CN115180947A - Preparation method of high-lumen-efficiency ceramic for laser illumination - Google Patents
Preparation method of high-lumen-efficiency ceramic for laser illumination Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000005286 illumination Methods 0.000 title claims abstract description 9
- 238000004321 preservation Methods 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 239000002002 slurry Substances 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 10
- 238000005498 polishing Methods 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000003825 pressing Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 9
- 238000000498 ball milling Methods 0.000 claims description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052721 tungsten Inorganic materials 0.000 claims description 4
- 239000010937 tungsten Substances 0.000 claims description 4
- 238000009694 cold isostatic pressing Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 4
- 239000013078 crystal Substances 0.000 abstract description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 abstract 2
- 229910001928 zirconium oxide Inorganic materials 0.000 abstract 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 description 4
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 4
- 238000000137 annealing Methods 0.000 description 3
- 229910019064 Mg-Si Inorganic materials 0.000 description 2
- 229910019406 Mg—Si Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910017970 MgO-SiO2 Inorganic materials 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/50—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
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Abstract
A preparation method of high lumen efficiency ceramic for laser illumination comprises the following steps: s1: respectively adding raw materials and ZrO in a grinding mechanism 2 Grinding the balls and alcohol to obtain slurry; zrO (zirconium oxide) 2 The mass ratio of the ball to the raw material is 3:2, wherein the raw material is Y 2.99 Mg x Al 5‑2x Si x O 12 :Ce 0.01 X is more than or equal to 2 and more than or equal to 0; s2: drying the slurry, and grinding the dried slurry again to obtain powder; s3: pressing the powder to obtain a prototype ceramic wafer; s4: placing the prototype ceramic wafer in vacuum equipment for heat preservation for a period of time, and performing rapid cooling after the heat preservation is finished; s5: taking out the prototype ceramic wafer after heat preservation, thinning and polishing; s6: after polishing, placing the prototype ceramic wafer in a muffle furnace for heat preservation for a set time, and preserving heatAnd cooling along with the furnace after the preparation is finished, and finishing the preparation. The invention achieves the effect of fog-like light uniformization under the condition of not influencing the quantum efficiency of YAG main crystal lattice, and greatly improves the lumen efficiency of the fluorescent ceramic.
Description
Technical Field
The invention relates to the field of illumination, in particular to a preparation method of high-lumen-efficiency ceramic for laser illumination.
Background
Laser lighting is a favorable competitor for next generation lighting by virtue of its advantages of small volume, high efficiency, long service life, environmental protection, etc. The main light conversion materials for white laser illumination include PiG (Phosphor in Glass), piS (Phosphor in silicon), and TPC (transmissive Phosphor ceramic). Among them, transparent fluorescent ceramics are widely spotlighted because of their high efficiency and high thermal stability. At present, white light laser illumination is realized mainly by exciting YAG (yttrium aluminum garnet) Ce or LuAG Ce transparent ceramics by a blue laser, and because high-quality transparent ceramics have high transmittance, the absorptivity of a ceramic phosphor for laser is too low when the laser passes through the transparent ceramics, so that the situation of low lumen efficiency is often shown.
Disclosure of Invention
The invention aims to solve the problem that when YAG-Ce ceramic is excited, a large amount of blue light is transmitted and cannot be absorbed, so that the quantum efficiency is low.
A preparation method of high lumen efficiency ceramic for laser lighting is provided, and the specific technical scheme is as follows:
a preparation method of high lumen efficiency ceramic for laser lighting is characterized by comprising the following steps:
the method comprises the following steps:
s1: respectively adding raw materials, zrO2 balls and alcohol into a grinding mechanism, and grinding to obtain slurry;
the mass ratio of the ZrO2 balls to the raw material is 3:2, wherein the raw material is Y 2.99 Mg x Al 5-2x Si x O 12 :Ce 0.01 Of (2) is stoichiometricRatio, x is more than or equal to 2 and more than or equal to 0;
s2: drying the slurry, and grinding the dried slurry again to obtain powder;
s3: pressing the powder to obtain a prototype ceramic wafer;
s4: placing the prototype ceramic wafer in vacuum equipment for heat preservation for a period of time, and performing rapid cooling after the heat preservation is finished;
s5: taking out the prototype ceramic wafer after heat preservation, thinning and polishing;
s6: and after polishing, placing the prototype ceramic wafer in a muffle furnace for heat preservation for a set time, and cooling along with the furnace after heat preservation is finished to finish preparation.
