CN109896851B - Ceramic composite with concentration gradient, preparation method and light source device - Google Patents
Ceramic composite with concentration gradient, preparation method and light source device Download PDFInfo
- Publication number
- CN109896851B CN109896851B CN201711288476.XA CN201711288476A CN109896851B CN 109896851 B CN109896851 B CN 109896851B CN 201711288476 A CN201711288476 A CN 201711288476A CN 109896851 B CN109896851 B CN 109896851B
- Authority
- CN
- China
- Prior art keywords
- oxide
- phase
- sintering
- light
- layer body
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Landscapes
- Luminescent Compositions (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses a ceramic composite with a concentration gradient, a preparation method and a light source device. The ceramic composite body has at least an upper layer body, a middle layer body and a lower layer body; the upper layer body consists of an oxide light-emitting phase, an oxide high thermal conductivity phase and an oxide luminescent phase; the intermediate layer body consists of an oxide light-emitting phase, an oxide high thermal conductivity phase and an oxide luminescent phase; the lower layer body consists of an oxide high thermal conductivity phase and an oxide luminescent phase, or consists of an oxide light-emitting phase, an oxide high thermal conductivity phase and an oxide luminescent phase. The invention has the beneficial effects that: the high-temperature fluorescence intensity is improved, and the uniformity of emergent fluorescence can be adjusted and controlled.
Description
Technical Field
The invention relates to the field of laser illumination light sources, in particular to a ceramic composite body with concentration gradient, a preparation method and a light source device.
Background
The laser diode has the characteristics of high photoelectric efficiency, high brightness, high collimation, long irradiation distance, small size and the like. Compared with a halogen lamp and a xenon lamp, the laser illumination light source has the advantages of long service life, high energy efficiency and lower carbon. Compared with an LED light source, the laser lighting light source has the advantages of high brightness, longer irradiation distance, flexible modeling design, high design freedom degree and simpler heat dissipation system. Compared with the LED light source product which is only suitable for the field of middle and low brightness, the laser light source can be suitable for all brightness requirements, and has incomparable advantages particularly in the fields of high brightness, high luminous efficiency, strong directivity and the like.
In view of the limitations of the luminous efficiency and the working temperature of red, green and blue lasers, the mainstream white light laser illuminating light source in the market at present uses the light distribution principle of a white light LED for reference, that is, a blue light laser with the wavelength of about 450nm is used as an exciting light source, and yttrium aluminum garnet, oxynitride fluorescent powder, fluorescent ceramic or single crystal are the preferred fluorescent materials for laser illumination. Among them, fluorescent ceramics are favored by the lighting industry because of their excellent optical properties, high concentration doping of RE, and good heat dissipation of the packaging method.
The intensity of blue light power which is suffered by the fluorescent material when the fluorescent material is operated relative to the white light LED light source is mostly 1W/mm 2 Below, maximum does not exceed5W/mm 2 Whereas the optical power density of a single laser diode (e.g., nichia-4.5W bare spot size of about 1.5 mm. About.0.5 mm) is about 1.5W/mm 2 In practical application, multiple lasers are usually adopted to converge on the surface of the fluorescent material, that is, the power density of the blue light irradiation required to be borne by the fluorescent material for laser illumination is ten times or even more than one hundred times that of the white light LED illumination. Therefore, the fluorescent material for laser illumination needs to have super-strong blue light irradiation resistance, excellent temperature quenching characteristic and excellent thermal shock resistance. At present, the effect of the fluorescent materials on the market is not ideal.
Disclosure of Invention
The invention aims to provide a ceramic composite with excellent high-temperature fluorescence characteristics and concentration gradient.
The invention further solves the technical problem of adding a light scattering design concept to reduce the burden of subsequent secondary formula light mixing and provide a ceramic composite body with concentration gradient.
In order to achieve the purpose, the technical scheme of the invention is as follows: a ceramic composite having a concentration gradient, the ceramic composite having at least an upper layer body, an intermediate layer body, and a lower layer body;
the upper layer body consists of an oxide light-emitting phase, an oxide high thermal conductivity phase and an oxide luminescent phase;
the intermediate layer body consists of an oxide light-emitting phase, an oxide high thermal conductivity phase and an oxide luminescent phase;
the lower layer body consists of an oxide high thermal conductivity phase and an oxide luminescent phase, or consists of an oxide scattered light phase, an oxide high thermal conductivity phase and an oxide luminescent phase;
the volume fractions of the oxide light-scattering phase of the upper layer body and the oxide light-scattering phase of the middle layer body are gradually increased;
the volume fractions of the oxide high thermal conductivity phase of the upper layer, the oxide high thermal conductivity phase of the middle layer and the oxide high thermal conductivity phase of the lower layer are gradually increased;
the volume fractions of the oxide light-emitting phase of the upper layer body, the oxide light-emitting phase of the middle layer body and the oxide light-emitting phase of the lower layer body are gradually reduced.
