CN106187197B - Carborundum plate product and its processing method - Google Patents
Carborundum plate product and its processing method Download PDFInfo
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- CN106187197B CN106187197B CN201610542507.9A CN201610542507A CN106187197B CN 106187197 B CN106187197 B CN 106187197B CN 201610542507 A CN201610542507 A CN 201610542507A CN 106187197 B CN106187197 B CN 106187197B
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Abstract
The present invention relates to a kind of carborundum plate product and its processing method, thickness is 0.5~50mm, and density is 2.70~2.85g/cm3, 100~130MPa of compressive resistance, 45~60MPa of flexural strength；Processing method its specific steps are：(1) preparation of carborundum plate performed polymer, the preparation of (two) carborundum plate：The carborundum plate performed polymer that step (1) is obtained, carborundum plate performed polymer is placed on pre-oxidation 1h~5h in 260~280 DEG C of Muffle furnaces, pre-oxidation carborundum plate material is prepared, then pre-oxidation carborundum plate is calcined in nitrogen atmosphere again 1.5~2.5h under the conditions of 1100~1200 DEG C, it is then transferred into argon gas atmosphere, 1~1.5h is calcined at 1500~1650 DEG C again, carborundum plate is prepared.The present invention utilizes multistep sintering process, not only can impurity content in reduction system, reduce system hole, while improving the compactness of carborundum plate, be conducive to improve the mechanical performance of carborundum plate；It is with important application prospects.
Description
Technical field
The present invention relates to a kind of carborundum plate product, especially a kind of carborundum plate product and its processing method.
Background technology
Carborundum plate is the important auxiliary material of ceramic industry, has high temperature resistant, intensity is big, and heat conductivility is good, anti-impact
The characteristics of hitting plays very important effect for the quality and cost that promote ceramic product.Simultaneously because carborundum plate is main
It is lamellar, large area, small thickness, and in use directly and flame contact, and there is supporting role to green compact, especially
It is to be badly in need of wanting certain weighing property during high-temperature calcination ceramic post sintering, it is also necessary to certain high temperature resistant and high temperature oxidation resisting
Property, the problems such as therefore requirement to carborundum plate is extremely stringent, causes silicon carbide price itself high, and service life is shorter.
Silicon carbide main production process is the ground and mixed using silicon source and carbon source at present, so that carbon source and silicon source is carried out uniform
Then mixing carries out high-temperature calcination technique, and produce the material of the silicon carbide not only fineness problem of grain size in by process of lapping
It influences, while also being influenced by the consistency problem of carbon source and silicon source itself, influence finished silicon carbide product rate and sintering process efficiency；
Prepared simultaneously for silicon carbide and mainly use novel carbon source and silicon source at present, and silicon source mixed with carbon source it is dispersed not only for
The yield rate of product impacts, and also has very important influence simultaneously for the quality of product, mixed due to carbon source and silicon source
Conjunction problem causes local proportion irregular, influences carborundum crystals crystal form, and making crystal, there are excessive defects, not only influence product
Performance, while also making the decrease in yield of product；Therefore the method studied at present mainly uses novel silicon source and carbon source, by opening
The mixing dispersing method for sending out new, the plank for preparing high finished product rate and haveing excellent performance.
Chinese patent CN2617571 discloses a kind of composite silicon carbide board, mainly solves common carborundum plate in strong oxygen
Change and is easily aoxidized in environment, influences the problem of service life.It includes silicon carbide substrate, and one layer is suppressed in silicon carbide substrate surface
The composite layer being made of composite material.Composite layer and SiC layer faying face are coarse, penetrate into mutually.The main component of composite layer is light
Burn α-Al2O3、ZrO2.Composite layer in the utility model is in all various aspects such as firing temperature, coefficient of thermal expansion, burning line variations
It is same or similar with SiC substrate, it will not fall off, remove in the variation of high temperature (1400 DEG C) room temperature, reach and be total to the service life with substrate,
And protect SiC substrate not oxidized.
A kind of production systems of carborundum plate of 105503221 A of Chinese patent CN, by using with continuous more suits
Carry out system single-candidate design is set, with grinding device successively, mixing device, humidifier, calciner, cooling device and packing machine
It is attached, and so that material is reentered secondary system utilization by production line tieback to grinding device in cooling device, save
Cost, avoids environmental pollution.
