CN111875388A - Preparation method of layered ceramic curved plate - Google Patents

Preparation method of layered ceramic curved plate Download PDF

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CN111875388A
CN111875388A CN202010723207.7A CN202010723207A CN111875388A CN 111875388 A CN111875388 A CN 111875388A CN 202010723207 A CN202010723207 A CN 202010723207A CN 111875388 A CN111875388 A CN 111875388A
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ceramic green
ceramic
curved plate
green sheet
preparing
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CN111875388B (en
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洪于喆
邬国平
谢方民
熊礼俊
戚明杰
于明亮
郭岱东
蔡宁宁
邹东平
杨连江
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Ningbo Vulcan Technology Co ltd
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Abstract

The invention discloses a preparation method of a layered ceramic curved plate, which comprises the following specific steps: 1) preparing a ceramic green sheet with the thickness of 0.1-5 mm; 2) cutting each layer of ceramic green sheet according to a plane development diagram of the prepared layered ceramic curved plate, wherein the cut ceramic green sheets ensure that a gap is formed between the edge and the inner wall of the die when the die is filled; 3) laminating the ceramic green sheets, cutting V-shaped opening at the region where material wrinkles are easily overlapped during molding, placing into steel mold, and molding at 30-380 deg.C and 50-500 kgf/cm2Pressing under pressure, and keeping the temperature for 0.5-5 h; the invention utilizes bondingThe fluidity of the agent is improved in a heating state, the fold overlapping is reduced by cutting the V-shaped opening, the powder is promoted to flow by heating and pressing molding, the green body is changed from normal equal height to vertical equal height, and the cut incision is healed.