As a preferable embodiment of the ceramic composite body having the concentration gradient, Y is used as the oxide light scattering phase 2 O 3 、La 2 O 3 Lanthanide series rare earth oxide, teO 2 、ZrO 2 、TiO 2 、ZnO、Nb 2 O 5 、Ta 2 O 5 、HfO 2 Further, the grain size of the oxide dispersed phase is less than 1000nm, and further, the grain size of the oxide dispersed phase is 50-800 nm.
As a preferable scheme of the ceramic composite body with concentration gradient, al is selected as the high-thermal-conductivity phase of the oxide 2 O 3 、Bi 2 O 3 、Cr 2 O 3 、MnO 2 、Sb 2 O 3 、Co 2 O 3 、TiO 2 、Ag 2 And O, further, the grain size of the oxide high thermal conductivity phase is less than 2000nm, and further, the grain size of the oxide high thermal conductivity phase is 50-500 nm.
As a preferable embodiment of the ceramic composite having a concentration gradient, the oxide luminescent phase has a garnet structure and is expressed by the general formula (Y) 1-x-y RE y Ce x ) 3 (Al 1-z M z ) 5 O 12 Wherein RE is one or more of Lu, tb, gd, la, pr, eu and Sm, M is one or more of Ga, cr, si, sr, mn, sc, ti and V, and x is more than or equal to 0.0001 and less than or equal to 0.05,0 and less than or equal to y is more than or equal to 0.5,0.0001 and less than or equal to z is less than or equal to 0.5.
In a preferable embodiment of the ceramic composite having a concentration gradient, the upper layer has a Ce doping content of 0.05 to 5.0at% in the oxide luminescent phase, and further has a Ce doping content of 0.3 to 2.0at% in the oxide luminescent phase; in the intermediate layer body, the Ce doping content in the oxide luminescent phase is 0.01-3.0 at%, and further the Ce doping content in the oxide luminescent phase is 0.1-1.0 at%.
In a preferred embodiment of the ceramic composite having a concentration gradient, the volume fraction of the oxide dispersed phase in the upper layer is 5 to 20%, the volume fraction of the oxide high thermal conductivity phase is 5 to 20%, and the volume fraction of the oxide luminescent phase is 70 to 90%, which add up to 100%; in the intermediate layer body, the volume fraction of the oxide light-emitting phase is 10-30%, the volume fraction of the oxide high thermal conductivity phase is 20-70%, and the volume fraction of the oxide light-emitting phase is 20-70%, wherein the sum of the three is 100%; in the lower layer body, the volume fraction of the oxide light-emitting phase is 0-10%, the volume fraction of the oxide high-thermal-conductivity phase is 70-99.99%, and the volume fraction of the oxide light-emitting phase is 0.01-20%, wherein the sum of the three is 100%.
The invention also provides a preparation method of the ceramic composite body with the concentration gradient, which is used for the ceramic composite body and comprises the following steps,
step S1, forming the lower layer body, the middle layer body and the upper layer body layer by layer to form a ceramic blank body;
s2, sintering the ceramic blank: sintering by adopting a vacuum sintering furnace, two-step sintering by adopting a vacuum sintering furnace and a hot isostatic pressing furnace or normal-pressure atmosphere sintering; further, in the sintering process of the vacuum sintering furnace and the normal pressure atmosphere sintering process, a weak reducing atmosphere is added, wherein the weak reducing atmosphere is H 2 -N 2 Or H 2 -Ar wherein H 2 The content of (A) is less than or equal to 4 percent;
step S3, annealing the ceramic blank: annealing at 1300-1600 deg.c in air or weak reducing atmosphere for 1-50 hr; furthermore, the annealing temperature is 1400-1500 ℃, and the annealing heat preservation time is 10-40 h; and the number of the first and second groups,
and S4, grinding and thinning the ceramic blank to obtain the ceramic composite.
