CN107540383B - The preparation method of silicon nitride combined silicon carbide refractory with double dispersing characteristics - Google Patents
The preparation method of silicon nitride combined silicon carbide refractory with double dispersing characteristics Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of silicon nitride combined silicon carbide refractory with double dispersing characteristics, include the following steps: the preparation of 1) initial slurry；2) preparation of primary billet；3) it nitrogenizes for the first time；4) preparation of intermediate pulp；5) preparation of intermediate green body；6) it nitrogenizes for second.Silicon nitride combined silicon carbide refractory prepared by the present invention, carbofrax strengthening particle has double dispersed distribution features, more traditional supercharged steam generator silicon nitride combined silicon carbide refractory, effectively improve its fracture toughness, and then improve its thermal shock resistance, the service life for extending burner hearth refractory brick in supercharged steam generator, improves the safety in utilization and reliability of dynamical system peculiar to vessel.
Description
Technical field
The present invention relates to technical field of fire resistant material production, and in particular to a kind of silicon nitride bonded silicon with double dispersing characteristics
The preparation method of silicon carbide refractory ceramics.
Background technique
Refractory brick for high-temperature hot protection is of crucial importance for Turbo-charged Marine Boiler, increases in the burner hearth of Turbo-charged Marine Boiler
Compression ignition is burnt, and maximum temperature can achieve 2000 DEG C, and heat flow density is up to about 20MW/m3, and wash away with high-speed flame and frequency
Numerous thermal shock proposes very harsh requirement to its refractory material.The failure of refractory material will result directly in boiler in burner hearth
Failure simultaneously loses ship power, and the performance of refractory material affects the security reliability of shiphoard machinery system.Silicon nitride bonded silicon
Thyrite is chosen as the raw material of refractory brick by its excellent high-temperature behavior.
However, the existing silicon nitride combined silicon carbide refractory in Turbo-charged Marine Boiler, is silicon carbide millimeter
Grade partial size bulky grain is dispersed in matrix, meets the requirement of above-mentioned use environment to a certain extent.But due to using ring
Thermal expansion between frequent thermal shock in border, and enhancing particle and matrix mismatches caused thermal stress, leads in use process
It causes crack initiation and extends, unexpected fracture failure can be caused in the thermal shock use environment of supercharged steam generator repeatedly.Due to milli
The presence of meter level silicon carbide bulky grain more exacerbates the unmatched consequence of above-mentioned thermal expansion, and thermal shock failure is caused to accelerate.Therefore it is existing
Some Turbo-charged Marine Boiler silicon nitride combined silicon carbide refractories, which remain, easily germinates fine fisssure under thermal shock use condition
Line extends the defect for causing service life to fall short of.
Summary of the invention
Present invention aims to overcome that the deficiency of above-mentioned background technique, and provide that a kind of thermal shock resistance is strong, service life
The preparation method of the long silicon nitride combined silicon carbide refractory with double dispersing characteristics.
To achieve the above object, the silicon nitride combined silicon carbide refractory with double dispersing characteristics provided by the present invention
Preparation method, include the following steps:
1) it the preparation of initial slurry: takes carborundum coarse particle, carbonization silicon fine particle, silicon powder to be placed in container, is added and combines
Agent, the dry-mixed stirring of dispersing agent, add water and stir, obtain initial slurry；
2) preparation of primary billet: by compression moulding after step 1) resulting initial slurry injection mold, then through at dry
Reason, obtains primary billet；
3) it nitrogenizes for the first time: first time nitrogen treatment will be carried out in the resulting primary billet merging nitriding furnace of step 2), then
It cools to room temperature with the furnace, finally takes out product successively by smashing, being ground up, sieved processing, obtain enhancing particle；
4) preparation of intermediate pulp: by the resulting enhancing particle of step 3) and carbonization silicon fine particle, silicon powder, bonding agent, divide
The dry-mixed stirring of powder, adds water and stirs, obtain intermediate pulp；
5) preparation of intermediate green body: by compression moulding after the resulting intermediate pulp injection mold of step 4), then through at dry
Reason, obtains intermediate green body；
6) it nitrogenizes for second: the resulting intermediate green body merging nitriding furnace of step 5) being subjected to second of nitrogen treatment, finally
Cool to room temperature with the furnace.
