CN114643632A - Ceramic forming method, ceramic preparation method and product - Google Patents

Ceramic forming method, ceramic preparation method and product Download PDF

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Publication number
CN114643632A
CN114643632A CN202210069377.7A CN202210069377A CN114643632A CN 114643632 A CN114643632 A CN 114643632A CN 202210069377 A CN202210069377 A CN 202210069377A CN 114643632 A CN114643632 A CN 114643632A
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Prior art keywords
ceramic
forming
blank
flat membrane
forming method
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Inventor
徐海森
郑凯
古娜
杨东亮
于洋
郭明玉
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Shandong Guiyuan Advanced Ceramics Co ltd
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Shandong Guiyuan Advanced Ceramics Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B1/00—Producing shaped prefabricated articles from the material
    • B28B1/26—Producing shaped prefabricated articles from the material by slip-casting, i.e. by casting a suspension or dispersion of the material in a liquid-absorbent or porous mould, the liquid being allowed to soak into or pass through the walls of the mould; Moulds therefor ; specially for manufacturing articles starting from a ceramic slip; Moulds therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B1/00—Producing shaped prefabricated articles from the material
    • B28B1/26—Producing shaped prefabricated articles from the material by slip-casting, i.e. by casting a suspension or dispersion of the material in a liquid-absorbent or porous mould, the liquid being allowed to soak into or pass through the walls of the mould; Moulds therefor ; specially for manufacturing articles starting from a ceramic slip; Moulds therefor
    • B28B1/261—Moulds therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B1/00—Producing shaped prefabricated articles from the material
    • B28B1/26—Producing shaped prefabricated articles from the material by slip-casting, i.e. by casting a suspension or dispersion of the material in a liquid-absorbent or porous mould, the liquid being allowed to soak into or pass through the walls of the mould; Moulds therefor ; specially for manufacturing articles starting from a ceramic slip; Moulds therefor
    • B28B1/261—Moulds therefor
    • B28B1/262—Mould materials; Manufacture of moulds or parts thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B11/00—Apparatus or processes for treating or working the shaped or preshaped articles
    • B28B11/24—Apparatus or processes for treating or working the shaped or preshaped articles for curing, setting or hardening
    • B28B11/243—Setting, e.g. drying, dehydrating or firing ceramic articles
    • 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
    • C04B35/10—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 aluminium oxide
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    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • 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
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    • 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
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    • 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
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • 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
    • C04B35/632—Organic additives
    • C04B35/634—Polymers
    • C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
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    • C04B35/632—Organic additives
    • C04B35/634—Polymers
    • C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
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    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/0051—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof characterised by the pore size, pore shape or kind of porosity
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Abstract

The invention belongs to the technical field of ceramic forming, and particularly relates to a ceramic forming method, a ceramic preparation method and a product, wherein the ceramic forming method comprises the steps of injecting ceramic slurry into a mold with a water filtering layer of a ceramic flat membrane, and curing and forming under the environment that the temperature is lower than 35 ℃ and the relative humidity is 50-80%; the pore diameter of the ceramic flat membrane is less than or equal to 0.1 mu m. The dehydration rates of the upper surface and the lower surface of the ceramic blank can be kept consistent by controlling the aperture of the ceramic flat membrane and the temperature and humidity in the environment, so that the upper size and the lower size of the blank are consistent in the forming process, and the bending deformation phenomenon after the blank is dried in the later period is reduced.

Description

Ceramic forming method, ceramic preparation method and product
Technical Field
The invention relates to the field of ceramic forming, in particular to a ceramic forming method, a ceramic preparation method and a product.
Background
The ceramic molding is a process for processing and preparing ceramic powder into ceramic with a certain size and shape, and the existing domestic molding methods at present comprise dry molding (dry pressing and isostatic pressing molding), plastic molding (extrusion, injection and calendaring molding), casting molding (grouting, filter pressing, tape casting, direct solidification, temperature induced flocculation and casting solidification molding) and special molding (3D printing).