As a preferable embodiment of the method for producing a ceramic composite body having a concentration gradient, in step S2,
sintering in a vacuum sintering furnace: the sintering heat preservation temperature is 1680-1820 ℃, and the sintering heat preservation time is 1-30 h; further, the sintering heat preservation temperature is 1720-1780 ℃, and the sintering heat preservation time is 5-15 h;
two-step sintering in vacuum sintering furnace and hot isostatic pressing furnaceAnd (3) knot: the first step is sintering in a vacuum sintering furnace with the vacuum degree of 10 -2 ～10 -4 Pa, the sintering heat preservation temperature is 1700-1800 ℃, the sintering heat preservation time is 1-10 h, further, the sintering heat preservation temperature is 1720-1760 ℃, and the sintering heat preservation time is 3-6 h; secondly, putting the ceramic block obtained in the first step into a hot isostatic pressing furnace for sintering, wherein the pressure is 150-200 MPa, the sintering heat preservation temperature is 1600-1700 ℃, the sintering heat preservation time is 1-10 h, further, the sintering heat preservation temperature is 1620-1680 ℃, and the sintering heat preservation time is 3-6 h;
sintering in normal pressure atmosphere: the sintering heat preservation temperature is 1650-1800 ℃, and the sintering heat preservation time is 1-20 h; furthermore, the sintering heat preservation temperature is 1750-1780 ℃, and the sintering heat preservation time is 3-6 h.
As a preferable embodiment of the method for producing a ceramic composite body having a concentration gradient, step S1 comprises,
step S11, weighing the raw materials corresponding to each layer: the starting material can be oxide or luminescent phase (Y, ce) 3 Al 5 O 12 Fluorescent powder and other oxides, and also can be raw material powder synthesized by using a coprecipitation technology;
step S12, weighing the sintering aid corresponding to each layer: li + ，Ca 2+ /Mg 2+ /Ba 2+ ， La 3+ /Y 3+ ，TEOS/SiO 2 The metal ions may be salts in the form of oxides, carbonates, fluorides, etc.;
step S13, preparing raw materials, sintering aids and dispersion media required by each layer body into slurry by using absolute ethyl alcohol respectively, and adding Al 2 O 3 Ball-milling for 5-20 h in a ball-milling tank, wherein the mass ratio of the raw materials, the milling balls and the dispersion medium is 1;
s14, performing casting molding, drying and laminating on the ball-milled slurry, and then performing tabletting and cold isostatic pressing; or, drying and sieving the ball-milled slurry, then sequentially putting the dried slurry into a die to dry and press layer by layer, and then applying cold isostatic pressing of 100-250 Mpa to form a biscuit; and the number of the first and second groups,
and S15, pre-sintering the biscuit in a muffle furnace at the temperature of 600-800 ℃, and preserving heat for 2-4 hours to obtain the ceramic body.
The invention also provides a light source device, comprising,
a blue light excitation light source; and the number of the first and second groups,
according to the ceramic composite, the top surface of the ceramic composite is plated with a blue light antireflection film, the bottom surface of the ceramic composite is plated with silver, and the bottom surface of the ceramic composite is welded on a copper heat dissipation base;
the blue light excitation light source irradiates the top surface of the ceramic composite body after being collimated and focused to be converted into yellow light, and the residual blue light and the emitted yellow light are mixed to obtain uniform white light.
Compared with the prior art, the invention has the beneficial effects that: since the fluorescent phase in the ceramic composite is uniformly distributed and contains scattering particles, uniform yellow fluorescence can be obtained. The ceramic composite contains a high thermal conductivity phase, and therefore has excellent heat resistance. In addition, since it is a bulk, it is not necessary to add a resin to the structure of the white light emitting device, and the fluorescence intensity and the white light mixing effect can be controlled according to the luminescent phase content, the Ce doping content, and the ceramic thickness. Therefore, a white light-emitting device comprising the composite ceramic body emits light uniformly and is very suitable for high output.
In addition to the technical problems addressed by the present invention, the technical features constituting the technical solutions, and the advantageous effects brought by the technical features of the technical solutions described above, other technical problems solved by the present invention, other technical features included in the technical solutions, and advantageous effects brought by the technical features will be described in further detail with reference to the accompanying drawings.
Drawings
FIG. 1 is a schematic structural view of a ceramic composite body according to the present invention.