Further, in the step 1), carborundum coarse particle: carbonization silicon fine particle: silicon powder: bonding agent: dispersing agent
Mass ratio is 6~10:5:1:0.1~0.3:0.1~0.3.
Further, in the step 1), carborundum coarse particle is technical grade black silicon carbide coarse granule, and the technical grade is black
The partial size of carborundum coarse particle is 0.3~0.6mm, and purity is higher than 98%.
Further, in the step 3), the temperature program of first time nitrogen treatment are as follows: risen within the scope of room temperature~1000 DEG C
Warm rate is 17 DEG C/min, and 1000 DEG C~1300 DEG C heating rates are 2.5 DEG C/min, 1300~1400 DEG C of heating rates are 2 DEG C/
Min, 1400 DEG C of 1~3h of heat preservation, finally cools to room temperature with the furnace.
Further, in the step 3), the partial size for enhancing particle is 2~4mm.
Further, in the step 4), in the step 4), enhance particle: carbonization silicon fine particle: silicon powder: bonding agent:
The mass ratio of dispersing agent is 4~8:6:1:0.1~0.3:0.1~0.3.
Further, in the step 1) and step 4), bonding agent is hydrated alumina, aluminous cement, phenolic resin
One of or it is a variety of.
Further, in the step 1) and step 4), dispersing agent is polyethyleneimine, polyvinyl alcohol, ammonium polyacrylate
One of or it is a variety of.
Still further, the silicon fine particle that is carbonized is by technical grade black silicon carbide fine grained, carbon in the step 1) and step 4)
SiClx superfine powder, SiC nano-powder are mixed according to 10~14:1:1 of mass ratio, wherein technical grade black silicon carbide fine grained
Partial size be 0.1~0.5mm, purity be higher than 98%；The silicon powder is the metallic silicon power of 98% or more purity, the silicon powder partial size
For 240 mesh；The partial size of the carbide fine powder is 200~240 mesh, and the partial size of the silicon carbide micro-powder is 1.0~3.0 μm.
Preferably, in the step 1) and step 4), the silicon fine particle that is carbonized is by technical grade black silicon carbide fine grained, silicon carbide
Superfine powder, SiC nano-powder are mixed according to 12~13:1:1 of mass ratio, wherein the fine grain grain of technical grade black silicon carbide
Diameter is 0.2~0.3mm, and purity is higher than 98%；The silicon powder is the metallic silicon power of 98% or more purity, and the silicon powder partial size is
240 mesh；The partial size of the carbide fine powder is 200~240 mesh, and the partial size of the silicon carbide micro-powder is 2.0~2.5 μm.
Further, in the step 4), the temperature program of second of nitrogen treatment are as follows: within the scope of room temperature~1000 DEG C
Heating rate is 17 DEG C/min；1000 DEG C~1300 DEG C heating rates are 2.5 DEG C/min, and 1300~1400 DEG C of heating rates are 2
DEG C/min, 1400 DEG C of 10~40h of heat preservation, last furnace cooling to room temperature.
Compared with prior art, there are following advantages by the present invention:
Carbofrax strengthening particle is in double dispersions in silicon nitride combined silicon carbide refractory made from preparation method of the present invention
Feature distribution can be improved its fracture toughness, compared with existing silicon nitride combined silicon carbide refractory, have preferably anti-
Thermal shock resistance properties, so extend supercharged steam generator in burner hearth refractory brick service life, improve dynamical system peculiar to vessel using safe
Property and reliability.In addition, the raw material sources of preparation method of the present invention are easy to get extensively, simple process is suitable for mass production.
Detailed description of the invention
Fig. 1 is traditional carbofrax strengthening particle monodisperse feature distribution schematic diagram；
Fig. 2 is the double dispersing character distribution schematic diagrams of carbofrax strengthening particle of the invention.
Specific embodiment
Below with reference to the embodiment performance that the present invention will be described in detail, but they and do not constitute a limitation of the invention,
It is only for example.Simultaneously by illustrating that advantages of the present invention will become clearer and be readily appreciated that.
