CN111362692A - High-strength multilayer ceramic co-fired structure and preparation method thereof - Google Patents
High-strength multilayer ceramic co-fired structure and preparation method thereof Download PDFInfo
- Publication number
- CN111362692A CN111362692A CN202010292960.5A CN202010292960A CN111362692A CN 111362692 A CN111362692 A CN 111362692A CN 202010292960 A CN202010292960 A CN 202010292960A CN 111362692 A CN111362692 A CN 111362692A
- Authority
- CN
- China
- Prior art keywords
- layer
- alumina
- powder
- zirconia
- parts
- 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
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
- C04B35/48—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 zirconium or hafnium oxides, zirconates, zircon or hafnates
-
- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
-
- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
- C04B41/90—Coating or impregnation for obtaining at least two superposed coatings having different compositions at least one coating being a metal
-
- 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
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
-
- 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
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5445—Particle size related information expressed by the size of the particles or aggregates thereof submicron sized, i.e. from 0,1 to 1 micron
-
- 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
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
- C04B2235/6025—Tape casting, e.g. with a doctor blade
-
- 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
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/612—Machining
-
- 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
-
- 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
- C04B2235/6583—Oxygen containing atmosphere, e.g. with changing oxygen pressures
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Laminated Bodies (AREA)
Abstract
The invention relates to the field of ceramic chips, in particular to a high-strength multilayer ceramic co-fired structure and a preparation method thereof. The ceramic co-firing structure comprises a first alumina layer, a second alumina layer and a zirconium oxide layer, wherein the zirconium oxide layer is fixed between the first alumina layer and the second alumina layer; the aluminum oxide layer I and the aluminum oxide layer II are respectively composed of the following components in parts by weight: 100 parts of alumina powder, 0-0.4 part of zirconium dioxide powder and 0-0.6 part of silicon dioxide powder; the zirconia layer comprises the following components in parts by weight: 100 parts of 5YSZ zirconia powder and 3-10 parts of alumina powder. The invention comprises a first alumina layer and a second alumina layer on the surface layers of the upper surface and the lower surface, and a zirconium oxide layer in the middle. On the basis of optimizing the components of the zirconia layer, the defect proportion in the chip is reduced and the strength and the toughness are improved by optimizing the structure of the multilayer co-fired ceramic and the sintering process.
Description
Technical Field
The invention relates to the field of ceramic chips, in particular to a high-strength multilayer ceramic co-fired structure and a preparation method thereof.
Background
The alumina-zirconia multilayer co-fired ceramic chip can be used for structural devices, and mainly utilizes the high strength and toughness of the chip; the gas sensitive property of the zirconium oxide can also be utilized for functional devices, such as an oxygen sensor sensing chip for a vehicle and the like. The ceramic induction chip of the integrated chip oxygen sensor mentioned in the previous patent ZL201010147931.6 adopts an alumina-zirconia co-firing process, and the bonding position is limited to the bottom plane and is used for integrating the heating circuit. The chip design and the method have high requirements on the shrinkage characteristic and the sintering characteristic of an alumina and zirconia material system, and the chip is easy to bend or crack due to mismatching of the sintering shrinkage characteristic, so that the product assembly and the strength characteristic of the chip are influenced.
Disclosure of Invention
In order to overcome the defect that the conventional ceramic chip is easy to bend and crack, the invention provides a high-strength multilayer ceramic co-fired structure and a preparation method thereof.
The technical scheme adopted by the invention for solving the technical problems is as follows: a high-strength multilayer ceramic co-fired structure comprises a first alumina layer, a second alumina layer and a zirconium oxide layer, wherein the zirconium oxide layer is fixed between the first alumina layer and the second alumina layer;
the aluminum oxide layer I and the aluminum oxide layer II are respectively composed of the following components in parts by weight: 100 parts of alumina powder, 0-0.4 part of zirconium dioxide powder and 0-0.6 part of silicon dioxide powder;
the zirconia layer comprises the following components in parts by weight: 100 parts of 5YSZ zirconia powder and 3-10 parts of alumina powder.
According to another embodiment of the invention, the aluminum oxide layer I and the aluminum oxide layer II are both composed of the following components in parts by weight: 100 parts of alumina powder;
the zirconia layer comprises the following components in parts by weight: 100 parts of 5YSZ zirconia powder and 6 parts of alumina powder.
