CN112028492B - YAG-Al2O3Nano laminated composite transparent ceramic and preparation method thereof - Google Patents

YAG-Al2O3Nano laminated composite transparent ceramic and preparation method thereof Download PDF

Info

Publication number
CN112028492B
CN112028492B CN202010922244.0A CN202010922244A CN112028492B CN 112028492 B CN112028492 B CN 112028492B CN 202010922244 A CN202010922244 A CN 202010922244A CN 112028492 B CN112028492 B CN 112028492B
Authority
CN
China
Prior art keywords
yag
nano
transparent ceramic
layered composite
composite transparent
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
Application number
CN202010922244.0A
Other languages
Chinese (zh)
Other versions
CN112028492A (en
Inventor
张乐
单迎双
陈东顺
邵岑
康健
李明
周天元
李延彬
陈浩
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jiangsu Normal University
Original Assignee
Jiangsu Normal University
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Jiangsu Normal University filed Critical Jiangsu Normal University
Priority to CN202010922244.0A priority Critical patent/CN112028492B/en
Publication of CN112028492A publication Critical patent/CN112028492A/en
Application granted granted Critical
Publication of CN112028492B publication Critical patent/CN112028492B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
    • C03B32/02—Thermal crystallisation, e.g. for crystallising glass bodies into glass-ceramic articles
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/12—Silica-free oxide glass compositions
    • C03C3/125—Silica-free oxide glass compositions containing aluminium as glass former

Abstract

The invention discloses a process for preparing M: YAG-Al2O3A nano-layered composite transparent ceramic and a preparation method thereof. The ceramic comprises fully crystallized M: YAG nanocrystalline and Al2O3Complex phase structure of thin layer; ball-milling and mixing raw materials of aluminum oxide, yttrium oxide and an oxide containing M, drying, calcining, pressing and forming, heating by adopting a high-power laser device to obtain a transparent glass material, grinding and polishing, and then carrying out annealing crystallization treatment to obtain the nano-layered composite transparent ceramic. The ceramic obtained by the invention is completely compact, the porosity is 0, no glass phase exists, and the density reaches 4.26-4.55 g/cm3The material has good mechanical strength, the hardness can reach 25-28 GPa, the Young modulus is 300-320 GPa, the transmittance of the material in a visible light waveband is 90-95% of the theoretical transmittance, the transmittance of the material in near infrared and intermediate infrared wavebands is 99.5-100% of the theoretical transmittance, the cutoff wavelength of the infrared waveband is 6.6-6.7 mu M, the material has lower phonon energy, high thermal conductivity and low radiationless transition probability, and M luminescent ions can realize higher photoluminescence efficiency and can be used in the fields of near infrared luminescence, biological imaging and the like.

