CN106278285A - A kind of formula of silicon nitride stalk and preparation method thereof - Google Patents
A kind of formula of silicon nitride stalk and preparation method thereof Download PDFInfo
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- CN106278285A CN106278285A CN201610645746.7A CN201610645746A CN106278285A CN 106278285 A CN106278285 A CN 106278285A CN 201610645746 A CN201610645746 A CN 201610645746A CN 106278285 A CN106278285 A CN 106278285A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
- C04B35/593—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride obtained by pressure sintering
- C04B35/5935—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride obtained by pressure sintering obtained by gas pressure sintering
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D18/00—Pressure casting; Vacuum casting
- B22D18/04—Low pressure casting, i.e. making use of pressures up to a few bars to fill the mould
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D18/00—Pressure casting; Vacuum casting
- B22D18/06—Vacuum casting, i.e. making use of vacuum to fill the mould
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5454—Particle size related information expressed by the size of the particles or aggregates thereof nanometer sized, i.e. below 100 nm
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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Abstract
The present invention relates to the formula of a kind of silicon nitride stalk, it is characterised in that: the powder body that stalk is mixed by silicon nitride powder and sintering aid is made, and wherein sintering aid accounts for the mass percent of silicon nitride powder is 1%～9%.Silicon nitride powder is made up of the nano silicon nitride powders mixing of the submicron silicon nitride powder that percentage by weight is 90%～95% and 5%～10%.The mixed powder that the silicon nitride stalk of the present invention is made up of silicon nitride powder and sintering aid carries out pelletize, molding, obtains the raw embryo of stalk, and described sintering aid is Al2O3 and Y2O3；Raw for described stalk embryo is carried out gas pressure sintering, obtains silicon nitride stalk.The present invention uses Al2O3 and Y2O3 to be sintering aid, is not only able to promote silicon nitride grain growth, reduces sintering temperature, and can reduce the decomposition of silicon nitride in sintering process.The silicon nitride material stalk of the present invention has high heat resisting temperature, can be heat-resisting 1800 DEG C, and low cost, can repeatedly use.
Description
Technical field
The present invention relates to the technical field of stalk, low pressure casting and vacuum that a kind of silicon nitride makes are inhaled
Formula of casting heat-resisting alloy stalk and preparation method thereof.
Background technology
Low pressure casting and very fast suction casting are a kind of casting methods between gravitational casting and compression casting, and stalk is
The key of this technology.At present low pressure casting and the very fast life-span inhaling the stalk that casting heat resisting steel is used are relatively low, thermal fatigue resistance with
High temperature oxidation corrosion resistance is poor, and some effects are preferable, but economical price is the most expensive, it is impossible to apply on producing.
Summary of the invention
Formula of silicon nitride stalk that it is an object of the invention to provide a kind of improvement and preparation method thereof, it can overcome
In prior art, the stalk life-span is relatively low, thermal fatigue resistance and the poor some shortcomings of high temperature oxidation corrosion resistance.
To achieve these goals, the technical scheme is that the formula of a kind of silicon nitride stalk, its feature exists
In: the powder body that described stalk is mixed by silicon nitride powder and sintering aid is made, and wherein sintering aid accounts for the matter of silicon nitride powder
Amount percentage ratio is 1%～9%.Silicon nitride powder by the submicron silicon nitride powder that percentage by weight is 90%～95% and 5%～
The nano silicon nitride powders mixing composition of 10%.Preferably, described sintering aid is nanometer Al2O3And Y2O3。
A kind of preparation method of silicon nitride stalk, it is characterised in that: described preparation method comprises the steps: a, general
Obtain mixed powder after silicon nitride powder and sintering aid mixing, then mixed powder is mixed with dehydrated alcohol, make slurry；B, general
The slurry obtained carries out spray drying granulation, obtains bulk material through discharging；C, bulk material is filled in stalk mould aftershaping,
The raw embryo of stalk is obtained after the demoulding；D, raw for described stalk embryo is carried out gas pressure sintering, obtain silicon nitride stalk.
Further, in a step, mixed powder configures according to the proportioning of 1:1-2 with the quality of dehydrated alcohol, and stirring is all
The slurry that solid content is 30 50% is obtained after even.
In b step, in 130-150 DEG C, prepared slurry being centrifuged spray drying granulation, rotating speed is 60r/min,
Temperature is that in the environment of 50-60 DEG C, discharging obtains bulk material.
In step c, bulk material pelletize obtained, by after 70 mesh sieves, uses vibrations charger to be filled with in a liter liquid
Also inserting while vibrate in pipe mold, vibration frequency is 150Hz, is then placed in equal pressing equipment by described crucible die,
Carry out cold isostatic compaction under the pressure of 200-300MPa, keep pressure 100s, after the demoulding, obtain stalk green compact.
