CN112174668B - Preparation method and application of transparent ceramic with multilayer composite structure - Google Patents

Preparation method and application of transparent ceramic with multilayer composite structure Download PDF

Info

Publication number
CN112174668B
CN112174668B CN202011113149.2A CN202011113149A CN112174668B CN 112174668 B CN112174668 B CN 112174668B CN 202011113149 A CN202011113149 A CN 202011113149A CN 112174668 B CN112174668 B CN 112174668B
Authority
CN
China
Prior art keywords
ceramic
powder
yag
biscuit
slurry
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
CN202011113149.2A
Other languages
Chinese (zh)
Other versions
CN112174668A (en
Inventor
张乐
郗晓倩
邵岑
康健
李明
周天元
王骋
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 CN202011113149.2A priority Critical patent/CN112174668B/en
Publication of CN112174668A publication Critical patent/CN112174668A/en
Application granted granted Critical
Publication of CN112174668B publication Critical patent/CN112174668B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

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
    • C04B35/50—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
    • C04B35/505—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 based on yttrium oxide
    • 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
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/638—Removal 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
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
    • 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
    • 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
    • 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

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Laminated Bodies (AREA)

Abstract

The invention discloses a preparation method and application of transparent ceramic with a multilayer composite structure. The invention firstly weighs Y2O3Powder and Al2O3Using the powder as ceramic powder, preparing YAG raw material powder, and taking Al2O3Preparation of Al from powder2O3Raw material powder; YAG slurry and Al were prepared by the same method2O3A ceramic slurry; then mixing YAG slurry with Al2O3Respectively carrying out defoaming treatment and tape casting treatment on the ceramic slurry, drying after complete gelation to obtain YAG single-layer biscuit and Al2O3A single-layer biscuit; mixing the obtained YAG single-layer biscuit with Al2O3And carrying out staggered lamination on the single-layer biscuit to obtain a casting sheet, carrying out warm isostatic pressing on the casting sheet to obtain a ceramic biscuit, and sequentially carrying out vacuum sintering, annealing and double-side polishing treatment after removing the glue to obtain the transparent ceramic with the multilayer composite structure. The invention adopts the idea of toughening the composite structure, and the fracture toughness of the obtained multilayer composite ceramic sheet reaches 20 Mpa.m1/2The above.