Description

YAG-Al2O3Nano laminated composite transparent ceramic and preparation method thereof
Technical Field
The invention belongs to the field of advanced functional transparent ceramics, and particularly relates to M: YAG-Al2O3A nano-layered composite transparent ceramic and a preparation method thereof.
Background
Yttrium aluminum garnet Y3Al5O12The (YAG) transparent ceramic is gradually a substitute of YAG single crystal due to its advantages of low cost, high concentration doping of rare earth ions, easy realization of composite structure preparation, etc., and can be used as the main body material of solid laser, phosphor and scintillator. YAG transparent ceramics are prepared by various sintering methods, such as spark plasma sintering, vacuum sintering, hot isostatic pressing sintering and the like. To ensure the sintering process, high quality nanoscale feedstock powders (e.g., high purity, no agglomerates), high pressures, high sintering temperatures, and the like are essential. The above requirements are on the one hand to eliminate light scattering centers (residual pores and second phases) in the ceramic body; on the other hand, the hall-pascal effect of nanocrystalline transparent ceramics will also significantly enhance the mechanical properties of the transparent ceramics compared to micron-sized (grain-sized) transparent ceramics, since rayleigh light scattering is greatly attenuated. Therefore, nanocrystalline transparent ceramics tend to be large. However, the realization of nanocrystalline transparent ceramics using conventional sintering techniques remains a great challenge due to the rapid growth of the grains at high sintering temperatures. For example, document 1(R. Dy)3+-doped Y3Al5O12A transparent ceramic for high efficiency circulating single-phase white-emitting phosphor, J.Am.chem.Soc.102(2019)3510--3Using Al under Pa vacuum2O3(200nm) and Y2O3、Dy2O3The (80nm) ultrafine powder is sintered at 1780 ℃ for 8 hours to prepare Dy: YAG transparent ceramic, and the grain size of the Dy: YAG transparent ceramic still reaches tens of microns.
At present, complete crystallization from molten and solidified glass has been considered as an effective method for synthesizing a fully dense transparent ceramic. Allix teach the subject group (documents 2-4, Enhanced Transmission through Second Phase Crystallization in BaAl)4O7 Scintillating Ceramics,Cryst.Growth Des. 16(2016)386-395.；Transparency through structural disorder a new concept for innovative transparent ceramics,Chem.Mater.27(2015)508-514.；Local disorder and tunable luminescence in Sr1-x/2Al2-xSixO4(0.2≤x≤0.5)transparent ceramics, inorg. chem.56(2017)14446-14458.) a series of micron-sized fully-crystallized transparent ceramics, including aluminates, aluminosilicates, etc., were successfully prepared by a pressureless glass crystallization process. However, the process required for the complete crystallization of the large-sized glass into the synthesized nanocrystalline transparent ceramic is very demanding. For example, silicate garnets require ultra-high external pressure during their production, LaAlO being produced3/t-ZrO2The transmittance of the nano ceramic at 800nm is only 55%, which is far lower than the theoretical transmittance. Until now, the practically available nanocrystalline transparent YAG ceramics that meet optical and mechanical performance requirements have not been directly realized.
Disclosure of Invention
The invention aims to provide M: YAG-Al2O3The nano-layered composite transparent ceramic has a nano-layered structure and high optical quality.
Another object of the present invention is to provide the above M: YAG-Al2O3The preparation method of the nano-layered composite transparent ceramic can realize transparent ceramic nanocrystals.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: YAG-Al2O3The nano-layered composite transparent ceramic comprises completely crystallized M: YAG nano-crystals and Al wrapped outside the M: YAG nano-crystals2O3The matrix of the complex phase structure of the thin layer is composed of the components shown in the following formula:
(100-x)Al2O3-(x)Y2O3
wherein x is more than or equal to 30 and less than or equal to 35, the thickness of the layered structure is controlled by the amount of yttrium oxide, and M is doped rare earth ions or transition metal ions capable of emitting light in near infrared and intermediate infrared bands.
Preferably, the grain size of the M: YAG nanocrystalline is 25-32 nm, and the outer layer of the grain is wrapped with Al2O3A layer having a thickness of 2 to 5 nm.
Preferably, the doping ion M is selected from Cr3+、Nd3+、Yb3+And Tm3+One or more of the ions.
Preferably, the molar concentration of the doping ions M in the YAG Al is 0.01-1%, or the molar concentration of the doping ions M in the YAG Y is 0.01-1%.
The invention provides the YAG-Al2O3The preparation method of the nano-layered composite transparent ceramic comprises the following specific steps:
(1) preparing materials: al according to the formula (100-x)2O3-(x)Y2O3Respectively weighing raw materials of alumina, yttrium oxide and oxide containing M according to the stoichiometric ratio of Al and Y and the doping concentration of M;