A kind of high-temperature resistant and energy-saving carborundum plates of 103833365 B of Chinese patent CN and its processing method, with different-grain diameter
The silicon carbide of size, silica flour and compound binding agent are bonded, then in surface spraying after dispensing, molding, drying and firing
High temperature anti-oxidation coating is made.The silicon carbide biscuit density that obtains by using vibration moulding forcing press compression moulding is high, grading
Rationally, plate face is uniform, improves compressive resistance and flexural strength；Using microwave drying, since microwave has penetration, carbonization
Silicon biscuit is inside and outside dry simultaneously, and internal temperature is slightly above surface temperature, makes to form outside pressure difference inside silicon carbide biscuit, add
The speed migration of moisture content, can reach the purpose of evenly drying；Refractory slab kiln group using natural gas firing and full residual heat integrative
It is energy-saving using power-saving technology, reduce discharge amount of exhaust gas, the flue gas of calcining kiln discharge is used for fire resisting slab as heat source
The energy and resource reutilization are realized in the drying of body；The firing of silicon carbide biscuit is fully chemically reacted within the scope of different temperatures,
Obtain the carborundum plate of uniform compressive resistance and flexural strength；Carborundum plate surface spraying high temperature anti-oxidation coating, has
Effect inhibits the oxidation of carborundum plate, extends life of product.
Invention content
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of carborundum plate product and its processing methods；
It is using the technique of in-situ blending, carbon source and silicon source is evenly dispersed, the silicon carbide nucleus sintering activating energy in sintering process is reduced,
The carborundum plate for preparing uniform resistance to oxidation has very important application prospect in the high temperature resistants sintering technology such as ceramics field.
The purpose of the present invention is achieved through the following technical solutions：
A kind of carborundum plate product, thickness are 0.5~50mm, and density is 2.70~2.85g/cm3, compressive resistance 100~
130MPa, 45~60MPa of flexural strength.
A kind of processing method of carborundum plate product, the specific steps are：
(1) preparation of carborundum plate performed polymer
Using polyacrylonitrile as carbon source, using the aqueous solution of n,N-Dimethylformamide as mixed solvent, using metasilicic acid as silicon source,
Carbon source and silicon source are dissolved in the mixed solvent at normal temperatures, the solidification stoste that viscosity is 50~100Pas is prepared, so
Again that the extruded die orifice extrusion of solidification stoste is preforming afterwards, preforming solidification stoste is cooled down through air section, then solidifying through sodium sulphate
Admittedly bathing solution, then after washing solidifies, then it is air-dried again at 145~155 DEG C, the residence time is that 45~60s is carbonized
Silicon plate performed polymer；
The mass values of the metasilicic acid and polyacrylonitrile are 1: 25~1: 50；
The polyacrylonitrile is 15~30% in the mass concentration of in the mixed solvent；
The volume ratio of the in the mixed solvent n,N-Dimethylformamide and water is 1: 0.05~1: 0.20；
Stoste is solidified in the preform process in 65~85 DEG C of the temperature of extrusion mould-outlet, the pump of extrusion is for amount
The thickness of 10~5000mL/min, extrusion mould-outlet are 0.75~75mm；
The air section cooling temperature is 20~25 DEG C, and the air section residence time is 10~15cm；
Sodium sulfate quality a concentration of 10~20% in the coagulating bath, solidification stoste is in the coagulating bath residence time 30~45
Second；The residence time is 10~15 seconds in water-washing process；
Polyacrylonitrile has abundant carbon source structure, is usually used in preparing the materials such as carbon fiber；Using the method for solution blending,
Polyacrylonitrile is mixed with material metasilicic acid, material is made to achieve the purpose that evenly dispersed and be blended；And metasilicic acid its
Itself has abundant element silicon, and can dissolve in aqueous solution, while metasilicic acid generates in the material containing sodium salt
Inorganic material sodium metasilicate, to realize, sodium metasilicate is precipitated while polyacrylonitrile solidifies, and to fixed silicon source material, keeps away
