments, the ceramic microspheres in the diffuse reflective layer may also be arranged in a different tiling pattern to achieve a better network structure. For convenience of description, the lying plane of the diffuse reflection layer or the substrate is set to a reference direction "X" axis direction and a "Y" axis direction, which are perpendicular to each other and parallel to the lying plane of the diffuse reflection layer or the substrate. In some embodiments, the ceramic microspheres 121 are loosely laid in a single layer in the diffusive reflective layer 120. By "loosely laid" is meant that any ceramic microsphere does not contact any other ceramic microsphere. In one embodiment, as shown in FIG. 4, the ceramic microspheres 121 are not in contact with any other ceramic microspheres. Meanwhile, the ceramic microspheres 121 are uniformly and uniformly arranged in the "X" axis and the "Y" axis, that is, the distances between the ceramic microspheres in the "X" axis and the "Y" axis are equal. It can be appreciated that this has the advantage of better consistency and better positioning of the ceramic microspheres through the fixed template during the manufacturing process. Of course, in other embodiments, the arrangement may be random at any distance.
Preferably, the ceramic microspheres 121 are laid flat in a single layer close-packed in the diffusive reflective layer 120. It should be noted that "closely spaced" herein means that the ceramic microspheres are in contact with at least one other ceramic microsphere. In particular embodiments, as shown in FIG. 5, ceramic microspheres 121 contact one another in both the "X" and "Y" directions; and the positions of the contact are all positioned on the straight line of the X axis and the Y axis or the parallel straight line. In still other embodiments, as shown in FIG. 6, any three ceramic microspheres closest to each other are in contact with each other. In still other embodiments, as shown in FIG. 7, any one of the ceramic microspheres is not in contact with other ceramic microspheres in the X-axis direction and is in contact with at least one ceramic microsphere closest thereto in the Y-axis direction.
It should be noted that the above-mentioned "contact" is not necessarily zero in an absolute sense; and in practical process, the absolute zero of the space distance is difficult to realize. Thus, it will be understood by those skilled in the art that "in contact" as used herein shall mean that the distance between the ceramic microspheres is sufficiently small in spatial distance that it can be considered to be in contact. On one hand, the uniform pores formed among the ceramic microspheres and the relatively smaller pore diameter can be realized, and the pore structure of the diffuse reflection layer can be refined, so that the shielding effect of diffuse reflection particles in the diffuse reflection layer on the surfaces of pores and a glass phase can be effectively improved, and the reflectivity of the diffuse reflection device is further improved; on the other hand, the distance is small enough, so that better thermal contact can be realized, namely, the thermal resistance between the ceramic microspheres is small, the heat in the plane direction can be quickly transferred, and the damage and the failure of the diffuse reflection device caused by overhigh local temperature in the use process can be avoided. The diffuse reflection device can radiate heat more uniformly and efficiently, and the thermal stability and the reflectivity under the high-temperature condition are improved. Meanwhile, the network body framework may also be understood to include at least one network structure in at least a thickness direction or in a plane direction of the diffuse reflection means; it will be appreciated that the more compact the body structure, i.e. there can be "thermal contact" both in the thickness direction and in the planar direction, and the better the "thermal contact", the higher the thermal stability of the diffuse reflective means.
Preferably, the thickness of the diffuse reflection layer is 0.1mm to 0.5 mm. It is understood that the thickness of the diffuse reflective layer is almost equal to the particle size of the ceramic microspheres.
The second aspect of the invention also provides a light-emitting device. As shown in fig. 8, the light emitting device includes any one of the diffuse reflection devices described above, and further includes a fluorescent layer 230 disposed on the diffuse reflection layer 220, wherein the fluorescent layer 230 can emit excited light under excitation of the excitation light.
Specifically, the light emitting device 200 includes a substrate 210, a diffuse reflection layer 220 and a fluorescent layer 230, which are sequentially stacked, wherein the diffuse reflection layer 220 includes ceramic microspheres 221, and diffuse reflection particles 222 and a binder coated on the surfaces of the ceramic microspheres 221 and/or filling gaps between the ceramic microspheres 221;
wherein the grain diameter of the ceramic microspheres 221 is 0.1 mm-0.5 mm; the particle size of the diffuse reflection particles 222 is 20nm to 200 nm.