FIG. 2 is a graph showing the high-temperature fluorescence characteristics of the present invention.
Fig. 3 is a schematic structural view (transmission type) of a laser-illuminated light-emitting device according to the present invention.
Fig. 4 is a schematic structural view of a laser-illuminated light-emitting device (reflective type) according to the present invention.
Detailed Description
The present invention will be described in further detail below with reference to specific embodiments and drawings. Here, the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Comparative example 1:
using high purity yttrium oxide (Y) 2 O 3 ) Alumina (Al) 2 O 3 ) Cerium oxide (CeO) 2 ) As raw materials, magnesium oxide (MgO) and Tetraethoxysilane (TEOS) are used as sintering aids. The addition amount of magnesium oxide (MgO) is 0.1 percent by mass, and the addition amount of Tetraethoxysilane (TEOS) is 0.6 percent by mass. According to (Y) 0.995 Ce 0.005 ) 3 Al 5 O 12 Preparing powder raw materials according to a stoichiometric ratio, taking absolute ethyl alcohol as a ball milling medium, putting the ball milling medium into an alumina ball milling tank, carrying out wet ball milling to prepare ceramic powder, and drying, sieving and tabletting the powder; then the ceramic blank is applied with 200MPa cold isostatic pressing to form a blank, the ceramic blank is pre-sintered after being preserved for 4 hours at 700 ℃, and then is put into a vacuum sintering furnace at 1750 ℃ and the vacuum degree of 10 -3 Sintering for 8 hours under the condition of Pa, and finally annealing for 20 hours at 1450 ℃ in a muffle furnace to obtain (Y) 0.995 Ce 0.005 ) 3 Al 5 O 12 And the obtained ceramic material is subjected to cutting, grinding and polishing processing to obtain the complex-phase fluorescent ceramic with the diameter of 12mm and the thickness of 0.5mm for white light illumination.
Example 1:
the upper layer (i.e., the light-emitting surface) contains (Y) 0.995 Ce 0.005 ) 3 Al 5 O 12 Volume fraction 80%, Y 2 O 3 Volume fraction 10%, al 2 O 3 The volume fraction was 10%, the diameter was 12mm, and the thickness was 1mm. The intermediate layer contains (Y) 0.99 Ce 0.01 ) 3 Al 5 O 12 Volume fraction 50%, Y 2 O 3 15% by volume, al 2 O 3 Volume fraction35%, diameter 12mm, thickness 0.3mm. The lower layer contains (Y) 0.99 Ce 0.01 ) 3 Al 5 O 12 10% by volume, al 2 O 3 Volume fraction of 90%, diameter of 12mm and thickness of 1mm. Respectively weighing raw material oxides and sintering aids (same as comparative example 1) required by corresponding layered structures according to the concentration gradient, respectively using absolute ethyl alcohol as a medium, carrying out ball milling and mixing, drying and sieving the slurry, sequentially putting each layer of raw materials into a mould, carrying out dry pressing layer by layer, then carrying out cold isostatic pressing at 200Mpa to prepare a biscuit, preparing a ceramic blank according to the ceramic sintering process in comparative example 1, and respectively grinding and thinning the two sides of the ceramic blank to obtain the complex phase fluorescent ceramic with the diameter of 12mm and the thickness of 0.5mm.
Example 2:
the upper layer (i.e., the light-emitting surface) contains (Y) 0.995 Ce 0.005 ) 3 Al 5 O 12 Volume fraction 80%, Y 2 O 3 10% by volume, al 2 O 3 The volume fraction is 10%, the diameter is 12mm, and the thickness is 0.5mm. The intermediate layer contains (Y) 0.99 Ce 0.01 ) 3 Al 5 O 12 Volume fraction 50%, Y 2 O 3 15% by volume, al 2 O 3 The volume fraction is 35%, the diameter is 12mm, and the thickness is 0.1mm. The lower layer contains (Y) 0.99 Ce 0.01 ) 3 Al 5 O 12 10% by volume, al 2 O 3 Volume fraction of 90%, diameter of 12mm and thickness of 0.5mm. And (2) respectively weighing raw material oxides and sintering aids (same as comparative example 1) required by corresponding layered structures according to the concentration gradient, ball-milling and mixing additives such as a connecting agent, a plasticizer, a dispersing agent, absolute ethyl alcohol and the like to prepare slurry, sequentially injecting the slurry into a casting machine for casting molding after vacuum defoaming, and drying, laminating, dry-pressing and cold isostatic pressing the casting sheet to prepare a biscuit. The ceramic body is pre-sintered after heat preservation for 4h at 800 ℃, and then is put into a vacuum sintering furnace at 1800 ℃ and the vacuum degree of 10 -3 Sintering for 2 hours under the Pa condition, cooling to 1720 ℃, preserving heat for 10 hours, and then annealing for 20 hours at 1450 ℃ in a muffle furnace. Finally, the two sides of the ceramic body are respectively ground and thinned to the same thicknessThe complex phase fluorescent ceramic with the diameter of 12mm and the thickness of 0.5mm is obtained.
