CN114621002A - Simple and efficient hot-pressing sintering preparation method of Ce: YAG transparent ceramic - Google Patents
Simple and efficient hot-pressing sintering preparation method of Ce: YAG transparent ceramic Download PDFInfo
- Publication number
- CN114621002A CN114621002A CN202210269674.6A CN202210269674A CN114621002A CN 114621002 A CN114621002 A CN 114621002A CN 202210269674 A CN202210269674 A CN 202210269674A CN 114621002 A CN114621002 A CN 114621002A
- Authority
- CN
- China
- Prior art keywords
- yag
- transparent ceramic
- ceramic
- pressing
- sintering
- 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.)
- Pending
Links
- 238000005245 sintering Methods 0.000 title claims abstract description 86
- 239000000919 ceramic Substances 0.000 title claims abstract description 74
- 238000007731 hot pressing Methods 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000010438 heat treatment Methods 0.000 claims abstract description 34
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 30
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000000654 additive Substances 0.000 claims abstract description 13
- 230000000996 additive effect Effects 0.000 claims abstract description 13
- 238000005516 engineering process Methods 0.000 claims abstract description 10
- 229910010293 ceramic material Inorganic materials 0.000 claims abstract description 6
- 238000003746 solid phase reaction Methods 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims description 53
- 229910052582 BN Inorganic materials 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 18
- 238000000137 annealing Methods 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 11
- 239000002270 dispersing agent Substances 0.000 claims description 9
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 7
- 238000001354 calcination Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000000465 moulding Methods 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 238000003825 pressing Methods 0.000 claims description 7
- 238000007873 sieving Methods 0.000 claims description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims description 7
- 239000010935 stainless steel Substances 0.000 claims description 7
- 229910000831 Steel Inorganic materials 0.000 claims description 6
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 6
- 229910052593 corundum Inorganic materials 0.000 claims description 6
- 239000010959 steel Substances 0.000 claims description 6
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052984 zinc sulfide Inorganic materials 0.000 claims 1
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 abstract description 48
- 238000000034 method Methods 0.000 abstract description 20
- 238000002834 transmittance Methods 0.000 abstract description 11
- 229910002804 graphite Inorganic materials 0.000 abstract description 8
- 239000010439 graphite Substances 0.000 abstract description 8
- 238000002845 discoloration Methods 0.000 abstract description 7
- 230000008569 process Effects 0.000 abstract description 6
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 55
- 238000005498 polishing Methods 0.000 description 11
- 238000011109 contamination Methods 0.000 description 6
- 238000000227 grinding Methods 0.000 description 6
- 239000011148 porous material Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000012512 characterization method Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 238000002490 spark plasma sintering Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 238000000280 densification Methods 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005261 decarburization Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 239000002223 garnet Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/44—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
- C04B35/645—Pressure sintering
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3201—Alkali metal oxides or oxide-forming salts thereof
- C04B2235/3203—Lithium oxide or oxide-forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3229—Cerium oxides or oxide-forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/444—Halide containing anions, e.g. bromide, iodate, chlorite
- C04B2235/445—Fluoride containing anions, e.g. fluosilicate
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/658—Atmosphere during thermal treatment
- C04B2235/6581—Total pressure below 1 atmosphere, e.g. vacuum
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/661—Multi-step sintering
- C04B2235/662—Annealing after sintering
- C04B2235/663—Oxidative annealing
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9646—Optical properties
- C04B2235/9653—Translucent or transparent ceramics other than alumina
Abstract
The invention belongs to the technical field of ceramic material preparation, and particularly relates to a simple and efficient hot-pressing sintering preparation method of Ce: YAG transparent ceramic. The preparation method disclosed by the invention combines the solid-phase reaction with the vacuum hot-pressing sintering (HP) technology, adopts lithium fluoride (LiF) as a sintering additive, uses Boron Nitride (BN) as a shielding layer to wrap a ceramic blank, and effectively solves the problem of carbon pollution caused by a graphite mold in the sintering process of a sample under the combined action of the lithium fluoride (LiF) and the Boron Nitride (BN), thereby effectively avoiding the phenomenon of reduced transparency of the ceramic after heat treatment due to pollution and discoloration, and expanding the application field for hot-pressing sintering. Finally, the Ce: YAG transparent ceramic with high transmittance and high density is prepared in a shorter sintering period under the conditions of lower sintering temperature and vacuum degree.
Description
Technical Field
The invention belongs to the technical field of ceramic material preparation, and particularly relates to a simple and efficient hot-pressing sintering preparation method of Ce: YAG transparent ceramic.