(2) ball milling: performing wet ball milling on the raw materials in the step (1) to obtain uniformly mixed slurry;
(3) drying and calcining: drying the slurry uniformly mixed in the step (2), and calcining in a muffle furnace after drying;
(4) laser melting vitrification: pressing the powder calcined in the step (3) into a block or a sheet, heating the block or the sheet in a certain atmosphere or in a vacuum state by using a high-power laser device, wherein the heating rate is 200-300 ℃/min, the heating temperature is 2000-2050 ℃, the heating time is 20-30 s, then closing the laser, and cooling to the room temperature at the speed of 200 ℃/s of 100-;
(5) processing: taking out the transparent glass material obtained in the step (4), grinding and polishing the transparent glass material into a disc shape, wherein the density of the transparent glass material is about 3.5-3.8 g/cm3；
(6) Annealing and ceramization: annealing and crystallizing the disc glass material in the step (5), wherein the annealing temperature is 945-955 ℃, the heating rate is 25-40 ℃/min, the heat preservation time is 1-3 h, and the annealing atmosphere is selected according to the selected M ion target valence state; cooling to room temperature along with the furnace to obtain the nano-layered composite transparent ceramic.
Preferably, the wet ball milling in the step (2) comprises the following specific steps: putting raw material powder into a ball milling tank in sequence, wherein high-purity alumina balls are selected as the grinding balls, and the ball-material ratio is 2-5: and 1, simultaneously adding a ball milling medium, and carrying out planetary ball milling, wherein the ball milling rotating speed is 120-300 r/min, and the ball milling time is 12-18 hours.
More preferably, the ball milling medium is absolute ethyl alcohol; the total mass ratio of the absolute ethyl alcohol to the raw material powder is 1: 1 to 2.
Preferably, the calcining temperature in the step (3) is 700-900 ℃, and the time is 3-8 hours.
Preferably, the annealing atmosphere in step (6) is selected from one or more of nitrogen, argon, hydrogen, oxygen, and air.
The mixed oxide glass frit is heated, the crystallization temperature is higher than the pure YAG crystallization temperature (about 940 ℃), and M is that YAG is firstly nucleated from a glass system in a large amount, then alumina is precipitated again, and the surface of the nucleated YAG is wrapped in a layered mode. The thin alumina layer limits the fusion growth among YAG crystal grains, namely the system has self-limiting effect to stop the grain growth. M is YAG nano-scale grain coating Al2O3Coating with thin layer by controlling Al in matrix2O3And Y2O3The relative amounts of (a) and (b) are used to control the thickness of the layered structure.
Meanwhile, the composition formula has high crystallization activation energy and retardation, the heating rate does not influence the nucleation number, and the glass crystallization process complies with the volume nucleation principle of three-dimensional crystal growth, namely the crystallization mechanism is the volume nucleation growth of the three-dimensional crystal growth. The glass phase is changed into ceramic, and the ceramic can be completely compact, the porosity is 0, and no glass phase exists.
Furthermore, since M is YAG-Al2O3The nano-layered composite transparent ceramic has small crystal grains, so the nano-layered composite transparent ceramic has high mechanical strength and weak light scattering effect. However, since YAG and Al2O3The difference of the refractive indexes between the two phases causes the transmittance of the nano ceramic in a visible light wave band to be poor. However, in the near infrared region and the intermediate infrared region, since the wavelength is far greater than the crystal grain size, the transmittance is almost the same, and can reach a theoretical value.
Compared with the prior art, the invention has the following beneficial effects:
(1) the nano-layered composite transparent ceramic prepared by the invention comprises fully crystallized YAG nano-crystals and Al2O3The thin-layer multiphase structure comprises YAG crystal grains of 25-32 nm in size, and Al wrapped on the outer layer of the crystal grains2O3A layer of a material selected from the group consisting of,the thickness is 2-5 nm. The ceramic is completely compact, the porosity is 0, no glass phase exists, and the density reaches 4.26-4.55 g/cm3The composite material has good mechanical strength, hardness of 25-28 GPa and Young modulus of 300-320 GPa.
(2) The nano-layered composite transparent ceramic prepared by the invention has better optical quality, because of the refractive index difference between the layers, the transmittance of the nano-layered composite transparent ceramic in a visible light wave band (400-800 nm) is 90-95% of the theoretical transmittance, the transmittance in a near infrared and middle infrared wave band (1-4 mu m) is 99.5-100% of the theoretical transmittance, and Cr is doped in the nano-layered composite transparent ceramic3+After the rare earth ions are used for near infrared luminescence and biological application, the method can be applied to the fields of near infrared luminescence, biological imaging and the like.