Example 3:
the upper layer (i.e., the light-emitting surface) contains (Y) 0.99 Ce 0.01 ) 3 Al 5 O 12 Volume fraction 85%, la 2 O 3 10% by volume, al 2 O 3 Volume fraction of 5%, diameter of 12mm and thickness of 0.6mm. The middle layer contains (Y) 0.99 Ce 0.01 ) 3 Al 5 O 12 Volume fraction 40%, la 2 O 3 20% by volume, al 2 O 3 The volume fraction is 40%, the diameter is 12mm, and the thickness is 0.1mm. The lower layer contains (Y) 0.99 Ce 0.01 ) 3 Al 5 O 12 Volume fraction of 5%, al 2 O 3 Volume fraction 95%, diameter 12mm, thickness 0.4mm. And (2) respectively weighing raw material oxides and sintering aids (same as comparative example 1) required by corresponding layered structures according to the concentration gradient, ball-milling and mixing additives such as a connecting agent, a plasticizer, a dispersing agent, absolute ethyl alcohol and the like to prepare slurry, sequentially injecting the slurry into a casting machine for casting molding after vacuum defoaming, and drying, laminating, dry-pressing and cold isostatic pressing the casting sheet to prepare a biscuit. The ceramic blank is pre-sintered at 800 ℃ for 4h and then is put into a vacuum sintering furnace at 1750 ℃ and the vacuum degree of 10 -3 Sintering for 5 hours under the Pa condition, then placing the ceramic blank into a hot isostatic pressing furnace, sintering for 5 hours under the conditions of 1650 ℃ and 200MPa, and then placing the obtained ceramic blank into a muffle furnace, and annealing for 20 hours at 1450 ℃. And finally, grinding the two surfaces of the ceramic blank respectively to reduce the thickness to the same thickness to obtain the complex phase fluorescent ceramic with the diameter of 12mm and the thickness of 0.5mm.
As can be seen from fig. 2, examples 1, 2 and 3 are superior to the comparative example, and the high-temperature fluorescence characteristics are significantly improved. Also, example 3 is significantly superior to examples 1 and 2.
Referring to fig. 3 to 4, the light source device containing the ceramic composite can realize white light illumination through a transmission type or reflection type light path. The method comprises the steps of utilizing a single or multiple lasers 1 as excitation light sources, collimating, bunching and homogenizing the light by a lens 2 and then irradiating the light to an upper layer body of a ceramic composite body 4, converting the wavelength 6 of the excitation light sources into yellow light or orange light by the ceramic composite body, and mixing the residual blue light with the emitted light of a ceramic plate to obtain uniform white light 7 with high brightness. The bottom surface of the lower layer body is plated with silver and welded in the copper heat dissipation base 5. The ceramic composite has excellent thermal shock resistance and light homogenizing capability, and is particularly suitable for high-power laser illumination.