Embodiment 1:
It is that 8:5:1:0.1:0.1 takes carborundum coarse particle, carbonization silicon fine particle, silicon powder, hydrated alumina according to mass ratio
(bonding agent) and polyethyleneimine (dispersing agent) is put into stirring-type batch mixer, dry-mixed 10 minutes, is then added with uniform speed
It is approximately equal to the moisture content of said mixture gross mass 8%, stirs 2 minutes and discharge, obtain initial slurry.Initial slurry is injected into mold
Compression moulding afterwards, after be dried to obtain primary billet.Primary billet after molding is put into nitriding furnace and is carried out at first time nitridation
It manages, heating rate is 17 DEG C/min within the scope of 20~1000 DEG C, and 1000 DEG C~1300 DEG C heating rates are 2.5 DEG C/min, 1300-
1400 DEG C of heating rates are 2 DEG C/min, 1400 DEG C of heat preservation 2h, last furnace cooling to room temperature.By first time, the product of nitridation is beaten
Broken, grinding, sieving obtains the enhancing particle having a size of 3mm.It is that 6:6:1:0.1:0.1 takes enhancing particle, carbonization according to mass ratio
Silicon fine particle, silicon powder, hydrated alumina (bonding agent) and polyethyleneimine (dispersing agent), are put into stirring-type batch mixer, and dry-mixed 10
Minute, it is then added with uniform speed and is approximately equal to the moisture content of said mixture gross mass 8%, stir 2 minutes and discharge, obtained
Between slurry.By intermediate pulp inject mold after compression moulding, after be dried to obtain intermediate green body.Intermediate green body after molding is put into
Second of nitrogen treatment is carried out in nitriding furnace, within the scope of 20~1000 DEG C heating rate be 17 DEG C/min, 1000 DEG C~1300 DEG C
Heating rate is 2.5 DEG C/min, and 1300-1400 DEG C of heating rate is 2 DEG C/min, 1400 DEG C of heat preservation 20h, and last furnace cooling is arrived
The silicon nitride combined silicon carbide refractory with double dispersing characteristics can be obtained in room temperature.
Embodiment 2:
It is that 10:5:1:0.3:0.3 takes carborundum coarse particle, carbonization silicon fine particle, silicon powder, hydrated alumina according to mass ratio
(bonding agent) and polyethyleneimine (dispersing agent) is put into stirring-type batch mixer, dry-mixed 10 minutes, is then added with uniform speed
It is approximately equal to the moisture content of said mixture gross mass 8%, stirs 2 minutes and discharge, obtain initial slurry.Initial slurry is injected into mold
Compression moulding afterwards, after be dried to obtain primary billet.Primary billet after molding is put into nitriding furnace and is carried out at first time nitridation
It manages, heating rate is 17 DEG C/min within the scope of 20~1000 DEG C, and 1000 DEG C~1300 DEG C heating rates are 2.5 DEG C/min, 1300-
1400 DEG C of heating rates are 2 DEG C/min, 1400 DEG C of heat preservation 1h, last furnace cooling to room temperature.By first time, the product of nitridation is beaten
Broken, grinding, sieving obtains the enhancing particle having a size of 3mm.It is that 4:6:1:0.3:0.3 takes enhancing particle, carbonization according to mass ratio
Silicon fine particle, silicon powder, hydrated alumina (bonding agent) and polyethyleneimine (dispersing agent), are put into stirring-type batch mixer, and dry-mixed 10
Minute, it is then added with uniform speed and is approximately equal to the moisture content of said mixture gross mass 8%, stir 2 minutes and discharge, obtained
Between slurry.By intermediate pulp inject mold after compression moulding, after be dried to obtain intermediate green body.Intermediate green body after molding is put into
Second of nitrogen treatment is carried out in nitriding furnace, heating rate is 17 DEG C/min within the scope of 20~1000 DEG C；1000 DEG C~1300 DEG C
Heating rate is 2.5 DEG C/min, and 1300-1400 DEG C of heating rate is 2 DEG C/min, 1400 DEG C of heat preservation 40h, and last furnace cooling is arrived
The silicon nitride combined silicon carbide refractory with double dispersing characteristics can be obtained in room temperature.