Exempt from the loss of later stage washing silicon source material, while may also reach up the purpose of even solidification, avoids being precipitated due to carbon source and silicon source
Object it is asynchronous, make the growth course of carborundum crystals in calcination process, and the silicon carbide whisker volume defect of part and after reducing
The yield rate of phase product；Avoid current silicon carbide articles using the method for solution blending needs high speed permanent in sintering procedure
Process of lapping, while sintering process activation energy is excessive between also solving the inorganic particle of multi phase state structure, and waste of energy,
And the self aggregation state of inorganic particle itself causes to easy to produce local defect in production process of plate, influences the finished product of product
Rate；
Using metasilicic acid material, using the silicon source structure that metasilicic acid is abundant, while polyacrylonitrile solidifies and sodium sulphate
Structure is silicon source and carbon source carries out blending process of setting, and generates silica at a temperature of 150 DEG C conducive to sodium metasilicate,
To achieve the purpose that carbon source and the evenly dispersed precipitation of silicon source, avoid phase itself existing for direct physical blending is difficult to phase
Hold, interface is excessive and the problem of be difficult to calcine forming；
(2) preparation of carborundum plate
Carborundum plate performed polymer is placed on 260~280 DEG C of Muffle furnaces by the carborundum plate performed polymer that step (1) is obtained
Pre-oxidation carborundum plate material is prepared, then again pre-oxidation carborundum plate in nitrogen atmosphere in middle pre-oxidation 1h~5h
Under the conditions of 1100~1200 DEG C calcine 1.5~2.5h, be then transferred into argon gas atmosphere, then at 1500~1650 DEG C calcining 1~
Carborundum plate is prepared in 1.5h；
Using first step pre-oxidation in polyacrylonitrile structure nitrogen and flammable hydrogen remove, while making polyacrylonitrile itself
Porous structure be further formed, be conducive to later stage calcination process, while in second nitrogen protection calcination process, utilizing high temperature item
Carbon source and silicon source are reacted under part, promote to produce silicon carbide precursor, while nitrogen protection process keeps carbon monoxide quick
Take away, avoid another secondary response, further high-temperature burning process, not only makes carborundum crystals generate in argon inert gas
It is more perfect, while system hole can also be reduced, improve the compactness of carborundum plate, be conducive to improve the machinery of carborundum plate
Performance；
The usefulness of the present invention and the prior art：
A kind of carborundum plate product of the present invention and its processing method reduce carbon source using the method for solution blending and silicon source are mixed
Difficulties in dispersion is closed, and leads in high-temperature burning process the raw material proportioning difference because of part, leads to carborundum crystals poor crystal form
It is different, make product poor quality；Use polyacrylonitrile and metasilicic acid for raw material, abundance, while passing through in preparation process
Silicon source solidification synchronous with carbon source is realized during coagulating bath, improves proportioning uniformity；Simultaneously because raw material proportioning is equal in raw material
Even process of setting realizes one of molding of product, using first one-step forming of the coagulating bath in process of setting, after avoiding powder from grinding
Be difficult to be molded the problem of carrying out product sintering, using multistep sintering process, not only can impurity content in reduction system, reduce body
It is hole, while improves the compactness of carborundum plate, is conducive to improve the mechanical performance of carborundum plate；A kind of carborundum plate of the present invention
Product and its processing method are with important application prospects in fields such as silicon carbide.
Description of the drawings
Fig. 1 is the XRD diffracting spectrums that a kind of carborundum plate of the application manufactures；
Specific implementation mode
The specific implementation mode of a kind of carborundum plate product of the present invention presented below and its processing method.
Embodiment 1
A kind of carborundum plate product, thickness are 0.5~50mm, and density is 2.70~2.85g/cm3, compressive resistance 100~
130MPa, 45~60MPa of flexural strength.