The foregoing merely represents embodiments of the present invention, which are described in some detail and detail, and are not to be construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (5)
1. A ceramic composite having a concentration gradient, wherein the ceramic composite has at least an upper layer body, an intermediate layer body, and a lower layer body;
the upper layer body consists of an oxide light-emitting phase, an oxide high thermal conductivity phase and an oxide luminescent phase;
the intermediate layer body consists of an oxide light-emitting phase, an oxide high thermal conductivity phase and an oxide luminescent phase;
the lower layer body consists of an oxide high thermal conductivity phase and an oxide luminescent phase, or consists of an oxide light-emitting phase, an oxide high thermal conductivity phase and an oxide luminescent phase;
the volume fractions of the oxide light-scattering phase of the upper layer body and the oxide light-scattering phase of the middle layer body are gradually increased;
the volume fractions of the oxide high thermal conductivity phase of the upper layer, the oxide high thermal conductivity phase of the intermediate layer, and the oxide high thermal conductivity phase of the lower layer are gradually increased;
the volume fractions of the oxide light-emitting phase of the upper layer body, the oxide light-emitting phase of the middle layer body and the oxide light-emitting phase of the lower layer body are gradually reduced;
in the upper layer body, the volume fraction of the oxide light-emitting phase is 5-20%, the volume fraction of the oxide high thermal conductivity phase is 5-20%, and the volume fraction of the oxide light-emitting phase is 70-90%; in the intermediate layer body, the volume fraction of the oxide light-emitting phase is 10-30%, the volume fraction of the oxide high thermal conductivity phase is 20-70%, and the volume fraction of the oxide light-emitting phase is 20-70%; in the lower layer body, the volume fraction of the oxide light-emitting phase is 0-10%, the volume fraction of the oxide high thermal conductivity phase is 70-99.99%, and the volume fraction of the oxide light-emitting phase is 0.01-20%;
the oxide light scattering phase adopts Y 2 O 3 、La 2 O 3 、TeO 2 、ZrO 2 、TiO 2 、ZnO、Nb 2 O 5 、Ta 2 O 5 、HfO 2 One or more of;
the high thermal conductivity phase of the oxide is Al 2 O 3 、Bi 2 O 3 、Cr 2 O 3 、MnO 2 、Sb 2 O 3 、Co 2 O 3 、TiO 2 、Ag 2 One or more of O;
the oxide light-emitting phase is of a garnet structure and has a general formula expressed as (Y) 1-x-y RE y Ce x ) 3 (Al 1-z M z ) 5 O 12 Wherein RE is one or more of Lu, tb, gd, la, pr, eu and Sm, M is one or more of Ga, cr, si, sr, mn, sc, ti and V, x is more than or equal to 0.0001 and less than or equal to 0.05,0 and less than or equal to 0.5,0.0001 and less than or equal to z and less than or equal to 0.5;
in the upper layer body, the doping content of Ce in the oxide luminescent phase is 0.05-5.0 at%; in the intermediate layer body, the Ce doping content in the oxide luminescent phase is 0.01-3.0 at%.
2. A method of making a ceramic composite body having a concentration gradient, the method comprising the steps of,
step S1, forming the lower layer body, the middle layer body and the upper layer body layer by layer to form a ceramic blank body;
s2, sintering the ceramic blank: sintering in a vacuum sintering furnace, sintering in two steps in the vacuum sintering furnace and a hot isostatic pressing furnace, or sintering in normal pressure atmosphere;
step S3, annealing the ceramic blank: annealing at 1300-1600 deg.c in air or weak reducing atmosphere for 1-50 hr; and the number of the first and second groups,
and S4, grinding and thinning the ceramic blank to obtain the ceramic composite.
3. The method of claim 2, wherein in step S2,
sintering in a vacuum sintering furnace: the sintering heat preservation temperature is 1680-1820 ℃, and the sintering heat preservation time is 1-30 h;
two-step sintering in a vacuum sintering furnace and a hot isostatic pressing furnace: the first step is sintering in a vacuum sintering furnace with the vacuum degree of 10 -2 ～10 -4 Pa, the heat preservation temperature is 1700-1800 ℃, and the sintering heat preservation time is 1-10 h; secondly, putting the ceramic block obtained in the first step into a hot isostatic pressing furnace for sintering, wherein the pressure is 150-200 MPa, the heat preservation temperature is 1600-1700 ℃, and the sintering heat preservation time is 1-10 h;
sintering in normal pressure atmosphere: the sintering heat preservation temperature is 1650-1800 ℃ and the sintering heat preservation time is 1-20 h.
4. The method of claim 2, wherein the step S1 comprises,
s11, weighing the raw materials corresponding to each layer body;
s12, weighing the sintering aid corresponding to each layer body;
step S13, preparing the raw materials, sintering aid and dispersion medium required by each layer body into slurry by using absolute ethyl alcohol respectively, and adding Al 2 O 3 Ball-milling for 5-20 h in a ball-milling tank, wherein the mass ratio of the raw materials, the milling balls and the dispersion medium is 1;
s14, performing casting molding, drying and laminating on the ball-milled slurry, and then performing tabletting and cold isostatic pressing; or, drying and sieving the ball-milled slurry, then sequentially putting the slurry into a mould to dry-press layer by layer, and then applying cold isostatic pressing at 100-250 Mpa to prepare a biscuit; and the number of the first and second groups,
and S15, pre-sintering the biscuit in a muffle furnace at the temperature of 600-800 ℃, and preserving heat for 2-4 hours to obtain the ceramic body.