The gel-casting technique has attracted much attention since the research and development of the national laboratory of oak ridge in the united states, and compared with the conventional process, the gel-casting technique has the following advantages: can be directly solidified and formed in a mould, and is suitable for preparing ceramics with complex shapes; the solid content of the slurry is high, the structure of the blank is uniform, and the density is high; simple equipment, convenient operation and suitability for industrial production. At present, the technology is mature to be applied to the field of high-technology ceramics abroad. In the gel injection molding process, slurry preparation, ceramic body curing and molding and body drying are key processes, but the body molding and drying processes occupy a long time in the existing gel injection molding ceramic production, consume a lot of resources and are not beneficial to industrial production.
Patent application CN 108748611A discloses a method for forming a ceramic body, which comprises the steps of dispersing ceramic powder, isobutylene and maleic anhydride copolymer in water, and mixing to obtain water-based ceramic slurry with the solid content of 40-61%; and injecting the obtained water-based ceramic slurry into a porous mold capable of filtering water to obtain a wet blank, discharging part of water in the wet blank under the action of pressure of 0.1-1 MPa, promoting the water to be spontaneously solidified and formed, and demolding and drying after solidification to obtain a ceramic blank. The method discharges the moisture in the slurry by applying pressure and assists spontaneous solidification forming to shorten the forming time, but the moisture in the ceramic slurry is filtered out through the bottom aperture under the method, so that the moisture removal rates in the upper part and the lower part of a blank are inconsistent, and the dried ceramic is easy to bend and deform.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the defect that the ceramic injection-setting molding in the prior art is easy to bend and deform, thereby providing a ceramic molding method, a ceramic preparation method and a ceramic product.
Therefore, the invention provides a ceramic forming method, which comprises the following steps: injecting the ceramic slurry into a die with a water filtering layer being a ceramic flat membrane, and curing and molding under the environment that the temperature is less than 35 ℃ and the relative humidity is 50-80%; the pore diameter of the ceramic flat membrane is less than or equal to 0.1 mu m.
Preferably, the pore diameter of the ceramic flat membrane is 0.05-0.1 μm.
Preferably, the temperature for curing and forming is 20-30 ℃.
Preferably, the relative humidity of the cured product is 60-70%.
Preferably, the flexural strength of the ceramic flat membrane is more than or equal to 40 MPa.
Preferably, the thickness of the ceramic flat membrane is 6-8 mm.
Preferably, the tolerance pH of the ceramic flat membrane is 2-14.
Preferably, the ceramic flat membrane has a tolerance temperature of 0-60 ℃.
Preferably, the ceramic flat membrane comprises a support body and a filter layer.
Preferably, the material of the supporting body and the filtering layer is selected from one or more of alumina ceramics, zirconia ceramics, titania ceramics, silica ceramics and silicon carbide ceramics.
Preferably, the water filtering layer can be directly used as a bottom plate of the mold, and can also be covered on a porous bottom plate.
Preferably, the roughness of the side wall of the die is less than or equal to Ra0.8um.
Preferably, the material of the side wall of the mold is selected from one or more of alumina ceramic, zirconia ceramic, titania ceramic, silica ceramic and silicon carbide ceramic.
Preferably, the step of sealing the side wall of the mold and the ceramic flat membrane with a mold release agent is further included before the curing molding.
Preferably, the release agent is white petrolatum.
Preferably, the ceramic slurry includes an additive and a ceramic powder.
Preferably, the additive is ammonium polyacrylate and/or an alternating copolymer of isobutylene and maleic anhydride.
Preferably, the ceramic powder is one or more selected from alumina ceramic powder, zirconia ceramic powder, titania ceramic powder, silica ceramic powder and silicon carbide ceramic powder.
Preferably, the ceramic slurry comprises 0.2-1 part of ammonium polyacrylate, 0.1-0.5 part of alternating copolymer of isobutene and maleic anhydride and 75-85 parts of ceramic powder in parts by weight.