(3) The nano-layered composite transparent ceramic prepared by the invention has higher light-light conversion efficiency, the cutoff wavelength of the nano-layered composite transparent ceramic in an infrared band is 6.6-6.7 mu m, the nano-layered composite transparent ceramic is farther than 6.1 mu m of a single crystal and ceramic (non-composite structure), the nano-layered composite transparent ceramic has lower phonon energy, high thermal conductivity and low probability of radiationless transition, and higher photoluminescence efficiency can be obtained.
(4) The preparation method of the nano-layered composite transparent ceramic provided by the invention has high level of process modernization and function integration, is convenient for controlling process parameters and processes, provides basis and guidance for converting glassy materials into compact polycrystalline materials, and is simple and easy to implement and good in popularization.
Drawings
Fig. 1 is an XRD chart of the nano-layered composite transparent ceramic prepared in examples 1, 2 and 3 of the present invention.
FIG. 2 shows that the Cr prepared in example 1 is YAG-Al2O3A light transmission effect diagram of a nano-layered composite transparent ceramic sample.
Detailed Description
The invention is described in further detail below with reference to the figures and specific examples.
Unless otherwise stated, the raw materials and reagents used in the examples of the present invention are commercially available products, and the raw materials are high-purity powders.
Example 1
The preparation method comprises the following steps:
(1) preparing materials: according to Cr, YAG-Al2O3(Cr3+Accounting for 1 percent of the molar concentration of Al in YAG) and weighing the raw material Al according to the stoichiometric ratio of each element in YAG2O3、Y2O3And Cr2O3In which Al is2O3And Y2O3The molar ratio is 70:30, i.e. x is 30;
(2) ball milling: carrying out wet ball milling on the raw materials in the step (1), sequentially putting raw material powder into a ball milling tank, wherein the grinding balls are high-purity alumina balls, and the ball-to-material ratio is 2: simultaneously adding absolute ethyl alcohol, wherein the total mass ratio of the absolute ethyl alcohol to the raw material powder is 1: 1, performing planetary ball milling at the ball milling rotation speed of 120r/min for 18 hours to fully and uniformly mix the raw materials;
(3) drying and calcining: drying the slurry uniformly mixed in the step (2) in a drying oven, and calcining the dried powder in a muffle furnace at 700 ℃ for 8 hours;
(4) laser melting vitrification: pressing the calcined powder in the step (3) into blocks or sheets, heating the blocks or sheets by using a high-power laser device in a vacuum state, wherein the heating rate is 250 ℃/min, the heating temperature is 2050 ℃, the heating time is 25s, then closing the laser, and cooling to the room temperature at the speed of 150 ℃/s;
(5) processing: taking out the transparent glass material obtained in the step (4), grinding and polishing the transparent glass material into a disc shape, wherein the density of the transparent glass material is about 3.5g/cm3；
(6) Annealing and ceramization: annealing and crystallizing the disc glass material in the step (5), wherein the annealing temperature is 945 ℃, the heating rate is 25 ℃/min, and the heat preservation time is 1 h; at O2Annealing in atmosphere, and cooling to room temperature along with the furnace to obtain the nano-layered composite transparent ceramic.
After testing, the density was 4.26g/cm3(ii) a The diffraction peak obtained by the X-ray diffraction test is shown in figure 1, and by comparing with a standard card, only YAG crystal phase and no other crystal phase appear in the sample. Observed by a field emission scanning electron microscope (FSEM), the YAG grain size is about 25nmThe outer layer of the crystal grain is wrapped with Al2O3A layer having a thickness of 5 nm; the hardness can reach 25GPa and the Young modulus can reach 300GPa when the test is carried out by adopting an indenter; and (3) carrying out tests of a spectrophotometer UV-VIS-NIR and an infrared spectrometer, wherein the transmittance of the sample in a visible light 500nm waveband is 92% of the theoretical transmittance, the transmittance of the sample in a near infrared and mid infrared 4-micron waveband is 99.5% of the theoretical transmittance, the cut-off wavelength of the infrared waveband is 6.6 microns, and the light transmission effect of the sample is shown in figure 2.
Example 2
The preparation method comprises the following steps:
(1) preparing materials: according to Tm: YAG-Al2O3(Tm3+Accounting for 0.8 percent of the molar concentration of Y in YAG) and weighing the raw material Al according to the stoichiometric ratio of each element in the YAG2O3、Y2O3And Tm2O3In which Al is2O3And Y2O3The molar ratio is 65:35, namely x is 35;