A kind of processing method of carborundum plate product, the specific steps are：
(1) preparation of carborundum plate performed polymer
Using polyacrylonitrile as carbon source, using the aqueous solution of n,N-Dimethylformamide as mixed solvent, using metasilicic acid as silicon source,
Carbon source and silicon source are dissolved in the mixed solvent at normal temperatures, the solidification stoste that viscosity is 50~100Pas is prepared, so
Again that the extruded die orifice extrusion of solidification stoste is preforming afterwards, preforming solidification stoste is cooled down through air section, then solidifying through sodium sulphate
Admittedly bathing solution, then after washing solidifies, then it is air-dried again at 145~155 DEG C, the residence time is that 45~60s is carbonized
Silicon plate performed polymer；
The mass values of the metasilicic acid and polyacrylonitrile are 1: 25；
The polyacrylonitrile is 15% in the mass concentration of in the mixed solvent；
The volume ratio of the in the mixed solvent n,N-Dimethylformamide and water is 1: 0.05；
Stoste is solidified in the preform process in 65~85 DEG C of the temperature of extrusion mould-outlet, the pump of extrusion is for amount
The thickness of 10~5000mL/min, extrusion mould-outlet are 0.75~75mm；
The air section cooling temperature is 20~25 DEG C, and the air section residence time is 10~15cm；
Sodium sulfate quality a concentration of 10~20% in the coagulating bath, solidification stoste is in the coagulating bath residence time 30~45
Second；The residence time is 10~15 seconds in water-washing process；
Polyacrylonitrile has abundant carbon source structure, is usually used in preparing the materials such as carbon fiber；Using the method for solution blending,
Polyacrylonitrile is mixed with material metasilicic acid, material is made to achieve the purpose that evenly dispersed and be blended；And metasilicic acid its
Itself has abundant element silicon, and can dissolve in aqueous solution, while metasilicic acid generates in the material containing sodium salt
Inorganic material sodium metasilicate, to realize, sodium metasilicate is precipitated while polyacrylonitrile solidifies, and to fixed silicon source material, keeps away
Exempt from the loss of later stage washing silicon source material, while may also reach up the purpose of even solidification, avoids being precipitated due to carbon source and silicon source
Object it is asynchronous, make the growth course of carborundum crystals in calcination process, and the silicon carbide whisker volume defect of part and after reducing
The yield rate of phase product；Avoid current silicon carbide articles using the method for solution blending needs high speed permanent in sintering procedure
Process of lapping, while sintering process activation energy is excessive between also solving the inorganic particle of multi phase state structure, and waste of energy,
And the self aggregation state of inorganic particle itself causes to easy to produce local defect in production process of plate, influences the finished product of product
Rate；
Using metasilicic acid material, using the silicon source structure that metasilicic acid is abundant, while polyacrylonitrile solidifies and sodium sulphate
Structure is silicon source and carbon source carries out blending process of setting, and generates silica at a temperature of 150 DEG C conducive to sodium metasilicate,
To achieve the purpose that carbon source and the evenly dispersed precipitation of silicon source, avoid phase itself existing for direct physical blending is difficult to phase
Hold, interface is excessive and the problem of be difficult to calcine forming；
(2) preparation of carborundum plate
Carborundum plate performed polymer is placed on 260~280 DEG C of Muffle furnaces by the carborundum plate performed polymer that step (1) is obtained
Pre-oxidation carborundum plate material is prepared, then again pre-oxidation carborundum plate in nitrogen atmosphere in middle pre-oxidation 1h~5h
Under the conditions of 1100~1200 DEG C calcine 1.5~2.5h, be then transferred into argon gas atmosphere, then at 1500~1650 DEG C calcining 1~
Carborundum plate is prepared in 1.5h；
Using first step pre-oxidation in polyacrylonitrile structure nitrogen and flammable hydrogen remove, while making polyacrylonitrile itself
Porous structure be further formed, be conducive to later stage calcination process, while in second nitrogen protection calcination process, utilizing high temperature item
Carbon source and silicon source are reacted under part, promote to produce silicon carbide precursor, while nitrogen protection process keeps carbon monoxide quick
Take away, avoid another secondary response, further high-temperature burning process, not only makes carborundum crystals produce in argon inert gas
It is more perfect, while system hole can also be reduced, improve the compactness of carborundum plate, be conducive to improve the machinery of carborundum plate
Performance；
Fig. 1 is a kind of XRD diffracting spectrums of carborundum plate manufacture of this patent；
Wherein 1 is the XRD diffraction maximums of silica, is 20.8 ° for 2 θ；2 be carbon in carbon fibre material after high-temperature calcination
XRD diffraction maximums, wherein 2 θ be 26.4 °；3 be the XRD diffraction maximums of silicon carbide, wherein producing the distinctive XRD diffraction of silicon carbide
Peak, for 2 θ be 35.6 °, 42.3 °, 60.0 ° and 71.8 ° its it is corresponding respectively in 111,200,220 and 311 crystal faces in silicon carbide,
Therefore production silicon carbide plank.
Embodiment 2
A kind of carborundum plate product, thickness are 0.5~50mm, and density is 2.70~2.85g/cm3, compressive resistance 100~
130MPa, 45~60MPa of flexural strength.