Description

Preparation method and application of transparent ceramic with multilayer composite structure
Technical Field
The invention belongs to the field of advanced ceramics, and relates to a preparation method and application of transparent ceramics with a multilayer composite structure.
Background
The transparent ceramic material is used as a new panel material, has ultrahigh hardness, better glossiness than glass, better chemical stability and thermal stability than a glass panel, ultrahigh wear resistance and high light transmittance, can prolong the service life of a product, has a market prospect far better than that of a glass panel material, has a very wide application market and has a very huge prospect.
Generally, the fracture toughness of the single-structure ceramic panel is not high, but the ceramic panel is toughened by methods such as fiber composite toughening, self toughening and phase change toughening, and the like, so that the operation is complex and the procedure is complicated. CN111253153A mentions that the toughened YAG ceramic is prepared based on the gel casting of an Isobam gel system, however, the toughening effect of the patent is not obvious and the uniformity of a blank in the forming process is not good.
The laminated ceramic composite ceramic is a novel composite ceramic, is different from the traditional ceramic aiming at eliminating defects essentially, is a defect-resistant toughening ceramic, and can greatly improve the fracture toughness, the impact toughness, the fracture work and the use reliability of the material while keeping the characteristics of low density, high strength and the like of the ceramic material.
The traditional dry pressing molding is easy to have the defects of unevenness, cracking, deformation and the like under the conditions of large size and extreme thinness; the optical quality of the transparent ceramic is certainly influenced by more organic matters in injection molding; the gel casting process is to perform casting by utilizing the polymerization principle of organic monomers. The method is that ceramic powder is dispersed in aqueous solution containing organic monomer and cross-linking agent to prepare concentrated suspension with low viscosity and high solid phase volume fraction (volume fraction is more than 50%), then initiator and catalyst are added to initiate organic monomer polymerization under certain temperature condition to increase the viscosity of suspension, thus leading in-situ solidification and forming, and obtaining smooth and uniform blank with certain strength and capable of being machined. Compared with organic tape casting, the use amount of organic matters in the slurry can be greatly reduced; and the key technical problems of easy agglomeration and difficult dispersion of powder, sensitive process parameters, drying cracking and warping and the like in the water-based tape casting slurry are also solved. The solid content of the slurry is improved, so that the uniformity, the density and the strength of the biscuit are improved, the environmental pollution is reduced, and the cost is obviously reduced. Therefore, gel casting will become the first choice for preparing large-size toughened composite ceramics.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method and application of a transparent ceramic with a multilayer composite structure.
In order to solve the problems of the prior art, the technical scheme adopted by the invention is as follows:
a process for preparing the transparent ceramic with multi-layer composite structure includes preparing Al by gel casting method2O3The YAG multilayer composite structure ceramic comprises the following specific steps:
step 1, according to the chemical formula Y3Al5O12The stoichiometric ratio of each element in (A) is measured by weighing Y2O3Powder of Al2O3The powder is used as ceramic powder; mixing the weighed ceramic powder, sintering aid, dispersant A, grinding balls and absolute ethyl alcohol, and ball-milling for 15-24 hours by using a planetary ball mill at the rotating speed of 180-220 r/min to obtain mixed slurry; drying the mixed slurry, sieving the dried mixed slurry by a 200-mesh sieve, and then placing the sieved powder in a muffle furnace for calcining to obtain YAG raw material powder formed by gel casting; further weighing Al equivalent to the ceramic powder2O3Powder treatment to obtain Al for gel casting2O3Processing the raw material powder in the same way;