Preferably, the fluorescent layer may be at least one of a fluorescent material single crystal, a fluorescent ceramic, a fluorescent glass, and a silica gel or resin-encapsulated fluorescent layer. Further preferably, the fluorescent layer is a fluorescent ceramic or a fluorescent glass. In particular, common fluorescent ceramics are generally classified into two types: one is a pure phase luminescent ceramic (i.e., a single phase luminescent ceramic), such as a YAG: Ce or LuAG: Ce ceramic, which has a ceramic phase in which the luminescent phase is the same phase as the luminescent phase and which can be sintered to a ceramic with high transparency, but the YAG: Ce or LuAG: Ce ceramic has low thermal conductivity. The other is a complex phase luminescent ceramic, such as Al2O3&YAG Ce ceramic or AlN&YAG Ce ceramics, etc. with Al as binder phase2O3Or AlN, etc. and the luminescent phase is YAG Ce fluorescent powder. Specifically, the fluorescent glass, that is, glass is used as an adhesive phase to encapsulate and adhere fluorescent powder serving as a luminescent phase. It is understood that any one of the existing luminescent materials can be arbitrarily selected as the fluorescent layer by those skilled in the art according to actual needs, and details are not described here.
The third aspect of the present invention also provides a method for manufacturing a diffuse reflection apparatus, comprising the steps of:
A. mixing and dispersing raw materials;
B. b, printing by adopting a silk screen or a steel screen mesh plate, and coating the slurry obtained in the step A on a substrate;
C. sintering or curing to obtain the diffuse reflection device.
Specifically, step a includes: selecting raw material diffuse reflection particles, ceramic microspheres and adhesive according to the mass ratio, and mixing and dispersing.
Wherein the grain diameter of the ceramic microspheres is 0.1 mm-0.5 mm; the particle size of the diffuse reflection particles is 20 nm-200 nm.
Preferably, the mass ratio of the diffuse reflection particles, the ceramic microspheres and the adhesive is (0.6-10) to (0.3-8): (1-5).
Preferably, the diffuse reflective particles are at least one of barium sulfate, aluminum oxide, magnesium oxide, titanium oxide, or zirconium oxide.
Preferably, the ceramic microspheres are at least one of alumina, magnesia, or boron nitride.
Preferably, the adhesive is one of glass, water glass, silica gel or resin. Preferably, the glass is one or more of silicate glass, lead silicate glass, aluminoborosilicate glass, aluminate glass, soda lime glass, quartz glass. The glasses have different softening points. Particularly preferably, the glass is silicate glass with a low expansion coefficient.
Preferably, the particle size of the raw material glass powder is selected to be 1-5 um, preferably less than or equal to 1 um. The refractive index of the glass frit can be selected from a variety of refractive indices of existing commercial glass frits. Since there has been no commercial glass frit of 1um or less for a while, in some embodiments, the particle size of the raw glass frit is 1 um.
Preferably, the substrate is a metal substrate or a ceramic substrate.
Specifically, step B includes: and B, printing by adopting a silk screen or a steel screen, and coating the slurry obtained in the step A on the substrate. Wherein the thickness of the coating layer is 0.1-0.6 mm.
Specifically, step C includes: sintering or curing to obtain the diffuse reflection device. Wherein, when water glass, silica gel or resin and the like are used as the adhesive, a curing process is adopted. Preferably, the curing process is light curing or temperature curing. It will be appreciated that one skilled in the art can select an appropriate curing temperature or light curing time depending on the particular type of water glass, silicone or resin. Preferably, the curing temperature is 80-200 ℃.
When glass is used as the binder, a sintering process is used. Preferably, the glass may be one or more of silicate glass, lead silicate glass, aluminoborosilicate glass, aluminate glass, soda lime glass, quartz glass. The glasses have different softening points and the person skilled in the art can determine the sintering temperature with more practical choices of the type of glass. It should be noted, however, that when the reflecting means is used in conjunction with a phosphor layer, the sintering temperature should be below the breakdown temperature of the phosphor. Specifically, the sintering temperature is 400-1000 ℃.
The present invention will be described with reference to specific examples.
Example one
Step A: TiO with the particle size of 20 nm-200 nm2The powder, the alumina ceramic microspheres with the diameter of 0.1mm and the silica gel are mixed according to the mass ratio of 1: 0.8: 1, proportioning. Wherein the alumina ceramic ball with the diameter of 0.1mm has the purity of 99.99 percent and the diameter is optimized to be 0.1 mm. The silica gel is 3000-5000 cp in viscosity and 150 ℃ in curing condition. The refractive index of the silica gel is preferably 1.41 for low refractive index silica gel. After the three materials are primarily dispersed by stirring, the three materials are dispersed by revolution and rotation dispersing equipment.
