CN111716494A - Method for preparing layered complex phase ceramic by using reaction sintering method - Google Patents
Method for preparing layered complex phase ceramic by using reaction sintering method Download PDFInfo
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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
- B28B3/00—Producing shaped articles from the material by using presses; Presses specially adapted therefor
- B28B3/02—Producing shaped articles from the material by using presses; Presses specially adapted therefor wherein a ram exerts pressure on the material in a moulding space; Ram heads of special form
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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
- 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
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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
- B28B13/00—Feeding the unshaped material to moulds or apparatus for producing shaped articles; Discharging shaped articles from such moulds or apparatus
- B28B13/02—Feeding the unshaped material to moulds or apparatus for producing shaped articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28C—PREPARING CLAY; PRODUCING MIXTURES CONTAINING CLAY OR CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28C5/00—Apparatus or methods for producing mixtures of cement with other substances, e.g. slurries, mortars, porous or fibrous compositions
- B28C5/003—Methods for mixing
Abstract
The invention discloses a method for preparing laminated multiphase ceramics by using a reaction sintering method, which mainly comprises the steps of preparing a single-layer casting sheet, stacking the casting sheets according to the required requirements, placing the stacked casting sheets in a press for press molding, controlling the interlayer gap by the molding pressure of the press, designing the gap of a dewaxed blank according to the requirement to form a porous micro carbon layer or a porous gap layer, and sintering the blank compactly by using a siliconizing reaction sintering process, wherein the porous micro carbon layer between the basic layers naturally forms an interface layer containing a large amount of silicon and a small amount of silicon carbide, and the formed porous gap layer is completely composed of free silicon; finally, the basic layer and the interface layer are mutually combined to form the layered complex phase ceramic with the required structure.
Description
Technical Field
The invention relates to the technical field of ceramic preparation, in particular to a method for preparing laminated complex-phase ceramic by using a reaction sintering method.
Background
The ceramic material has high hardness, high strength, high wear resistance, low thermal expansion coefficient and excellent chemical stability, and is widely applied to the industrial fields of armor protection, petrochemical industry, ferrous metallurgy, mechanical electronics, aerospace and the like. However, conventional ceramic materials are highly susceptible to chipping during impact, resulting in failure of the material due to the extreme tendency for cracks to propagate within the ceramic material. The introduction of the layered interface layer changes the propagation path of the crack in the ceramic material into a path extending along the layers, so that the crack does not penetrate through the whole blank, the toughness of the material is improved, and the impact resistance is improved.
The prior preparation method of the laminated structure complex phase ceramic comprises a multistep dry pressing forming technology, a gel injection molding forming technology, a direct tape casting lamination and other preparation methods, but the technology needs to independently introduce a layer of special interface material, the bonding strength between the independently introduced interface layer and a substrate layer is relatively weak, and the problems of component layer, warping, fault layer, cracking and the like are easily caused by adopting a pressureless sintering process due to different expansion coefficients and sintering shrinkage rates of the substrate layer and the interface layer, so the laminated structure complex phase ceramic is prepared by adopting a hot pressing sintering process, and the preparation cost and the productivity are greatly limited. In addition, the interface layer added separately in the preparation process makes the preparation process relatively complicated.
The publication No. CN104329988A 'A bulletproof ceramic sheet and its preparation method' adopts a method of multiple feeding and multiple dry pressing to successfully prepare a bulletproof ceramic sheet with a composite sandwich structure, the sintering method used in the structure is a normal pressure sintering process, the material components of each layer have large difference in the sintering process, the sintering shrinkage and sintering temperature of each layer of components have large difference, the process is very difficult to control, and the phenomena of cracking, layering and the like between layers are easily caused.
The preparation method of the boron carbide/silicon carbide laminated composite ceramic material with the publication number of CN109111231A adopts a gel injection molding method to alternately cast a solidified green body of ceramic slurry of a substrate layer and a separating layer in a mould, and then obtains laminated structure ceramic by a hot-pressing sintering technology. In the process, the hot-pressing sintering technology is adopted to ensure that the boron carbide and the silicon carbide layer are relatively well combined, but because the sintering temperatures of the silicon carbide and the boron carbide are different, even if the hot-pressing sintering technology is adopted and the two layered structures are extremely difficult to control in the same sintering temperature range, the phenomenon of overburning of one material is easily caused, and the performance of the material is greatly reduced.