Description

Preparation method of layered ceramic curved plate
Technical Field
The invention relates to the technical field of ceramic material preparation, in particular to a preparation method of a layered ceramic curved plate.
Background
The ceramic material has the characteristics of high strength, high hardness and low density, and has wide application in the fields of national defense, chemical engineering, machinery and the like. However, ceramic, which is a brittle material, has poor toughness and is prone to catastrophic fracture under the action of high-speed impact, alternating stress and the like. The layered composite ceramic utilizes the alternate lamination of different materials to increase the energy required by crack propagation, thereby greatly improving the toughness and the fracture work of the materials and reducing the defect sensitivity, thereby improving the brittleness of the ceramic. The preparation of the laminated composite ceramic material can be divided into an integral forming method and a prefabricated sheet laminating method. The integral forming method directly prepares the ceramic green body with a laminated structure by methods such as laminating, grouting and the like, and is often low in production efficiency and not beneficial to batch production. The prefabricated sheet lamination method is that prefabricated ceramic green body prefabricated sheets are prepared, and then the prefabricated sheets are dry-pressed, laminated and sintered according to the design. Compared with other processes such as gel injection molding, roller and the like, the tape casting has the advantages of simple process and high production efficiency in the common preparation method of the prefabricated sheet. Patent CN110156486A proposes a method for preparing laminated ceramic by combining tape casting with hot pressing sintering, the ceramic layer structure of which can be flexibly designed, and the product density is high. However, because of the limited process, the ceramic green sheets can only be flat and thin, and thus the method is limited to the preparation of flat ceramic. There are two main difficulties associated with the production of layered ceramic curved panels from ceramic green sheets. On the one hand, it is known from geometric analysis that a ceramic green sheet cut into a flat shape cannot be completely fitted to a desired curved surface after being laminated, and that the flat green sheet inevitably has wrinkles after being bent. This brings about a phenomenon that material wrinkles overlap in a partial region of the green sheet during the pressing process, thereby affecting uneven pressing of the curved plate. On the other hand, if the thickness of the planar preform laminate is equal at each location, the height of the curved surface in the normal direction of the curved surface is also equal at each location after bending. Since the pressing direction of the press is generally perpendicular to the plane, for points on the curved surface where the normal direction is not parallel to the pressing direction, the height h' in the pressing direction will be greater than the height h of the normal direction of the curved surface, as shown in fig. 1 a. The absolute value of the compression amount is in direct proportion to the height of the material, so that the compression amount of each position on the plate is inconsistent in the pressing process of the normal equal-height curved plate, and the condition that the stress of each position of the curved plate is uneven is greatly aggravated. This problem is not present if the green bodies are vertically level, as shown in fig. 1 b. The larger the curvature of the curved surface, the more significant the two problems described above. The powder in the prefabricated sheet is in a bonding state, powder particles are tightly stacked, the flowability is poor, and the deformation of the green sheet can not be realized through the flowing of the powder so as to fit a curved surface and change the deformation into vertical equal height.
Disclosure of Invention
Aiming at the problem that the layered ceramic curved plate is difficult to form, the invention utilizes the improvement of the fluidity of the binder in a heating state, reduces the fold overlapping by cutting the V-shaped opening, promotes the flow of the powder by heating and pressing for forming, enables the green body to be changed from normal equal height to vertical equal height, and heals the cut.
The technical problem to be solved by the invention is to overcome the defects of the prior art: the preparation method of the layered ceramic curved plate comprises the following specific steps:
1) preparing a ceramic green sheet with the thickness of 0.1-5 mm;
2) cutting each layer of ceramic green sheet according to a plane development diagram of the prepared layered ceramic curved plate, wherein the cut ceramic green sheets ensure that a gap is formed between the edge and the inner wall of the die when the die is filled;
3) laminating the ceramic green sheets, cutting V-shaped opening at the region where material wrinkles are easily overlapped during molding, placing into steel mold, and molding at 30-380 deg.C and 50-500 kgf/cm2Pressing under pressure, and keeping the temperature for 0.5-5 h;
4) heating to 450-850 ℃ at the speed of 0.1-5 ℃/min, and preserving heat for 2-3h to perform dewaxing treatment on the green body;
5) heating to 1450-2350 deg.c at 10-20 deg.c/min, maintaining at 0.5-2 hr and sintering pressure of 0-40MPa in argon, nitrogen or vacuum atmosphere, and cooling to room temperature.
The preparation method of the ceramic green sheet in the step 1) is not particularly limited, and the preparation process known by the technical personnel in the field can be adopted, specifically, the preparation process comprises tape casting, gel casting, rolling and the like;
in the step 1), the binder in the ceramic green sheet is one or more of polyvinyl alcohol, polyvinyl butyral, polyacrylate, hydroxypropyl methylcellulose and polymethyl methacrylate, and the content of the binder is 5-30 wt%;
the ceramic green sheets cut in the step 2) ensure that the edge has a gap of 0.1-10mm from the inner wall of the die when the die is filled.
The invention has the beneficial effects that:
1. the V-shaped opening is cut in the region with serious partial wrinkle overlap on the ceramic green sheet, and when the complex curved plate is pressed, two sides of the opening can be just closed, so that the situation that materials are overlapped in partial wrinkles in the pressing process is greatly reduced;
2. when the temperature is higher than the glass transition temperature of the organic binder and lower than the decomposition temperature, the fluidity of the binder is greatly improved compared with the normal temperature, and the small-amplitude plastic deformation and flowing of the tape-casting sheet can be realized under certain pressure. By utilizing this property, when the complex curved plate is pressed at a suitable temperature and pressure, the material on both sides of the "V" shaped opening can self-heal by flow deformation without affecting the performance of the final product.
3. The reserved gap between the casting sheet and the die provides a space for material flow, the material flow capacity is improved at a proper temperature, small-amplitude plastic deformation and flow energy can be generated under the combined action of the casting sheet and the die in the heating and pressing process, the casting sheet is promoted to be attached to the curved surface of the die, the whole green body is changed from normal equal height to vertical equal height, and the internal stress of the material is reduced;
4. when the ceramic green sheet is cut, only one specification is needed, and the ceramic green sheet does not need to be laminated in sequence, so that the ceramic green sheet is convenient for mass production.
Drawings
Fig. 1 is a schematic view of a pressed structure of a curved plate according to the prior art.
Wherein, fig. 1a shows that the height h' in the pressure direction is larger than the height h of the normal direction of the curved surface, and fig. 1b shows that the heights in the pressure direction are the same.
Detailed Description
The present invention will be described in further detail with reference to the following examples, but the present invention is not limited to the following examples.
Examples
Preparing a compact silicon carbide curved plate according to the following steps:
1) the ceramic raw material powder is silicon carbide powder, silicon nitride powder and graphite powder, and the mixing ratio is 94: 4: 2, taking 100 parts of mixed powder, 20 parts of polyvinyl butyral as a binder, 6 parts of epoxidized soybean oil as a plasticizer, 3 parts of herring oil as a dispersant, 120 parts of absolute ethyl alcohol as a solvent and 80 parts of trichloroethylene as a solvent. Mixing the components and performing ball milling to obtain ceramic slurry;
2) preparing a ceramic green sheet from the ceramic slurry by using a tape casting process, wherein the thickness of the tape casting layer is 0.1 mm;
3) cutting each layer of ceramic green sheet according to the planar development of the prepared layered ceramic curved plate; designing a V-shaped opening at the position where the folds are easy to overlap; whereas the fold-prone overlap may be determined by pre-pressing.
4) Laminating the cut casting sheets, placing the laminated sheets into a steel die, and placing the steel die at 180 ℃ and 500 kgf/cm2Pressing and forming under pressure;
5) heating to 850 ℃ at the speed of 5 ℃/min, preserving heat for 2h, and carrying out dewaxing treatment on the green body;
6) heating to 1950 ℃ at the speed of 10 ℃/min, preserving the heat for 1h, keeping the sintering pressure at 5MPa, and cooling to room temperature along with the furnace, wherein the sintering atmosphere is vacuum;
obtaining a compact silicon carbide multi-curved-surface plate with the density>3.15g/cm3No obvious deformation and cracking, and the V-shaped opening is completely healed when cut.
The above are merely characteristic embodiments of the present invention, and do not limit the scope of the present invention in any way. All technical solutions formed by equivalent exchanges or equivalent substitutions fall within the protection scope of the present invention.