step 2, mixing deionized water, acrylamide, a cross-linking agent, a dispersing agent B, grinding balls and YAG raw material powder, performing ball milling, adjusting the pH value of the system to 9-11 by using a pH regulator, performing ball milling for 6-12 h, adding a plasticizer, and performing ball milling for 6-12 h to obtain YAG slurry with the solid content of 55-65 wt.%; preparing the solid content of 55-6 by the same method5 wt.% Al2O3A ceramic slurry;
step 3, respectively aligning YAG slurry and Al2O3Carrying out defoaming treatment on the ceramic slurry under the following treatment conditions: degassing for 2-5 min under a vacuum environment of-50 to-20 kPa; then YAG slurry and Al2O3Respectively pouring the ceramic slurry into a trough of a casting machine for casting, drying after complete gelation, and forming to obtain YAG single-layer biscuit and Al with the thickness of 0.08-0.4 mm2O3A single-layer biscuit;
step 4, mixing the prepared YAG single-layer biscuit with Al2O3The single-layer biscuit is staggered and laminated to obtain a tape-casting sheet, wherein the YAG single-layer biscuit and Al2O3Respectively stacking 3-8 layers of single-layer biscuit, wherein the total number of the obtained laminated layers of the composite tape-casting sheet is 6-16; placing the tape-casting sheet under 150-300 Mpa for warm isostatic pressing, and keeping the pressure for 1-10 min to obtain a biscuit, wherein the thickness of the biscuit is 0.48-6 mm;
and 5, placing the ceramic biscuit in a muffle furnace for glue discharging treatment, then placing the ceramic biscuit in a vacuum furnace for sintering, finally placing the ceramic biscuit in the muffle furnace for annealing and double-sided polishing to obtain the multilayer composite structure transparent ceramic.
Preferably, in step 1, the sintering aid is a mixture of magnesium oxide and ethyl orthosilicate, the addition amount of the sintering aid is 0.1 to 0.5 wt.% of the total mass of the ceramic powder, the dispersant a is polyetherimide, the addition amount of the dispersant a is 0.1 to 0.8 wt.% of the total mass of the ceramic powder, and the grinding balls are high-purity Al2O3The grinding ball and the ceramic powder are in a total mass ratio of 1-3: 1; the muffle furnace calcining temperature is 600-1000 DEG CoAnd C, keeping the temperature for 4-9 hours.
Preferably, in the step 2, the addition amount of the acrylamide is 2.5-5 wt.% of the mass of the ceramic powder; the cross-linking agent is any one of Ethylene Dimethacrylate (EDMA), diethylene glycol diacrylate (DEGDA) or N, N' -Methylene Bisacrylamide (MBAM), and the addition amount of the cross-linking agent is 1/10-1/15 of the total mass of the acrylamide; the dispersing agent B is any one of ammonium citrate, polyacrylic acid or polyethylene glycol, and the adding amount of the dispersing agent B is 0.2-0.5 wt% of the mass of the ceramic powder; the plasticizer is glycerol or ethylene glycol, and the adding amount of the plasticizer is 1-5 wt% of the mass of the ceramic powder; the pH regulator is ammonia water or tetramethyl ammonium hydroxide.
Preferably, the step 5 of removing the glue comprises the following specific steps: raising the temperature to 400-500 ℃ at the speed of 0.5-2 ℃/min at room temperature, preserving the heat for 4-8 h, raising the temperature to 800-900 ℃ at the speed of 0.5-2 ℃/min, and preserving the heat for 4-8 h.
Preferably, the vacuum sintering temperature in the step 5 is 1650-1870oC; the vacuum degree in the furnace chamber is kept at 10-3~10-4 Pa; the ceramic annealing atmosphere is air, and the annealing temperature is 1200-1600 DEGoC。
The application of the transparent ceramic with the multilayer composite structure in preparing a display panel.
Has the advantages that:
compared with the prior art, the preparation method and the application of the transparent ceramic with the multilayer composite structure have the following advantages:
1. al used in the present invention2O3The YAG layered composite ceramic material has different elastic modulus and linear expansion coefficient of each layer, so that macroscopic stress is generated among the layers, strain energy can be absorbed to the maximum extent when the surface is acted by external force, and cracks generate repeated deflection and inflection along the interface, so that the aims of improving the surface performance and the overall toughness are fulfilled. The idea of toughening the composite structure is adopted to prepare the Al2O3YAG multilayer composite ceramic sheet with fracture toughness up to 20 Mpa.m1/2The above.
2. Compared with organic tape casting and water-based tape casting, the gel tape casting technology for the transparent ceramic with the multilayer composite structure provided by the invention can greatly reduce the use amount of organic matters in slurry and improve the solid content of the slurry, so that the uniformity, density and strength of a biscuit are improved, and the light transmittance of the biscuit can reach more than 85% after vacuum sintering and polishing.