To better implement the invention, the method can further comprise the following steps:
in S1, the raw materials, zrO2 balls and alcohol seal are placed in a planetary ball mill, the rotating speed is 180rpm, and the ball milling time is 12 hours.
Further:
in S3, the diameter of the prototype ceramic chip is 15mm, the mass of the single chip is 0.8mg, and after the prototype ceramic chip is pressed, the prototype ceramic chip is subjected to cold isostatic pressing for 3min under the pressure of 200 MPa.
Further:
in S4, the vacuum equipment is a vacuum tungsten filament furnace, and the vacuum pressure is lower than 3 x 10 -5 And (3) keeping the temperature of the Pa and 1600-1800 ℃ for 8h, and quickly cooling at the cooling speed of 50 ℃/min after the temperature is kept.
Further:
in S6, the temperature was maintained in a muffle furnace at 1400 ℃ for 4h.
The invention has the beneficial effects that:
according to the invention, mgO-SiO2 nano powder is added as a fluxing agent, high-quality fluorescent transparent ceramic is obtained at 1800 ℃, and then low-temperature annealing is carried out, so that Mg-Si is precipitated at a crystal boundary, and thus, under the condition of not influencing YAG host lattice quantum efficiency, a mist light homogenizing effect is achieved, and the lumen efficiency of the fluorescent ceramic is greatly improved.
The addition of MgO-SiO2 serving as a fluxing agent ensures the sintering quality (YAG) of the transparent ceramic, and then low-temperature annealing is carried out to cause the precipitation of Mg-Si with a low melting point, so that the effect of light uniformization is achieved, and the lumen efficiency is improved to 230lm/W from 150lm/W before annealing.
Drawings
FIG. 1 is a flow chart of the operation of the present invention;
FIG. 2 is a diagram illustrating the effect of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in fig. 1 and 2:
a preparation method of high lumen efficiency ceramic for laser illumination comprises the following steps,
s1: according to Y 2.99 Mg x Al 5-2x Si x O 12 :Ce 0.01 Accurately weighing raw materials in a stoichiometric ratio of more than or equal to 2 and more than or equal to 0, placing the raw materials in a 250ml nylon ball milling tank, adding ZrO2 balls according to the ball-material mass ratio of 3:2, adding alcohol to submerge the balls, sealing, placing in a planetary ball mill, rotating at 180rpm, and carrying out ball milling for 12 hours to obtain slurry after ball milling is completed;
s2: placing the slurry ball-milled by the planetary ball mill in an air blower for drying, and grinding to obtain powder for later use;
s3: pressing the powder into a prototype ceramic sheet body with the diameter of 15mm and the mass of a single sheet of 0.8mg by a tablet press;
s4: carrying out cold isostatic pressing on the prototype ceramic sheet body for 3min under the pressure of 200 MPa;
s5: placing the prototype ceramic sheet body in a vacuum tungsten filament furnace, wherein the vacuum pressure is lower than 3 x 10 -5 Pa, heat preservation at 1600-1800 ℃ for 8h, and rapidly cooling at a cooling speed of 50 ℃/min after finishing heat preservation;
s6: taking out the prototype ceramic sheet after the temperature reduction in the vacuum tungsten filament furnace, and thinning and polishing;
s7: and after polishing, placing the ceramic wafer in a muffle furnace, keeping the temperature at 1400 ℃ for 4h in an air atmosphere, and cooling along with the furnace after the temperature is kept. The preparation is finished.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (5)
1. A preparation method of high lumen efficiency ceramic for laser illumination is characterized in that:
the method comprises the following steps:
s1: respectively adding raw materials and ZrO in a grinding mechanism 2 Grinding the balls and alcohol to obtain slurry;
ZrO 2 the mass ratio of the ball to the raw material is 3:2, wherein the raw material is Y 2.99 Mg x Al 5-2x Si x O 12 :Ce 0.01 X is more than or equal to 2 and more than or equal to 0;
s2: drying the slurry, and grinding the dried slurry again to obtain powder;
s3: pressing the powder to obtain a prototype ceramic wafer;
s4: placing the prototype ceramic wafer in vacuum equipment for heat preservation for a period of time, and performing rapid cooling after the heat preservation is finished;
s5: taking out the prototype ceramic wafer after heat preservation, thinning and polishing;
s6: and after polishing, placing the prototype ceramic wafer in a muffle furnace for heat preservation for a set time, and cooling along with the furnace after heat preservation is finished to finish preparation.