According to another embodiment of the invention, the aluminum oxide layer I and the aluminum oxide layer II are both composed of the following components in parts by weight: 100 parts of alumina powder, 0.4 part of zirconium dioxide powder and 0.2 part of silicon dioxide powder;
the zirconia layer comprises the following components in parts by weight: 100 parts of 5YSZ zirconia powder and 4 parts of alumina powder.
According to another embodiment of the present invention, the purity of the alumina powder further including the alumina layer one and the alumina layer two is 99.7%, and the particle size of the alumina powder of the alumina layer one and the alumina layer two is 0.3 to 0.5 μm;
the purity of the alumina powder of the zirconia layer is 99.7%, and the particle size of the alumina powder of the zirconia layer is 0.3-1 μm.
According to another embodiment of the present invention, the method further comprises a step of setting a thickness ratio of the first alumina layer to the second alumina layer to be 1: 0.6-1: 1.5, the thickness ratio of the first alumina layer to the first zirconia layer is 1: 20-1:50
A preparation method of a high-strength multilayer ceramic co-fired structure comprises the following steps:
A. firstly, mixing 5YSZ zirconia powder and alumina powder according to a ratio, performing ball milling to prepare slurry, then performing tape casting molding, naturally drying to prepare a green tape, and then laminating 3 layers of the green tape into a zirconia layer by using a mold;
B. preparing alumina slurry for screen printing from alumina powder, zirconia powder and silicon dioxide powder according to a ratio, and then screen printing the slurry on two surfaces of a zirconia layer to form an alumina layer I and an alumina layer II;
C. and finally, sintering the alumina layer I, the alumina layer II and the zirconia layer for 1-3 hours at 1300-1550 ℃ in an air environment to obtain the flat multilayer co-fired ceramic chip.
According to another embodiment of the invention, further comprising step a, the green tape thickness is 0.3-0.5 mm; the length of the zirconia blank is 20-40 mm, the width is 3-4 mm, and the thickness is 1.0 mm.
According to another embodiment of the present invention, the method further comprises a step B, wherein the temperature in the air environment is 1400 ℃ to 1450 ℃, and the sintering time is 2 hours.
The invention has the beneficial effects that the aluminum oxide coating comprises an aluminum oxide layer I and an aluminum oxide layer II on the surface layers of the upper surface and the lower surface, and a zirconium oxide layer in the middle. On the basis of optimizing the components of the zirconia layer, the defect proportion in the chip is reduced and the strength and the toughness are improved by optimizing the structure of the multilayer co-fired ceramic and the sintering process.
Drawings
The invention is further illustrated with reference to the following figures and examples.
FIG. 1 is a schematic structural view of the invention;
in the figure, 1, an alumina layer I, 2, an alumina layer II and 3, a zirconia layer.
Detailed Description
Fig. 1 is a schematic structural diagram of the invention. The technical scheme adopted by the invention for solving the technical problems is as follows:
a high-strength multilayer ceramic co-fired structure comprises a first alumina layer, a second alumina layer and a zirconium oxide layer, wherein the zirconium oxide layer is fixed between the first alumina layer and the second alumina layer;
the aluminum oxide layer I and the aluminum oxide layer II are respectively composed of the following components in parts by weight: 100 parts of alumina powder, 0-0.4 part of zirconium dioxide powder and 0-0.6 part of silicon dioxide powder;
the zirconia layer comprises the following components in parts by weight: 100 parts of 5YSZ zirconia powder and 3-10 parts of alumina powder.
The aluminum oxide layer I and the aluminum oxide layer II are respectively composed of the following components in parts by weight: 100 parts of alumina powder;
the zirconia layer comprises the following components in parts by weight: 100 parts of 5YSZ zirconia powder and 6 parts of alumina powder.
The aluminum oxide layer I and the aluminum oxide layer II are respectively composed of the following components in parts by weight: 100 parts of alumina powder, 0.4 part of zirconium dioxide powder and 0.2 part of silicon dioxide powder;
the zirconia layer comprises the following components in parts by weight: 100 parts of 5YSZ zirconia powder and 4 parts of alumina powder.