Background
Among many novel fluorescent light conversion materials, transparent ceramics have low cost, short production period, easy realization of high doping concentration,The advantages of high thermal conductivity (about 14W/mK), high mechanical strength and the like are rapidly developed, among which, Y3Al5O12: Ce3+Transparent ceramics (Ce: YAG) have been studied most extensively. The vacuum sintering of a furnace adopting a tungsten heating element is the most common preparation method of the Ce: YAG transparent ceramic at present. But the method has higher sintering temperature, longer sintering period and higher production cost. Compared with non-pressure sintering, pressure-assisted sintering technologies such as hot-pressing sintering (HP) and Spark Plasma Sintering (SPS) can provide more sintering driving force, inhibit grain growth, and achieve densification of a sample at a lower temperature and in a shorter time. However, these techniques require the use of graphite molds, making the samples susceptible to carbon contamination during sintering, which greatly affects the optical properties of the Ce: YAG transparent ceramics.
Research shows that lithium fluoride (LiF) plays a role in better particle rearrangement, higher densification rate and inhibition of carbon contamination in poor sintering environment during sintering of transparent ceramics. In 1994, Majima et al discovered that the use of LiF as a sintering aid significantly improved the transparency of the samples when preparing yttria ceramics by hot press sintering. There have been many studies to prepare a YAG powder having a high sintering activity by a chemical coprecipitation method and then to add LiF to successfully prepare a high-transparency YAG transparent ceramic free from carbon contamination. We have found that LiF does not effectively eliminate carbon contamination of graphite molds when YAG transparent ceramics are prepared by solid phase reaction in combination with hot press sintering using commercial alumina and yttria powders. Luzhou Kogyo ceramics of Huazhong science and technology university also encounters the problem in the research on YAG transparent ceramics, and a sample using LiF as a sintering aid can be transparent through annealing, but has very low transmittance, and black impurity residues which cannot be removed through annealing can be observed in a physical photograph; and the sample without using LiF in the experiment can not eliminate the discoloration problem after annealing. Other effective measures for removing carbon contamination must be found.
Disclosure of Invention
The invention provides a new idea for preparing Ce: YAG transparent ceramic by a hot-pressing sintering method, aiming at the problem of carbon pollution caused by a graphite mould in the process of preparing a ceramic sample by traditional pressure-assisted sintering technologies such as hot-pressing sintering (HP), Spark Plasma Sintering (SPS) and the like. BN powder is selected as a carbon shielding material to wrap a ceramic blank, LiF is used as a sintering aid in a combined manner, and the two decarburization methods are combined to prepare the Ce: YAG transparent ceramic material with high transparency and high compactness.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a novel carbon shielding material, which is used for preparing a carbon shielding material in Ce: YAG ceramic by using BN (boron nitride) as hot-pressing sintering. BN has a low coefficient of friction, excellent high temperature stability and high thermal conductivity, and is often used as a high temperature release agent in HP.
In the research, the effect of completely removing carbon pollution in the hot-pressing sintering process cannot be achieved only by adding LiF or wrapping the mixture by using BN, so that the influence of the combination of two decarburization methods on the hot-pressing sintering of the Ce: YAG transparent ceramic is researched by using hexagonal boron nitride (BN-h) powder as a carbon shielding material and using LiF as a sintering auxiliary agent. Finally, the problem of carbon pollution caused by a graphite die in hot-pressing sintering is successfully solved by adopting a simple and effective boron nitride shielding technology, and a new idea is provided for solving the problem of carbon pollution in HP and SPS technologies.
A simple and efficient hot-pressing sintering preparation method of Ce: YAG transparent ceramic comprises the following steps:
(1) using high purity commercial powder Al2O3、Y2O3、CeO2Weighing the powder serving as the original powder according to a stoichiometric ratio, adding a certain amount of PEI serving as a dispersing agent, and taking LiF as a sintering additive to obtain a mixture; the chemical formula of the Ce: YAG is as follows: (Y)1- xCex)3Al5O12(x = 0-0.01); the PEI dispersing agent is an absolute ethyl alcohol diluted solution, and the addition amount of PEI is 0-0.5 wt.%; the addition amount of the LiF is 0-1 wt.%.
