CN110054497A - A kind of preparation method of the nanometer toughening silicon carbide complex phase ceramic of densification - Google Patents
A kind of preparation method of the nanometer toughening silicon carbide complex phase ceramic of densification Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of the nanometer toughening silicon carbide complex phase ceramic of densification, described method includes following steps: Step 1: using α-SiC particle as raw material, nanometer β-SiC particle is toughening phase, add sintering aid and binder, it is put into aluminum oxide ball grinder after preparing raw material, distilled water is added, investment mill ball is ground, and the evenly dispersed slurry of component is obtained；Step 2: being granulated using atomizing granulating technology；Step 3: pelletizing is dry-pressing formed, obtain biscuit；It carries out normal pressure-sintered Step 4: biscuit is placed in vacuum sintering furnace, obtains fine and close nanometer toughening silicon carbide complex phase ceramic.The present invention solves the brittleness problems of ceramics, improves intensity and toughness, and easy to operate, securely and reliably, low in cost, has good popularization and application foreground.
Description
Technical field
The invention belongs to ceramic materials preparation technology fields, are related to a kind of method for preparing carborundum composite-phase ceramic.
Background technique
SiC ceramic has many excellent performances, such as the features such as high rigidity, high intensity, low thermal coefficient of expansion, extensively
General is applied to the numerous areas such as petro chemical industry, automobile manufacture, semiconductor material.Wherein, SiC ceramic is in addition to density
Outside feature small, thermal conductivity is high, have the characteristics that high hardness, high temperature resistant and chemical property are stable.Therefore, SiC ceramic is answered
With also more and more extensive, the bearing made of SiC ceramic, engine components and refractory material etc. are in automobile, aerospace, space
Multiple industries such as technology are widely used.
SiC ceramic has many advantages, such as high rigidity, high intensity, low thermal coefficient of expansion, is widely used in taking under harsh environment
Labour, shows higher stability and good mechanical performance.But due to the brittleness of ceramics, i.e., under the action of external applied load, pottery
Unexpected fracture can occur for ceramic material, show as impact resistance is low, damage tolerance is low etc..It, can to solve this defect of SiC ceramic
Performance is improved by the way that ceramic material is prepared into ceramic matric composite.The appearance of nanotechnology is improving ceramic material
The aspect of energy shows great advantage, and nanometer, which is added, mutually can be improved the toughness of material.
At this stage, the raw material of SiC ceramic preparation mainly uses α-SiC powder, and compared with common α-SiC, β-SiC belongs to
Low temperature crystal form can be converted into α-SiC when more than 1800 DEG C, and volume changes in the conversion process, and tissue is finer and close, from
And improve the intensity and toughness of SiC ceramic.
Summary of the invention
In order to solve the problems, such as that preparation SiC ceramic intensity and toughness existing in the prior art are lower, the present invention provides
A kind of preparation method of fine and close nanometer toughening silicon carbide complex phase ceramic low in cost, easy to operate.This method is with α-SiC
It is main, nanometer β-SiC is added and is used as toughening phase, β-SiC particle can be undergone phase transition at a high temperature of 1800 DEG C or more generates long shaft-like
Crystal can crack deflection and the effect of bridging, play the role of toughening.The present invention solves the brittleness problems of ceramics, mentions
High intensity and toughness, and it is easy to operate, it is securely and reliably, low in cost, there is good popularization and application foreground.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of preparation method of the nanometer toughening silicon carbide complex phase ceramic of densification, using α-SiC particle as raw material, nanometer β-SiC
Son is toughening phase, and certain sintering aid and binder is added, and carries out high temperature sintering, ultimately forms a nanometer toughening silicon carbide complex phase
Ceramics.Specifically comprise the following steps:
Step 1: the preparation of nanometer β-SiC particle: carbon dust, silicon powder and silicon dioxide powder are uniformly mixed, are sintered at high temperature,
Obtain a nanometer β-SiC particle, in which: the molar ratio of carbon dust, silicon powder and silicon dioxide powder is 1:3~7:1；Incorporation time be 30~
90min；Sintering temperature is 1200~1900 DEG C, and sintering time is 2~6h；
Step 2: mixing: using wet blending process, using α-SiC particle as raw material, nanometer β-SiC particle is toughening phase, addition sintering
Auxiliary agent and binder are put into aluminum oxide ball grinder after preparing raw material, and distilled water is added, and investment mill ball is ground,
Obtain the evenly dispersed slurry of component, in which: the mass ratio of α-SiC particle and toughening phase nanometer β-SiC particle for 1:0.05~
1；The mass ratio of raw material, mill ball and distilled water is 3:6~9:1；Sintering aid is B4C, additive amount be total mass of raw material 1~
5%；Binder is phenolic resin, and additive amount is the 10~15% of total mass of raw material；The revolving speed of grinding is 300~390r/min；When
Between be 8~12h；
Step 3: being granulated: using atomizing granulating technology, be passed through clear water with peristaltic pump first, after whole system obtains wetting, lead to
Enter uniformly mixed slurry, be granulated under certain revolving speed of spray dryer spray head, collect pelletizing, in which: is spraying dry
The rotating speed of shower nozzle of dry machine is 20000~24000r/min；
Step 4: molding: pelletizing is dry-pressing formed, obtain biscuit, in which: briquetting pressure is 100~600MPa；
Step 5: sintering: biscuit being placed in vacuum sintering furnace and carries out normal pressure-sintered, obtains fine and close nanometer toughening silicon carbide
Complex phase ceramic, in which: sintering atmosphere is inert gas, and sintering temperature is 1900~2100 DEG C, and the time is 0.5~2h.
The above method can occur to chemically react as follows during β-SiC particle generates in system:
One, solid-gas is reacted:
C (s)+Si (s)=SiC (s) (1)；
SiO (g)+2C (s)=SiC (s)+CO (g) (2)；
Two, gas phase reaction:
SiO2(s) (3)+Si (s)=2SiO (g)；
SiO2(s)+C (s)=SiO (g)+CO (g) (4)；
C(s)+ CO2(g)=2CO (g) (5)；
SiO(g)+3CO(g) = SiC(s) + 2CO2(g) (6).
Compared with the prior art, the present invention has the advantage that
1, the present invention provides a kind of method of SiC nanocomposites that preparation that is easy, being easy to amplify is fine and close, the party
Method improves the brittleness of ceramics, plays the effect of reinforcing and toughening, the ceramic high-temperature resistant of preparation, excellent in mechanical performance.
2, the present invention adjusts the microscopic appearance and power of carborundum composite-phase ceramic by changing the dosage of nanometer β-SiC particle
Learn performance.
3, the present invention use nanometer β-SiC particle as toughening phase, and the local elongation stress around nanoparticle, which induces, to be worn
Crystalline substance fracture, and since solid particles generate toughening to the reflex of crack tip.
4, the binder that the present invention uses is phenolic resin, and at high temperature, phenolic resin can be carbonized and generate 65%
Carbon residue provides a small amount of carbon source for sintering, is conducive to the progress of sintering densification.
5, the present invention when sintering at high temperature, by changing sintering temperature and soaking time, make pottery by adjustable silicon carbide complex phase
The consistency and mechanical performance of porcelain.
Detailed description of the invention
Fig. 1 is the sample drawing of nanometer toughening silicon carbide complex phase ceramic prepared by embodiment 1；
Fig. 2 is the SEM photograph of nanometer toughening silicon carbide complex phase ceramic prepared by embodiment 1；
Fig. 3 is the XRD diagram of nanometer toughening silicon carbide complex phase ceramic prepared by embodiment 1；
Fig. 4 is the SEM photograph of nanometer toughening silicon carbide complex phase ceramic prepared by embodiment 2；
Fig. 5 is the XRD photo of nanometer toughening silicon carbide complex phase ceramic prepared by embodiment 2；
Fig. 6 is the SEM photograph of nanometer toughening silicon carbide complex phase ceramic prepared by embodiment 3；
Fig. 7 is the XRD diagram of nanometer toughening silicon carbide complex phase ceramic prepared by embodiment 3；
Fig. 8 is the compressive strength of the nanometer toughening silicon carbide complex phase ceramic of Examples 1 to 5 preparation.
Specific embodiment
Below with reference to embodiment, further description of the technical solution of the present invention, and however, it is not limited to this, all right
Technical solution of the present invention is modified or replaced equivalently, and without departing from the spirit and scope of the technical solution of the present invention, should all be contained
Lid is within the protection scope of the present invention.