A kind of processing method of carborundum plate product, the specific steps are：
(1) preparation of carborundum plate performed polymer
Using polyacrylonitrile as carbon source, using the aqueous solution of n,N-Dimethylformamide as mixed solvent, using metasilicic acid as silicon source,
Carbon source and silicon source are dissolved in the mixed solvent at normal temperatures, the solidification stoste that viscosity is 50~100Pas is prepared, so
Again that the extruded die orifice extrusion of solidification stoste is preforming afterwards, preforming solidification stoste is cooled down through air section, then solidifying through sodium sulphate
Admittedly bathing solution, then after washing solidifies, then it is air-dried again at 145~155 DEG C, the residence time is that 45~60s is carbonized
Silicon plate performed polymer；
The mass values of the metasilicic acid and polyacrylonitrile are 1: 35；
The polyacrylonitrile is 20% in the mass concentration of in the mixed solvent；
The volume ratio of the in the mixed solvent n,N-Dimethylformamide and water is 1: 0.15；
Stoste is solidified in the preform process in 65~85 DEG C of the temperature of extrusion mould-outlet, the pump of extrusion is for amount
The thickness of 10~5000mL/min, extrusion mould-outlet are 0.75~75mm；
The air section cooling temperature is 20~25 DEG C, and the air section residence time is 10~15cm；
Sodium sulfate quality a concentration of 10~20% in the coagulating bath, solidification stoste is in the coagulating bath residence time 30~45
Second；The residence time is 10~15 seconds in water-washing process；
Polyacrylonitrile has abundant carbon source structure, is usually used in preparing the materials such as carbon fiber；Using the method for solution blending,
Polyacrylonitrile is mixed with material metasilicic acid, material is made to achieve the purpose that evenly dispersed and be blended；And metasilicic acid its
Itself has abundant element silicon, and can dissolve in aqueous solution, while metasilicic acid generates in the material containing sodium salt
Inorganic material sodium metasilicate, to realize, sodium metasilicate is precipitated while polyacrylonitrile solidifies, and to fixed silicon source material, keeps away
Exempt from the loss of later stage washing silicon source material, while may also reach up the purpose of even solidification, avoids being precipitated due to carbon source and silicon source
Object not to step, make the growth course of carborundum crystals in calcination process, and the silicon carbide whisker volume defect of part and after reducing
The yield rate of phase product；Avoid current silicon carbide articles using the method for solution blending needs high speed permanent in sintering procedure
Process of lapping, while sintering process activation energy is excessive between also solving the inorganic particle of multi phase state structure, and waste of energy,
And the self aggregation state of inorganic particle itself causes to easy to produce local defect in production process of plate, influences the finished product of product
Rate；
Using metasilicic acid material, using the silicon source structure that metasilicic acid is abundant, while polyacrylonitrile solidifies and sodium sulphate
Structure is silicon source and carbon source carries out blending process of setting, and generates silica at a temperature of 150 DEG C conducive to sodium metasilicate,
To achieve the purpose that carbon source and the evenly dispersed precipitation of silicon source, avoid phase itself existing for direct physical blending is difficult to phase
Hold, interface is excessive and the problem of be difficult to calcine forming；
(2) preparation of carborundum plate
Carborundum plate performed polymer is placed on 260~280 DEG C of Muffle furnaces by the carborundum plate performed polymer that step (1) is obtained
Pre-oxidation carborundum plate material is prepared, then again pre-oxidation carborundum plate in nitrogen atmosphere in middle pre-oxidation 1h~5h
Under the conditions of 1100~1200 DEG C calcine 1.5~2.5h, be then transferred into argon gas atmosphere, then at 1500~1650 DEG C calcining 1~
Carborundum plate is prepared in 1.5h；
Using first step pre-oxidation in polyacrylonitrile structure nitrogen and flammable hydrogen remove, while making polyacrylonitrile itself
Porous structure be further formed, be conducive to later stage calcination process, while in second nitrogen protection calcination process, utilizing high temperature item
Carbon source and silicon source are reacted under part, promote to produce silicon carbide precursor, while nitrogen protection process keeps carbon monoxide quick
Take away, avoid another secondary response, further high-temperature burning process, not only makes carborundum crystals produce in argon inert gas
It is more perfect, while system hole can also be reduced, improve the compactness of carborundum plate, be conducive to improve the machinery of carborundum plate
Performance；
Embodiment 3
A kind of carborundum plate product, thickness are 0.5~50mm, and density is 2.70~2.85g/cm3, compressive resistance 100~
130MPa, 45~60MPa of flexural strength.