(2) Placing the mixture in a planetary ball mill for ball milling for 8-24 hours, drying, sieving by using a 200-mesh sieve, then pressing and molding the sieved powder by using a steel mold with the diameter of 19mm, and then placing in a muffle furnace for calcining at 800 ℃ to completely remove organic components in a blank;
(3) adopting BN-h powder to coat the calcined ceramic body to obtain a BN-YAG structure,
the method comprises the following steps: firstly, paving a layer of BN powder at the bottom of a stainless steel die with the diameter of 20mm, applying uniaxial pressure of 20MPa to the BN powder to ensure that the BN powder has certain strength, then putting a ceramic blank (phi 19mm) into the center of the die, uniformly placing the BN powder above and around the blank, and applying uniaxial pressure of 20MPa again to form a BN-YAG inclusion;
(4) transferring the BN-YAG inclusion into a hot-pressing die, placing the BN-YAG inclusion into a vacuum hot-pressing furnace for sintering, heating and pressurizing according to a certain system, wherein the heating rate is 5-15 ℃ per min, the temperature in the furnace is 1550-1700 ℃, the pressure is 50MPa, and the vacuum degree is about 10-1Keeping the mixture for 1 to 3 hours under the condition of Pa to prepare Ce: YAG transparent ceramic;
(5) annealing the ceramic sample after hot-pressing sintering in air at 1200-1400 ℃ to remove oxygen vacancies, and finally grinding and polishing the double surfaces of the sample to the thickness of 1mm for characterization test.
According to the method, a solid-phase reaction is combined with a vacuum hot-pressing sintering (HP) technology, lithium fluoride (LiF) is used as a sintering additive, Boron Nitride (BN) is used as a shielding layer to wrap a ceramic blank, and the two technologies act together to effectively solve the problem of carbon pollution caused by a graphite mold in the sintering process of a sample, effectively avoid the phenomenon of reduced transparency of the ceramic after heat treatment due to pollution and color change, and expand the application field of hot-pressing sintering. Finally, the Ce: YAG transparent ceramic with high transmittance and high density is prepared in a shorter sintering period under the conditions of lower sintering temperature and vacuum degree.
Advantageous effects
The invention discloses a simple and efficient hot-pressing sintering preparation method of a Ce: YAG transparent ceramic, which has the following beneficial effects:
(1) the pressure-assisted sintering technology can provide more driving force and inhibit the growth of crystal grains, and compared with other sintering methods, the vacuum hot-pressing sintering method can realize the densification of the ceramic sample at a lower sintering temperature and in a shorter sintering period, thereby meeting the requirements of industrial production.
(2) BN powder is selected as a carbon shielding material to wrap the ceramic blank, LiF is combined to serve as a sintering additive, the preparation process is simple, pollution caused by a graphite mold in the vacuum hot-pressing sintering process is finally eliminated, and a new thought is provided for solving the problem of carbon pollution in the HP and SPS technologies.
(3) The Ce-YAG transparent ceramic material prepared by the method has high transparency and density and is a transparent ceramic material with excellent performance.
Drawings
FIG. 1 is an XRD pattern of a sample A, B, C of Ce: YAG prepared in examples 1-3 before heat treatment (a);
FIG. 2 is an XRD pattern of a sample A, B, C of Ce: YAG prepared in examples 1-3 after heat treatment and polishing (b);
FIG. 3 is a photograph of a Ce: YAG sample A, B, C made in examples 1-3;
FIG. 4 is a graph of the linear transmittance of the Ce: YAG sample A, B, C after heat treatment and polishing prepared in examples 1-3;
FIG. 5 is a scanning electron microscope image of the hot-etched surface of the Ce: YAG sample A prepared in example 1;
FIG. 6 is a scanning electron microscope image of the hot-etched surface of the Ce: YAG sample B prepared in example 2;
FIG. 7 is a scanning electron microscope image of the hot-etched surface of the Ce: YAG sample C prepared in example 3.
Detailed Description
Hereinafter, the present invention will be described in detail. Before the description is made, it should be understood that the terms used in the present specification and the appended claims should not be construed as limited to general and dictionary meanings, but interpreted based on the meanings and concepts corresponding to technical aspects of the present invention on the basis of the principle that the inventor is allowed to define terms appropriately for the best explanation. Accordingly, the description proposed herein is just a preferable example for the purpose of illustrations only, not intended to limit the scope of the invention, so it should be understood that other equivalents and modifications could be made thereto without departing from the spirit and scope of the invention.
The following examples are given by way of illustration of embodiments of the invention and are not to be construed as limiting the invention, and it will be understood by those skilled in the art that modifications may be made without departing from the spirit and scope of the invention. Unless otherwise specified, reagents and equipment used in the following examples are commercially available products.