Preferably, the solid content of the ceramic slurry is 50-56 vol%, and the viscosity is less than or equal to 0.5Pa & S.
Preferably, the ceramic slurry is prepared by the following steps: adding water into the alternating copolymer of the ammonium polyacrylate, the isobutene and the maleic anhydride for dissolving, and then adding the ceramic powder for uniform dispersion to obtain the composite material.
Preferably, the ceramic slurry is prepared by the following steps: adding water into the alternating copolymer of ammonium polyacrylate, isobutene and maleic anhydride for dissolving, ball-milling, mixing, stirring and dispersing for 10-20min at the speed of 150 plus one 250r/min, then reducing the rotating speed to 30-100r/min, adding ceramic powder for several times, adding 1/45-1/10 of the total amount of the ceramic powder each time, uniformly dispersing the ceramic powder, increasing the rotating speed to the speed of 150 plus one 250r/min, ball-milling, mixing, stirring and dispersing for 60-90min, and exhausting in vacuum for 15-30min to obtain the high-performance polyurethane adhesive.
Preferably, the step of coating a release agent on the inner wall of the mould is further included before the curing and forming.
The invention further provides a preparation method of the ceramic, which comprises the forming method and also comprises the steps of demoulding, drying and sintering.
Preferably, the drying is performed by means of staged heating, and preferably, the drying is performed by standing for 20-30h at 20-25 ℃; heating to 28-32 ℃, and standing for 10-15 h; heating to 38-42 deg.C, standing for 8-12 h; heating to 48-52 deg.C, standing for 6-10 h; heating to 58-62 ℃, and standing for 4-8 h; heating to 75-85 deg.C, standing for 2-5 h; heating to 95-100 deg.c to constant weight.
Preferably, the sintering temperature is 1560-1600 ℃, and the time is 2-5 h.
The invention also provides the ceramic prepared by the preparation method of the ceramic.
The technical scheme of the invention has the following advantages:
1. the invention provides a ceramic forming method, which comprises the following steps: injecting the ceramic slurry into a die with a water filtering layer being a ceramic flat membrane, and curing and molding under the environment that the temperature is less than 35 ℃ and the relative humidity is 50-80%; the pore diameter of the ceramic flat membrane is less than or equal to 0.1 mu m. By controlling the aperture of the ceramic flat membrane and the temperature and humidity in the environment, the dehydration rates of the upper surface and the lower surface of the ceramic blank can be kept consistent, so that the upper size and the lower size of the blank in the forming process are consistent, the bending deformation phenomenon after the blank is sintered at the later stage is reduced, and the forming rate and the qualification rate of products are greatly improved.
2. The invention selects the ceramic flat membrane with the aperture of 0.05-0.1 μm, on one hand, the curing time of the ceramic blank body can be prolonged when the aperture of the ceramic flat membrane is too small, and on the other hand, the curing time can be shortened when the aperture is too large, but fine particles in the ceramic slurry can block the ceramic flat membrane along with the curing time, so that the blank body can only volatilize water through the upper surface of the die, the shrinkage rates of the upper surface and the lower surface of the blank body are inconsistent, and severe bending deformation can occur after sintering.
3. The ceramic body is cured at the temperature of 20-30 ℃, the curing time is prolonged due to too low temperature, the industrial production is not facilitated, the moisture on the upper surface is volatilized fast in the curing process due to too high temperature, the shrinkage rates of the upper surface and the lower surface of the body are inconsistent, and the body is easy to bend and deform after being sintered.
4. The invention is cured in the environment with the relative humidity of 60-70%, when the relative humidity is lower, the moisture on the upper surface of the green body is volatilized faster, so that the shrinkage rates of the upper surface and the lower surface of the green body are inconsistent, and the green body is easy to bend and deform after being sintered; when the humidity is too high, the curing time of the blank is correspondingly prolonged, and the industrial production cost is increased.
5. The ceramic flat membrane with the breaking strength of more than or equal to 40MPa is adopted, so that the requirement on strength in the process of forming the ceramic blank body can be met, and the ceramic blank body can be smoothly formed. In addition, the ceramic flat membrane is suitable for slurry with pH of 2-14, can adapt to the environmental temperature of 0-60 ℃, and has wide application range.