A kind of processing method of carborundum plate product, the specific steps are：
(1) preparation of carborundum plate performed polymer
Using polyacrylonitrile as carbon source, using the aqueous solution of n,N-Dimethylformamide as mixed solvent, using metasilicic acid as silicon source,
Carbon source and silicon source are dissolved in the mixed solvent at normal temperatures, the solidification stoste that viscosity is 50~100Pas is prepared, so
Again that the extruded die orifice extrusion of solidification stoste is preforming afterwards, preforming solidification stoste is cooled down through air section, then solidifying through sodium sulphate
Admittedly bathing solution, then after washing solidifies, then it is air-dried again at 145~155 DEG C, the residence time is that 45~60s is carbonized
Silicon plate performed polymer；
The mass values of the metasilicic acid and polyacrylonitrile are 1: 50；
The polyacrylonitrile is 30% in the mass concentration of in the mixed solvent；
The volume ratio of the in the mixed solvent n,N-Dimethylformamide and water is 1: 0.20；
Stoste is solidified in the preform process in 65~85 DEG C of the temperature of extrusion mould-outlet, the pump of extrusion is for amount
The thickness of 10~5000mL/min, extrusion mould-outlet are 0.75~75mm；
The air section cooling temperature is 20~25 DEG C, and the air section residence time is 10~15cm；
Sodium sulfate quality a concentration of 10~20% in the coagulating bath, solidification stoste is in the coagulating bath residence time 30~45
Second；The residence time is 10~15 seconds in water-washing process；
Polyacrylonitrile has abundant carbon source structure, is usually used in preparing the materials such as carbon fiber；Using the method for solution blending,
Polyacrylonitrile is mixed with material metasilicic acid, material is made to achieve the purpose that evenly dispersed and be blended；And metasilicic acid its
Itself has abundant element silicon, and can dissolve in aqueous solution, while metasilicic acid generates in the material containing sodium salt
Inorganic material sodium metasilicate, to realize, sodium metasilicate is precipitated while polyacrylonitrile solidifies, and to fixed silicon source material, keeps away
Exempt from the loss of later stage washing silicon source material, while may also reach up the purpose of even solidification, avoids being precipitated due to carbon source and silicon source
Object it is asynchronous, make the growth course of carborundum crystals in calcination process, and the silicon carbide whisker volume defect of part and after reducing
The yield rate of phase product；Avoid current silicon carbide articles using the method for solution blending needs high speed permanent in sintering procedure
Process of lapping, while sintering process activation energy is excessive between also solving the inorganic particle of multi phase state structure, and waste of energy,
And the self aggregation state of inorganic particle itself causes to easy to produce local defect in production process of plate, influences the finished product of product
Rate；
Using metasilicic acid material, using the silicon source structure that metasilicic acid is abundant, while polyacrylonitrile solidifies and sodium sulphate
Structure is silicon source and carbon source carries out blending process of setting, and generates silica at a temperature of 150 DEG C conducive to sodium metasilicate,
To achieve the purpose that carbon source and the evenly dispersed precipitation of silicon source, avoid phase itself existing for direct physical blending is difficult to phase
Hold, interface is excessive and the problem of be difficult to calcine forming；
(2) preparation of carborundum plate
Carborundum plate performed polymer is placed on 260~280 DEG C of Muffle furnaces by the carborundum plate performed polymer that step (1) is obtained
Pre-oxidation carborundum plate material is prepared, then again pre-oxidation carborundum plate in nitrogen atmosphere in middle pre-oxidation 1h~5h
Under the conditions of 1100~1200 DEG C calcine 1.5~2.5h, be then transferred into argon gas atmosphere, then at 1500~1650 DEG C calcining 1~
Carborundum plate is prepared in 1.5h；
Using first step pre-oxidation in polyacrylonitrile structure nitrogen and flammable hydrogen remove, while making polyacrylonitrile itself
Porous structure be further formed, be conducive to later stage calcination process, while in second nitrogen protection calcination process, utilizing high temperature item
Carbon source and silicon source are reacted under part, promote to produce silicon carbide precursor, while nitrogen protection process keeps carbon monoxide quick
Take away, avoid another secondary response, further high-temperature burning process, not only makes carborundum crystals produce in argon inert gas
It is more perfect, while system hole can also be reduced, improve the compactness of carborundum plate, be conducive to improve the machinery of carborundum plate
Performance；
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
Member, without departing from the inventive concept of the premise, can also make several improvements and modifications, these improvements and modifications also should be regarded as
In protection scope of the present invention.