The purity of the alumina powder of the alumina layer I and the alumina layer II is 99.7 percent, and the granularity of the alumina powder of the alumina layer I and the alumina layer II is 0.3-0.5 mu m;
the purity of the alumina powder of the zirconia layer is 99.7%, and the particle size of the alumina powder of the zirconia layer is 0.3-1 μm.
The thickness ratio of the first alumina layer to the second alumina layer is 1: 0.6-1: 1.5, the thickness ratio of the first alumina layer to the first zirconia layer is 1: 20-1:50
A preparation method of a high-strength multilayer ceramic co-fired structure comprises the following steps:
A. firstly, mixing 5YSZ zirconia powder and alumina powder according to a ratio, performing ball milling to prepare slurry, then performing tape casting molding, naturally drying to prepare a green tape, and then laminating 3 layers of the green tape into a zirconia layer by using a mold;
B. preparing alumina slurry for screen printing from alumina powder, zirconia powder and silicon dioxide powder according to a ratio, and then screen printing the slurry on two surfaces of a zirconia layer to form an alumina layer I and an alumina layer II;
C. and finally, sintering the alumina layer I, the alumina layer II and the zirconia layer for 1-3 hours at 1300-1550 ℃ in an air environment to obtain the flat multilayer co-fired ceramic chip.
In the step A, the thickness of the green tape is 0.3-0.5 mm; the length of the zirconia blank is 20-40 mm, the width is 3-4 mm, and the thickness is 1.0 mm.
In the step B, in the step C, the temperature is 1400-1450 ℃ in the air environment, and the sintering time is 2 hours.
And (4) optimizing the zirconium oxide composition. Because the alumina and zirconia materials have different sintering characteristics, the materials can be deformed due to the unmatched shrinkage when directly co-fired; therefore, different doping needs to be carried out on the alumina powder and the zirconia powder to adjust the shrinkage characteristics of the alumina powder and the zirconia powder, so that the sintering shrinkage tends to be consistent as much as possible. The alumina powder can properly reduce the shrinkage mismatch condition by doping zirconia powder and silica powder and doping alumina with proper proportion and granularity (0.3-1 mu m) in a zirconia layer.
As shown in figure 1, the relative thicknesses of the alumina layer I1, the alumina layer II 2 and the zirconia layer 3 are designed. According to the invention, the alumina layer I1 and the alumina layer II 2 are respectively arranged on two sides of the zirconia layer 3, so that a 3-layer symmetrical structure is formed. The treatment is beneficial to reducing the shrinkage difference of different materials in the multi-layer ceramic co-firing, thereby improving the straightness of the product and the stability of the strength; in addition, due to the difference of sintering driving forces of the alumina and the zirconia, compressive stress is formed in the surface layer alumina, so that the bending strength and the fracture toughness of the whole chip are improved. The key point is that the relative thicknesses of the zirconia layer 3, the alumina layer I1 and the alumina layer II 2 are not effective if the alumina layer I1 and the alumina layer II 2 are too thin; when the thickness of the alumina layer one 1 and the alumina layer two 2 is too large, reverse bending is caused. The range we have determined experimentally and computationally is: the thickness of the first alumina layer 1 and the second alumina layer 2 on the two sides is 0.02-0.06mm, and the thickness of the middle zirconia layer 3 is 0.8-1.0 mm. The thickness ratio within this range, in combination with a suitable sintering process, can achieve high strength and stability of the final product. In summary, the invention can be used as a basic frame of a high-temperature gas sensor chip structure, and can be directly used as a high-temperature gas sensor chip by combining with specific designs such as a sensitive electrode, a diffusion channel and the like.
The first embodiment is as follows:
preparation of zirconia layer 3: the method comprises the steps of doping 6 parts of alumina powder (99.7% purity alumina, granularity 0.3-1 mu m) into 100 parts of 5YSZ zirconia powder, mixing and ball-milling to prepare slurry, then carrying out tape casting forming through a double-knife-edge technology, naturally drying to prepare a green belt with the thickness of 0.3mm, and then stamping 3 layers of green belts into a zirconia blank with the thickness of 1.0mm (length and width: 20-40 mm) through a die. Before lamination, the multilayer green tape can be screen-printed with appropriate Pt lines, diffusion gaps, air channels and the like to meet the requirements of gas detection performance.