6. The ceramic slurry used in the invention adopts polyacrylamide as a dispersing agent, and an alternating copolymer of isobutylene and maleic anhydride as the dispersing agent and a coagulant, and has the dispersing and coagulation promoting effects through the change of the function of functional groups in a molecular chain, the addition amount of the two auxiliaries is very small, the emission of organic matters is reduced in the production process, the ceramic slurry is environment-friendly, and the two auxiliaries are decomposed in the later sintering process, so that the green body is not polluted.
7. The ceramic forming method provided by the invention has a wide application range, and can select a proper mold according to the material variety of the ceramic slurry, so that the pollution of the mold to the slurry is effectively avoided; white vaseline is used as a release agent before forming, the high viscosity performance of the white vaseline can ensure the sealing performance of the material, can also ensure that the slurry can avoid the influence of cracking and the like caused by wall adhesion in the process of dehydration and shrinkage, and can be directly decomposed in the later sintering process, so that the product cannot be polluted.
8. The ceramic forming method provided by the invention can realize rapid gel forming of the ceramic blank, obvious shrinkage gaps can appear between the blank and the die within 2h, curing and demoulding can be completed within 24h, and the method is simple, high in repeatability and convenient for industrial production.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the prior art descriptions will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is an SEM electron micrograph of an alumina ceramic body prepared in example 1 of the present invention;
FIG. 2 is a photograph of the gap between the green body and the mold after 2 hours of dehydration in the alumina ceramic molding process according to example 1 of the present invention;
FIG. 3 is a picture showing the appearance of a green body obtained by removing the mold by the alumina ceramic molding method according to example 1 of the present invention.
Detailed Description
The following examples are provided to further understand the present invention, not to limit the scope of the present invention, but to provide the best mode, not to limit the content and the protection scope of the present invention, and any product similar or similar to the present invention, which is obtained by combining the present invention with other prior art features, falls within the protection scope of the present invention.
The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field. The reagents or instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.
The alternating copolymer of isobutylene and maleic anhydride used in the invention can be prepared by persons skilled in the art by themselves by using isobutylene and maleic anhydride, and can also be purchased directly without influencing the experimental effect of the invention. The alternating copolymer of isobutylene and maleic anhydride adopted in the embodiment of the invention is purchased from Jiaxing Puxin commercial Co., Ltd, and has the trade name of Isobam104 and the molecular weight of 55000-65000.
The ceramic flat membrane used in the invention is a flat ceramic membrane, and the purpose of the invention can be realized by meeting the following conditions: the average pore diameter is less than or equal to 0.1 mu m. The specific manufacturer of the ceramic flat sheet membrane is not limited, and the ceramic flat sheet membrane can meet the conditions, for example, the ceramic flat sheet membrane is produced by Shandong silicon element membrane material science and technology Limited company, the batch number is 20200320-1, the average pore diameter is 0.1 mu m, the breaking strength is more than or equal to 40MPa, the tolerance pH range is 2-14, and the tolerance temperature range is 0-60 ℃.
The bending strength is measured by a three-point bending method, a testing instrument is a WDW-3100 type universal electronic testing machine, the span is 80mm, the moving speed of a pressure head is 0.5mm/min, the maximum load when the sample is broken and the distance of a lower knife edge are measured, and then the bending strength of the sample is calculated according to a formula: sigmaf＝3×P×l/(2×b×h2) In the formula: sigmaf-bending strength (Mpa); p-the maximum load (N) at which the specimen breaks; l-distance of lower knife edge (cm); b-width of the sample (cm); h-thickness of the sample (cm).
The side wall of the die used in the following examples of the invention was purchased from Shandong silicon element New materials GmbH, the roughness of the side wall was Ra0.7 μm, and the roughness was tested by a TR200 roughness meter of Shenzhen Shenlidaxin instruments GmbH.