Drawings
FIG. 1 is a schematic structural diagram of a transparent ceramic with a multilayer composite structure obtained in example 2 of the present invention, 1-Al2O3Single-layer biscuit, 2-YAG single-layer biscuit, 3-stress, 4-crack;
FIG. 2 is a three-point bending resistance test chart of the transparent ceramic with a multilayer composite structure obtained in example 2 of the present invention;
FIG. 3 is a graph showing the transmittance of a transparent ceramic having a multilayer composite structure obtained in example 2 of the present invention.
Detailed Description
The present invention is further illustrated by the following examples, which should not be construed as limiting the scope of the invention. Unless otherwise stated, the starting materials used in the following examples are all commercially available products.
Example 1
A preparation method of a transparent ceramic with a multilayer composite structure comprises the following steps:
(1) according to Y3Al5O12Stoichiometric ratio of Y2O3Powder of Al2O3The total amount of the powder was 60 g. Absolute ethyl alcohol is used as a ball milling medium. Accurately weighed ceramic powder, polyetherimide, MgO and TEOS are respectively placed in a ball milling tank to be ball milled for 15 hours at a speed of 220 r/min, and mixed slurry which is evenly mixed is obtained. Drying the ball-milled slurry, sieving with 200 mesh sieve, placing in a muffle furnace at 600 deg.CoAnd calcining at the temperature of C to obtain YAG raw material powder for gel tape casting. Then, 60 g of Al is weighed in addition2O3Powder treatment to obtain Al for gel casting2O3Processing the raw material powder in the same way;
(2) deionized water, acrylamide, EDMA, ammonium citrate, YAG raw material powder and grinding balls are subjected to pH value adjustment to 9 by using tetramethylammonium hydroxide, ball milling is carried out for 6 hours, 0.6 g of plasticizer glycerol is added, and then ball milling is carried out for 6 hours, so that YAG slurry with the solid content of 55 wt.% is prepared; al having a solid content of 55 wt.% was prepared in the same manner2O3A ceramic slurry;
(3) respectively aligning YAG slurry and Al2O3Carrying out defoaming treatment on the ceramic slurry under the following treatment conditions: degassing for 2 min under a vacuum environment of-50 kPa; then YAG slurry and Al2O3The ceramic slurry being poured separately into casting machinesCasting in a trough, drying after complete gelation, and molding to obtain YAG single-layer biscuit and Al2O3A single-layer biscuit, the thickness of which is 0.08 mm;
(4) mixing the obtained YAG single-layer biscuit with Al2O3Carrying out staggered lamination on the single-layer biscuit to obtain 6 layers of casting sheets, and placing the casting sheets at 150 MPa to obtain a ceramic biscuit;
(5) and (3) placing the ceramic biscuit in a muffle furnace, heating to 400 ℃ at the speed of 0.5 ℃/min, preserving heat for 4 h, heating to 800 ℃ at the speed of 0.5 ℃/min, preserving heat for 4 h, and discharging the glue. The ceramic biscuit is then placed in a vacuum furnace at 1650oC, sintering at a vacuum degree of 10 in a furnace chamber-3Pa, finally placing the ceramic in a muffle furnace at 1200oAnd C, annealing. Double-side polishing, fracture toughness up to 20 Mpa.m1/2The light transmittance can reach 85%.
Example 2
A preparation method of a transparent ceramic with a multilayer composite structure comprises the following steps:
(1) according to Y3Al5O12Respectively weighing Y in the stoichiometric ratio of2O3Powder of Al2O3The total amount of the powder was 60 g. Absolute ethyl alcohol is used as a ball milling medium. Accurately weighed raw material powder, polyetherimide, MgO and TEOS are respectively placed in a ball milling tank to be ball milled for 20 hours at a speed of 200 r/min, and evenly mixed slurry is obtained. Drying the ball-milled slurry, sieving with 200 mesh sieve, placing in a muffle furnace at 800 deg.CoAnd calcining at the temperature of C to obtain YAG raw material powder for gel tape casting. Further, 60 g of Al was additionally weighed2O3Powder treatment to obtain Al for gel casting2O3Processing the raw material powder in the same way;