And B: and coating the slurry on a substrate by adopting a screen printing mode, wherein the thickness of the coating layer is 0.1-0.12 mm. Wherein the substrate is made of Al2O3Substrate (alumina ceramic substrate).
And C: the diffuse reflection device is prepared by adopting the curing temperature of 150 ℃ and the baking time of 120 min.
The diffuse reflection device manufactured by the first embodiment comprises an aluminum oxide ceramic substrate and a diffuse reflection layer which are stacked; wherein the diffuse reflection layer comprises alumina ceramic microspheres and TiO coated on the surfaces of the alumina ceramic microspheres and/or filled in gaps among the alumina ceramic microspheres2Diffuse reflective particles and silica gel binder; meanwhile, the grain diameter of the alumina ceramic microspheres is 0.1 mm; TiO22The grain diameter of the diffuse reflection particles is 20 nm-200 nm. TiO22The mass ratio of the alumina ceramic microspheres to the silica gel is about 1: 0.8: 1.
example two
Similar to the first embodiment, the second embodiment is different from the first embodiment in that the diffuse reflection particles further include particles of 20nm to 200nmAl2O3And (3) powder. And TiO2 powder, Al2O3The mass ratio of the powder, the alumina ceramic balls and the silica gel is 3:2:1: 3. The rest of the process parameters and the process flow are the same as the first embodiment.
In the diffuse reflection apparatus according to example two, the diffuse reflection particles include TiO particles having a particle size of 20nm to 200nm2And Al2O3(ii) a And TiO2 powder, Al2O3The mass ratio of the powder, the alumina ceramic balls and the silica gel is 3:2:1: 3.
Experiments show that the diffuse reflection device prepared in the second embodiment has basically equivalent light reflection characteristics to the diffuse reflection device prepared in the first embodiment.
EXAMPLE III
Step A: TiO with the particle size of 20 nm-200 nm2Powder, 20 nm-200 nm Al2O3The powder, the alumina ceramic ball with the diameter of 0.1mm and the glass powder are mixed according to the mass ratio of 3:2:1: 4. The four materials are mixed with an organic carrier and stirred for primary dispersion, and then dispersed by revolution and rotation dispersion (or ball milling) dispersion equipment.
Wherein the purity of the alumina ceramic ball with the diameter of 0.1mm is 99.99%. The glass powder can be one or more of silicate glass, lead silicate glass, aluminoborosilicate glass, aluminate glass, soda-lime glass and quartz glass with different softening points. In this embodiment, silicate glass having a low expansion coefficient is preferable. The grain size of the glass powder is selected to be 1-5 um, preferably less than or equal to 1 um. The particle size of the glass frit in this example was selected to be 1 um. The refractive index of the glass frit can be selected from a variety of refractive indices of existing commercial glass frits.
The organic carrier is used for mixing and dispersing the raw material powder. In this embodiment, the organic carrier specifically includes an organic carrier formed by mixing and dissolving ethyl cellulose, terpineol, butyl carbitol, and butyl carbitol ester. In other embodiments, the organic vehicle may also consist of other types of cellulose and alcohols; the person skilled in the art can choose arbitrarily according to the actual requirements.
And B: adopting a screen printing mode to print the product obtained in the step AThe slurry is coated on a substrate, and the thickness of the coated layer is 0.1-0.12 mm. Wherein the substrate is Al2O3A substrate.
And C: pre-drying the substrate coated with the slurry in the step B at the drying temperature of 60-200 ℃ for 2-60 min, and then sintering in a muffle furnace at the temperature of 800-1000 ℃ for 1 h; and finally, manufacturing the diffuse reflection device. In other embodiments, the sintering time may be 2min to 1 h.
The diffuse reflection device manufactured in the third embodiment comprises an alumina ceramic substrate and a diffuse reflection layer which are stacked; wherein the diffuse reflection layer comprises alumina ceramic microspheres and TiO coated on the surfaces of the alumina ceramic microspheres and/or filled in gaps among the alumina ceramic microspheres2And Al2O3Diffuse reflective particles and a glass binder phase; meanwhile, the grain diameter of the alumina ceramic microspheres is 0.1 mm; TiO22And Al2O3The grain diameter of the diffuse reflection particles is 20 nm-200 nm. TiO22、Al2O3The mass ratio of the alumina ceramic microspheres to the glass is about 3:2:1: 4.
Example four
Similar to example three, example four differs from example one in that the ceramic microspheres used were boron nitride ceramic microspheres. The grain diameter of the boron nitride ceramic microspheres is also 0.1 mm.