The laminated bulletproof ceramic material with high toughness and the preparation method of the laminated bulletproof ceramic material with the publication number of CN110156486A and the combination of the tape casting method and the hot-pressing sintering method are adopted to prepare the laminated bulletproof ceramic material, the interface layer is made of BN (boron nitride) or graphite or WC (wolfram carbide) and the like, the required interface layer needs to be prepared separately in the process, then the difference between the interface layer and the substrate layer is utilized to form a laminated structure, the laminated ceramic with the difference can only be prepared by the hot-pressing sintering process, and the separate preparation process of the interface layer causes relative complexity.
Disclosure of Invention
Aiming at the problems and the defects in the preparation technology of the laminated structure complex phase ceramic, the invention provides a method for preparing the laminated structure complex phase ceramic by combining a tape casting lamination technology and a siliconizing reaction sintering process.
Preparing a single-layer casting sheet, stacking the casting sheets according to the required requirements, placing the stacked casting sheets in a press for press forming, wherein the interlayer gap can be controlled through the forming pressure of the press, the gap of a dewaxed blank can be designed according to the requirement to form a porous micro carbon layer or a porous layer, and sintering the blank by using a siliconizing reaction sintering process to ensure that the blank is sintered compactly, wherein the casting sheet layer forms a base layer consisting of silicon carbide, a ceramic phase and a small amount of free silicon, the porous micro carbon layer between the base layers naturally forms an interface layer containing a large amount of silicon and a small amount of silicon carbide, and the formed porous layer gap layer completely consists of the free silicon; finally, the basic layer and the interface layer are mutually combined to form the layered complex phase ceramic with the required structure.
The technical solution of the invention is as follows: a method for preparing laminated complex phase ceramics by using a reaction sintering method comprises the following steps:
(1) uniformly mixing ceramic powder, a carbon source, a modifier, a dispersant, a binder, a solvent, a plasticizer and a defoaming agent, ball-milling for 1-48h, and then carrying out vacuum defoaming on the ball-milled slurry in a vacuum defoaming machine for 10-180min to prepare ceramic slurry;
(2) carrying out tape casting on the ceramic slurry to obtain a ceramic tape casting roll with required thickness, and then cutting the ceramic tape casting roll into ceramic tape casting sheets with required size;
(3) according to the structural design of the layered complex phase ceramic, the prepared ceramic tape casting sheets are laminated to a biscuit with required thickness, then the biscuit is placed in a mould and loaded with required pressure, the ceramic tape casting sheets approach to each other under the action of the pressure, so that gaps between layers are reduced, and meanwhile, the ceramic tape casting sheets are mutually adhered under the action of organic matters; controlling the bonding degree between layers by controlling the pressure, and measuring the final thickness of the pressed biscuit;
(4) then dewaxing the biscuit, siliconizing, reacting and sintering to obtain the layered complex phase ceramic product with the required structure.
The ceramic powder is any one or mixture of silicon carbide, boron carbide and silicon nitride.
The carbon source is one or a mixture of more of colloidal graphite, crystalline flake graphite, carbon black, resin, cellulose, organic residual carbon of saccharides and petroleum coke powder.
The modifier comprises one or more of graphene, carbon fiber, carbon nano tube, silicon carbide fiber and silicon carbide whisker.
The dispersing agent is one or more of tetramethylammonium hydroxide, ammonium polyacrylate, herring oil, castor oil, polyvinyl alcohol, triethyl phosphate and BYK-160;
the binder category comprises two types of residual carbon after dewaxing and non-residual carbon after dewaxing, wherein the residual carbon is contained in the binder and is bound by one or more of phenolic resin, furan resin, epoxy resin and sodium lignosulfonate, and the binder without the residual carbon comprises one or more of polyvinyl alcohol, polyvinyl butyral and hydroxypropyl methyl cellulose.
The solvent is one or a mixture of deionized water, absolute ethyl alcohol, n-butyl alcohol and butanone.
The plasticizer is one or more of dimethyl phthalate, dibutyl phthalate, dioctyl phthalate, glycerol, polyethylene glycol, epoxidized soybean oil and dioctyl adipate.
The defoaming agent is one of n-octanol and silicone oil.
The ceramic slurry in the step (1) comprises the following components in parts by weight: 70-100 parts of ceramic powder, 1-50 parts of carbon source, 0.1-20 parts of modifier, 0.1-20 parts of dispersant, 1-18 parts of binder, 70-700 parts of solvent, 1-20 parts of plasticizer and 0.001-5 parts of defoaming agent.
The thickness of the ceramic casting sheet in the step (2) is 0.05-5 mm.