(2) deionized water, acrylamide, MBAM, ammonium citrate, YAG raw material powder and grinding balls are subjected to pH adjustment to 10 by ammonia water, after ball milling is carried out for 8 hours, 3 g of plasticizer ethylene glycol and 0.6 g of glycerol are added, and then ball milling is carried out for 10 hours, so that YAG slurry with the solid content of 60 wt.% is prepared; al having a solid content of 55 wt.% was prepared in the same manner2O3A ceramic slurry;
(3) respectively aligned to YAG slurryMaterial and Al2O3Carrying out defoaming treatment on the ceramic slurry under the following treatment conditions: degassing for 3 min under vacuum environment of-40 kPa; then YAG slurry and Al2O3Respectively pouring the ceramic slurry into a trough of a casting machine for casting, drying after complete gelation, and forming to obtain YAG single-layer biscuit and Al2O3A single-layer biscuit, the thickness of which is 0.2 mm;
(4) mixing the obtained YAG single-layer biscuit with Al2O3Carrying out staggered lamination on the single-layer biscuit to obtain cast sheets, wherein the number of the cast sheets is 12, and placing the cast sheets at 200 MPa to obtain a ceramic biscuit;
(5) and (3) placing the ceramic biscuit in a muffle furnace, heating to 450 ℃ at the speed of 1 ℃/min, preserving heat for 6 h, heating to 850 ℃ at the speed of 1 ℃/min, preserving heat for 6 h, and discharging the glue. The ceramic biscuit was then placed in a vacuum furnace at 1750oC, sintering at a vacuum degree of 10 in a furnace chamber-3Pa, finally placing the ceramic in a muffle furnace at 1400 DEG CoAnd C, annealing. Double-side polishing, fracture toughness up to 21 Mpa.m1/2The light transmittance can reach 88%.
FIG. 2 is a three-point bending resistance test object diagram of the composite ceramic, which is uniform in whole and has better strength and toughness.
FIG. 3 is Al2O3YAG is a multilayer composite ceramic transmittance graph.
Example 3
A preparation method of a transparent ceramic with a multilayer composite structure comprises the following steps:
(1) according to Y3Al5O12Respectively weighing Y in the stoichiometric ratio of2O3Powder of Al2O3The total amount of the powder was 60 g. Absolute ethyl alcohol is used as a ball milling medium. Accurately weighed raw material powder, polyetherimide, MgO and TEOS are respectively placed in a ball milling tank to be ball milled for 24 hours at 180 r/min, and evenly mixed slurry is obtained. Drying the ball-milled slurry, sieving with 200 mesh sieve, placing in a muffle furnace at 800 deg.CoAnd calcining at the temperature of C to obtain YAG raw material powder for gel tape casting. Further, 60 g of Al was additionally weighed2O3Powder treatment to obtain Al for gel casting2O3Processing the raw material powder in the same way;
(2) deionized water, acrylamide, DEGDA, polyethylene glycol, YAG raw material powder and grinding balls are subjected to pH value adjustment to 11 by using tetramethylammonium hydroxide, 3 g of plasticizer ethylene glycol is added after ball milling for 12 h, and then ball milling is carried out for 12 h to prepare YAG slurry with the solid content of 65 wt.%; al having a solid content of 65 wt.% was prepared in the same manner2O3A ceramic slurry;
(3) respectively aligning YAG slurry and Al2O3Carrying out defoaming treatment on the ceramic slurry under the following treatment conditions: degassing for 2 min under a vacuum environment of-50 kPa; then YAG slurry and Al2O3Respectively pouring the ceramic slurry into a trough of a casting machine for casting, drying after complete gelation, and forming to obtain YAG single-layer biscuit and Al2O3A single-layer biscuit, the thickness of which is 0.4 mm;
(4) mixing the obtained YAG single-layer biscuit with Al2O3Carrying out staggered lamination on the single-layer biscuit to obtain 16 layers of casting sheets, and placing the casting sheets at the temperature of 300 MPa and the like to obtain a ceramic biscuit;
(5) and (3) placing the ceramic biscuit in a muffle furnace, heating to 500 ℃ at the speed of 2 ℃/min, preserving heat for 8 h, heating to 900 ℃ at the speed of 2 ℃/min, preserving heat for 8 h, and discharging the glue. The ceramic biscuit is then placed in a vacuum furnace at 1870oC, sintering at a vacuum degree of 10 in a furnace chamber-4Pa, finally placing the ceramic in a muffle furnace at 1600 DEG CoAnd C, annealing. Double-side polishing, fracture toughness up to 20.5 Mpa.m1/2The light transmittance can reach 87%.
The above description is only a preferred embodiment of the present invention, and the scope of the present invention is not limited thereto, and any simple modifications or equivalent substitutions of the technical solutions that can be obviously obtained by those skilled in the art within the technical scope of the present invention are within the scope of the present invention.