Embodiment 3:
It is that 6:5:1:0.2:0.2 takes carborundum coarse particle, carbonization silicon fine particle, silicon powder, hydrated alumina according to mass ratio
(bonding agent) and polyethyleneimine (dispersing agent) is put into stirring-type batch mixer, dry-mixed 10 minutes, is then added with uniform speed
It is approximately equal to the moisture content of said mixture gross mass 8%, stirs 2 minutes and discharge, obtain initial slurry.Initial slurry is injected into mold
Compression moulding afterwards, after be dried to obtain primary billet.Primary billet after molding is put into nitriding furnace and is carried out at first time nitridation
It manages, heating rate is 17 DEG C/min within the scope of 20~1000 DEG C, and 1000 DEG C~1300 DEG C heating rates are 2.5 DEG C/min, 1300-
1400 DEG C of heating rates are 2 DEG C/min, 1400 DEG C of heat preservation 3h, last furnace cooling to room temperature.By first time, the product of nitridation is beaten
Broken, grinding, sieving obtains the enhancing particle having a size of 3mm.It is that 8:6:1:0.2:0.2 takes enhancing particle, carbonization according to mass ratio
Silicon fine particle, silicon powder, hydrated alumina (bonding agent) and polyethyleneimine (dispersing agent), are put into stirring-type batch mixer, and dry-mixed 10
Minute, it is then added with uniform speed and is approximately equal to the moisture content of said mixture gross mass 8%, stir 2 minutes and discharge, obtained
Between slurry.By intermediate pulp inject mold after compression moulding, after be dried to obtain intermediate green body.Intermediate green body after molding is put into
Second of nitrogen treatment is carried out in nitriding furnace, within the scope of 20~1000 DEG C heating rate be 17 DEG C/min, 1000 DEG C~1300 DEG C
Heating rate is 2.5 DEG C/min, and 1300-1400 DEG C of heating rate is 2 DEG C/min, 1400 DEG C of heat preservation 20h, and last furnace cooling is arrived
The silicon nitride combined silicon carbide refractory with double dispersing characteristics can be obtained in room temperature.
Embodiment 4:
It is that 6:5:1:0.1:0.3 takes carborundum coarse particle, carbonization silicon fine particle, silicon powder, aluminous cement according to mass ratio
(bonding agent) and polyvinyl alcohol (dispersing agent) is put into stirring-type batch mixer, dry-mixed 10 minutes, is then added about with uniform speed
Equal to the moisture content of said mixture gross mass 8%, stirs 2 minutes and discharge, obtain initial slurry.After initial slurry is injected mold
Compression moulding, after be dried to obtain primary billet.Primary billet after molding is put into progress first time nitrogen treatment in nitriding furnace,
Heating rate is 17 DEG C/min within the scope of 20~1000 DEG C, and 1000 DEG C~1300 DEG C heating rates are 2.5 DEG C/min, 1300-
1400 DEG C of heating rates are 2 DEG C/min, 1400 DEG C of heat preservation 3h, last furnace cooling to room temperature.By first time, the product of nitridation is beaten
Broken, grinding, sieving obtains the enhancing particle having a size of 3mm.It is that 8:6:1:0.1:0.3 takes enhancing particle, carbonization according to mass ratio
Silicon fine particle, silicon powder, aluminous cement (bonding agent) and polyvinyl alcohol (dispersing agent), are put into stirring-type batch mixer, and dry-mixed 10 points
Then the moisture content for being approximately equal to said mixture gross mass 8% is added in clock with uniform speed, stir 2 minutes and discharge, obtain centre
Slurry.By intermediate pulp inject mold after compression moulding, after be dried to obtain intermediate green body.Intermediate green body after molding is put into nitrogen
Change in furnace and carry out second of nitrogen treatment, heating rate is 17 DEG C/min within the scope of 20~1000 DEG C, and 1000 DEG C~1300 DEG C rise
Warm rate is 2.5 DEG C/min, and 1300-1400 DEG C of heating rate is 2 DEG C/min, 1400 DEG C of heat preservation 20h, last furnace cooling to room
The silicon nitride combined silicon carbide refractory with double dispersing characteristics can be obtained in temperature.