Preparation of alumina layer one 1 and alumina layer two 2: alumina powder of 99.7% purity having a particle size of 0.3 to 0.5 μm was prepared into alumina slurry for screen printing. Forming an alumina insulating layer (containing a Pt heating circuit) and an alumina covering layer on the other side on the surface of the zirconia blank by screen printing; the thickness of the insulating layer was 30 μm and the thickness of the covering layer was 20 μm. The alumina layer I1 or the alumina layer II 2 is provided with a Pt heating circuit which is an alumina insulating layer, and the alumina covering layer without the Pt heating circuit.
Co-firing the multilayer ceramic structure: sintering at 1300-1550 ℃ for 1-3 hours in an air environment to obtain the flat multilayer co-fired ceramic chip. The three-point bending strength mean value of 20 chips is 900MPa, and the Weibull modulus is 13.
Example two:
preparation of zirconia layer 3: after 100 parts of 5YSZ zirconia powder is doped with 4 parts of alumina powder (alumina with the purity of 99.7 percent and the granularity of 0.3-1 mu m), the mixture is prepared into slurry through sanding-ball milling, then the slurry is cast and molded through a double-knife-edge technology, a green belt with the thickness of 0.5mm is prepared after natural drying, and then 2 layers of green belts are punched into a zirconia blank with the thickness of 0.9mm (the length and width are 20-40 mm) through a die. The multilayer green tape is screen printed with appropriate Pt wiring, diffusion gaps, air channels, etc. prior to lamination to meet the requirements for gas detection performance.
Preparation of alumina layer one 1 and alumina layer two 2: on the basis of 100 parts of alumina powder (granularity is 0.3-0.5 mu m, purity is 99.7%), 0.4 part of zirconia powder and 0.2 part of silicon dioxide powder (granularity is about 0.3 mu m) are doped, the doping process is realized by chemical deposition on the surface of the alumina powder, and the alumina slurry for screen printing is prepared. Forming an alumina insulating layer (containing a Pt heating circuit) and an alumina covering layer on the other side on the surface of the zirconia blank by screen printing; the thickness of the insulating layer is 60 μm, and the thickness of the covering layer is 40 μm. The alumina layer I1 or the alumina layer II 2 is provided with a Pt heating circuit which is an alumina insulating layer, and the alumina covering layer without the Pt heating circuit.
Co-firing the multilayer ceramic structure: sintering at 1400-1450 deg.c for 2 hr in air environment to obtain flat multilayer co-fired ceramic chip. The three-point bending strength mean value of 16 chips is 800MPa, and the Weibull modulus is 15.
Claims (8)
1. A high-strength multilayer ceramic co-fired structure is characterized by comprising a first alumina layer (1), a second alumina layer (2) and a zirconia layer (3), wherein the zirconia layer (3) is fixed between the first alumina layer (1) and the second alumina layer (2);
the aluminum oxide layer I (1) and the aluminum oxide layer II (2) are respectively composed of the following components in parts by weight: 100 parts of alumina powder, 0-0.4 part of zirconium dioxide powder and 0-0.6 part of silicon dioxide powder;
the zirconia layer (3) consists of the following components in parts by weight: 100 parts of 5YSZ zirconia powder and 3-10 parts of alumina powder.
2. The high-strength multilayer ceramic co-fired structure of claim 1, wherein the first alumina layer (1) and the second alumina layer (2) are composed of the following components in parts by weight: 100 parts of alumina powder;
the zirconia layer (3) consists of the following components in parts by weight: 100 parts of 5YSZ zirconia powder and 6 parts of alumina powder.
3. The high-strength multilayer ceramic co-fired structure of claim 1, wherein the first alumina layer (1) and the second alumina layer (2) are composed of the following components in parts by weight: 100 parts of alumina powder, 0.4 part of zirconium dioxide powder and 0.2 part of silicon dioxide powder;
the zirconia layer (3) consists of the following components in parts by weight: 100 parts of 5YSZ zirconia powder and 4 parts of alumina powder.
4. The high strength multi-layer ceramic co-fired structure according to any one of claims 1 to 3, wherein the alumina powder of the alumina layer I (1) and the alumina layer II (2) has a purity of 99.7%, and the alumina powder of the alumina layer I (1) and the alumina layer II (2) has a particle size of 0.3-0.5 μm;
the purity of the alumina powder of the zirconia layer (3) is 99.7%, and the particle size of the alumina powder of the zirconia layer (3) is 0.3-1 μm.