The loading pressure in the step (3) is 5-200 MPa.
The final thickness of the biscuit is 1-30 mm.
When the binder formed by the formula contains residual carbon, a porous micro carbon layer with certain residual carbon is formed between the casting sheets by the blank after dewaxing, and the thickness of the porous micro carbon layer is 0.05-2 mm; when the binder formed by the formula does not contain residual carbon, a blank can form a gap layer between the casting sheets after dewaxing, and the thickness of the gap layer is 0.05-2 mm;
the laminated multiphase ceramic structure of the green body obtained by siliconizing reaction sintering is a base layer formed by silicon carbide, ceramic powder and a small amount of free silicon which are generated by reaction and are formed by a casting layer phase composition. When the adhesive formed by the formula contains residual carbon, a small amount of silicon carbide generated by reaction in the porous micro carbon layer between the casting layers and a large amount of free silicon form an interface layer, wherein the thickness of the interface layer is equivalent to that of the porous micro carbon layer; when the formula composition adhesive does not contain residual carbon, the gap layer between the casting layers can form an interface layer with the component of free silicon; finally, the basic layer and the interface layer are mutually combined to form the layered complex phase ceramic with the required structure.
The invention has the beneficial effects that: the layered complex phase ceramic structure prepared by adopting the steps has the following advantages: a) the laminated complex phase ceramic is prepared by adopting a siliconizing reaction sintering process, so that overburning and undercurning caused by different sintering temperature differences caused by different layer components are solved; b) by controlling the type of the binder in the formula, an interface layer containing a small amount of silicon carbide and a large amount of free composition or an interface layer entirely composed of free silicon can be formed; c) meanwhile, the phenomena of layered delamination, cracking and the like caused by sintering shrinkage difference caused by different layer component difference are solved; d) the process for preparing the layered ceramic by adopting the process ensures that the connection between the substrate layer and the interface layer is made of the metal silicon, so that the bonding strength between the substrate layer and the interface is high, and the layered complex-phase ceramic continuously has stronger toughness without reducing the strength of the substrate layer; e) the interface layer of the layered multiphase ceramic is formed by a small amount of silicon carbide and a large amount of free silicon which are produced by reacting with silicon in the porous micro carbon layer with dewaxing performance, and the interface layer does not need to be manufactured separately, so that the process is simple in preparation and beneficial to mass production.
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.
Example 1
(1) Mixing 70 parts of silicon carbide powder, 30 parts of colloidal graphite, 0.5 part of tetramethylammonium hydroxide, 20 parts of phenolic resin, 10 parts of glycerol, 50 parts of deionized water and 0.05 part of n-octanol, adding the mixture into a ball milling barrel, adding 200 parts of silicon carbide ball milling medium, ball milling for 24 hours, and then carrying out vacuum defoaming on the ball milled slurry in a vacuum defoaming machine for 60 minutes to prepare matrix layer ceramic slurry;
(2) carrying out tape casting on the substrate layer ceramic slurry to obtain a substrate ceramic tape casting roll, and then cutting the substrate ceramic tape casting roll into a 100x100mm square tape casting sheet, wherein the thickness of the tape casting sheet layer is 0.2 mm;
(4) according to the structural design of the laminated composite ceramic, 50 pieces of matrix casting sheets are selected to be laminated layer by layer, placed in a 100x100mm square die, and then subjected to pressure forming under a press with the forming pressure of 100MPa to obtain a required laminated ceramic blank with the thickness of 9.5 mm;
(5) slowly heating the pressed layered ceramic biscuit to 900 ℃ in a dewaxing furnace in vacuum atmosphere for dewaxing and cooling to obtain a layered ceramic biscuit; then embedding the biscuit into metal silicon powder and placing the biscuit in a vacuum sintering furnace for sintering, wherein the sintering temperature is 1500 ℃, the heat preservation time is 3 hours, cooling and then processing the residual silicon on the surface of the biscuit to obtain the required layered complex phase ceramic biscuit;
(6) the cross-section metallographic observation shows that the layered structure of the green body consists of a matrix layer of about 0.18mm and an interface layer of 0.01mm, wherein the matrix comprises α -SiC, β -SiC and trace Si, the interface layer consists of a large amount of Si and a small amount of β -SiC, and the overall structure consists of the matrix layer and the interface layer alternately, the bending strength of the matrix layer is 350MPa, and the fracture toughness of the matrix layer is 7.5 MPa.m1/2。
Example 2