Claims (6)

1. The preparation method of the transparent ceramic with the multilayer composite structure is characterized in that Al is prepared by a gel casting forming method2O3YAG multilayer composite structure ceramicThe method comprises the following steps:
step 1, according to the chemical formula Y3Al5O12The stoichiometric ratio of each element in (A) is measured by weighing Y2O3Powder of Al2O3The powder is used as ceramic powder; mixing the weighed ceramic powder, sintering aid, dispersant A, grinding balls and absolute ethyl alcohol, and ball-milling for 15-24 hours by using a planetary ball mill at the rotating speed of 180-220 r/min to obtain mixed slurry; drying the mixed slurry, sieving the dried mixed slurry by a 200-mesh sieve, and then placing the sieved powder in a muffle furnace for calcining to obtain YAG raw material powder formed by gel casting; further weighing Al equivalent to the ceramic powder2O3Powder treatment to obtain Al for gel casting2O3Processing the raw material powder in the same way;
step 2, mixing deionized water, acrylamide, a cross-linking agent, a dispersing agent B, grinding balls and YAG raw material powder, performing ball milling, adjusting the pH value of the system to 9-11 by using a pH regulator, performing ball milling for 6-12 h, adding a plasticizer, and performing ball milling for 6-12 h to obtain YAG slurry with the solid content of 55-65 wt.%; preparing Al with the solid content of 55-65 wt.% according to the same method2O3A ceramic slurry;
step 3, respectively aligning YAG slurry and Al2O3Carrying out defoaming treatment on the ceramic slurry under the following treatment conditions: degassing for 2-5 min under a vacuum environment of-50 to-20 kPa; then YAG slurry and Al2O3Respectively pouring the ceramic slurry into a trough of a casting machine for casting, drying after complete gelation, and forming to obtain YAG single-layer biscuit and Al with the thickness of 0.08-0.4 mm2O3A single-layer biscuit;
step 4, mixing the prepared YAG single-layer biscuit with Al2O3The single-layer biscuit is staggered and laminated to obtain a tape-casting sheet, wherein the YAG single-layer biscuit and Al2O3Respectively stacking 3-8 layers of single-layer biscuit, wherein the total number of the obtained laminated layers of the composite tape-casting sheet is 6-16; placing the tape-casting sheet under 150-300 Mpa for warm isostatic pressing, and keeping the pressure for 1-10 min to obtain a biscuit, wherein the thickness of the biscuit is 0.48-6 mm;
and 5, placing the ceramic biscuit in a muffle furnace for glue discharging treatment, then placing the ceramic biscuit in a vacuum furnace for sintering, finally placing the ceramic biscuit in the muffle furnace for annealing and double-sided polishing to obtain the multilayer composite structure transparent ceramic.
2. The method for preparing the transparent ceramic with the multilayer composite structure according to claim 1, wherein in the step 1, the sintering aid is a mixture of magnesium oxide and ethyl orthosilicate, the addition amount of the sintering aid is 0.1-0.5 wt% of the total mass of the ceramic powder, the dispersant A is polyetherimide, the addition amount of the dispersant A is 0.1-0.8 wt% of the total mass of the ceramic powder, and the grinding balls are high-purity Al2O3The grinding ball and the ceramic powder are in a total mass ratio of 1-3: 1; the muffle furnace calcining temperature is 600-1000 DEG CoAnd C, keeping the temperature for 4-9 hours.
3. The method for preparing the transparent ceramic with the multilayer composite structure according to claim 1, wherein in the step 2, the addition amount of the acrylamide is 2.5-5 wt.% of the mass of the ceramic powder; the cross-linking agent is any one of ethyl dimethacrylate, diethylene glycol diacrylate or N, N' -methylene bisacrylamide, and the addition amount of the cross-linking agent is 1/10-1/15 of the total mass of the acrylamide; the dispersing agent B is any one of ammonium citrate, polyacrylic acid or polyethylene glycol, and the adding amount of the dispersing agent B is 0.2-0.5 wt% of the mass of the ceramic powder; the plasticizer is glycerol or ethylene glycol, and the adding amount of the plasticizer is 1-5 wt% of the mass of the ceramic powder; the pH regulator is ammonia water or tetramethyl ammonium hydroxide.
4. The method for preparing the transparent ceramic with the multilayer composite structure according to claim 1, wherein the step 5 of removing the glue comprises the following specific steps: raising the temperature to 400-500 ℃ at the speed of 0.5-2 ℃/min at room temperature, preserving the heat for 4-8 h, raising the temperature to 800-900 ℃ at the speed of 0.5-2 ℃/min, and preserving the heat for 4-8 h.
5. The method of claim 1, wherein the ceramic is a multilayer composite structure transparent ceramicIn the step 5, the vacuum sintering temperature is 1650-1870oC; the vacuum degree in the furnace chamber is kept at 10-3~10-4 Pa; the ceramic annealing atmosphere is air, and the annealing temperature is 1200-1600 DEGoC。
6. Use of a transparent ceramic based on a multilayer composite structure according to any of claims 1 to 5 for the production of display panels.
CN202011113149.2A 2020-10-17 2020-10-17 Preparation method and application of transparent ceramic with multilayer composite structure Active CN112174668B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202011113149.2A CN112174668B (en) 2020-10-17 2020-10-17 Preparation method and application of transparent ceramic with multilayer composite structure