5. The high strength multi-layer ceramic co-fired structure according to any one of claims 1 to 3, wherein the thickness ratio of the alumina layer I (1) to the alumina layer II (2) is 1: 0.6-1: 1.5, the thickness ratio of the first alumina layer (1) to the zirconia layer (3) is 1: 20-1:50.
6. The method for preparing a high-strength multilayer ceramic co-fired structure according to any one of claims 1 to 3, characterized in that the method comprises the steps of:
A. firstly, mixing 5YSZ zirconia powder and alumina powder according to a ratio, performing ball milling to prepare slurry, then performing tape casting molding, naturally drying to prepare a green tape, and then laminating 3 layers of the green tape into a zirconia layer (3) by using a mold;
B. preparing alumina slurry for screen printing from alumina powder, zirconia powder and silicon dioxide powder according to a ratio, and then screen printing the slurry on two surfaces of a zirconia layer (3) to form an alumina layer I (1) and an alumina layer II (2);
C. and finally, sintering the alumina layer I (1), the alumina layer II (2) and the zirconia layer (3) for 1-3 hours at 1300-1550 ℃ in an air environment to obtain the flat multi-layer co-fired ceramic chip.
7. The method according to claim 6, wherein in step A, the green tape has a thickness of 0.3-0.5 mm; the length of the zirconia blank is 20-40 mm, the width is 3-4 mm, and the thickness is 1.0 mm.
8. The method according to claim 6, wherein in step B, the temperature in air environment is 1400-1450 ℃, and the sintering time is 2 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010292960.5A CN111362692A (en) | 2020-04-15 | 2020-04-15 | High-strength multilayer ceramic co-fired structure and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010292960.5A CN111362692A (en) | 2020-04-15 | 2020-04-15 | High-strength multilayer ceramic co-fired structure and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111362692A true CN111362692A (en) | 2020-07-03 |
Family
ID=71203305
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010292960.5A Pending CN111362692A (en) | 2020-04-15 | 2020-04-15 | High-strength multilayer ceramic co-fired structure and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111362692A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112010648A (en) * | 2020-09-11 | 2020-12-01 | 东莞理工学院 | Preparation method of high-density zirconia ceramic |
| CN114736005A (en) * | 2022-03-14 | 2022-07-12 | 中国电子科技集团公司第四十三研究所 | Tungsten metallization-multilayer alumina black porcelain substrate and preparation method thereof |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101045625A (en) * | 2007-03-13 | 2007-10-03 | 广东风华高新科技集团有限公司 | Manufacturing method of composite ceramic plate and composit ceramic |
| CN101806768A (en) * | 2010-04-16 | 2010-08-18 | 常州联德电子有限公司 | Integrated chip type oxygen sensor and manufacturing method thereof |
| CN105330268A (en) * | 2015-12-03 | 2016-02-17 | 广东工业大学 | Manufacturing method of laminated ceramics |
| CN105459516A (en) * | 2014-08-28 | 2016-04-06 | 比亚迪股份有限公司 | Ceramic substrate and preparation method thereof, and power module |
| CN105732008A (en) * | 2016-02-17 | 2016-07-06 | 同济大学 | Co-firing method and application of laminated type zirconium oxide and aluminium oxide ceramic |
| CN107266067A (en) * | 2017-06-14 | 2017-10-20 | 东莞华晶粉末冶金有限公司 | A kind of layered composite ceramic plate, preparation method and mobile terminal device |
| CN207108835U (en) * | 2017-06-14 | 2018-03-16 | 东莞华晶粉末冶金有限公司 | A kind of layered composite ceramic plate and mobile terminal device |
| CN108760822A (en) * | 2018-06-06 | 2018-11-06 | 成都科锐传感技术有限公司 | A kind of chip oxygen sensor and preparation method thereof containing two parts zirconia structure |
-
2020
- 2020-04-15 CN CN202010292960.5A patent/CN111362692A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101045625A (en) * | 2007-03-13 | 2007-10-03 | 广东风华高新科技集团有限公司 | Manufacturing method of composite ceramic plate and composit ceramic |