In the diffuse reflection apparatus according to example IV, the diffuse reflection particles include TiO particles having a particle size of 20nm to 200nm2And Al2O3(ii) a And TiO2 powder, Al2O3The mass ratio of the powder, the boron nitride ceramic balls and the silica gel is 3:2:1: 4.
EXAMPLE five
This example further prepares a phosphor layer on the diffuse reflection layer prepared in the first example.
The prepared fluorescent ceramic sheet was used as a fluorescent layer, and the fluorescent ceramic was directly attached to the diffuse reflection layer of the diffuse reflection device prepared in one of the examples. Since the diffuse reflection layer of the first embodiment is encapsulated by the silicone gel, the present embodiment also uses the silicone gel as the adhesive between the fluorescent layer and the diffuse reflection layer.
A light emitting device according to the fifth embodiment includes an alumina ceramic substrate, a diffuse reflection layer, and a fluorescent layer stacked one on another; wherein the diffuse reflection layer comprises alumina ceramic microspheres and TiO coated on the surfaces of the alumina ceramic microspheres and/or filled in gaps among the alumina ceramic microspheres2Diffuse reflective particles and silica gel binder; meanwhile, the grain diameter of the alumina ceramic microspheres is 0.1 mm; TiO22The grain diameter of the diffuse reflection particles is 20 nm-200 nm. TiO22The mass ratio of the alumina ceramic microspheres to the silica gel is about 1: 0.8: 1.
EXAMPLE six
In this example, a phosphor layer was further prepared on the diffuse reflection layer prepared in example three.
The prepared fluorescent ceramic sheet is used as a fluorescent layer. The fluorescent ceramic was directly attached on the diffuse reflection layer of the diffuse reflection device prepared in example three. And high temperature resistant glue is used for bonding the fluorescent layer and the diffuse reflection layer.
A light emitting device according to a sixth embodiment includes an alumina ceramic substrate, a diffuse reflection layer, and a fluorescent layer stacked one on another; wherein the diffuse reflection layer comprises alumina ceramic microspheres and TiO coated on the surfaces of the alumina ceramic microspheres and/or filled in gaps among the alumina ceramic microspheres2And Al2O3Diffuse reflective particles and a glass binder phase; meanwhile, the grain diameter of the alumina ceramic microspheres is 0.1 mm; TiO22And Al2O3The grain diameter of the diffuse reflection particles is 20 nm-200 nm. TiO22、Al2O3The mass ratio of the alumina ceramic microspheres to the glass is about 3:2:1: 4.
EXAMPLE seven
This example further prepares a phosphor layer on the diffuse reflection layer prepared in example four.
Similarly to the sixth embodiment, the already-prepared fluorescent ceramic sheet was also used as the fluorescent layer. The fluorescent ceramic was directly attached on the diffuse reflection layer of the diffuse reflection device prepared in the four examples. And high temperature resistant glue is used for bonding the fluorescent layer and the diffuse reflection layer.
The light-emitting device obtained in example seven is different from that obtained in example six in that the ceramic microspheres are boron nitride ceramic microspheres.
Comparative example 1
TiO with the particle size of 20 nm-200 nm2The mass ratio of the powder to the silica gel is 1.8: 1.
The silica gel is baked for 120min at the temperature of 150 ℃ under the curing condition of 3000-5000 cp, and the refractive index of the silica gel is 1.41. After the two materials are primarily dispersed by stirring, the two materials are dispersed by revolution and rotation dispersing equipment. The substrate is coated by adopting a silk screen or a steel screen printing mode, and the thickness of the coating layer is 0.1-0.12 mm. Wherein the substrate is an Al2O3 ceramic substrate.
Comparative example I diffuse reflection clothes made only contain 20 nm-200 nm TiO2Diffusely reflecting the particles.
Comparative example No. two
This comparative example further prepared a fluorescent layer on the diffuse reflection layer prepared in comparative example one. The prepared fluorescent ceramic sheet was used as a fluorescent layer, and the fluorescent ceramic was directly attached onto the diffuse reflection layer of the diffuse reflection device prepared in the comparative example. Since the diffuse reflection layer of the comparative example was encapsulated with the silicone gel, the present example also employed the silicone gel as the adhesive between the fluorescent layer and the diffuse reflection layer.