The alumina ceramic powder used in the following examples of the present invention was obtained from light metal Japan K.K., Al2O3The content is more than or equal to 99.8 percent; the zirconia ceramic powder is purchased from zirconium science and technology Co., Ltd, Guangdong Oriental zirconium industry, and the zirconia content is more than or equal to 99%.
The ceramic flat membrane used in the invention can be directly used as a bottom plate of a mould, white vaseline is adopted to seal the side wall of the mould, and the ceramic flat membrane can also be directly covered on a porous bottom plate of the mould for use, and the purpose of the invention can be realized in any mode.
Example 1
The embodiment provides a ceramic forming method, which comprises the following steps:
(1) weighing 29.12g of polyacrylamide and 12.48g of Isobam104, adding 960g of deionized water, stirring for dissolving, pouring into a ball-milling stirring tank, ball-milling and stirring for 10min at 200r/min, reducing the rotating speed to 50r/min, adding 100g of alumina ceramic powder, continuing to add 100g of alumina ceramic powder after uniform dispersion, repeating the operation until 4160g of alumina ceramic powder is completely and uniformly dispersed, increasing the rotating speed to 200r/min, stirring for 1h, pouring the slurry into a vacuum stirring kettle, and performing vacuum degassing for 20min to obtain alumina ceramic slurry with the solid content of 54% and the room temperature of vol 0.4 Pa.S;
(2) the bottom plate of the mould is a ceramic flat membrane with the aperture of 0.1mm (the ceramic flat membrane support body and the filter layer are made of alumina ceramic), the side wall of the mould is made of alumina ceramic with the content of 99.5 percent, the ceramic flat membrane and the side wall are sealed by coating white vaseline, and the inner wall of the mould is coated with white vaseline with the thickness of 0.4mm as a release agent;
(3) and (3) injecting the alumina ceramic slurry into a mold, and curing and molding at 25 ℃ in an environment with the relative humidity of 60%, wherein the curing and molding time is 18 h.
Fig. 2 is a picture of a gap between the ceramic blank and the mold when the ceramic blank is cured and molded for 2 hours in the embodiment, and it can be seen that an obvious gap can be formed between the ceramic blank and the mold when the time is 2 hours.
The embodiment also provides a ceramic and a preparation method thereof, and the preparation method comprises the steps of demoulding, drying and sintering the cured and molded ceramic blank.
Fig. 3 is an appearance picture of the ceramic green body obtained after demolding, and it can be seen that the green body obtained after curing and molding by the method of the present embodiment and demolding has a complete appearance and no defect.
Wherein, the drying conditions are as follows: and (3) standing the demoulded blank for 24h at room temperature, heating to 30 ℃, standing for 12h, standing for 10h at 40 ℃, standing for 8h at 50 ℃, standing for 6h at 60 ℃, standing for 4h at 80 ℃, and standing for 100 ℃ until the blank is constant in weight.
The sintering conditions are as follows: and (4) insulating the blank at 1580 ℃ for 2h, and sintering to obtain the ceramic.
Example 2
The embodiment provides a ceramic forming method, which comprises the following steps:
(1) weighing 11.2g of polyacrylamide and Isobam1042.24g, adding 220g of deionized water, stirring for dissolving, then pouring into a ball-milling stirring tank, ball-milling and stirring at 250r/min for 10min, then reducing the rotating speed to 100r/min, adding 100g of alumina ceramic powder, after uniform dispersion, continuing to add 100g of alumina ceramic powder, repeatedly operating until 1120g of alumina ceramic powder is completely and uniformly dispersed, increasing the rotating speed to 250r/min, stirring for 1h, then pouring the slurry into a vacuum stirring kettle, and carrying out vacuum degassing for 15min to obtain alumina ceramic slurry with the solid content of 56 vol% and the room temperature of 0.5 Pa.S;
(2) the bottom plate of the mould is a ceramic flat membrane with the aperture of 0.1mm (the ceramic flat membrane support body and the filter layer are made of alumina ceramic), the side wall of the mould is made of alumina ceramic with the content of 99.0 percent, the ceramic flat membrane and the side wall are sealed by coating white vaseline, and the inner wall of the mould is coated with white vaseline with the thickness of 0.4mm as a release agent;
(3) and (3) injecting the alumina ceramic slurry into a mold, and curing and molding at 30 ℃ in an environment with the relative humidity of 60%, wherein the curing and molding time is 14 h.