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202011113149.2A CN112174668B (en) 2020-10-17 2020-10-17 Preparation method and application of transparent ceramic with multilayer composite structure

Publications (2)

Publication Number Publication Date
CN112174668A CN112174668A (en) 2021-01-05
CN112174668B true CN112174668B (en) 2022-04-01

Family

ID=73950710

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202011113149.2A Active CN112174668B (en) 2020-10-17 2020-10-17 Preparation method and application of transparent ceramic with multilayer composite structure

Country Status (1)

Country Link
CN (1) CN112174668B (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113149631B (en) * 2021-01-20 2022-06-07 江苏师范大学 Method for preparing YAG transparent ceramic by colloidal state curing molding
CN113716951B (en) * 2021-08-26 2022-04-29 新沂市锡沂高新材料产业技术研究院有限公司 Preparation method of YAG-based transparent ceramic with large-size sheet composite structure
CN116177995B (en) * 2022-09-07 2024-03-12 中国科学院上海硅酸盐研究所 Preparation method of fluorescent ceramic based on 3D printing composite structure

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6013592A (en) * 1998-03-27 2000-01-11 Siemens Westinghouse Power Corporation High temperature insulation for ceramic matrix composites
WO2002000409A2 (en) * 2000-06-29 2002-01-03 Cook Composites And Polymers Company, Inc. Curing of a gel coat on a mold
CN102011215A (en) * 2010-10-15 2011-04-13 陕西理工学院 Process for preparing yttrium aluminum garnet-based continuous fibers through sol-gel method
WO2011097137A1 (en) * 2010-02-04 2011-08-11 Nitto Denko Corporation Light emissive ceramic laminate and method of making same
CN103508729A (en) * 2012-06-19 2014-01-15 中国科学院上海硅酸盐研究所 Method for preparing yttrium aluminum garnet-based transparent ceramic through aqueous tape casting
CN104725052A (en) * 2014-12-18 2015-06-24 徐州市江苏师范大学激光科技有限公司 Preparation method of multilayer composite structured transparent ceramic
WO2020173151A1 (en) * 2019-02-26 2020-09-03 中国科学院上海硅酸盐研究所 Method for preparing amorphous oxide ceramic composite coating simultaneously having toughness, thermal conductivity and high-temperature structural stability
CN112389039A (en) * 2020-11-02 2021-02-23 宁波伏尔肯科技股份有限公司 Preparation method of high-strength and high-toughness layered complex-phase ceramic