In Step d, the temperature of gas pressure sintering is 1900 DEG C～2000 DEG C, the pressure 1-10MPa of gas pressure sintering.
During use, the mixed powder that the silicon nitride stalk of the present invention is made up of silicon nitride powder and sintering aid is made
Grain, molding, obtain the raw embryo of stalk, and described sintering aid is Al2O3And Y2O3；Raw for described stalk embryo is carried out gas pressure sintering,
To silicon nitride stalk.The present invention uses Al2O3And Y2O3For sintering aid, it is not only able to promote silicon nitride grain growth, reduces and burn
Junction temperature, and the decomposition of silicon nitride in sintering process can be reduced.The silicon nitride material stalk of the present invention has high
Heat resisting temperature, can be heat-resisting 1800 DEG C, and low cost, can repeatedly use.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described.
The invention mainly comprises the formula of a kind of silicon nitride stalk, its difference with the prior art is: described liter
The powder body that liquid pipe is mixed by silicon nitride powder and sintering aid is made, and wherein sintering aid accounts for the mass percent of silicon nitride powder and is
1%～9%.Silicon nitride powder is by the submicron silicon nitride powder that percentage by weight is 90%～95% and the nanometer nitrogen of 5%～10%
SiClx powder mixing composition.
Preferably, described sintering aid is nanometer Al2O3And Y2O3, combustion adjuvant here is to mix in 1:1 ratio.
A kind of preparation method of silicon nitride stalk, it is characterised in that: described preparation method comprises the steps: a, general
Obtain mixed powder after silicon nitride powder and sintering aid mixing, then mixed powder is mixed with dehydrated alcohol, make slurry；B, general
The slurry obtained carries out spray drying granulation, obtains bulk material through discharging；C, bulk material is filled in stalk mould aftershaping,
The raw embryo of stalk is obtained after the demoulding；D, raw for described stalk embryo is carried out gas pressure sintering, obtain silicon nitride stalk.
Optionally, in a step, silicon nitride powder is by the submicron silicon nitride powder and 5% that percentage by weight is 90%～95%
～the nano silicon nitride powders mixing composition of 10%；It is 1%～9% that sintering aid accounts for the mass percent of silicon nitride powder.Mixed powder
Configure according to the proportioning of 1:1-2 with the quality of dehydrated alcohol, after stirring, obtain the slurry that solid content is 30 50%；
Described sintering aid is nanometer Al2O3And Y2O3。
In b step, in 130-150 DEG C, prepared slurry being centrifuged spray drying granulation, rotating speed is 60r/min,
Temperature is that in the environment of 50-60 DEG C, discharging obtains bulk material.
In step c, bulk material pelletize obtained, by after 70 mesh sieves, uses vibrations charger to be filled with in a liter liquid
Also inserting while vibrate in pipe mold, vibration frequency is 150Hz, is then placed in equal pressing equipment by described crucible die,
Carry out cold isostatic compaction under the pressure of 200-300MPa, keep pressure 100s, after the demoulding, obtain stalk green compact.
In Step d, the temperature of gas pressure sintering is 1900 DEG C～2000 DEG C, the pressure 1-10MPa of gas pressure sintering.Enter one
The stalk green compact obtained are placed in gas pressure sintering stove, evacuation electrified regulation by step, after being heated to 900 DEG C, add continuing
While heat, being filled with the nitrogen that purity is 99.99% and pressurize in stove, being heated to pressure when 1100 DEG C is 0.3MPa,
After insulation 1h, continue to be heated to 1400 DEG C, while continuing heating, continue to be filled with the nitrogen that purity is 99.99% in stove
Gas pressurizes, reach the temperature of gas pressure sintering be 1900 DEG C, pressure be 5-10MPa, after gas pressure sintering terminates, stop heating
And close intake valve, and cooling to 100 DEG C with the furnace and start release, blow-on also carries out polish and product inspection, obtains silicon nitride liter
Liquid pipe.