Example 1
A simple and efficient hot-pressing sintering preparation method of Ce: YAG transparent ceramic comprises the following steps:
1. using high purity commercial powder Al2O3、Y2O3、CeO2The raw powder is weighed according to the stoichiometric ratio, 0.5wt.% of PEI is added as a dispersing agent, and 1wt.% of LiF is added as a sintering additive, so as to obtain a mixture.
2. And placing the mixture in a planetary ball mill for ball milling for 24 hours, drying, sieving by using a 200-mesh sieve, then pressing and molding the sieved powder by using a steel mold with the diameter of 19mm, and then placing in a muffle furnace for calcining at 800 ℃ to completely remove organic components in a blank.
3. And (3) wrapping the calcined ceramic body with BN-h powder to obtain a BN-YAG structure. The method comprises the following steps: firstly, a layer of BN-h powder is paved at the bottom of a stainless steel die with the diameter of 20mm, uniaxial pressure of 20MPa is applied to the powder to enable the powder to have certain strength, then a ceramic blank (phi 19mm) is placed in the center of the die, the BN-h powder is uniformly placed above and around the blank, and uniaxial pressure of 20MPa is applied again to form a BN-YAG inclusion.
4. And transferring the BN-YAG inclusion into a hot-pressing die, and sintering in a vacuum hot-pressing furnace. Heating and pressurizing according to a certain system, firstly heating to 1000 ℃ at the speed of 10 ℃/min, and then slowly heating to 1600 ℃ at the heating speed of 5 ℃/min. At 1200 ℃ the slow addition is startedPressing until 50MPa is reached. The temperature in the furnace is 1600 ℃, the pressure is 50MPa, and the vacuum degree is about 10-1And keeping the mixture for 1 hour under the condition of Pa to prepare the Ce: YAG transparent ceramic.
5. Annealing the ceramic sample after hot-pressing sintering in air at 1300 ℃ to remove oxygen vacancies, and finally grinding and polishing the double surfaces of the sample until the thickness is 1mm, marking as a sample A, and performing characterization test.
Example 2
A simple and efficient hot-pressing sintering preparation method of a Ce: YAG transparent ceramic is used as a reference of example 1 and comprises the following steps:
1. using high purity commercial powder Al2O3、Y2O3、CeO2The powder is taken as original powder and weighed according to the stoichiometric ratio, 0.5wt.% of PEI is added to be taken as a dispersing agent, TEOS is taken as a sintering additive, and a mixture is obtained.
2. And placing the mixture in a planetary ball mill for ball milling for 24 hours, drying, sieving by using a 200-mesh sieve, then pressing and molding the sieved powder by using a steel mold with the diameter of 19mm, and then placing in a muffle furnace for calcining at 800 ℃ to completely remove organic components in a blank.
3. And (3) wrapping the calcined ceramic body with BN-h powder to obtain a BN-YAG structure. The method comprises the following steps: firstly, a layer of BN-h powder is paved at the bottom of a stainless steel die with the diameter of 20mm, uniaxial pressure of 20MPa is applied to the powder to enable the powder to have certain strength, then a ceramic blank (phi 19mm) is placed in the center of the die, the BN-h powder is uniformly placed above and around the blank, and uniaxial pressure of 20MPa is applied again to form a BN-YAG inclusion.
4. Transferring the BN-YAG inclusion into a hot-pressing die, and sintering in a vacuum hot-pressing furnace. Heating and pressurizing according to a certain system, firstly heating to 1000 ℃ at the rate of 10 ℃/min, and then slowly heating to 1600 ℃ at the heating rate of 5 ℃/min. The slow pressurization was started at 1200 ℃ until 50MPa was reached. The temperature in the furnace is 1600 ℃, the pressure is 50MPa, and the vacuum degree is about 10-1And keeping the mixture for 1 hour under the condition of Pa to prepare the Ce: YAG transparent ceramic.
5. Annealing the ceramic sample after hot-pressing sintering in air at 1300 ℃ to remove oxygen vacancies, and finally grinding and polishing the double surfaces of the sample until the thickness is 1mm, marking as a sample B, and performing characterization test.
Example 3
YAG transparent ceramic simple high-efficient hot pressing sintering preparation method, this example is as the reference of example 1, includes the following steps:
1. using high purity commercial powder Al2O3、Y2O3、CeO2The raw powder is weighed according to the stoichiometric ratio, 0.5wt.% of PEI is added as a dispersing agent, and 1wt.% of LiF is added as a sintering additive, so as to obtain a mixture.