(1) Mixing 70 parts of silicon carbide powder, 30 parts of colloidal graphite, 0.5 part of tetramethylammonium hydroxide, 10 parts of polyvinyl alcohol, 10 parts of glycerol, 50 parts of deionized water and 0.05 part of n-octanol, adding the mixture into a ball milling barrel, adding 200 parts of silicon carbide ball milling medium, ball milling for 24 hours, and then carrying out vacuum defoaming on the ball milled slurry in a vacuum defoaming machine for 60 minutes to prepare matrix layer ceramic slurry;
(2) carrying out tape casting on the substrate layer ceramic slurry to obtain a substrate ceramic tape casting roll, and then cutting the substrate ceramic tape casting roll into a 100x100mm square tape casting sheet, wherein the thickness of the tape casting sheet layer is 0.8 mm;
(4) according to the structural design of the laminated composite ceramic, 15 pieces of matrix casting sheets are selected to be laminated layer by layer, placed in a 100x100mm square die, and then subjected to pressure forming under a press with the forming pressure of 50MPa to obtain a required laminated ceramic blank with the thickness of 12.4 mm;
(5) slowly heating the pressed layered ceramic biscuit to 900 ℃ in a dewaxing furnace in vacuum atmosphere for dewaxing and cooling to obtain a layered ceramic biscuit; then embedding the biscuit into metal silicon powder and placing the biscuit in a vacuum sintering furnace for sintering, wherein the sintering temperature is 1500 ℃, the heat preservation time is 3 hours, cooling and then processing the residual silicon on the surface of the biscuit to obtain the required layered complex phase ceramic biscuit;
(6) the cross-section metallographic observation shows that the layered structure of the blank consists of a matrix layer of about 0.78mm and an interface layer of 0.05mm, wherein the matrix consists of α -SiC, β -SiC and trace Si, the interface layer consists of Si, and the overall structure consists of the matrix layer and the interface layer alternately, the bending strength of the base is 380MPa, and the fracture toughness of the base is 7.0 MPa.m1/2。
Example 3
(1) Mixing 60 parts of boron carbide powder, 30 parts of colloidal graphite, 0.5 part of ammonium polyacrylate, 10 parts of phenolic resin, 3 parts of carbon fiber, 10 parts of glycerol, 50 parts of deionized water and 0.05 part of n-octanol, stirring and mixing for 48 hours by adopting a stirring process, and then carrying out vacuum defoaming on the uniformly stirred slurry in a vacuum defoaming machine for 60 minutes to prepare substrate layer ceramic slurry;
(2) carrying out tape casting on the substrate layer ceramic slurry to obtain a substrate ceramic tape casting roll, and then cutting the substrate ceramic tape casting roll into a 100x100mm square tape casting sheet, wherein the thickness of the tape casting sheet layer is 0.8 mm;
(4) according to the structural design of the laminated composite ceramic, 15 pieces of matrix casting sheets are selected to be laminated layer by layer, placed in a 100x100mm square die, and then subjected to pressure forming under a press with the forming pressure of 50MPa to obtain a required laminated ceramic blank with the thickness of 12.4 mm;
(5) slowly heating the pressed layered ceramic biscuit to 900 ℃ in a dewaxing furnace in vacuum atmosphere for dewaxing and cooling to obtain a layered ceramic biscuit; then embedding the biscuit into metal silicon powder and placing the biscuit in a vacuum sintering furnace for sintering, wherein the sintering temperature is 1500 ℃, the heat preservation time is 3 hours, cooling and then processing the residual silicon on the surface of the biscuit to obtain the required layered complex phase ceramic biscuit;
(6) the composition of the layered structure of the blank can be found through cross-section metallographic observation: the matrix layer is about 0.78mm, the thickness of the interface layer is 0.05mm, and the component of the matrix is B4C. β -SiC, carbon fiber and trace Si, wherein the interface layer consists of a large amount of Si and a small amount of β -SiC, the integral structure consists of a substrate layer and interface layers which are alternately arranged, the bending strength is 450MPa, and the fracture toughness is 8.5 MPa.m1/2。
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 (10)
1. A method for preparing laminated complex phase ceramics by using a reaction sintering method is characterized by comprising the following steps:
(1) uniformly mixing ceramic powder, a carbon source, a modifier, a dispersant, a binder, a solvent, a plasticizer and a defoaming agent, ball-milling for 1-48h, and then carrying out vacuum defoaming on the ball-milled slurry in a vacuum defoaming machine for 10-180min to prepare ceramic slurry;
(2) carrying out tape casting on the ceramic slurry to obtain a ceramic tape casting roll with required thickness, and then cutting the ceramic tape casting roll into ceramic tape casting sheets with required size;
(3) according to the structural design of the layered complex phase ceramic, the prepared ceramic tape casting sheets are laminated to a biscuit with required thickness, then the biscuit is placed in a mould and loaded with required pressure, the ceramic tape casting sheets approach to each other under the action of the pressure, so that gaps between layers are reduced, and meanwhile, the ceramic tape casting sheets are mutually adhered under the action of organic matters; controlling the bonding degree between layers by controlling the pressure, and measuring the final thickness of the pressed biscuit;
(4) then dewaxing the biscuit, siliconizing, reacting and sintering to obtain the layered complex phase ceramic product with the required structure.