Embodiment 5:
It is that 6:5:1:0.3:0.1 takes carborundum coarse particle, carbonization silicon fine particle, silicon powder, phenolic resin (knot according to mass ratio
Mixture) and ammonium polyacrylate (dispersing agent), it is put into stirring-type batch mixer, dry-mixed 10 minutes, is then added about with uniform speed
Equal to the moisture content of said mixture gross mass 8%, stirs 2 minutes and discharge, obtain initial slurry.After initial slurry is injected mold
Compression moulding, after be dried to obtain primary billet.Primary billet after molding is put into progress first time nitrogen treatment in nitriding furnace,
Heating rate is 17 DEG C/min within the scope of 20~1000 DEG C, and 1000 DEG C~1300 DEG C heating rates are 2.5 DEG C/min, 1300-
1400 DEG C of heating rates are 2 DEG C/min, 1400 DEG C of heat preservation 3h, last furnace cooling to room temperature.By first time, the product of nitridation is beaten
Broken, grinding, sieving obtains the enhancing particle having a size of 3mm.It is that 4:6:1:0.3:0.1 takes enhancing particle, carbonization according to mass ratio
Silicon fine particle, silicon powder, phenolic resin and ammonium polyacrylate, are put into stirring-type batch mixer, and dry-mixed 10 minutes, then with uniform speed
The moisture content for being approximately equal to said mixture gross mass 8% is added in degree, stirs 2 minutes and discharges, obtains intermediate pulp.Intermediate pulp is infused
Enter compression moulding after mold, after be dried to obtain intermediate green body.Intermediate green body after molding is put into nitriding furnace and is carried out second
Nitrogen treatment, heating rate is 17 DEG C/min within the scope of 20~1000 DEG C, 1000 DEG C~1300 DEG C heating rates are 2.5 DEG C/
Min, 1300-1400 DEG C of heating rates are 2 DEG C/min, 1400 DEG C of heat preservation 10h, and tool can be obtained in last furnace cooling to room temperature
There is the silicon nitride combined silicon carbide refractory of double dispersing characteristics.
Embodiment 6:
It is that 6:5:1:0.3:0.1 takes carborundum coarse particle, carbonization silicon fine particle, silicon powder, bonding agent (hydration according to mass ratio
Aluminium oxide, aluminous cement, phenolic resin are mixed according to mass ratio 1:2:3) and dispersing agent (polyethyleneimine, polyethylene
Alcohol, ammonium polyacrylate are mixed according to mass ratio 1:2:3), it is put into stirring-type batch mixer, dry-mixed 10 minutes, then with uniform
Speed be added and be approximately equal to the moisture content of said mixture gross mass 8%, stir 2 minutes and discharge, obtain initial slurry.It will initially starch
Material injection mold after compression moulding, after be dried to obtain primary billet.Primary billet after molding is put into nitriding furnace and carries out
Nitrogen treatment, heating rate is 17 DEG C/min within the scope of 20~1000 DEG C, and 1000 DEG C~1300 DEG C heating rates are 2.5
DEG C/min, 1300-1400 DEG C of heating rate is 2 DEG C/min, 1400 DEG C of heat preservation 3h, last furnace cooling to room temperature.It will be for the first time
The product of nitridation is smashed, and grinding, sieving obtains the enhancing particle having a size of 3mm.It is that 4:6:1:0.3:0.1 takes increasing according to mass ratio
Strong particle, carbonization silicon fine particle, silicon powder, (hydrated alumina, aluminous cement, phenolic resin are according to mass ratio 1:2:3 for bonding agent
Mix) and (polyethyleneimine, polyvinyl alcohol, ammonium polyacrylate are mixed according to mass ratio 1:2:3), it is put into stirring-type
Batch mixer dry-mixed 10 minutes, is added the moisture content for being approximately equal to said mixture gross mass 8% then with uniform speed, stirs 2 points
Clock discharging, obtains intermediate pulp.By intermediate pulp inject mold after compression moulding, after be dried to obtain intermediate green body.After forming
Intermediate green body be put into nitriding furnace and carry out second of nitrogen treatment, heating rate is 17 DEG C/min within the scope of 20~1000 DEG C,
1000 DEG C~1300 DEG C heating rates are 2.5 DEG C/min, and 1300-1400 DEG C of heating rate is 2 DEG C/min, 1400 DEG C of heat preservation 10h,
The silicon nitride combined silicon carbide refractory with double dispersing characteristics can be obtained to room temperature in last furnace cooling.