2. And placing the mixture in a planetary ball mill for ball milling for 24 hours, drying, sieving by using a 200-mesh sieve, then pressing and molding the sieved powder by using a steel mold with the diameter of 19mm, and then placing in a muffle furnace for calcining at 800 ℃ to completely remove organic components in a blank.
3. Transferring the calcined ceramic body into a hot-pressing die, separating the ceramic body from a graphite gasket by using carbon paper, and sintering in a vacuum hot-pressing furnace. Heating and pressurizing according to a certain system, firstly heating to 1000 ℃ at the rate of 10 ℃/min, and then slowly heating to 1600 ℃ at the heating rate of 5 ℃/min. The slow pressurization was started at 1200 ℃ until 50MPa was reached. The temperature in the furnace is 1600 ℃, the pressure is 50MPa, and the vacuum degree is about 10-1And keeping the mixture for 1 hour under the condition of Pa to prepare the Ce: YAG transparent ceramic.
4. Annealing the ceramic sample after hot-pressing sintering in air at 1300 ℃ to remove oxygen vacancies, and finally grinding and polishing the double surfaces of the sample until the thickness is 1mm, marking as a sample C, and performing characterization test.
Example 4
A simple and efficient hot-pressing sintering preparation method of Ce: YAG transparent ceramic comprises the following steps:
1. using high purity commercial powder Al2O3、Y2O3、CeO2Weighing the raw powder according to the stoichiometric ratio, adding 0.5wt.% of PEI as a dispersing agent and 1wt.% of LiF as a sintering additive to obtain the powderAnd (4) mixing the materials.
2. And (3) placing the mixture into a planetary ball mill for ball milling for 24 hours, drying, sieving by using a 200-mesh sieve, then pressing and molding the sieved powder by using a steel mold with the diameter of 19mm, and then placing the powder into a muffle furnace for calcining at 800 ℃ to completely remove organic components in the blank.
3. And (3) wrapping the calcined ceramic body with BN-h powder to obtain a BN-YAG structure. The method comprises the following steps: firstly, a layer of BN-h powder is paved at the bottom of a stainless steel die with the diameter of 20mm, uniaxial pressure of 20MPa is applied to the powder to enable the powder to have certain strength, then a ceramic blank (phi 19mm) is placed in the center of the die, the BN-h powder is uniformly placed above and around the blank, and uniaxial pressure of 20MPa is applied again to form a BN-YAG inclusion.
4. Transferring the BN-YAG inclusion into a hot-pressing die, and sintering in a vacuum hot-pressing furnace. Heating and pressurizing according to a certain system, firstly heating to 1000 ℃ at the speed of 10 ℃/min, and then slowly heating to 1550 ℃ at the heating speed of 5 ℃/min. The slow pressurization was started at 1200 ℃ until 50MPa was reached. The temperature in the furnace is 1550 ℃, the pressure is 50MPa, and the vacuum degree is about 10-1And keeping the mixture for 2 hours under the condition of Pa to prepare the Ce: YAG transparent ceramic.
5. Annealing the ceramic sample after hot-pressing sintering in air at 1300 ℃ to remove oxygen vacancies, and finally grinding and polishing the double surfaces of the sample until the thickness is 1mm, marking as a sample D, and performing characterization test.
Examples of the experiments
YAG sample A, B, C of Ce prepared in examples 1-3 above was heat treated and polished, and then X-ray diffraction was performed on the samples before heat treatment (a), after heat treatment and after polishing (b), respectively, and XRD patterns of the samples before heat treatment (a), after heat treatment and after polishing (b) are shown in FIGS. 1 and 2, respectively. From fig. 1 and 2, it can be seen that the diffraction peaks of Ce: YAG can well meet the standard mode of YAG (JCPDS33-0040), indicating that pure garnet crystal structure is obtained.
The photographs of the Ce: YAG sample A, B, C obtained in examples 1-3 above are shown in FIG. 3. Sample (a) was prepared with LiF as sintering additive; the sample (B) is prepared by taking TEOS as a sintering additive and BN-h as a shielding material; the sample (C) was prepared using LiF as a sintering additive and BN-h as a shielding material. In fig. 3, the part above the red line is a photograph of the hot-pressed sintered sample after simple grinding and polishing, and the part below the red line is a photograph of the same sample after annealing and final polishing. As can be seen from FIG. 3, after vacuum hot-pressing sintering, the sample B, C shows black/brown discoloration, which is generally considered to be caused by carbon pollution or oxygen vacancy, and the discoloration can be solved by high-temperature heat treatment, so that the original yellow color of the Ce: YAG is restored, but the light transmittance of the Ce: YAG ceramic is reduced due to the generation of micro-structural pores of the ceramic. It is demonstrated that the problems of carbon contamination and discoloration cannot be solved by using BN or LiF only in the hot-pressing sintering process, and particularly, sample C has not only serious discoloration but also extremely low light transmittance after annealing. And the sample A protects the ceramic body by combining BN-h with LiF, thereby effectively avoiding carbon pollution, eliminating color change and having higher transparency after annealing.