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6013592A (en) * 1998-03-27 2000-01-11 Siemens Westinghouse Power Corporation High temperature insulation for ceramic matrix composites
WO2002000409A2 (en) * 2000-06-29 2002-01-03 Cook Composites And Polymers Company, Inc. Curing of a gel coat on a mold
WO2011097137A1 (en) * 2010-02-04 2011-08-11 Nitto Denko Corporation Light emissive ceramic laminate and method of making same
CN102011215A (en) * 2010-10-15 2011-04-13 陕西理工学院 Process for preparing yttrium aluminum garnet-based continuous fibers through sol-gel method
CN103508729A (en) * 2012-06-19 2014-01-15 中国科学院上海硅酸盐研究所 Method for preparing yttrium aluminum garnet-based transparent ceramic through aqueous tape casting
CN104725052A (en) * 2014-12-18 2015-06-24 徐州市江苏师范大学激光科技有限公司 Preparation method of multilayer composite structured transparent ceramic
WO2020173151A1 (en) * 2019-02-26 2020-09-03 中国科学院上海硅酸盐研究所 Method for preparing amorphous oxide ceramic composite coating simultaneously having toughness, thermal conductivity and high-temperature structural stability
CN112389039A (en) * 2020-11-02 2021-02-23 宁波伏尔肯科技股份有限公司 Preparation method of high-strength and high-toughness layered complex-phase ceramic

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
"A1203(YAG)/LaP04层状陶瓷复合材料研究";仝建峰等;《航空材料学报》;20060630;第163-164页 *
"Oxidation Resistance of Double-Ceramic-Layered Thermal Barrier Coating System with an Intermediate Al2O3-YAG Layer";Saemi, H等;《JOURNAL OF THERMAL SPRAY TECHNOLOGY》;20210430;第1049-1058页 *

Also Published As

Publication number Publication date
CN112174668A (en) 2021-01-05

Similar Documents

Publication Publication Date Title
CN112174668B (en) Preparation method and application of transparent ceramic with multilayer composite structure
CN111253153A (en) Method for preparing toughened large-size ultrathin YAG transparent ceramic biscuit based on Isodam gel system
CN100503507C (en) Low temperature sintered 99 aluminium oxide ceramic and its production method and use
CN106966709B (en) Method for preparing transparent alumina ceramic through 3D printing based on photocuring molding
CN107721424B (en) Method for preparing YAG transparent ceramic by gel casting
CN101671179B (en) High strength and high wear-resistance zirconium-aluminum-silicon composite self-release glazed ceramic material and manufacture method thereof
CN108516818A (en) A method of YAG crystalline ceramics is prepared based on improved Isobam gel rubber systems
CN112939582B (en) Zirconia-doped alumina ceramic and preparation method thereof
CN111170726B (en) Method for preparing uniform YAG transparent ceramic biscuit based on AM gel casting
CN111533540A (en) Preparation method of alumina ceramic with complex shape
CN104591709A (en) High-strength magnesia porcelain ultrathin plate and preparation method thereof
CN112279650A (en) Preparation method of high-density silicon carbide ceramic composite material
CN113716951A (en) Preparation method of YAG-based transparent ceramic with large-size sheet composite structure
CN114702321A (en) Sintering process of tape-casting alumina sheet
CN114853467B (en) ITO planar target and preparation method thereof
CN113045310B (en) Method for preparing lanthanum gadolinium zirconate transparent ceramic by AM gel casting process
CN113880563B (en) High-temperature creep-resistant ceramic material and preparation method thereof
CN115636672A (en) Tape casting production method of large-size AlON transparent ceramic
CN113997681A (en) Method for improving shock resistance of thin ceramic plate
CN104628376A (en) Centrifugal forming method for preparing transparent ceramic laser bar
CN117417187B (en) Preparation method of solid electrolyte casting film
CN115611619B (en) Ceramic material for temperature controller and preparation method thereof
CN112851375A (en) Binder for preparing zirconium oxide grinding beads
CN116874304B (en) Ceramic material with high heat dissipation performance and preparation method and application thereof
CN114890678B (en) Large-size low-expansion glass-based composite material and slip casting 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
GR01 Patent grant
GR01 Patent grant