Embodiment 7:
It is that 6:5:1:0.2:0.2 takes carborundum coarse particle, carbonization silicon fine particle, silicon powder, bonding agent (hydration according to mass ratio
Aluminium oxide, aluminous cement, phenolic resin are mixed according to mass ratio 1:1:1) and dispersing agent (polyethyleneimine, polyethylene
Alcohol, ammonium polyacrylate are mixed according to mass ratio 1:1:1), it is put into stirring-type batch mixer, dry-mixed 10 minutes, then with uniform
Speed be added and be approximately equal to the moisture content of said mixture gross mass 8%, stir 2 minutes and discharge, obtain initial slurry.It will initially starch
Material injection mold after compression moulding, after be dried to obtain primary billet.Primary billet after molding is put into nitriding furnace and carries out
Nitrogen treatment, heating rate is 17 DEG C/min within the scope of 20~1000 DEG C, and 1000 DEG C~1300 DEG C heating rates are 2.5
DEG C/min, 1300-1400 DEG C of heating rate is 2 DEG C/min, 1400 DEG C of heat preservation 3h, last furnace cooling to room temperature.It will be for the first time
The product of nitridation is smashed, and grinding, sieving obtains the enhancing particle having a size of 3mm.It is that 4:6:1:0.2:0.2 takes increasing according to mass ratio
Strong particle, carbonization silicon fine particle, silicon powder, (hydrated alumina, aluminous cement, phenolic resin are according to mass ratio 1:1:1 for bonding agent
Mix) and (polyethyleneimine, polyvinyl alcohol, ammonium polyacrylate are mixed according to mass ratio 1:1:1), it is put into stirring-type
Batch mixer dry-mixed 10 minutes, is added the moisture content for being approximately equal to said mixture gross mass 8% then with uniform speed, stirs 2 points
Clock discharging, obtains intermediate pulp.By intermediate pulp inject mold after compression moulding, after be dried to obtain intermediate green body.After forming
Intermediate green body be put into nitriding furnace and carry out second of nitrogen treatment, heating rate is 17 DEG C/min within the scope of 20~1000 DEG C,
1000 DEG C~1300 DEG C heating rates are 2.5 DEG C/min, and 1300-1400 DEG C of heating rate is 2 DEG C/min, 1400 DEG C of heat preservation 10h,
The silicon nitride combined silicon carbide refractory with double dispersing characteristics can be obtained to room temperature in last furnace cooling.
Embodiment 8:
It is that 8:5:1:0.2:0.2 takes carborundum coarse particle, carbonization silicon fine particle, silicon powder, bonding agent (hydration according to mass ratio
Aluminium oxide, aluminous cement are mixed according to mass ratio 1:2) and dispersing agent (polyethyleneimine, polyvinyl alcohol, polyacrylic acid
Ammonium is mixed according to mass ratio 1:4:5), it is put into stirring-type batch mixer, dry-mixed 10 minutes, is then added about with uniform speed
Equal to the moisture content of said mixture gross mass 8%, stirs 2 minutes and discharge, obtain initial slurry.After initial slurry is injected mold
Compression moulding, after be dried to obtain primary billet.Primary billet after molding is put into progress first time nitrogen treatment in nitriding furnace,
Heating rate is 17 DEG C/min within the scope of 20~1000 DEG C, and 1000 DEG C~1300 DEG C heating rates are 2.5 DEG C/min, 1300-
1400 DEG C of heating rates are 2 DEG C/min, 1400 DEG C of heat preservation 3h, last furnace cooling to room temperature.By first time, the product of nitridation is beaten
Broken, grinding, sieving obtains the enhancing particle having a size of 3mm.It is that 6:6:1:0.2:0.2 takes enhancing particle, carbonization according to mass ratio
Silicon fine particle, silicon powder, bonding agent (hydrated alumina, aluminous cement, phenolic resin are mixed according to mass ratio 1:1:1) and
(polyethyleneimine, polyvinyl alcohol are mixed according to mass ratio 1:2), is put into stirring-type batch mixer, dry-mixed 10 minutes, then with
The moisture content for being approximately equal to said mixture gross mass 8% is added in uniform speed, stirs 2 minutes and discharges, obtains intermediate pulp.Will in
Between slurry injection mold after compression moulding, after be dried to obtain intermediate green body.By intermediate green body after molding be put into nitriding furnace into
Second of nitrogen treatment of row, heating rate is 17 DEG C/min within the scope of 20~1000 DEG C, and 1000 DEG C~1300 DEG C heating rates are
2.5 DEG C/min, 1300-1400 DEG C of heating rate is 2 DEG C/min, 1400 DEG C of heat preservation 10h, last furnace cooling to room temperature
Obtain the silicon nitride combined silicon carbide refractory with double dispersing characteristics.
In the embodiment of the present invention 1~8, carborundum coarse particle is technical grade black silicon carbide coarse granule, technical grade black silicon carbide
Coarse grained partial size is 0.3~0.6mm, and purity is higher than 98%.The partial size for enhancing particle is 2~4mm.Silicon fine particle be carbonized by work
Industry grade black silicon carbide fine grained, silicon carbide ultrafine powder, SiC nano-powder are mixed according to 10~14:1:1 of mass ratio,
In, the fine grain partial size of technical grade black silicon carbide is 0.1~0.5mm, and purity is higher than 98%；The partial size of carbide fine powder is 200
~240 mesh, the partial size of silicon carbide micro-powder are 1.0~3.0 μm.
The double dispersion implementation methods of carbofrax strengthening particle used by embodiments of the present invention, raw material sources are easy extensively
, simple process.Silicon nitride combined silicon carbide refractory prepared by the present invention, carbofrax strengthening particle have double dispersions point
Cloth feature, more traditional supercharged steam generator silicon nitride combined silicon carbide refractory effectively improve its fracture toughness, and then improve
Its thermal shock resistance, extend supercharged steam generator in burner hearth refractory brick service life, improve dynamical system peculiar to vessel using safe
Property and reliability.
The content that this specification is not described in detail belongs to the prior art well known to professional and technical personnel in the field.
Claims (9)
1. a kind of preparation method of the silicon nitride combined silicon carbide refractory with double dispersing characteristics, which is characterized in that including
Following steps:
1) it the preparation of initial slurry: takes carborundum coarse particle, carbonization silicon fine particle, silicon powder to be placed in container, bonding agent is added, divides
The dry-mixed stirring of powder, adds water and stirs, obtain initial slurry；
2) it the preparation of primary billet: by compression moulding after the resulting initial slurry injection mold of step 1), then is dried, is obtained
To primary billet；
3) it nitrogenizes for the first time: first time nitrogen treatment will be carried out in the resulting primary billet merging nitriding furnace of step 2, then with furnace
It is cooled to room temperature, finally takes out product successively by smashing, being ground up, sieved processing, obtain enhancing particle；
4) preparation of intermediate pulp: by the resulting enhancing particle of step 3) and carbonization silicon fine particle, silicon powder, bonding agent, dispersing agent
Dry-mixed stirring adds water and stirs, obtains intermediate pulp；
5) it the preparation of intermediate green body: by compression moulding after the resulting intermediate pulp injection mold of step 4), then is dried, is obtained
To intermediate green body；
6) it nitrogenizes for second: the resulting intermediate green body merging nitriding furnace of step 5) being subjected to second of nitrogen treatment, finally with furnace
It is cooled to room temperature.