YAG sample A, B, C of Ce prepared in examples 1-3 was heat treated and polished for in-line transmittance testing and the in-line transmittance curve of sample A, B, C is shown in FIG. 4. As can be seen from FIG. 4, under the dual actions of BN-h and LiF, the on-line transmittance of sample A at 800nm reaches 71.5%; the sample B using BN-h as an external shield has a high transmittance of 57.1 percent at 800nm, but still has discoloration; the in-line transmission at 800nm for sample C was only 21.3%. It can be seen that the light transmittance of the color-changed sample is obviously reduced after the heat treatment, and the appearance color change of the sample is closely related to carbon pollution. Carbon purification mechanism studies for LiF generally suggest that LiF reacts with carbon at high temperatures to form (CF)nA gas, which is then released; the mechanism of action of BN-h is to reduce the diffusion of elemental carbon by a simple external shield to avoid direct contact between the carbon mold and the sample. LiF has poor effect on eliminating carbon pollution, but can solve the problem of color change caused by carbon pollution when combined with a BN-h shielding material.
The thermal corrosion surface of the Ce: YAG sample A, B, C prepared in examples 1-3 was examined by sem, and the sem images of the thermal corrosion surface of sample A, B, C are shown in fig. 5, 6, and 7, respectively. As can be seen from FIGS. 5 to 7, the average grain size of all three samples was about 1 to 3 μm, and all had regular grains and clean grain boundaries. The samples A and B which are subjected to the BN-h coating treatment have fewer pores, while the sample C does not have the shielding effect of the BN-h, so that most of carbon impurities enriched at grain boundaries are permeated, a large number of open pores are left at the grain boundaries after the heat treatment, a small number of closed pores are generated in the grain boundaries, and the optical properties of the samples are greatly reduced by the pores. The BN-h is adopted as the barrier, so that the number of pores of the crystal boundary is reduced, the density of the sample is increased, and the optical performance of the sample is improved.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions.
Claims (9)
1. A simple and efficient hot-pressing sintering preparation method of a Ce: YAG transparent ceramic is characterized in that a solid-phase reaction is combined with a vacuum hot-pressing sintering technology to prepare the Ce: YAG transparent ceramic material, and specifically comprises the following steps:
(1) weighing original powder, wherein the original powder comprises Al2O3、Y2O3、CeO2Adding a dispersing agent and a sintering additive into the original powder to obtain a mixture;
(2) ball-milling the mixture obtained in the step (1), drying, sieving, then pressing and molding the sieved powder, and then calcining to completely remove organic components in the blank to obtain a ceramic blank;
(3) wrapping the ceramic blank obtained in the step (2) with boron nitride powder to obtain a ceramic blank with a BN-YAG structure;
(4) transferring the ceramic blank with the BN-YAG structure obtained in the step (3) into a hot-pressing die, sintering in a vacuum hot-pressing furnace, and heating and pressurizing to obtain a Ce: YAG transparent ceramic sample;
(5) and (4) annealing the Ce: YAG transparent ceramic sample obtained in the step (4) to remove oxygen vacancies, thus obtaining the Ce: YAG transparent ceramic.
2. The simple and efficient hot-pressing sintering preparation method of the Ce: YAG transparent ceramic is characterized in that in the step (1), the dispersant is PEI; the sintering additive is LiF.
3. YAG transparent ceramic simple and efficient hot-pressing sintering preparation method according to claim 2, wherein in the step (1), the used PEI dispersant is absolute ethyl alcohol diluted solution, and the addition amount of PEI is 0-0.5 wt.%; the addition amount of the LiF is 0-1 wt.%.
4. The simple and efficient hot-pressing sintering preparation method of the Ce: YAG transparent ceramic according to claim 1, characterized in that in the step (2), the mixture is placed in a planetary ball mill for ball milling for 8-24 hours, after drying, a 200-mesh screen is used for sieving, then a steel die with the diameter of 19mm is used for pressing and molding the sieved powder, and then the powder is placed in a muffle furnace for calcining at 800 ℃.