Claims (4)

1. The preparation method of the layered ceramic curved plate is characterized by comprising the following specific steps of:
1) preparing a ceramic green sheet with the thickness of 0.1-5 mm;
2) cutting each layer of ceramic green sheet according to a plane development diagram of the prepared layered ceramic curved plate, wherein the cut ceramic green sheets ensure that a gap is formed between the edge and the inner wall of the die when the die is filled;
3) laminating the ceramic green sheets, cutting V-shaped opening at the region where material wrinkles are easily overlapped during molding, placing into steel mold, and molding at 30-380 deg.C and 50-500 kgf/cm2Pressing under pressure, and keeping the temperature for 0.5-5 h;
4) heating to 450-850 ℃ at the speed of 0.1-5 ℃/min, and preserving heat for 2-3h to perform dewaxing treatment on the green body;
5) heating to 1450-2350 deg.c at 10-20 deg.c/min, maintaining at 0.5-2 hr and sintering pressure of 0-40MPa in argon, nitrogen or vacuum atmosphere, and cooling to room temperature.
2. The method for preparing a layered ceramic curved plate according to claim 1, wherein the ceramic green sheet in step 1) is prepared by casting, gel casting, and rolling.
3. The method for preparing a layered ceramic curved plate according to claim 1, wherein the binder used in step 1) for preparing the ceramic green sheet is one or more selected from polyvinyl alcohol, polyvinyl butyral, polyacrylate, hydroxypropyl methylcellulose, and polymethyl methacrylate, and the binder content is 5wt% to 30 wt%.
4. The method for preparing a layered ceramic curved plate according to claim 1, wherein the ceramic green sheet cut in step 2) is secured to the inner wall of the mold with a gap of 0.1-10mm from the edge when the mold is installed.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114634366A (en) * 2022-02-17 2022-06-17 福建闽航电子有限公司 Preparation method of ceramic tube shell based on fiber alumina

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CN101289328A (en) * 2008-05-20 2008-10-22 西安理工大学 Method for preparing metal-ceramic composite material
CN103591846A (en) * 2013-11-18 2014-02-19 宁波伏尔肯机械密封件制造有限公司 Integral type silicon carbide ceramic elasticity-proof plate and manufacturing method thereof
CN107573074A (en) * 2017-08-30 2018-01-12 西北工业大学 A kind of method of RMI methods low temperature preparation stratiform SiC base shock resistance composite ceramic materials
CN207468477U (en) * 2017-10-09 2018-06-08 蓝思科技(长沙)有限公司 A kind of cavity plate and mold of the 3D glass for being used to produce stable dimensions
US20190144286A1 (en) * 2017-11-10 2019-05-16 Skckolon Pi Inc. Graphite sheet having excellent thermal conductivity and method for preparing the same
CN109761482A (en) * 2019-03-26 2019-05-17 信利光电股份有限公司 A kind of preparation method of 3D cover board
CN110156486A (en) * 2019-05-23 2019-08-23 西北工业大学 The preparation method of high tenacity stratiform bullet-resistant ceramic material and the tape casting combination hot pressing sintering method

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101289328A (en) * 2008-05-20 2008-10-22 西安理工大学 Method for preparing metal-ceramic composite material
CN103591846A (en) * 2013-11-18 2014-02-19 宁波伏尔肯机械密封件制造有限公司 Integral type silicon carbide ceramic elasticity-proof plate and manufacturing method thereof
CN107573074A (en) * 2017-08-30 2018-01-12 西北工业大学 A kind of method of RMI methods low temperature preparation stratiform SiC base shock resistance composite ceramic materials
CN207468477U (en) * 2017-10-09 2018-06-08 蓝思科技(长沙)有限公司 A kind of cavity plate and mold of the 3D glass for being used to produce stable dimensions
US20190144286A1 (en) * 2017-11-10 2019-05-16 Skckolon Pi Inc. Graphite sheet having excellent thermal conductivity and method for preparing the same
CN109761482A (en) * 2019-03-26 2019-05-17 信利光电股份有限公司 A kind of preparation method of 3D cover board
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