Embodiment 1
According to the mass ratio of 9: 1, by purity be 99.99% by 95% submicron silicon nitride powder and 5% nano silicon nitride powders group
The silicon nitride powder and the nano-silica powder that become carry out dispensing, after obtaining mixed powder, according to mixed powder and dehydrated alcohol
Mass ratio is the ratio of 4: 6, adds dehydrated alcohol and stir 10min in mixed powder, and making uniform solid content is 40%
Slurry, prepared slurry is centrifuged spray drying granulation in 150 DEG C, rotating speed is 60r/min, at the ring that temperature is 60 DEG C
In border, discharging obtains bulk material；
Bulk material pelletize obtained, by after 70 mesh sieves, uses vibrations charger to be filled with in stalk mould and limit
Inserting limit vibration, vibration frequency is 150Hz, is then placed in equal pressing equipment by described crucible die, at the pressure of 200MPa
Under carry out cold isostatic compaction, keep pressure 100s, after the demoulding, obtain stalk green compact；
The stalk green compact obtained are placed in gas pressure sintering stove, evacuation electrified regulation, after being heated to 900 DEG C, are continuing
While heating, being filled with the nitrogen that purity is 99.99% and pressurize in stove, being heated to pressure when 1100 DEG C is 0.3MPa,
After insulation 1h, continue to be heated to 1400 DEG C, while continuing heating, continue to be filled with the nitrogen that purity is 99.99% in stove
Pressurize, reach the temperature of gas pressure sintering be 1900 DEG C, pressure be 5MPa, after gas pressure sintering terminates, stop heating and also close
Intake valve, cools to 100 DEG C with the furnace and starts release, and blow-on also carries out polish and product inspection, obtains silicon nitride stalk.System
Silicon nitride material stalk after one-tenth has high heat resisting temperature, can be heat-resisting 1800 DEG C, and low cost, can be repeated several times
Use.
Embodiment 2
According to the mass ratio of 8: 2, by purity be 99.99% by 90% submicron silicon nitride powder and 10% nano silicon nitride powders
Silicon nitride powder and the nano-silica powder of composition carry out dispensing, after obtaining mixed powder, according to mixed powder and dehydrated alcohol
Mass ratio be 5: 5, add dehydrated alcohol and also stir 10min, make the slurry that uniform solid content is 50%, by prepared slurry
Expecting to be centrifuged spray drying granulation in 150 DEG C, rotating speed is 60r/min, and in the environment that temperature is 60 DEG C, discharging obtains powder
Body；
Bulk material pelletize obtained, by after 70 mesh sieves, uses vibrations charger to be filled with in stalk mould and limit
Inserting limit vibration, vibration frequency is 150Hz, is then placed in equal pressing equipment by described crucible die, at the pressure of 300MPa
Under carry out cold isostatic compaction, keep pressure 100s, after the demoulding, obtain stalk green compact；
The stalk green compact obtained are placed in gas pressure sintering stove, evacuation electrified regulation, after being heated to 900 DEG C, are continuing
While heating, being filled with the nitrogen that purity is 99.99% and pressurize in stove, being heated to pressure when 1100 DEG C is 0.3MPa,
After insulation 1h, continue to be heated to 1400 DEG C, while continuing heating, continue to be filled with the nitrogen that purity is 99.99% in stove
Pressurize, reach the temperature of gas pressure sintering be 1900 DEG C, pressure be 10MPa, after gas pressure sintering terminates, stop heating and also close
Intake valve, cools to 100 DEG C with the furnace and starts release, and blow-on also carries out polish and product inspection, obtains silicon nitride stalk.
Embodiment 3
First obtain mixed powder after silicon nitride powder and sintering aid being mixed, then mixed powder is mixed with dehydrated alcohol, system
Form slurry, specifically, silicon nitride powder is by the submicron silicon nitride powder that percentage by weight is 92% and the nano silicon nitride powders of 8%
Mixing composition, mixed powder configures according to the proportioning of 1:1.5 with the quality of dehydrated alcohol, obtains solid content after stirring
It it is the slurry of 30 50%；Sintering aid account for the mass percent of silicon nitride powder be 5% sintering aid be nanometer Al2O3And Y2O3。
Secondly, in 140 DEG C, prepared slurry being centrifuged spray drying granulation, rotating speed is 60r/min, is 55 in temperature
DEG C environment in discharging obtain bulk material.
Then, bulk material pelletize obtained, by after 70 mesh sieves, uses vibrations charger to be filled with in stalk mould
Also inserting while vibrate in tool, vibration frequency is 150Hz, is then placed in equal pressing equipment by described crucible die, at 200-
Carry out cold isostatic compaction under the pressure of 300MPa, keep pressure 100s, after the demoulding, obtain stalk green compact.
Finally, raw for described stalk embryo is carried out gas pressure sintering, obtains silicon nitride stalk.Wherein, the temperature of gas pressure sintering
Degree is 1900 DEG C, the pressure 8MPa of gas pressure sintering.Being placed in gas pressure sintering stove by the stalk green compact obtained, evacuation is also energized
Heating, after being heated to 900 DEG C, while continuing heating, is filled with the nitrogen that purity is 99.99% in stove and pressurizes, add
Heat to pressure when 1100 DEG C is 0.3MPa, after insulation 1h, continues to be heated to 1400 DEG C, while continuing heating, continues in stove
Continuous be filled with the nitrogen that purity is 99.99% and pressurize, reach the temperature of gas pressure sintering be 1900 DEG C, pressure be 5-10MPa, gas
Pressure after sintering terminates, stops heating and also closes intake valve, cools to 100 DEG C with the furnace and starts releases, blow-on and carry out polish and
Product inspection, obtains silicon nitride stalk.
Above content is to combine concrete preferred implementation further description made for the present invention, it is impossible to assert
The present invention is embodied as being confined to these explanations above-mentioned.For general technical staff of the technical field of the invention,
Without departing from the inventive concept of the premise, it is also possible to make some simple deduction or replace, all should be considered as belonging to the present invention
Protection domain.
Claims (9)
1. the formula of a silicon nitride stalk, it is characterised in that: described stalk is by silicon nitride powder and sintering aid mixing
The powder body become is made, and wherein sintering aid accounts for the mass percent of silicon nitride powder is 1%～9%；
Silicon nitride powder is by the submicron silicon nitride powder that percentage by weight is 90%～95% and the nano silicon nitride powders of 5%～10%
Mixing composition.
The formula of a kind of silicon nitride stalk the most according to claim 1, it is characterised in that: described sintering aid is nanometer
Al2O3And Y2O3, combustion adjuvant here is to mix in 1:1 ratio.
3. the preparation method of a silicon nitride stalk, it is characterised in that: described preparation method comprises the steps: a, by nitrogen
Obtain mixed powder after SiClx powder and sintering aid mixing, then mixed powder is mixed with dehydrated alcohol, make slurry；B, will
To slurry carry out spray drying granulation, obtain bulk material through discharging；C, bulk material is filled in stalk mould aftershaping, de-
The raw embryo of stalk is obtained after mould；D, raw for described stalk embryo is carried out gas pressure sintering, obtain silicon nitride stalk.
The preparation method of a kind of silicon nitride stalk the most according to claim 3, it is characterised in that: in a step, silicon nitride
Powder is made up of the nano silicon nitride powders mixing of the submicron silicon nitride powder that percentage by weight is 90%～95% and 5%～10%；
It is 1%～9% that sintering aid accounts for the mass percent of silicon nitride powder.
The preparation method of a kind of silicon nitride stalk the most according to claim 3, it is characterised in that: in a step, mixed powder
Body configures according to the proportioning of 1:1-2 with the quality of dehydrated alcohol, obtains the slurry that solid content is 30 50% after stirring
Material；
Described sintering aid is nanometer Al2O3And Y2O3。
The preparation method of a kind of silicon nitride stalk the most according to claim 3, it is characterised in that: in b step, will prepare
Slurry be centrifuged spray drying granulation in 130-150 DEG C, rotating speed is 60r/min, goes out in the environment that temperature is 50-60 DEG C
Material obtains bulk material.
The preparation method of a kind of silicon nitride stalk the most according to claim 3, it is characterised in that: in step c, by pelletize
The bulk material obtained, by after 70 mesh sieves, uses vibrations charger to be filled with in stalk mould and insert while shake
Dynamic, vibration frequency is 150Hz, is then placed in equal pressing equipment by described crucible die, enters under the pressure of 200-300MPa
Row cold isostatic compaction, keeps pressure 100s, obtains stalk green compact after the demoulding.
The preparation method of a kind of silicon nitride stalk the most according to claim 3, it is characterised in that: in Step d, air pressure burns
The temperature of knot is 1900 DEG C～2000 DEG C, the pressure 1-10MPa of gas pressure sintering.
The preparation method of a kind of silicon nitride stalk the most according to claim 8, it is characterised in that: the stalk that will obtain
Green compact are placed in gas pressure sintering stove, evacuation electrified regulation, after being heated to 900 DEG C, while continuing heating, fill in stove
Entering the nitrogen that purity is 99.99% to pressurize, being heated to pressure when 1100 DEG C is 0.3MPa, after insulation 1h, continues to add
Heat, to 1400 DEG C, while continuing heating, continues to be filled with the nitrogen that purity is 99.99% in stove and pressurizes, reach gas
The temperature of pressure sintering is 1900 DEG C, pressure is 5-10MPa, after gas pressure sintering terminates, stops heating and also closes intake valve, with stove
Being cooled to 100 DEG C and start release, blow-on also carries out polish and product inspection, obtains silicon nitride stalk.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108407075A (en) * | 2018-01-02 | 2018-08-17 | 上海华培动力科技股份有限公司 | A kind of stalk preparation method for suction pouring |
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| 董英鸽等: "加入纳米氮化硅对氮化硅陶瓷性能与结构影响", 《陶瓷学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108407075A (en) * | 2018-01-02 | 2018-08-17 | 上海华培动力科技股份有限公司 | A kind of stalk preparation method for suction pouring |
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