5. The simple and efficient hot-pressing sintering preparation method of the Ce: YAG transparent ceramic according to claim 1, wherein in the step (3), the used boron nitride powder comprises one or more of hexagonal boron nitride, rhombohedral boron nitride, cubic boron nitride and wurtzite boron nitride.
6. The simple and efficient hot-pressing sintering preparation method of the Ce: YAG transparent ceramic according to claim 5, characterized in that hexagonal boron nitride powder is adopted as a carbon shielding material.
7. YAG transparent ceramic simple and efficient hot-pressing sintering preparation method according to claim 6, wherein in the step (3), the specific steps for obtaining the BN-YAG structure are as follows: firstly, laying a layer of BN-h powder at the bottom of a stainless steel die, applying uniaxial pressure of 20MPa to the stainless steel die to enable the stainless steel die to have certain strength, then placing a ceramic blank into the center of the die, uniformly placing the BN-h powder above and around the blank, and applying uniaxial pressure of 20MPa again to form a BN-YAG inclusion.
8. The simple and efficient hot-pressing sintering preparation method of the Ce: YAG transparent ceramic according to claim 1, wherein in the step (4), the heating and pressurizing treatment specifically comprises the following steps: the heating rate is 5-15 ℃/min, the temperature in the furnace is 1550-1700 ℃, the pressure is 50MPa, and the vacuum degree is 10-1Keeping the temperature for 1 to 3 hours under the condition of Pa.
9. The simple and efficient hot-pressing sintering preparation method of the Ce: YAG transparent ceramic is characterized in that in the step (5), the Ce: YAG transparent ceramic sample is annealed in air at 1200-1400 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210269674.6A CN114621002A (en) | 2022-03-18 | 2022-03-18 | Simple and efficient hot-pressing sintering preparation method of Ce: YAG transparent ceramic |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210269674.6A CN114621002A (en) | 2022-03-18 | 2022-03-18 | Simple and efficient hot-pressing sintering preparation method of Ce: YAG transparent ceramic |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114621002A true CN114621002A (en) | 2022-06-14 |
Family
ID=81902931
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210269674.6A Pending CN114621002A (en) | 2022-03-18 | 2022-03-18 | Simple and efficient hot-pressing sintering preparation method of Ce: YAG transparent ceramic |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114621002A (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120088649A1 (en) * | 2009-06-24 | 2012-04-12 | Nahum Frage | Manufacturing transparent yttrium aluminum garnet by spark plasma sintering |
| CN102910899A (en) * | 2012-11-16 | 2013-02-06 | 北京雷生强式科技有限责任公司 | Preparation method of yttrium aluminium garnet doped transparent laser ceramics |
| CN102924073A (en) * | 2012-11-16 | 2013-02-13 | 北京雷生强式科技有限责任公司 | Method for preparing rare earth ion-doped yttrium aluminum garnet (Re: YAG) transparent laser ceramic by using hot-pressing post treatment |
| US20130160492A1 (en) * | 2011-12-23 | 2013-06-27 | Guillermo R Villalobos | Polished, hot pressed, net shape ceramics |
| RU2685305C1 (en) * | 2018-05-28 | 2019-04-17 | Федеральное государственное автономное образовательное учреждение высшего образования "Дальневосточный федеральный университет" (ДВФУ) | Method of obtaining transparent ceramics of yttrium-aluminum garnet |
| CN112209714A (en) * | 2020-10-16 | 2021-01-12 | 长春理工大学 | Preparation technology of one-step-formed sintered aluminum-based garnet type luminescent ceramic |
| RU2746912C1 (en) * | 2020-09-03 | 2021-04-22 | Федеральное государственное автономное образовательное учреждение высшего образования «Дальневосточный федеральный университет» (ДВФУ) | Method for producing transparent yag ceramics |
-
2022
- 2022-03-18 CN CN202210269674.6A patent/CN114621002A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120088649A1 (en) * | 2009-06-24 | 2012-04-12 | Nahum Frage | Manufacturing transparent yttrium aluminum garnet by spark plasma sintering |
| US20130160492A1 (en) * | 2011-12-23 | 2013-06-27 | Guillermo R Villalobos | Polished, hot pressed, net shape ceramics |