5. The light source device is characterized by comprising,
a blue light excitation light source; and the number of the first and second groups,
the ceramic composite body of claim 1, wherein the top surface of the ceramic composite body is plated with a blue light antireflection film, the bottom surface of the ceramic composite body is plated with silver, and the bottom surface of the ceramic composite body is welded to a copper heat dissipation base;
the blue light excitation light source irradiates the top surface of the ceramic composite body after being collimated and focused to be converted into yellow light, and the residual blue light is mixed with the emitted yellow light to obtain uniform white light.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711288476.XA CN109896851B (en) | 2017-12-07 | 2017-12-07 | Ceramic composite with concentration gradient, preparation method and light source device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711288476.XA CN109896851B (en) | 2017-12-07 | 2017-12-07 | Ceramic composite with concentration gradient, preparation method and light source device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109896851A CN109896851A (en) | 2019-06-18 |
| CN109896851B true CN109896851B (en) | 2023-02-10 |
Family
ID=66939569
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711288476.XA Active CN109896851B (en) | 2017-12-07 | 2017-12-07 | Ceramic composite with concentration gradient, preparation method and light source device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109896851B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112174647B (en) * | 2019-07-04 | 2023-06-09 | 上海航空电器有限公司 | Low-temperature cofiring fluorescent ceramic composite for white light illumination, preparation method and light source device |
| CN113024242A (en) * | 2019-12-09 | 2021-06-25 | 上海航空电器有限公司 | Superfine ceramic phosphor for obtaining high lumen laser illumination and preparation method thereof |
| CN110981481B (en) * | 2019-12-31 | 2022-02-01 | 江苏师范大学 | Preparation method of stepped complex-phase fluorescent ceramic for high-luminous-efficiency white light LED |
| WO2022199623A1 (en) * | 2021-03-24 | 2022-09-29 | 中国科学院福建物质结构研究所 | Enhanced single-matrix ceramic phosphor for white light led, preparation method therefor, and application thereof |
| CN115490508B (en) * | 2022-10-12 | 2023-11-03 | 中国科学院上海光学精密机械研究所 | Composite fluorescent ceramic for white light LD illumination and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008109120A (en) * | 2006-09-27 | 2008-05-08 | Kyocera Corp | Multilayer ceramic capacitor and its fabrication process |
| WO2011125422A1 (en) * | 2010-03-31 | 2011-10-13 | 宇部興産株式会社 | Ceramic composites for light conversion, process for production thereof, and light-emitting devices provided with same |
| CN102891432A (en) * | 2011-07-19 | 2013-01-23 | 中国科学院理化技术研究所 | Function-doping based transparent ceramic slab pumping device |
| CN104245881A (en) * | 2012-03-30 | 2014-12-24 | 宇部兴产株式会社 | Ceramic complex for light conversion and light-emitting device using same |
| WO2016173528A1 (en) * | 2015-04-30 | 2016-11-03 | 深圳市光峰光电技术有限公司 | Luminescent ceramic used for high-power light source, and light-emitting device |
| WO2017177923A1 (en) * | 2016-04-12 | 2017-10-19 | 深圳市绎立锐光科技开发有限公司 | Method for preparing fluorescent ceramic having aluminum oxide substrate, and related fluorescent ceramic |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100566490C (en) * | 2005-03-14 | 2009-12-02 | 皇家飞利浦电子股份有限公司 | Phosphor in the polycrystalline ceramic structure and the light-emitting component that comprises this phosphor |
| US20110104491A1 (en) * | 2009-10-30 | 2011-05-05 | The Government Of The United States Of America As Represented By The Secretary Of The Navy | Functionally Doped Polycrystalline Ceramic Laser Materials |
| CN103347982B (en) * | 2010-12-01 | 2016-05-25 | 日东电工株式会社 | There is emissivity ceramic material and manufacture method and the using method of doping content gradient |
| CN103253937B (en) * | 2013-05-30 | 2014-11-26 | 东北大学 | Yttrium oxide laser transparent ceramic material with incentive elements in continuous gradient distribution and preparation method thereof |
| CN104446428B (en) * | 2013-09-23 | 2017-02-15 | 中国科学院上海硅酸盐研究所 | Complex phase transparent ceramic for white-light LED devices and preparation method of complex phase transparent ceramic |