The embodiment also provides a ceramic and a preparation method thereof, and the preparation method comprises the steps of demoulding, drying and sintering the cured and molded ceramic blank.
Wherein, the drying conditions are as follows: and (3) standing the demoulded blank for 24h at room temperature, heating to 30 ℃, standing for 12h, standing for 10h at 40 ℃, standing for 8h at 50 ℃, standing for 6h at 60 ℃, standing for 4h at 80 ℃, and standing for 100 ℃ until the blank is constant in weight.
The sintering conditions are as follows: and (4) keeping the temperature of the green body at 1600 ℃ for 5 hours for sintering to obtain the ceramic.
Example 3
The embodiment provides a ceramic forming method, which comprises the following steps:
(1) weighing 24g of polyacrylamide and Isobam 10430 g, adding 1000g of deionized water, stirring and dissolving, then pouring into a ball-milling stirring tank, ball-milling and stirring at 150r/min for 20min, reducing the rotating speed to 30r/min, adding 150g of zirconia ceramic powder, continuing to add 150g of zirconia ceramic powder after uniform dispersion, repeatedly operating until 6000g of zirconia ceramic powder is completely and uniformly dispersed, increasing the rotating speed to 150r/min, stirring for 1.5h, then pouring the slurry into a vacuum stirring kettle, and carrying out vacuum degassing for 30min to obtain zirconia ceramic slurry with the solid content of 50 vol% and the room temperature of 0.2 Pa.S;
(2) the bottom plate of the mould is a ceramic flat membrane with the aperture of 0.1mm (the ceramic flat membrane support body and the filter layer are made of zirconia ceramic), the side wall of the mould is made of 99% zirconia ceramic, the ceramic flat membrane and the side wall are sealed by coating white vaseline, and the inner wall of the mould is coated with white vaseline with the thickness of 0.5mm as a release agent;
(3) and (3) injecting the zirconia ceramic slurry into a mold, and curing and molding at 25 ℃ in an environment with the relative humidity of 60%, wherein the curing and molding time is 24 h.
The embodiment also provides a ceramic and a preparation method thereof, and the preparation method comprises the steps of demoulding, drying and sintering the ceramic blank after curing and forming.
Wherein, the drying conditions are as follows: and (3) standing the demoulded blank for 24h at room temperature, heating to 30 ℃, standing for 12h, standing for 10h at 40 ℃, standing for 8h at 50 ℃, standing for 6h at 60 ℃, standing for 4h at 80 ℃, and drying at 100 ℃ until the blank is constant in weight.
The sintering conditions are as follows: and (4) insulating the blank at 1580 ℃ for 3h, and sintering to obtain the ceramic.
Example 4
This example provides a method of forming a ceramic, which differs from example 1 in that the temperature at curing is 20 ℃. The curing and molding time of the ceramic body in the embodiment is 22 h.
Example 5
This example provides a ceramic molding method, which is different from example 1 in that the mold base is a ceramic flat membrane having a pore size of 0.05 μm. The curing and molding time of the ceramic body in the embodiment is 21 h.
Example 6
This example provides a method of forming a ceramic, which differs from example 1 in that the ambient relative humidity at the time of curing is 50%. The curing and molding time of the ceramic body in the embodiment is 18 h.
Example 7
This example provides a method of forming a ceramic, which differs from example 1 in that the ambient relative humidity at the time of curing is 80%. The curing and molding time of the ceramic body in the embodiment is 19.5 h.
Comparative example 1
This comparative example provides a ceramic forming process, which is distinguished from example 1 by a curing temperature of 35 ℃.