| CN102910899A (en) * | 2012-11-16 | 2013-02-06 | 北京雷生强式科技有限责任公司 | Preparation method of yttrium aluminium garnet doped transparent laser ceramics |
| CN102924073A (en) * | 2012-11-16 | 2013-02-13 | 北京雷生强式科技有限责任公司 | Method for preparing rare earth ion-doped yttrium aluminum garnet (Re: YAG) transparent laser ceramic by using hot-pressing post treatment |
| RU2685305C1 (en) * | 2018-05-28 | 2019-04-17 | Федеральное государственное автономное образовательное учреждение высшего образования "Дальневосточный федеральный университет" (ДВФУ) | Method of obtaining transparent ceramics of yttrium-aluminum garnet |
| RU2746912C1 (en) * | 2020-09-03 | 2021-04-22 | Федеральное государственное автономное образовательное учреждение высшего образования «Дальневосточный федеральный университет» (ДВФУ) | Method for producing transparent yag ceramics |
| CN112209714A (en) * | 2020-10-16 | 2021-01-12 | 长春理工大学 | Preparation technology of one-step-formed sintered aluminum-based garnet type luminescent ceramic |
Non-Patent Citations (4)
| Title |
|---|
| AURELIEN KATZ等: "role of LiF addictive on spark plasma sintered transparent YAG ceramics", 《CERAMICS INTERNATIONAL》 * |
| QINGLE PANG: "improved optical properties of BN powder shielded Ce:YAG ceramics prepared by hot pressing", 《CERAMICS INTERNATIONAL》 * |
| 李兴旺等: "埋粉热压后处理制备Nd:YAG激光陶瓷", 《硅酸盐学报》 * |
| 陆艺莹: "热压烧结制备YAG透明陶瓷及其阻抗谱分析研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107721406B (en) | Method for preparing high-light-transmittance magnesia-alumina spinel transparent ceramic | |
| WO2012118315A2 (en) | Method for preparing polycrystalline aluminum oxynitride having enhanced transparency | |
| Bhandhubanyong et al. | Forming of silicon nitride by the HIP process | |
| CN101935208B (en) | Rare earth aluminate single-phase or complex-phase nanocrystalline transparent ceramic material and preparation method thereof | |
| CN107352994B (en) | Preparation method of magnesia-alumina spinel transparent ceramic | |
| TWI464133B (en) | Polycrystalline MgO sintered body and its manufacturing method and MgO target for sputtering | |
| Min et al. | Fabrication of transparent γ-AlON by direct 2-step pressureless sintering of Al2O3 and AlN using an AlN-deficient composition | |
| Sutorik et al. | Transparent solid solution magnesium aluminate spinel polycrystalline ceramic with the alumina‐rich composition MgO· 1.2 Al2O3 | |
| JP4878343B2 (en) | Translucent rare earth gallium garnet sintered body, manufacturing method thereof and magneto-optical device | |
| CN112299861B (en) | AlON transparent ceramic pseudo-sintering agent and application thereof, and preparation method of transparent ceramic | |
| JP2011121837A (en) | Translucent terbium oxide sintered compact for magneto-optical element | |
| RU2746912C1 (en) | Method for producing transparent yag ceramics | |
| CN114105639A (en) | Infrared transparent ceramic material and preparation method thereof | |
| Fang et al. | Effect of heat treatment of green bodies on the sintering and optical properties of large-size and thick transparent YAG ceramics | |
| Baek et al. | AlN with high strength and high thermal conductivity based on an MCAS-Y2O3-YSZ multi-additive system | |
| Ni et al. | Textured HfB2-based ultrahigh-temperature ceramics with anisotropic oxidation behavior | |
| CN107473730B (en) | Method for preparing fine-grain and high-strength magnesia-alumina spinel transparent ceramic | |
| Gan et al. | Fabrication of submicron-grained IR-transparent Y2O3 ceramics from commercial nano-raw powders | |
| Wang et al. | Effects of YH2 addition on pressureless sintered AlN ceramics | |
| Xiang et al. | Transparent AlN ceramics sintered from nanopowders produced by the wet chemical method | |
| CN114621002A (en) | Simple and efficient hot-pressing sintering preparation method of Ce: YAG transparent ceramic | |
| CN102815945A (en) | Lanthanum gadolinium zirconate transparent ceramic material and preparation method thereof | |
| JP2856734B2 (en) | High thermal conductive aluminum nitride sintered body | |
| Li et al. | Low-temperature sintering of high-density aluminium nitride ceramics without additives at high pressure | |
| CN111499380B (en) | Zirconium-aluminum-based multi-phase composite ceramic and preparation method thereof |
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 | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20220614 |