Claims (6)
1. a kind of processing method of carborundum plate product, which is characterized in that its specific steps are：
（One）The preparation of carborundum plate performed polymer
Using polyacrylonitrile as carbon source, using the aqueous solution of n,N-Dimethylformamide as mixed solvent, using metasilicic acid as silicon source, normal
Carbon source and silicon source are dissolved in the mixed solvent under temperature, the solidification stoste that viscosity is 50~100Pas is prepared, then again
The extruded die orifice extrusion of solidification stoste is preforming, and preforming solidification stoste is cooled down through air section, then through sodium sulphate coagulating bath
Solution, then after washing solidifies, be then air-dried again at 145~155 DEG C, the residence time is that 45~60s obtains carborundum plate
Performed polymer；
（Two）The preparation of carborundum plate
Step（One）Carborundum plate performed polymer is placed in 260~280 DEG C of Muffle furnaces in advance by obtained carborundum plate performed polymer
1h~5h is aoxidized, pre-oxidation carborundum plate material is prepared, then again pre-oxidation carborundum plate 1100 in nitrogen atmosphere
1.5~2.5h is calcined under the conditions of~1200 DEG C, is then transferred into argon gas atmosphere, then 1~1.5h is calcined at 1500~1650 DEG C,
Carborundum plate is prepared.
2. a kind of processing method of carborundum plate product as described in claim 1, which is characterized in that in carborundum plate performed polymer
Preparation in, the mass values of the metasilicic acid and polyacrylonitrile are 1:25~1:50.
3. a kind of processing method of carborundum plate product as described in claim 1, which is characterized in that in carborundum plate performed polymer
Preparation in, the polyacrylonitrile in the mixed solvent mass fraction be 15~30%.
4. a kind of processing method of carborundum plate product as described in claim 1, which is characterized in that in carborundum plate performed polymer
Preparation in, the volume ratio of the in the mixed solvent n,N-Dimethylformamide and water is 1:0.05~1:0.20.
5. a kind of processing method of carborundum plate product as described in claim 1, which is characterized in that in carborundum plate performed polymer
Preparation in, stoste is solidified in the preform process in 65~85 DEG C of the temperature of extrusion mould-outlet, the pump of extrusion is for amount
Thickness for 10~5000 mL/min, extrusion mould-outlet is 0.75~75mm.
6. a kind of processing method of carborundum plate product as described in claim 1, which is characterized in that in carborundum plate performed polymer
Preparation in, in the coagulating bath sodium sulfate quality score be 10~20%, solidification stoste in the coagulating bath residence time 30~45
Second；The residence time is 10~15 seconds in water-washing process.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1793038A (en) * | 2005-11-18 | 2006-06-28 | 清华大学 | Process for sintering Sialong binding silicon carbide refractory by microwave tech. |
| CN101423412A (en) * | 2008-11-27 | 2009-05-06 | 中钢集团洛阳耐火材料研究院有限公司 | Method for preparing high performance silicon oxide combining silicon carbide refractory by low-temperature sintering |
| CN103833365A (en) * | 2012-11-29 | 2014-06-04 | 宜兴中村窑业有限公司 | High-temperature-resistant energy-saving silicon carbide plate and preparation method thereof |
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| JPS60226406A (en) * | 1984-04-23 | 1985-11-11 | Natl Inst For Res In Inorg Mater | Preparation of beta-silicon carbide |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1793038A (en) * | 2005-11-18 | 2006-06-28 | 清华大学 | Process for sintering Sialong binding silicon carbide refractory by microwave tech. |
| CN101423412A (en) * | 2008-11-27 | 2009-05-06 | 中钢集团洛阳耐火材料研究院有限公司 | Method for preparing high performance silicon oxide combining silicon carbide refractory by low-temperature sintering |
| CN103833365A (en) * | 2012-11-29 | 2014-06-04 | 宜兴中村窑业有限公司 | High-temperature-resistant energy-saving silicon carbide plate and preparation method thereof |
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| SiO2－SiC棚板的性能优化研究;陈永强等;《耐火材料》;20140831;第48卷(第4期);第285～287页 * |
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