(2) ball milling: carrying out wet ball milling on the raw materials in the step (1), sequentially putting raw material powder into a ball milling tank, wherein the grinding balls are high-purity alumina balls, and the ball-to-material ratio is 5: simultaneously adding absolute ethyl alcohol, wherein the total mass ratio of the absolute ethyl alcohol to the raw material powder is 1: 1, carrying out planetary ball milling at the ball milling rotation speed of 300r/min for 12 hours to fully and uniformly mix the raw materials;
(3) drying and calcining: drying the slurry uniformly mixed in the step (2) in a drying oven, and calcining the dried powder in a muffle furnace at 900 ℃ for 3 hours;
(4) laser melting vitrification: pressing the dried powder in the step (3) into a block or a sheet, heating the block or the sheet in a vacuum state by using a high-power laser device, wherein the heating rate is 300 ℃/min, the heating temperature is 2000 ℃, the heating time is 30s, then closing the laser, and cooling to the room temperature at the speed of 200 ℃/s;
(5) processing: taking out the transparent glass material obtained in the step (4), grinding and polishing the transparent glass material into a disc shape, wherein the density of the transparent glass material is about 3.8g/cm3；
(6) Annealing and ceramization: annealing and crystallizing the disc glass material in the step (5), wherein the annealing temperature is 955 ℃, the heating rate is 40 ℃/min, and the heat preservation time is 3 h; annealing in air atmosphere, and cooling to room temperature along with the furnace to obtain the nano-layered composite transparent ceramic.
After testing, the density was 4.53g/cm3(ii) a The X-ray diffraction test shows that the diffraction peak is shown in fig. 1, and compared with a standard card, only YAG crystal phase and no other crystal phase appear. Observing with field emission scanning electron microscope FSEM, wherein YAG crystal grain size is about 32nm, and Al is wrapped on the outer layer of the crystal grain2O3A layer having a thickness of 2 nm; the hardness can reach 28GPa and the Young modulus can reach 320GPa when the test is carried out by adopting an indenter; the transmittance of the visible light in a wave band of 500nm is 93 percent of the theoretical transmittance, the transmittance of the near infrared and middle infrared in a wave band of 4 mu m is 99.6 percent of the theoretical transmittance, and the cutoff wavelength of the infrared wave band is 6.6 mu m.
Example 3
The preparation method comprises the following steps:
(1) preparing materials: according to Yb: YAG-Al2O3(Yb3+Accounting for 0.2 percent of the molar concentration of Y in YAG) and weighing the raw material Al according to the stoichiometric ratio of each element in the YAG2O3、Y2O3And Yb2O3In which Al is2O3And Y2O3The molar ratio is 68:32, namely x is 32;
(2) ball milling: carrying out wet ball milling on the raw materials in the step (1), sequentially putting raw material powder into a ball milling tank, wherein the grinding balls are high-purity alumina balls, and the ball-to-material ratio is 4: simultaneously adding absolute ethyl alcohol, wherein the total mass ratio of the absolute ethyl alcohol to the raw material powder is 1: 2, carrying out planetary ball milling at the ball milling rotation speed of 180r/min for 15 hours to fully and uniformly mix the raw materials;
(3) drying and calcining: drying the slurry uniformly mixed in the step (2) in a drying oven, and calcining the dried powder in a muffle furnace at 800 ℃ for 4 hours;
(4) laser melting vitrification: pressing the dried powder in the step (3) into a block or a sheet, heating the block or the sheet by adopting a high-power laser device in a vacuum state at the heating rate of 200 ℃/min at the heating temperature of 2020 ℃ for 20s, then closing the laser, and cooling the block or the sheet to the room temperature at the speed of 100 ℃/s;
(5) processing: taking out the transparent glass material obtained in the step (4), grinding and polishing the transparent glass material into a disc shape, wherein the density of the transparent glass material is about 3.65g/cm3；
(6) Annealing and ceramization: annealing and crystallizing the disc glass material in the step (5), wherein the annealing temperature is 950 ℃, the heating rate is 35 ℃/min, and the heat preservation time is 2 h; at H2Annealing in atmosphere, and cooling to room temperature along with the furnace to obtain the nano-layered composite transparent ceramic.
After testing, the density was 4.41g/cm3(ii) a The X-ray diffraction test shows that the diffraction peak is shown in fig. 1, and compared with a standard card, only YAG crystal phase and no other crystal phase appear. Observing with field emission scanning electron microscope FSEM, wherein YAG crystal grain size is 28nm, and Al is coated on the outer layer of the crystal grain2O3A layer having a thickness of 3 nm; the hardness can reach 26GPa and the Young modulus can reach 310GPa when the test is carried out by adopting an indenter; the transmittance of the visible light in a wave band of 500nm is 94 percent of the theoretical transmittance, the transmittance of the near-infrared and mid-infrared 4 mu m wave bands is 99.8 percent of the theoretical transmittance, and the cutoff wavelength of the infrared wave band is 6.6 mu m.