| CN104628375A (en) * | 2014-05-12 | 2015-05-20 | 长春理工大学 | Laminated forming method of rare-earth ion-doped yttrium aluminum garnet laser ceramics |
| CN107253854B (en) * | 2017-05-18 | 2020-10-02 | 北京科技大学 | Gradient doped laser transparent ceramic and preparation method thereof |
-
2017
- 2017-12-07 CN CN201711288476.XA patent/CN109896851B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008109120A (en) * | 2006-09-27 | 2008-05-08 | Kyocera Corp | Multilayer ceramic capacitor and its fabrication process |
| WO2011125422A1 (en) * | 2010-03-31 | 2011-10-13 | 宇部興産株式会社 | Ceramic composites for light conversion, process for production thereof, and light-emitting devices provided with same |
| CN102891432A (en) * | 2011-07-19 | 2013-01-23 | 中国科学院理化技术研究所 | Function-doping based transparent ceramic slab pumping device |
| CN104245881A (en) * | 2012-03-30 | 2014-12-24 | 宇部兴产株式会社 | Ceramic complex for light conversion and light-emitting device using same |
| WO2016173528A1 (en) * | 2015-04-30 | 2016-11-03 | 深圳市光峰光电技术有限公司 | Luminescent ceramic used for high-power light source, and light-emitting device |
| WO2017177923A1 (en) * | 2016-04-12 | 2017-10-19 | 深圳市绎立锐光科技开发有限公司 | Method for preparing fluorescent ceramic having aluminum oxide substrate, and related fluorescent ceramic |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109896851A (en) | 2019-06-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109896851B (en) | Ceramic composite with concentration gradient, preparation method and light source device | |
| JP6834491B2 (en) | Manufacturing method of sintered phosphor, light emitting device, lighting device, vehicle headlight, and sintered phosphor | |
| CN109467453B (en) | Fluorescent ceramic with characteristic microstructure and preparation method and application thereof | |
| JP5454473B2 (en) | Phosphor ceramics, method for producing the same, and light emitting device | |
| CN108863317B (en) | Fluorescent composite ceramic and preparation method and application thereof | |
| CN109896852B (en) | Complex phase fluorescent ceramic for blue light excited white light illumination, preparation method and light source device | |
| CN109642156B (en) | Sintered phosphor, light-emitting device, lighting device, and display lamp for vehicle | |
| KR20090089384A (en) | Illumination system comprising monolithic ceramic luminescence converter | |
| CN109896853B (en) | Ceramic composite with lower expansion coefficient, preparation method and light source device | |
| CN101697367A (en) | Method for preparing LED by using transparent ceramics | |
| CN108503352B (en) | Garnet-based red fluorescent ceramic material and preparation method thereof | |
| CN109437900A (en) | A kind of fluorescence ceramics block, preparation method and its application in laser lighting | |
| WO2018154869A1 (en) | Light wavelength conversion member and light emitting device | |
| JP6449963B2 (en) | Light wavelength conversion member and light emitting device | |
| WO2018028265A1 (en) | Wavelength conversion device and preparation method therefor, light-emitting device and projection device | |
| TW201527487A (en) | Wavelength-conversion member and light-emitting device | |
| CN109987932B (en) | Complex phase fluorescent ceramic for white light illumination, preparation method and light source device | |
| JP4916469B2 (en) | Phosphor | |
| CN108484168B (en) | Red transparent fluorescent ceramic and preparation method thereof | |
| Liu et al. | Spectrum regulation of YAG: Ce/YAG: Cr/YAG: Pr phosphor ceramics with barcode structure prepared by tape casting | |
| CN114031400B (en) | Single-phase warm white fluorescent ceramic and preparation method and application thereof | |
| WO2021248445A1 (en) | Transparent complex-phase fluorescent ceramic and preparation method therefor | |
| WO2021015261A1 (en) | Fluorescent member, method for producing same, and light-emitting device | |
| CN113024253B (en) | High-color-rendering edge-covering composite structure wavelength conversion ceramic for laser illumination and preparation method thereof | |
| TW201638297A (en) | Light emitting material composite ceramic and process for its production |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |