CN105130445B - Method of co-sintering joined silicon-carbide-based composite ceramic green bodies - Google Patents
Method of co-sintering joined silicon-carbide-based composite ceramic green bodies Download PDFInfo
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Abstract
The invention relates to a method of co-sintering joined silicon-carbide-based composite ceramic green bodies, relates to a joint and sintering method of composite ceramic green bodies, and aims at solving the technical problem that hot stress exists during an application process due to an existing silicon carbide ceramic connection way. The method comprises the following steps: I, joining silicon-carbide-based composite material green bodies; II, heating the joined silicon-carbide composite material green bodies processed in the step I under the condition that the sintering atmosphere is argon or nitrogen and the atmospheric pressure is 0.1MPa to 0.5MPa, preserving the heat, cooling the ceramic green bodies to the room temperature along with a furnace, and obtaining silicon-carbide ceramic. The shear strength of a prepared silicon-carbide ceramic connector can reach 150MPa. The invention belongs to the field of preparation of the silicon-carbide-based composite ceramic.
Description
Technical field
The invention belongs to the connection of composite ceramicses green compact and sintering method.
Background technology
Silicon carbide ceramics is due to its excellent performance, such as high intensity, fusing point, heat conductivity so as to become 1400 DEG C
Below most valuable structural ceramic material, has a good application prospect in all kinds of engineer applieds.Due to carborundum pottery
Porcelain mainly has covalent bond and ionic bond to constitute, and its densification process is more difficult, while large scale high-compactness part or complexity
Structure silicon-carbide-based composite ceramic is difficult to prepare.This causes the application of silicon carbide ceramics to be subject to larger restriction.
Ceramic joining technology is the effective means for realizing that this kind of engineering ceramics of carborundum is practical, at present conventional connection side
Formula has Reaction-diffusion terms weldering, active metal brazing etc..But diffusion welding (DW) Joining Technology is complicated, higher to equipment requirements；Active metal
Soldering has under the high temperature conditions larger restriction.In addition, the metal or its compound and mother metal thermal expansion of diffusion welding (DW) and soldering introducing
Coefficient difference is larger, there is larger thermal stress in connection and application process.
The content of the invention
The invention aims to solving existing silicon carbide ceramics connected mode causes the presence of hot answering in application process
The technical problem of power, there is provided a kind of method of co-sintering after silicon-carbide-based composite ceramic green compact connection.
The method of co-sintering is as follows after the connection of silicon-carbide-based composite ceramic green compact：
First, the preparation of silicon carbide green body adhesive sheet：
By the mixing of aluminium oxide or aluminium nitride, carborundum, carbon, silicon and yittrium oxide, obtain silicon carbide green body binding agent and be combined
Powder body；
Described carbon is 1 ︰ 1 with the mol ratio of silicon, and described aluminium oxide or the mol ratio of aluminium nitride and yittrium oxide is 2 ︰ 1,
Mass fraction of the carborundum in carborundum, carbon and silicon mixture is 40%～60%, and the mixture of carborundum, carbon and silicon is in carbon
Mass fraction in SiClx base substrate binding agent composite granule is 75%～90%；
By silicon carbide green body binding agent composite granule wet ball grinding, slurry is obtained, then by slurry in 50 DEG C～70 DEG C bars
It is dried under part, then pressurize 60s～300s under conditions of pressure 150MPa～250MPa, obtains final product thickness for 200 μm～500 μm
Silicon carbide green body adhesive sheet；
2nd, the preparation of phenolic resin alcoholic solution：
By phenolic resin, hexamethylenamine, silica flour and dehydrated alcohol according to the ratio that mass ratio is the ︰ (10～20) of 10 ︰, 1 ︰ 15
Mixing, with 100r/min～150r/min, mechanical agitation speed stirring 10min～15min, obtain final product phenolic resin alcoholic solution；
3rd, the connection of carborundum based material green compact：Silicon carbide green body adhesive sheet is immersed in into phenolic resin alcohol
In solution, take out silicon carbide green body adhesive sheet and be positioned over applying 1MPa～5MPa pressures between composite material of silicon carbide green compact again
Power is attached, and is then at ambient temperature dried the composite material of silicon carbide green compact for connecting, then in temperature in air furnace
Spend for heat treatment 5min～15min under conditions of 150 DEG C～170 DEG C；
4th, in sintering atmosphere it is argon or nitrogen by the composite material of silicon carbide green compact for connecting processed through step 3
Gas, atmosphere pressures are under conditions of 0.1MPa～0.5MPa, with the programming rate of 3 DEG C/min～20 DEG C/min, from room temperature
To 1250 DEG C～1450 DEG C, 30min～90min is incubated；
5th, again with the programming rate of 3 DEG C/min～20 DEG C/min, further heat up to 1800 DEG C～2100 DEG C, be incubated
60min～180min, then cool to room temperature with the furnace, obtain final product silicon carbide ceramics.
Advantages of the present invention：
First, the present invention realizes silicon carbide-based composite ceramic using the mode of co-sintering after the connection of silicon-carbide-based composite ceramic green compact
The connection of porcelain.Using anti-during connection and silicon-carbide-based composite ceramic blank Densification between silicon-carbide-based composite ceramic base substrate
Sintering mechanism is answered, the difficulty during ceramic joining is reduced.The connection of ceramics simultaneously is carried out simultaneously with densification process, is reduced
The situation of post bake, it is to avoid crystal grain is grown up and a large amount of save energies.
2nd, the shear strength of silicon carbide ceramics joint prepared by the present invention can reach 150MPa.
Specific embodiment
Technical solution of the present invention is not limited to act specific embodiment set forth below, also including between each specific embodiment
Combination in any.
Specific embodiment one：The method of co-sintering is as follows after the connection of present embodiment silicon-carbide-based composite ceramic green compact：
First, the preparation of silicon carbide green body adhesive sheet：
By the mixing of aluminium oxide or aluminium nitride, carborundum, carbon, silicon and yittrium oxide, obtain silicon carbide green body binding agent and be combined
Powder body；
Described carbon is 1 ︰ 1 with the mol ratio of silicon, and described aluminium oxide or the mol ratio of aluminium nitride and yittrium oxide is 2 ︰ 1,
Mass fraction of the carborundum in carborundum, carbon and silicon mixture is 40%～60%, and the mixture of carborundum, carbon and silicon is in carbon
Mass fraction in SiClx base substrate binding agent composite granule is 75%～90%；
By silicon carbide green body binding agent composite granule wet ball grinding, slurry is obtained, then by slurry in 50 DEG C～70 DEG C bars
It is dried under part, then pressurize 60s～300s under conditions of pressure 150MPa～250MPa, obtains final product thickness for 200 μm～500 μm
Silicon carbide green body adhesive sheet；
2nd, the preparation of phenolic resin alcoholic solution：
By phenolic resin, hexamethylenamine, silica flour and dehydrated alcohol according to the ratio that mass ratio is the ︰ (10～20) of 10 ︰, 1 ︰ 15
Mixing, with 100r/min～150r/min, mechanical agitation speed stirring 10min～15min, obtain final product phenolic resin alcoholic solution；
3rd, the connection of carborundum based material green compact：Silicon carbide green body adhesive sheet is immersed in into phenolic resin alcohol
In solution, take out silicon carbide green body adhesive sheet and be positioned over applying 1MPa～5MPa pressures between composite material of silicon carbide green compact again
Power is attached, and is then at ambient temperature dried the composite material of silicon carbide green compact for connecting, then in temperature in air furnace
Spend for heat treatment 5min～15min under conditions of 150 DEG C～170 DEG C；
4th, in sintering atmosphere it is argon or nitrogen by the composite material of silicon carbide green compact for connecting processed through step 3
Gas, atmosphere pressures are under conditions of 0.1MPa～0.5MPa, with the programming rate of 3 DEG C/min～20 DEG C/min, from room temperature
To 1250 DEG C～1450 DEG C, 30min～90min is incubated；
5th, again with the programming rate of 3 DEG C/min～20 DEG C/min, further heat up to 1800 DEG C～2100 DEG C, be incubated
60min～180min, then cool to room temperature with the furnace, obtain final product silicon carbide ceramics.
For diameter 10mm～10cm, the component of thickness 3mm～15mm, programming rate is 10 DEG C/min～20 DEG C/min,
For more than diameter 10cm, the component of thickness more than 2cm, programming rate are 3 DEG C/min～10 DEG C/min.
The preparation of composite material of silicon carbide green compact in present embodiment：
By aluminium oxide or the mixing of aluminium nitride, carborundum and yittrium oxide, silicon carbide composite powder is obtained, silicon carbide composite powder is wet
Method ball milling, obtains slurry, and the mass fraction of silicon carbide composite powder is 40%～60% in slurry, then by slurry 50 DEG C～70
It is dried under the conditions of DEG C, then pressurize 60s～300s under conditions of pressure 150MPa～250MPa, obtains final product composite material of silicon carbide
Green compact；
The mass fraction of carborundum is 75%～90% wherein in silicon carbide composite powder, aluminium oxide or aluminium nitride and yittrium oxide
Mol ratio be 2 ︰ 1, the particle diameter of the carborundum is 0.3 μm～0.7 μm, and the particle diameter of aluminium oxide or aluminium nitride is 0.5 μm～1 μ
M, the particle diameter of yittrium oxide is 2 μm～3 μm.
Specific embodiment two：Present embodiment from step one unlike specific embodiment one in described carbonization
The particle diameter of silicon is 0.3 μm～0.7 μm, and the particle diameter of aluminium oxide or aluminium nitride is 0.5 μm～1 μm, and the particle diameter of yittrium oxide is 2 μm～3 μ
M, the particle diameter of silica flour is 35 μm～50 μm, and the particle diameter of carbon dust is 1 μm～2 μm.Other are identical with specific embodiment one.
Specific embodiment three：Present embodiment is carbonized from step one unlike specific embodiment one or one of two
Mass fraction of the silicon in carborundum, carbon and silicon mixture is 50%.Other are identical with specific embodiment one or one of two.
Specific embodiment four：It is carbonized in step one unlike one of present embodiment and specific embodiment one to three
Mass fraction of the mixture of silicon, carbon and silicon in silicon carbide green body binding agent composite granule is 85%.Other be embodied as
One of mode one to three is identical.
Specific embodiment five：With 4 in step 4 unlike one of present embodiment and specific embodiment one to four
DEG C/programming rate of min～19 DEG C/min, from room temperature to 1300 DEG C, it is incubated 35min～85min.Other be embodied as
One of mode one to four is identical.
Specific embodiment six：With 8 in step 4 unlike one of present embodiment and specific embodiment one to five
DEG C/programming rate of min～15 DEG C/min, from room temperature to 1350 DEG C, it is incubated 40min～80min.Other be embodied as
One of mode one to five is identical.
Specific embodiment seven：With 10 in step 4 unlike one of present embodiment and specific embodiment one to six
DEG C/programming rate of min～13 DEG C/min, from room temperature to 1400 DEG C, it is incubated 60min.Other and specific embodiment one
It is identical to one of six.
Specific embodiment eight：In step 5 unlike one of present embodiment and specific embodiment one to seven again with
The programming rate of 5 DEG C/min～18 DEG C/min, further heats up to 1800 DEG C, is incubated 60min～180min.Other and concrete reality
Apply one of mode one to seven identical.
Specific embodiment nine：In step 5 unlike one of present embodiment and specific embodiment one to eight again with
The programming rate of 3 DEG C/min～10 DEG C/min, further heats up to 1800 DEG C～2100 DEG C, is incubated 60min～180min.Other
It is identical with one of specific embodiment one to eight.
Specific embodiment ten：In step 5 unlike one of present embodiment and specific embodiment one to nine again with
The programming rate of 10 DEG C/min～15 DEG C/min, further heats up to 1800 DEG C～2100 DEG C, is incubated 60min～180min.Its
It is identical with one of specific embodiment one to nine.
Using following experimental verification the inventive method：
Experiment one：
The method of co-sintering is as follows after the connection of silicon-carbide-based composite ceramic green compact：
First, the preparation method of composite material of silicon carbide green compact：
By the mixing of carborundum, aluminium oxide and yittrium oxide, silicon carbide composite powder is obtained；
The mass fraction of carborundum is 85% in silicon carbide composite powder, and wherein aluminium oxide and the mol ratio of yittrium oxide are 2 ︰ 1,
The particle diameter of the carborundum is 0.3 μm, and the particle diameter of aluminium oxide is 0.5 μm, and the particle diameter of yittrium oxide is 2 μm～3 μm；
By silicon carbide composite powder wet ball grinding, slurry is obtained, the mass fraction of silicon carbide composite powder is 50% in slurry, it
Carry out pelletize and die-filling to powder body afterwards, reuse the further molding of isostatic cool pressing technique, briquetting pressure 200MPa, dwell time
100s, obtains final product composite material of silicon carbide green compact.
2nd, the preparation method of silicon carbide green body adhesive sheet：
By the mixing of carborundum, carbon, silicon, aluminium oxide and yittrium oxide, silicon carbide green body binding agent composite granule is obtained；
Described carbon is 1 ︰ 1 with the mol ratio of silicon, and described aluminium oxide and the mol ratio of yittrium oxide is 2 ︰ 1, and carborundum exists
Mass fraction in carborundum, carbon and silicon mixture is 60%, and the mixture of carborundum, carbon and silicon is in silicon carbide green body binding agent
Mass fraction in composite granule is 85%；
The particle diameter of described carborundum is 0.3 μm, and the particle diameter of aluminium oxide is 0.5 μm, and the particle diameter of yittrium oxide is 2 μm, silica flour
Particle diameter be 35 μm, the particle diameter of carbon dust is 1 μm；
2nd, by silicon carbide green body binding agent composite granule wet ball grinding, slurry is obtained, then by slurry under the conditions of 50 DEG C
It is dried, then the pressurize 60s under conditions of pressure 150MPa, obtains final product silicon carbide green body adhesive sheet, the silicon carbide green body
Adhesive sheet thickness is 200 μm.
Phenolic resin, hexamethylenamine, silica flour and dehydrated alcohol are mixed according to the ratio that mass ratio is the ︰ 10 of 10 ︰, 1 ︰ 15, with
100r/min, mechanical agitation speed stirring 10min, obtain final product phenolic resin alcoholic solution.
3rd, the connection of carborundum based material green compact：Silicon carbide green body adhesive sheet is immersed in into phenolic resin alcohol
In solution, then it is positioned over again between composite material of silicon carbide green compact and applies 1MPa pressure and be attached, then will connects
Composite material of silicon carbide green compact are dried at ambient temperature, then in air furnace temperature be 150 DEG C～170 DEG C under conditions of heat
Process 5min～15min；
4th, in sintering atmosphere it is argon or nitrogen by the composite material of silicon carbide green compact for connecting processed through step one
Gas, atmosphere pressures are under conditions of 0.2MPa, with the programming rate of 10 DEG C/min, from room temperature to 1300 DEG C, to be incubated
60min, then with the programming rate of 10 DEG C/min, further heat up to 2000 DEG C, 120min is incubated, then cool to room temperature with the furnace,
Obtain final product silicon carbide ceramics.
Experiment two：
The method of co-sintering is as follows after the connection of silicon-carbide-based composite ceramic green compact：
First, the preparation method of composite material of silicon carbide green compact：
By the mixing of carborundum, aluminium nitride and yittrium oxide, silicon carbide composite powder is obtained；
The mass fraction of carborundum is 85% in silicon carbide composite powder, wherein or the mol ratio of aluminium nitride and yittrium oxide is 2 ︰
1, the particle diameter of the carborundum is 0.4 μm, and the particle diameter of aluminium nitride is 0.6 μm, and the particle diameter of yittrium oxide is 2 μm；
By silicon carbide composite powder wet ball grinding, slurry is obtained, the mass fraction of silicon carbide composite powder is 60% in slurry, it
Carry out pelletize and die-filling to powder body afterwards, reuse the further molding of isostatic cool pressing technique, briquetting pressure 200MPa, dwell time
100s, obtains final product composite material of silicon carbide green compact.
2nd, the preparation method of silicon carbide green body adhesive sheet：
By the mixing of carborundum, carbon, silicon, aluminium oxide and yittrium oxide, silicon carbide green body binding agent composite granule is obtained；
Described carbon is 1 ︰ 1 with the mol ratio of silicon, and described aluminium oxide and the mol ratio of yittrium oxide is 2 ︰ 1, and carborundum exists
Mass fraction in carborundum, carbon and silicon mixture is 50%, and the mixture of carborundum, carbon and silicon is in silicon carbide green body binding agent
Mass fraction in composite granule is 80%；
The particle diameter of described carborundum is 0.4 μm, and the particle diameter of aluminium nitride is 0.7 μm, and the particle diameter of yittrium oxide is 3 μm, silica flour
Particle diameter be 40 μm, the particle diameter of carbon dust is 1.5 μm；
2nd, by silicon carbide green body binding agent composite granule wet ball grinding, slurry is obtained, then by slurry under the conditions of 70 DEG C
It is dried, then the pressurize 120s under conditions of pressure 200MPa, obtains final product silicon carbide green body adhesive sheet, the silicon carbide green body
Adhesive sheet thickness is 200 μm.
Phenolic resin, hexamethylenamine, silica flour and dehydrated alcohol are mixed according to the ratio that mass ratio is the ︰ 10 of 10 ︰, 1 ︰ 15, with
120r/min, mechanical agitation speed stirring 13min, obtain final product phenolic resin alcoholic solution.
3rd, the connection of carborundum based material green compact：Silicon carbide green body adhesive sheet is immersed in into phenolic resin alcohol
In solution, then it is positioned over again between composite material of silicon carbide green compact and applies 3MPa pressure and be attached, then will connects
Composite material of silicon carbide green compact are dried at ambient temperature, then in air furnace temperature be 150 DEG C under conditions of heat treatment
10min；
4th, in sintering atmosphere it is argon or nitrogen by the composite material of silicon carbide green compact for connecting processed through step one
Gas, atmosphere pressures are under conditions of 0.2MPa, with the programming rate of 10 DEG C/min, from room temperature to 1400 DEG C, to be incubated
60min, then with the programming rate of 10 DEG C/min, further heat up to 2000 DEG C, 120min is incubated, then cool to room temperature with the furnace,
Obtain final product silicon carbide ceramics.
Experiment three：
The method of co-sintering is as follows after the connection of silicon-carbide-based composite ceramic green compact：
First, the preparation method of composite material of silicon carbide green compact：
By the mixing of carborundum, aluminium oxide and yittrium oxide, silicon carbide composite powder is obtained；
The mass fraction of carborundum is 85% in silicon carbide composite powder, and wherein aluminium oxide and the mol ratio of yittrium oxide are 2 ︰ 1,
The particle diameter of the carborundum is 0.5 μm, and the particle diameter of aluminium oxide is 0.7 μm, and the particle diameter of yittrium oxide is 3 μm；
By silicon carbide composite powder wet ball grinding, slurry is obtained, the mass fraction of silicon carbide composite powder is 60% in slurry, it
Carry out pelletize and die-filling to powder body afterwards, reuse the further molding of isostatic cool pressing technique, briquetting pressure 200MPa, dwell time
100s, obtains final product composite material of silicon carbide green compact.
2nd, the preparation method of silicon carbide green body adhesive sheet：
By the mixing of carborundum, carbon, silicon, aluminium oxide and yittrium oxide, silicon carbide green body binding agent composite granule is obtained；
Described carbon is 1 ︰ 1 with the mol ratio of silicon, and described aluminium oxide and the mol ratio of yittrium oxide is 2 ︰ 1, and carborundum exists
Mass fraction in carborundum, carbon and silicon mixture is 60%, and the mixture of carborundum, carbon and silicon is in silicon carbide green body binding agent
Mass fraction in composite granule is 85%；
The particle diameter of described carborundum is 0.5 μm, and the particle diameter of aluminium oxide is 0.6 μm, and the particle diameter of yittrium oxide is 3 μm, silica flour
Particle diameter be 35 μm～50 μm, the particle diameter of carbon dust is 1 μm～2 μm；
2nd, by silicon carbide green body binding agent composite granule wet ball grinding, slurry is obtained, then by slurry under the conditions of 70 DEG C
It is dried, then the pressurize 120s under conditions of pressure 200MPa, obtains final product silicon carbide green body adhesive sheet, the silicon carbide green body
Adhesive sheet thickness is 300 μm.
Phenolic resin, hexamethylenamine, silica flour and dehydrated alcohol are mixed according to the ratio that mass ratio is the ︰ 10 of 10 ︰, 1 ︰ 15, with
130r/min, mechanical agitation speed stirring 13min, obtain final product phenolic resin alcoholic solution.
3rd, the connection of carborundum based material green compact：Silicon carbide green body adhesive sheet is immersed in into phenolic resin alcohol
In solution, then it is positioned over again between composite material of silicon carbide green compact and applies 3MPa pressure and be attached, then will connects
Composite material of silicon carbide green compact are dried at ambient temperature, then in air furnace temperature be 160 DEG C under conditions of heat treatment
10min；
4th, in sintering atmosphere it is argon or nitrogen by the composite material of silicon carbide green compact for connecting processed through step one
Gas, atmosphere pressures are under conditions of 0.2MPa, with the programming rate of 10 DEG C/min, from room temperature to 1300 DEG C, to be incubated
60min, then with the programming rate of 10 DEG C/min, further heat up to 1900 DEG C, 120min is incubated, then cool to room temperature with the furnace,
Obtain final product silicon carbide ceramics.
Experiment four：
The method of co-sintering is as follows after the connection of silicon-carbide-based composite ceramic green compact：
First, the preparation method of composite material of silicon carbide green compact：
By the mixing of carborundum, aluminium nitride and yittrium oxide, silicon carbide composite powder is obtained；
The mass fraction of carborundum is 90% in silicon carbide composite powder, and wherein aluminium nitride and the mol ratio of yittrium oxide are 2 ︰ 1,
The particle diameter of the carborundum is 0.6 μm, and the particle diameter of aluminium nitride is 0.5 μm～0.7 μm, and the particle diameter of yittrium oxide is 2 μm～3 μm；
By silicon carbide composite powder wet ball grinding, slurry is obtained, the mass fraction of silicon carbide composite powder is 50% in slurry, it
Carry out pelletize and die-filling to powder body afterwards, reuse the further molding of isostatic cool pressing technique, briquetting pressure 200MPa, dwell time
100s, obtains final product composite material of silicon carbide green compact.
2nd, the preparation method of silicon carbide green body adhesive sheet：
By the mixing of carborundum, carbon, silicon, aluminium oxide and yittrium oxide, silicon carbide green body binding agent composite granule is obtained；
Described carbon is 1 ︰ 1 with the mol ratio of silicon, and described aluminium oxide and the mol ratio of yittrium oxide is 2 ︰ 1, and carborundum exists
Mass fraction in carborundum, carbon and silicon mixture is 60%, and the mixture of carborundum, carbon and silicon is in silicon carbide green body binding agent
Mass fraction in composite granule is 90%；
The particle diameter of described carborundum is 0.3 μm～0.7 μm, and the particle diameter of aluminium oxide is 0.5 μm～1 μm, the grain of yittrium oxide
Footpath is 2 μm～3 μm, and the particle diameter of silica flour is 35 μm～50 μm, and the particle diameter of carbon dust is 1 μm～2 μm；
2nd, by silicon carbide green body binding agent composite granule wet ball grinding, slurry is obtained, then by slurry under the conditions of 70 DEG C
It is dried, then the pressurize 120s under conditions of pressure 200MPa, obtains final product silicon carbide green body adhesive sheet, the silicon carbide green body
Adhesive sheet thickness is 300 μm.
Phenolic resin, hexamethylenamine, silica flour and dehydrated alcohol are mixed according to the ratio that mass ratio is the ︰ 10 of 10 ︰, 1 ︰ 15, with
130r/min, mechanical agitation speed stirring 13min, obtain final product phenolic resin alcoholic solution.
3rd, the connection of carborundum based material green compact：Silicon carbide green body adhesive sheet is immersed in into phenolic resin alcohol
In solution, then it is positioned over again between composite material of silicon carbide green compact and applies 3MPa pressure and be attached, then will connects
Composite material of silicon carbide green compact are dried at ambient temperature, then in air furnace temperature be 150 DEG C under conditions of heat treatment
10min；
4th, in sintering atmosphere it is argon or nitrogen by the composite material of silicon carbide green compact for connecting processed through step one
Gas, atmosphere pressures are under conditions of 0.2MPa, with the programming rate of 10 DEG C/min, from room temperature to 1300 DEG C, to be incubated
60min, then with the programming rate of 10 DEG C/min, further heat up to 2000 DEG C, 120min is incubated, then cool to room temperature with the furnace,
Obtain final product silicon carbide ceramics.
Experiment five：
The method of co-sintering is as follows after the connection of silicon-carbide-based composite ceramic green compact：
First, the preparation method of composite material of silicon carbide green compact：
By the mixing of carborundum, aluminium oxide and yittrium oxide, silicon carbide composite powder is obtained；
The mass fraction of carborundum is 90% in silicon carbide composite powder, and wherein aluminium oxide and the mol ratio of yittrium oxide are 2 ︰ 1,
The particle diameter of the carborundum is 0.3 μm～0.7 μm, and the particle diameter of aluminium oxide is 0.5 μm～0.6 μm, the particle diameter of yittrium oxide is 2 μm～
3μm；
By silicon carbide composite powder wet ball grinding, obtain slurry, in slurry the mass fraction of silicon carbide composite powder be 40%～
60%, carry out pelletize and die-filling to powder body afterwards, the further molding of isostatic cool pressing technique is reused, briquetting pressure 200MPa is protected
Pressure time 100s, obtains final product composite material of silicon carbide green compact.
2nd, the preparation method of silicon carbide green body adhesive sheet：
By the mixing of carborundum, carbon, silicon, aluminium oxide and yittrium oxide, silicon carbide green body binding agent composite granule is obtained；
Described carbon is 1 ︰ 1 with the mol ratio of silicon, and described aluminium oxide and the mol ratio of yittrium oxide is 2 ︰ 1, and carborundum exists
Mass fraction in carborundum, carbon and silicon mixture is 40%, and the mixture of carborundum, carbon and silicon is in silicon carbide green body binding agent
Mass fraction in composite granule is 90%；
The particle diameter of described carborundum is 0.3 μm～0.7 μm, and the particle diameter of aluminium oxide is 0.5 μm～1 μm, the grain of yittrium oxide
Footpath is 2 μm～3 μm, and the particle diameter of silica flour is 35 μm～50 μm, and the particle diameter of carbon dust is 1 μm～2 μm；
2nd, by silicon carbide green body binding agent composite granule wet ball grinding, slurry is obtained, then by slurry under the conditions of 60 DEG C
It is dried, then the pressurize 120s under conditions of pressure 200MPa, obtains final product silicon carbide green body adhesive sheet, the silicon carbide green body
Adhesive sheet thickness is 200 μm～500 μm.
Phenolic resin, hexamethylenamine, silica flour and dehydrated alcohol are mixed according to the ratio that mass ratio is the ︰ 10 of 10 ︰, 1 ︰ 15, with
150r/min, mechanical agitation speed stirring 15min, obtain final product phenolic resin alcoholic solution.
3rd, the connection of carborundum based material green compact：Silicon carbide green body adhesive sheet is immersed in into phenolic resin alcohol
In solution, then it is positioned over again between composite material of silicon carbide green compact and applies 5MPa pressure and be attached, then will connects
Composite material of silicon carbide green compact are dried at ambient temperature, then in air furnace temperature be 170 DEG C under conditions of heat treatment
10min；
4th, in sintering atmosphere it is argon or nitrogen by the composite material of silicon carbide green compact for connecting processed through step one
Gas, atmosphere pressures are under conditions of 0.3MPa, with the programming rate of 10 DEG C/min, from room temperature to 1300 DEG C, to be incubated
60min, then with the programming rate of 10 DEG C/min, further heat up to 1900 DEG C, 120min is incubated, then cool to room temperature with the furnace,
Obtain final product silicon carbide ceramics.
Claims (9)
1. the method for co-sintering after silicon-carbide-based composite ceramic green compact connect, it is characterised in that silicon-carbide-based composite ceramic green compact connect
The method for connecing rear co-sintering is as follows：
First, the preparation of silicon carbide green body adhesive sheet：
One kind in aluminium oxide and aluminium nitride is mixed with carborundum, carbon, silicon and yittrium oxide, silicon carbide green body binding agent is obtained and is answered
Close powder body；
Described carbon is 1 ︰ 1 with the mol ratio of silicon, and described aluminium oxide or the mol ratio of aluminium nitride and yittrium oxide is 2 ︰ 1, is carbonized
Mass fraction of the silicon in carborundum, carbon and silicon mixture is 40%～60%, and the mixture of carborundum, carbon and silicon is in carborundum
Mass fraction in base substrate binding agent composite granule is 75%～90%；
By silicon carbide green body binding agent composite granule wet ball grinding, slurry is obtained, then by slurry under the conditions of 50 DEG C～70 DEG C
It is dried, then pressurize 60s～300s under conditions of pressure 150MPa～250MPa, obtains final product thickness for 200 μm～500 μm carbonizations
Silicon base substrate adhesive sheet；
2nd, the preparation of phenolic resin alcoholic solution：
Ratio by phenolic resin, hexamethylenamine, silica flour and dehydrated alcohol according to mass ratio for the ︰ (10～20) of 10 ︰, 1 ︰ 15 mixes,
With 100r/min～150r/min, mechanical agitation speed stirring 10min～15min, obtain final product phenolic resin alcoholic solution；
3rd, the connection of carborundum based material green compact：Silicon carbide green body adhesive sheet is immersed in into phenolic resin alcoholic solution
In, taking-up silicon carbide green body adhesive sheet is positioned over again applying 1MPa～5MPa pressure between composite material of silicon carbide green compact and enters
Row connection, is then at ambient temperature dried the composite material of silicon carbide green compact for connecting, then is in temperature in air furnace
Heat treatment 5min～15min under conditions of 150 DEG C～170 DEG C；
4th, in sintering atmosphere it is argon or nitrogen, gas by the composite material of silicon carbide green compact for connecting processed through step 3
Atmosphere pressure is under conditions of 0.1MPa～0.5MPa, with the programming rate of 3 DEG C/min～20 DEG C/min, from room temperature to 1250
DEG C～1450 DEG C, it is incubated 30min～90min；
5th, again with the programming rate of 3 DEG C/min～20 DEG C/min, further heat up to 1800 DEG C～2100 DEG C, insulation 60min～
180min, then cool to room temperature with the furnace, obtain final product silicon carbide ceramics.
2. the method for co-sintering after according to claim 1 silicon-carbide-based composite ceramic green compact connect, it is characterised in that step
Mass fraction of the carborundum in carborundum, carbon and silicon mixture is 50% in one.
3. the method for co-sintering after according to claim 1 silicon-carbide-based composite ceramic green compact connect, it is characterised in that step
Mass fraction of the mixture of carborundum, carbon and silicon in silicon carbide green body binding agent composite granule is 85% in one.
4. the method for co-sintering after according to claim 1 silicon-carbide-based composite ceramic green compact connect, it is characterised in that step
With the programming rate of 4 DEG C/min～19 DEG C/min in four, from room temperature to 1300 DEG C, 35min～85min is incubated.
5. the method for co-sintering after according to claim 1 silicon-carbide-based composite ceramic green compact connect, it is characterised in that step
With the programming rate of 8 DEG C/min～15 DEG C/min in four, from room temperature to 1350 DEG C, 40min～80min is incubated.
6. the method for co-sintering after according to claim 1 silicon-carbide-based composite ceramic green compact connect, it is characterised in that step
With the programming rate of 10 DEG C/min～13 DEG C/min in four, from room temperature to 1400 DEG C, 60min is incubated.
7. the method for co-sintering after according to claim 1 silicon-carbide-based composite ceramic green compact connect, it is characterised in that step
Again with the programming rate of 5 DEG C/min～18 DEG C/min in five, further heat up to 1800 DEG C, be incubated 60min～180min.
8. the method for co-sintering after according to claim 1 silicon-carbide-based composite ceramic green compact connect, it is characterised in that step
Again with the programming rate of 3 DEG C/min～10 DEG C/min in five, further heat up to 1800 DEG C～2100 DEG C, insulation 60min～
180min。
9. the method for co-sintering after according to claim 1 silicon-carbide-based composite ceramic green compact connect, it is characterised in that step
Again with the programming rate of 10 DEG C/min～15 DEG C/min in five, further heat up to 1800 DEG C～2100 DEG C, insulation 60min～
180min。
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| CN106866149B (en) * | 2017-03-14 | 2019-08-02 | 株洲湘火炬火花塞有限责任公司 | A kind of preparation method of carborundum based material mechanical seal slide unit |
| CN107540385A (en) * | 2017-09-01 | 2018-01-05 | 安徽青花坊瓷业股份有限公司 | A kind of green compact leaching liquid for improving ceramics strength |
| CN109516828B (en) * | 2018-10-15 | 2021-03-30 | 广东工业大学 | Novel connection method of silicon carbide ceramic for core, silicon carbide ceramic prepared by connection method and application of silicon carbide ceramic |
| CN110452010B (en) * | 2019-07-19 | 2021-07-09 | 广东工业大学 | High-entropy alloy-connected silicon carbide ceramic connecting piece and preparation method and application thereof |
| CN111454063B (en) * | 2020-04-03 | 2022-09-09 | 广东工业大学 | Ceramic connecting piece with compact connecting layer and connecting method and application thereof |
| CN113040430A (en) * | 2020-04-27 | 2021-06-29 | 四川三联新材料有限公司 | Heating element for heating appliance and preparation method thereof |
| CN114478043B (en) * | 2022-01-12 | 2023-05-09 | 中国科学院上海硅酸盐研究所 | Connecting method of silicon carbide ceramic based on liquid phase sintering |
| CN116161985B (en) * | 2023-01-12 | 2024-07-23 | 哈尔滨工业大学 | Surface treatment method before welding silicon carbide and welding method of silicon carbide and high-temperature alloy |
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