2. the preparation method of the silicon nitride combined silicon carbide refractory with double dispersing characteristics according to claim 1,
It is characterized by: in the step 1), carborundum coarse particle: carbonization silicon fine particle: silicon powder: bonding agent: the mass ratio of dispersing agent
For 6 ~ 10:5:1:0.1 ~ 0.3:0.1 ~ 0.3.
3. the preparation side of the silicon nitride combined silicon carbide refractory with double dispersing characteristics according to claim 1 or 2
Method, it is characterised in that: in the step 1), carborundum coarse particle is technical grade black silicon carbide coarse granule, the black carbon of technical grade
The coarse grained partial size of SiClx is 0.3 ~ 0.6mm, and purity is higher than 98%.
4. the preparation method of the silicon nitride combined silicon carbide refractory with double dispersing characteristics according to claim 1,
It is characterized by: in the step 3), the temperature program of first time nitrogen treatment are as follows: heating rate is within the scope of 20 ~ 1000 DEG C
17 DEG C/min, 1000 DEG C ~ 1300 DEG C heating rates are 2.5 DEG C/min, and 1300 ~ 1400 DEG C of heating rates are 2 DEG C/min, 1400 DEG C
1 ~ 3h is kept the temperature, finally cools to room temperature with the furnace.
5. the preparation method of the silicon nitride combined silicon carbide refractory with double dispersing characteristics according to claim 1,
It is characterized by: the partial size for enhancing particle is 2 ~ 4mm in the step 3).
6. the preparation method of the silicon nitride combined silicon carbide refractory with double dispersing characteristics according to claim 1,
It is characterized by: in the step 4), enhance particle: carbonization silicon fine particle: silicon powder: bonding agent: the mass ratio of dispersing agent is 4 ~
8:6:1: 0.1~0.3:0.1~0.3。
7. the preparation method of the silicon nitride combined silicon carbide refractory with double dispersing characteristics according to claim 1,
It is characterized by: in the step 1) and step 4), bonding agent is hydrated alumina, aluminous cement, one in phenolic resin
Kind is a variety of.
8. the preparation method of the silicon nitride combined silicon carbide refractory with double dispersing characteristics according to claim 1,
It is characterized by: in the step 1) and step 4), dispersing agent is polyethyleneimine, polyvinyl alcohol, one in ammonium polyacrylate
Kind is a variety of.
9. the preparation method of the silicon nitride combined silicon carbide refractory with double dispersing characteristics according to claim 1,
It is characterized by: in the step 4), the temperature program of second of nitrogen treatment are as follows: heating rate is within the scope of 20 ~ 1000 DEG C
17℃/min；1000 DEG C ~ 1300 DEG C heating rates are 2.5 DEG C/min, and 1300 ~ 1400 DEG C of heating rates are 2 DEG C/min, 1400 DEG C
Keep the temperature 10 ~ 40h, last furnace cooling to room temperature.
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| CN102746013A (en) * | 2012-08-13 | 2012-10-24 | 南京工业大学 | Light high-strength silicon nitride bonded silicon carbide refractory and preparation method thereof |
| CN104744048A (en) * | 2015-03-20 | 2015-07-01 | 中原工学院 | Preparation method of compact in-situ Si4N3-SiC composite material |
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| JPS56125276A (en) * | 1980-03-06 | 1981-10-01 | Kurosaki Refractories Co | Beta-sic-si3n4 composite specific heat-resistant ceramics and manufacture |
| JPS6121976A (en) * | 1984-07-10 | 1986-01-30 | 日本重化学工業株式会社 | Manufacture of silicon nitride base sintered body |
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| CN101591187A (en) * | 2009-03-19 | 2009-12-02 | 宜兴新威利成耐火材料有限公司 | High strength silicon nitride combined silicon carbide material and preparation method thereof |
| CN102746013A (en) * | 2012-08-13 | 2012-10-24 | 南京工业大学 | Light high-strength silicon nitride bonded silicon carbide refractory and preparation method thereof |
| CN104744048A (en) * | 2015-03-20 | 2015-07-01 | 中原工学院 | Preparation method of compact in-situ Si4N3-SiC composite material |
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