2. The method for preparing the layered complex-phase ceramic by using the reaction sintering method according to claim 1, wherein the ceramic powder is any one or a mixture of more of silicon carbide, boron carbide and silicon nitride.
3. The method for preparing the layered complex-phase ceramic according to claim 1, wherein the carbon source is any one or a mixture of colloidal graphite, crystalline flake graphite, carbon black, resin, cellulose, organic residual carbon of saccharides and petroleum coke powder.
4. The method for preparing the layered complex-phase ceramic by using the reactive sintering method as claimed in claim 1, wherein the modifier comprises one or more of graphene, carbon fiber, carbon nanotube, silicon carbide fiber and silicon carbide whisker.
5. The method for preparing the layered complex phase ceramic using the reactive sintering method as claimed in claim 1, wherein the dispersant is one or more of tetramethylammonium hydroxide, ammonium polyacrylate, herring oil, castor oil, polyvinyl alcohol, triethyl phosphate, BYK-160.
6. The method of claim 1, wherein the binder includes two types of residual carbon after dewaxing and non-residual carbon after dewaxing, the binder containing residual carbon is one or more of phenolic resin, furan resin, epoxy resin and sodium lignosulfonate, and the binder without residual carbon comprises one or more of polyvinyl alcohol, polyvinyl butyral and hydroxypropyl methylcellulose.
7. The method for preparing the layered complex-phase ceramic by using the reaction sintering method as claimed in claim 1, wherein the solvent is one or more of deionized water, absolute ethyl alcohol, n-butanol and butanone.
8. The method for preparing the layered complex-phase ceramic by using the reaction sintering method according to claim 1, wherein the ceramic slurry in the step (1) comprises the following components in parts by weight: 70-100 parts of ceramic powder, 1-50 parts of carbon source, 0.1-20 parts of modifier, 0.1-20 parts of dispersant, 1-18 parts of binder, 70-700 parts of solvent, 1-20 parts of plasticizer and 0.001-5 parts of defoaming agent.
9. The method for preparing the layered complex phase ceramic using the reaction sintering method as claimed in claim 1, wherein the thickness of the ceramic casting sheet in the step (2) is 0.05-5 mm.
10. The method for preparing the layered composite ceramic using the reaction sintering method as claimed in claim 1, wherein the loading pressure in the step (3) is 5 to 200 MPa.
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Cited By (4)
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| CN112390649A (en) * | 2020-11-09 | 2021-02-23 | 镇江华核装备有限公司 | Preparation method of composite fiber reinforced boron carbide ceramic plate |
| CN112408953A (en) * | 2020-12-11 | 2021-02-26 | 湖南人文科技学院 | Forming method of arc-shaped composite ceramic tile |
| CN113149632A (en) * | 2021-04-23 | 2021-07-23 | 江苏师范大学 | High-hardness YAG-based composite-structure transparent ceramic and preparation method thereof |
| CN116003133A (en) * | 2021-10-22 | 2023-04-25 | 宁波伏尔肯科技股份有限公司 | Method for controlling residual stress of layered ceramic material, method for producing layered ceramic material, layered ceramic material and use thereof |
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| CN112408953A (en) * | 2020-12-11 | 2021-02-26 | 湖南人文科技学院 | Forming method of arc-shaped composite ceramic tile |
| CN113149632A (en) * | 2021-04-23 | 2021-07-23 | 江苏师范大学 | High-hardness YAG-based composite-structure transparent ceramic and preparation method thereof |
| CN116003133A (en) * | 2021-10-22 | 2023-04-25 | 宁波伏尔肯科技股份有限公司 | Method for controlling residual stress of layered ceramic material, method for producing layered ceramic material, layered ceramic material and use thereof |
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Application publication date: 20200929 |