Claims (9)

1. YAG-Al2O3The nano-layered composite transparent ceramic is characterized by comprising completely crystallized M: YAG nano-crystals and Al wrapped outside the M: YAG nano-crystals2O3The matrix of the complex phase structure of the thin layer is composed of the components shown in the following formula:
(100-x)Al2O3-(x)Y2O3
wherein x is more than or equal to 30 and less than or equal to 35, and M is doped rare earth ions or transition metal ions capable of emitting light in near-infrared and mid-infrared bands.
2. According to claimYAG-Al as described in claim 12O3The nano-layered composite transparent ceramic is characterized in that the grain size of the M: YAG nano-crystal is 25-32 nm, and the Al is2O3The thickness of the thin layer is 2-5 nm.
3. YAG-Al as in claim 12O3The nano-layered composite transparent ceramic is characterized in that the doping ions M are selected from Cr3+、Nd3+、Yb3+And Tm3+One or more of the ions.
4. YAG-Al as in claim 1 or 32O3The nano layered composite transparent ceramic is characterized in that the molar concentration of doping ions M in Al in YAG is 0.01-1%, or the molar concentration of doping ions M in Y in YAG is 0.01-1%.
5. YAG-Al as claimed in any one of claims 1 to 42O3The preparation method of the nano-layered composite transparent ceramic is characterized by comprising the following specific steps of:
(1) preparing materials: al according to the formula (100-x)2O3-(x)Y2O3Respectively weighing raw materials of alumina, yttrium oxide and oxide containing M according to the stoichiometric ratio of Al and Y and the doping concentration of M;
(2) ball milling: carrying out wet ball milling on the raw material powder in the step (1) to obtain uniformly mixed slurry;
(3) drying and calcining: drying the slurry uniformly mixed in the step (2), and calcining in a muffle furnace after drying;
(4) laser melting vitrification: pressing the powder calcined in the step (3) into blocks or sheets, heating the blocks or sheets in a certain atmosphere or vacuum state by using a high-power laser device, wherein the heating rate is 200-300 ℃/min, the heating temperature is 2000-2050 ℃, the heating time is 20-30 s, then closing a laser, and cooling to the room temperature at the speed of 100-200 ℃/s;
(5) processing: taking out the transparent glass material obtained in the step (4), and grinding and polishing the transparent glass material into a disc shape;
(6) annealing and ceramization: annealing and crystallizing the disc glass material in the step (5), wherein the annealing temperature is 945-955 ℃, the heating rate is 25-40 ℃/min, the heat preservation time is 1-3 h, and the annealing atmosphere is selected according to the selected M ion target valence state; cooling to room temperature along with the furnace to obtain the nano-layered composite transparent ceramic.
6. YAG-Al as in claim 52O3The preparation method of the nano-layered composite transparent ceramic is characterized in that the wet ball milling in the step (2) comprises the following specific steps: putting raw material powder into a ball milling tank in sequence, wherein high-purity alumina balls are selected as the grinding balls, and the ball-material ratio is 2-5: and 1, simultaneously adding a ball milling medium, and carrying out planetary ball milling, wherein the ball milling rotating speed is 120-300 r/min, and the ball milling time is 12-18 hours.
7. YAG-Al as in claim 62O3The preparation method of the nano-layered composite transparent ceramic is characterized in that the ball milling medium is absolute ethyl alcohol, and the total mass ratio of the absolute ethyl alcohol to the raw material powder is 1: 1 to 2.
8. YAG-Al as in claim 52O3The preparation method of the nano-layered composite transparent ceramic is characterized in that the calcining temperature in the step (3) is 700-900 ℃, and the time is 3-8 hours.
9. YAG-Al as in claim 52O3The preparation method of the nano-layered composite transparent ceramic is characterized in that the annealing atmosphere in the step (6) is selected from one or more of nitrogen, argon, hydrogen, oxygen and air.
CN202010922244.0A 2020-09-04 2020-09-04 YAG-Al2O3Nano laminated composite transparent ceramic and preparation method thereof Active CN112028492B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010922244.0A CN112028492B (en) 2020-09-04 2020-09-04 YAG-Al2O3Nano laminated composite transparent ceramic and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010922244.0A CN112028492B (en) 2020-09-04 2020-09-04 YAG-Al2O3Nano laminated composite transparent ceramic and preparation method thereof