Comparative example 2
This comparative example provides a ceramic molding method, which is different from example 1 in that the mold base is an alumina ceramic flat membrane having a pore size of 0.2 μm.
Comparative example 3
This comparative example provides a ceramic forming process, which differs from example 1 in that the ambient relative humidity at the time of curing is 20%.
Examples of the experiments
The upper and lower diameters of the dried bodies of examples 1 to 7 and comparative examples 1 to 3 were measured for their difference in shrinkage, and the results are shown in Table 1.
The diameter shrinkage difference refers to that when the solidified and molded blank body is dried to constant weight (weighing twice, the difference value is not more than 0.3mg), the diameter of the upper surface and the diameter of the lower surface of the blank body are measured, and the difference value of the two is the diameter shrinkage difference.
TABLE 1 comparison of the effects of different shaping methods
Figure BDA0003480536110000111
As can be seen from the above table, the ceramic forming method provided by the invention adopts the ceramic flat membrane with the aperture less than or equal to 0.1 μm as the water filtering layer, and simultaneously controls the environmental temperature less than 35 ℃ and the relative humidity between 50 and 80 percent, so that the deviation of the upper diameter and the lower diameter of the blank after shrinkage is less than or equal to 1.1mm, and the deviation effectively avoids the problem of bending deformation of the blank within an acceptable range; comparative example 1 the curing temperature was 35 ℃, the volatilization speed of the moisture on the upper surface of the green body was faster than that on the bottom, resulting in inconsistent shrinkage of the upper and lower surfaces of the green body, with the shrinkage difference being significantly greater than that of the examples; the filter layer adopted in the comparative example 2 is a ceramic flat membrane with the average membrane pore diameter of 0.2um, and the phenomenon of inconsistent shrinkage occurs at the bottom and the upper part of the blank body, because the fine ceramic particles with the particle diameter of 0.1-0.2um block partial membrane pore drainage channels, so that the vertical discharge rate of water is inconsistent, and the vertical shrinkage drop is larger than 2 mm. Comparative example 3 the relative humidity was 20% when curing, the air was relatively dry in the environment, the volatilization rate of the upper surface of the blank was greater than that of the lower surface, resulting in a significantly greater difference in upper and lower shrinkage than in the examples, and the blank had a bending problem.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.

Claims (10)

1. A method of forming a ceramic, comprising the steps of: the ceramic slurry is injected into a die of which the water filtering layer is a ceramic flat membrane with the aperture less than or equal to 0.1 mu m, and is cured and molded under the environment that the temperature is less than 35 ℃ and the relative humidity is 50-80 percent.
2. The ceramic molding method according to claim 1, wherein the pore size of the ceramic flat membrane is 0.05 to 0.1 μm.
3. The ceramic forming method according to claim 1 or 2, wherein the temperature of the solidification forming is 20 to 30 ℃.
4. The ceramic forming method according to any one of claims 1 to 3, wherein the relative humidity of the cured form is 60 to 70%.
5. The ceramic forming method according to any one of claims 1 to 4, wherein the flexural strength of the ceramic flat sheet membrane is not less than 40 MPa.
6. The ceramic forming method according to any one of claims 1 to 5, wherein the ceramic slurry includes an additive and a ceramic powder.
7. The ceramic forming method according to claim 6, wherein the additive is ammonium polyacrylate and/or an alternating copolymer of isobutylene and maleic anhydride.
8. The ceramic forming method according to claim 7, wherein the ceramic slurry comprises 0.2 to 1 part by weight of ammonium polyacrylate, 0.1 to 0.5 part by weight of alternating copolymer of isobutylene and maleic anhydride, and 75 to 85 parts by weight of ceramic powder.
9. A method of making a ceramic comprising the method of forming of any one of claims 1-8, further comprising the steps of demolding, drying and sintering.
10. A ceramic produced by the production method according to claim 9.
CN202210069377.7A 2022-01-20 2022-01-20 Ceramic forming method, ceramic preparation method and product Pending CN114643632A (en)

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