The diffuse reflection layers prepared in the above examples one, three and four and the comparative example one were measured for their reflectivity using a spectrophotometer, and the results are shown in fig. 9. As can be seen from fig. 9, the reflectivity of the diffuse reflection device added with the ceramic microspheres is higher than that of the diffuse reflection device without the ceramic microspheres in the comparative example, which is beneficial for the diffuse reflection layer added with the ceramic spheres to be thicker, the internal pores to be smaller, and the like to achieve better shielding effect of the diffuse reflection particles.
The results of measuring the light emission intensity of the fluorescent layer under different excitation light powers in the above examples five to seven and comparative example two are shown in fig. 10. As can be seen from fig. 10, the diffuse reflection layer after adding the ceramic microspheres is beneficial to improving the light emitting efficiency of the fluorescent layer. The reflectivity of the diffuse reflection device added with the ceramic microspheres is improved, so that the utilization rate of the fluorescent layer to exciting light is improved, and the absorption loss of the fluorescent excited by the fluorescent layer is reduced. Meanwhile, the results in fig. 10 also show that the luminescent intensity of the fluorescent layer is continuously increased along with the increase of power, and the fluorescent layer has a better linear relationship, which indicates that the diffuse reflection layer added with the ceramic microspheres does not have a reduced heat conduction performance due to the increase of thickness, mainly because the heat conductivity coefficients of the added ceramic spheres are higher, and the ceramic microspheres form a network structure in the diffuse reflection layer, so that heat generated when the fluorescent layer is excited can be well transferred to the substrate, and the ceramic microspheres not only have a good reflection effect but also have excellent heat conduction performance in the diffuse reflection layer.
The above-mentioned serial numbers of the embodiments of the present invention are merely for description and do not represent the merits of the embodiments. The above description is only a part of the embodiments of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the contents of the present specification and the drawings, or applied to other related technical fields directly or indirectly, are included in the scope of the present invention.
Claims (10)
1. A diffuse reflection device is characterized by comprising a substrate and a diffuse reflection layer which are superposed, wherein the diffuse reflection layer comprises ceramic microspheres, diffuse reflection particles and adhesives, and the diffuse reflection particles and the adhesives are coated on the surfaces of the ceramic microspheres and/or are filled in gaps among the ceramic microspheres;
wherein the grain diameter of the ceramic microspheres is 0.1 mm-0.5 mm; the particle size of the diffuse reflection particles is 20 nm-200 nm.
2. The diffuse reflective device of claim 1, wherein said ceramic microspheres are at least one of alumina, magnesia, or boron nitride.
3. The diffuse reflective device of claim 1, wherein said diffuse reflective particles are at least one of barium sulfate, aluminum oxide, magnesium oxide, titanium oxide, or zirconium oxide.
4. The diffuse reflective device of claim 1, wherein said adhesive is one of glass, water glass, silica gel, or resin; or, the substrate is a metal substrate or a ceramic substrate.
5. The diffuse reflection device according to claim 1, wherein the mass ratio of the diffuse reflection particles, the ceramic microspheres and the binder is (0.6-10): (0.3-8): (1-5).
6. The diffuse reflective device of claim 1, wherein said ceramic microspheres are in a single-layer tiled arrangement in said diffuse reflective layer.
7. The diffuse reflective device of claim 6, wherein said ceramic microspheres are laid in a single layer close-packed arrangement in said diffuse reflective layer.
8. The diffuse reflecting device of claim 1, wherein said diffuse reflecting layer has a thickness of 0.1mm to 0.5 mm.
9. A light emitting device comprising the diffuse reflection device according to any one of claims 1 to 8, further comprising a fluorescent layer provided on the diffuse reflection layer, wherein the fluorescent layer is capable of emitting excited light under excitation of the excited light.
10. A method of making a diffuse reflective device, comprising the steps of:
A. mixing and dispersing raw materials to obtain slurry, wherein the raw materials comprise diffuse reflection particles, ceramic microspheres and an adhesive, and the particle size of the ceramic microspheres is 0.1-0.5 mm; the particle size of the diffuse reflection particles is 20 nm-200 nm;
B. b, printing by adopting a silk screen or a steel screen, and coating the slurry obtained in the step A on a substrate;
C. sintering or curing to obtain the diffuse reflection device.
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| CN201811099651.5A CN110927844B (en) | 2018-09-20 | 2018-09-20 | Diffuse reflection device, preparation method thereof and wavelength conversion device |
| PCT/CN2019/100481 WO2020057297A1 (en) | 2018-09-20 | 2019-08-14 | Diffuse reflection device and preparation method thereof, and wavelength conversion device |
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