2. The method according to claim 1, wherein the method comprises the steps of:
in S1, raw material, zrO 2 The ball and the alcohol seal are placed in a planetary ball mill, the rotating speed is 180rpm, and the ball milling time is 12h.
3. The method according to claim 2, wherein the ceramic is prepared by a method comprising the following steps:
in S3, the diameter of the prototype ceramic chip is 15mm, the mass of the single chip is 0.8mg, and after the prototype ceramic chip is pressed, the prototype ceramic chip is subjected to cold isostatic pressing for 3min under the pressure of 200 MPa.
4. The method according to claim 3, wherein the ceramic has a high luminous efficiency, and comprises:
in S4, the vacuum equipment is a vacuum tungsten filament furnace, and the vacuum pressure is lower than 3 x 10 -5 And (3) keeping the temperature of the Pa and 1600-1800 ℃ for 8h, and quickly cooling at the cooling speed of 50 ℃/min after the temperature is kept.
5. The method of claim 4, wherein the ceramic comprises:
in S6, the temperature was maintained in a muffle furnace at 1400 ℃ for 4h.
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| CN202210662282.6A CN115180947A (en) | 2022-06-13 | 2022-06-13 | Preparation method of high-lumen-efficiency ceramic for laser illumination |
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| CN202210662282.6A CN115180947A (en) | 2022-06-13 | 2022-06-13 | Preparation method of high-lumen-efficiency ceramic for laser illumination |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108947516A (en) * | 2018-08-29 | 2018-12-07 | 江苏师范大学 | A kind of (Cu, Ce): YAG transparent fluorescent ceramic and the preparation method and application thereof |
| CN111018512A (en) * | 2019-12-30 | 2020-04-17 | 江苏师范大学 | Preparation method of high-luminous-efficiency and high-color-rendering-index fluorescent ceramic with gradient refractive index structure |
| CN112174646A (en) * | 2020-09-28 | 2021-01-05 | 东北大学 | High-thermal-conductivity fluorescent ceramic for laser illumination and preparation method thereof |
| CN113480311A (en) * | 2021-06-29 | 2021-10-08 | 南通大学 | Preparation method of Ce: YAG fluorescent ceramic emitting warm white light |
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- 2022-06-13 CN CN202210662282.6A patent/CN115180947A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108947516A (en) * | 2018-08-29 | 2018-12-07 | 江苏师范大学 | A kind of (Cu, Ce): YAG transparent fluorescent ceramic and the preparation method and application thereof |
| CN111018512A (en) * | 2019-12-30 | 2020-04-17 | 江苏师范大学 | Preparation method of high-luminous-efficiency and high-color-rendering-index fluorescent ceramic with gradient refractive index structure |
| CN112174646A (en) * | 2020-09-28 | 2021-01-05 | 东北大学 | High-thermal-conductivity fluorescent ceramic for laser illumination and preparation method thereof |
| CN113480311A (en) * | 2021-06-29 | 2021-10-08 | 南通大学 | Preparation method of Ce: YAG fluorescent ceramic emitting warm white light |
Non-Patent Citations (2)
| Title |
|---|
| YOUNG HYUN SONG ET AL.: "Design of laser-driven high-efficiency Al2O3/YAG:Ce3+ ceramicconverter for automotive lighting: Fabrication, luminous emittance,and tunable color space" * |
| 雷婷等: "荧光粉Y3Mg2AlSi2O12:Ce3+的合成及光谱性能研究" * |
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Application publication date: 20221014 |