Publications (2)

Publication Number Publication Date
CN112028492A CN112028492A (en) 2020-12-04
CN112028492B true CN112028492B (en) 2022-03-08

Family

ID=73592127

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010922244.0A Active CN112028492B (en) 2020-09-04 2020-09-04 YAG-Al2O3Nano laminated composite transparent ceramic and preparation method thereof

Country Status (1)

Country Link
CN (1) CN112028492B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116477930A (en) * 2023-03-17 2023-07-25 江苏师范大学 Method for preparing large-size nanocrystalline transparent ceramic through nano metal nucleating agent

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107915481A (en) * 2017-11-22 2018-04-17 中国科学院过程工程研究所 A kind of nanostructured Yt aluminum garnet-base transparent ceramic material, preparation method and the usage
CN109896857A (en) * 2017-12-07 2019-06-18 上海航空电器有限公司 Composite ceramics fluorophor, preparation method and light supply apparatus for high power laser light illumination

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107915481A (en) * 2017-11-22 2018-04-17 中国科学院过程工程研究所 A kind of nanostructured Yt aluminum garnet-base transparent ceramic material, preparation method and the usage
CN109896857A (en) * 2017-12-07 2019-06-18 上海航空电器有限公司 Composite ceramics fluorophor, preparation method and light supply apparatus for high power laser light illumination

Also Published As

Publication number Publication date
CN112028492A (en) 2020-12-04

Similar Documents

Publication Publication Date Title
US10727493B2 (en) Oriented apatite-type doped rare earth silicate and/or germanate ion conductor and method for manufacturing same
Chen et al. New opportunities for transparent ceramics
CN107721406B (en) Method for preparing high-light-transmittance magnesia-alumina spinel transparent ceramic
CN104557013B (en) Preparation method of transparent tetravalent chromium-doped yttrium aluminum garnet ceramics
CN101935208B (en) Rare earth aluminate single-phase or complex-phase nanocrystalline transparent ceramic material and preparation method thereof
WO2003004437A1 (en) Translucent rare earth oxide sintered article and method for production thereof
CN101993240B (en) Preparation method of Ce3+doped lutetium silicate (Lu2SiO5) polycrystalline flashing optical ceramic
de Camargo et al. Structural and spectroscopic properties of rare-earth (Nd 3+, Er 3+, and Yb 3+) doped transparent lead lanthanum zirconate titanate ceramics
US7022262B2 (en) Yttrium aluminum garnet powders and processing
Su et al. Effect of Ca2+ and Mn2+ ions on the radiation properties of LaAlO3
CN103601484A (en) Preparation method for lutetium-aluminum garnet-based transparent ceramic
CN114773048A (en) Preparation method and application of composite ceramic material
CN102815941B (en) Rare-earth-ion-doped lanthanum gadolinium zirconate transparent ceramic material and preparation method thereof
CN112028492B (en) YAG-Al2O3Nano laminated composite transparent ceramic and preparation method thereof
Liu et al. Uniform and fine Mg-γ-AlON powders prepared from MgAl2O4: A promising precursor material for highly-transparent Mg-γ-AlON ceramics
Milisavljevic et al. Crystallization of glass materials into transparent optical ceramics
CN114105639A (en) Infrared transparent ceramic material and preparation method thereof
Luo et al. Fabrication and spectral properties of hot-pressed Co: MgAl2O4 transparent ceramics for saturable absorber
Carreaud et al. Fabrication and optical properties of transparent fine-grained Zn1. 1Ga1. 8Ge0. 1O4 and Ni2+ (or Cr3+)-doped Zn1. 1Ga1. 8Ge0. 1O4 spinel ceramics
Fu et al. Ce3+: Lu3Al5O12–Al2O3 optical nanoceramic scintillators elaborated via a low-temperature glass crystallization route
He et al. Preparation of Ce-doped (Y, Gd) 3Al5O12 nanoceramics by sintering and crystallization of glass microspheres
CN106342083B (en) A kind of low temperature is prepared the method for aluminum nitride oxygen transparent ceramic
CN110550945B (en) Preparation method of LuAG Ce transparent ceramic and LuAG Ce transparent ceramic
JP7027338B2 (en) Transparent AlN sintered body and its manufacturing method
Tang et al. CoO-doped MgO–Al 2 O 3–SiO 2-colored transparent glass–ceramics with high crystallinity

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