| CN101806768A (en) * | 2010-04-16 | 2010-08-18 | 常州联德电子有限公司 | Integrated chip type oxygen sensor and manufacturing method thereof |
| CN105459516A (en) * | 2014-08-28 | 2016-04-06 | 比亚迪股份有限公司 | Ceramic substrate and preparation method thereof, and power module |
| CN105330268A (en) * | 2015-12-03 | 2016-02-17 | 广东工业大学 | Manufacturing method of laminated ceramics |
| CN105732008A (en) * | 2016-02-17 | 2016-07-06 | 同济大学 | Co-firing method and application of laminated type zirconium oxide and aluminium oxide ceramic |
| CN107266067A (en) * | 2017-06-14 | 2017-10-20 | 东莞华晶粉末冶金有限公司 | A kind of layered composite ceramic plate, preparation method and mobile terminal device |
| CN207108835U (en) * | 2017-06-14 | 2018-03-16 | 东莞华晶粉末冶金有限公司 | A kind of layered composite ceramic plate and mobile terminal device |
| CN108760822A (en) * | 2018-06-06 | 2018-11-06 | 成都科锐传感技术有限公司 | A kind of chip oxygen sensor and preparation method thereof containing two parts zirconia structure |
Non-Patent Citations (1)
| Title |
|---|
| 陈蓓: "Al2O3/ZrO2层状复合陶瓷组织控制及工艺优化", 《中国学术期刊（光盘版）》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112010648A (en) * | 2020-09-11 | 2020-12-01 | 东莞理工学院 | Preparation method of high-density zirconia ceramic |
| CN114736005A (en) * | 2022-03-14 | 2022-07-12 | 中国电子科技集团公司第四十三研究所 | Tungsten metallization-multilayer alumina black porcelain substrate and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US7691469B2 (en) | Ceramic multilayer substrate and method for manufacturing the same | |
| US11866370B2 (en) | Grain-grade zirconia toughened alumina ceramic substrate and method for preparing the same | |
| KR101290089B1 (en) | Ceramic material for low-temperature sintering, and ceramic substrate | |
| CN111362692A (en) | High-strength multilayer ceramic co-fired structure and preparation method thereof | |
| KR100451955B1 (en) | Method of manufacturing ceramic multi-layer substrate, and unbaked composite laminated body | |
| CN101806768B (en) | Integrated chip type oxygen sensor and manufacturing method thereof | |
| US20090004438A1 (en) | Dielectric ceramic composition, ceramic substrate, and method for producing the same | |
| CN107266067B (en) | Layered composite ceramic plate, manufacturing method and mobile terminal device | |
| JPS6036369A (en) | Ceramic manufacture | |
| US20180072627A1 (en) | Multilayer ceramic substrate and method for manufacturing multilayer ceramic substrate | |
| KR20080002944A (en) | Method for manufacturing thin-film capacitor | |
| CN106145914A (en) | The rapid shaping of a kind of ultrathin low-temperature co-fired ceramic substrate and sintering method | |
| CN110988084A (en) | Durable sheet type oxygen sensor | |
| CN107921744A (en) | Layered product and electronic unit | |
| JP3517986B2 (en) | Manufacturing method of oxygen sensor | |
| US5110442A (en) | Reinforced electrolyte function elements | |
| JP2966375B2 (en) | LAMINATED CERAMIC AND PROCESS FOR PRODUCING THE SAME | |
| JP3320947B2 (en) | Ceramic member having fine through holes | |
| JPH0629664A (en) | Multilayered ceramic wiring board | |
| CN114660154B (en) | Nitrogen-oxygen sensor chip and preparation method thereof | |
| US20050074638A1 (en) | Ceramic substrate and method of manufacturing same | |
| KR20110043440A (en) | Low temperature co-fired ceramic material, low temperature co-fired ceramic body, and multilayer ceramic substrate | |
| CN111433017A (en) | Method for producing metal semi-finished product, method for producing metal-ceramic substrate, and metal-ceramic substrate | |
| CN109640517A (en) | A kind of LTCC base cantilever beam structure and its manufacturing method | |
| EP0987101A2 (en) | Method for producing a ceramic diaphragm structure |
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: 20200703 |