Embodiment 1:
A kind of preparation method of the nanometer toughening silicon carbide complex phase ceramic of densification is present embodiments provided, the method is by following
What step was completed:
One, the preparation of nanometer β-SiC particle: by carbon dust, silicon powder and silicon dioxide powder with the molar ratio of 1:4:1 in high-speed mixer
Middle mixing 60min, is sintered at 1600 DEG C；
Two, mixing: using wet blending process, and using α-SiC particle as raw material, nanometer β-SiC particle is toughening phase, adds B4C and phenol
Urea formaldehyde, in which: the mass ratio of α-SiC particle and toughening phase nanometer β-SiC particle is 1:0.05, B4The additive amount of C is raw material
The 3% of gross mass；The additive amount of phenolic resin is the 10% of total mass of raw material, after preparing raw material by the formula of design, puts into oxygen
Change aluminum ball grinder in, be added distilled water, put into mill ball, in which: raw material, mill ball, distilled water mass ratio be 3:8:1,
9h is ground with the revolving speed of 380r/min, obtains the evenly dispersed experimental slurries of component；
Three, it is granulated: using atomizing granulating technology, be passed through clear water with peristaltic pump first, after whole system obtains wetting, be passed through mixed
Uniform slurry is closed, under the 19000r/min revolving speed of spray dryer spray head, is granulated and completes, then under spray dryer
Collect pelletizing in side；
Four, it forms: pelletizing is dry-pressing formed under the pressure of 500MPa, obtain biscuit；
Five, be sintered: the biscuit of compacting is placed in graphite crucible, using inert gas as protect gas, in high temperature sintering furnace in
It is sintered 1.5h at 2000 DEG C, is cooled to room temperature, fine and close nanometer toughening silicon carbide complex phase ceramic is obtained.
Fig. 1 is the sample drawing of complex phase SiC ceramic manufactured in the present embodiment, and You Tuzhong can be seen that surface flawless, without bright
Aobvious gross imperfection, and there is a degree of volume contraction.
Fig. 2 is that the SEM of complex phase SiC ceramic manufactured in the present embodiment schemes, and You Tuzhong can be seen that the sample for being added to β-SiC
Product section, crystal boundary is fuzzy, and in concave-convex new clothes, its fracture mode is along crystalline substance/transcrystalline mixed fracture mode, in the mistake that crackle generates
Cheng Zhong, crystal boundary, which extends it, produces obstruction, to improve the intensity of material.
Fig. 3 is the XRD diagram of complex phase SiC ceramic manufactured in the present embodiment, and You Tuzhong can be seen that the master of sintered material
Wanting crystal phase is 6H-SiC phase, and the β-SiC of addition has been completely converted into α-SiC.
Embodiment 2:
The present embodiment and 1 difference of embodiment are: the ratio of α-SiC particle and toughening phase nanometer β-SiC particle is 1:0.1.
Fig. 4 is that the SEM of complex phase SiC ceramic manufactured in the present embodiment schemes, You Tuzhong can be seen that β-SiC content improve with
Afterwards, material sample consistency obtained improves.
Fig. 5 is the XRD diagram of complex phase SiC ceramic manufactured in the present embodiment, and You Tuzhong can be seen that the master of sintered material
Wanting crystal phase is 6H-SiC phase, and the β-SiC of addition has been completely converted into α-SiC.
Embodiment 3:
The present embodiment and 1 difference of embodiment are: the ratio of α-SiC particle and toughening phase nanometer β-SiC particle is 1:0.2.
Fig. 6 is that the SEM of complex phase SiC ceramic manufactured in the present embodiment schemes, and You Tuzhong can be seen that β-SiC content continues to mention
Height, material sample consistency obtained improve.
Fig. 7 is the XRD diagram of complex phase SiC ceramic manufactured in the present embodiment, and You Tuzhong can be seen that the master of sintered material
Wanting crystal phase is 6H-SiC phase, and the β-SiC of addition has been completely converted into α-SiC.
Embodiment 4:
The present embodiment and 1 difference of embodiment are: the ratio of α-SiC particle and toughening phase nanometer β-SiC particle is 1:0.3.
Embodiment 5:
The present embodiment and 1 difference of embodiment are: the ratio of α-SiC particle and toughening phase nanometer β-SiC particle is 1:0.4.
Fig. 8 is the compressive strength of the complex phase SiC ceramic of Examples 1 to 5 preparation, and You Tuzhong, which can be seen that, to be worked as: α-SiC
When the ratio of son and toughening phase nanometer β-SiC particle is 1:0.2, the compressive strength of complex phase SiC ceramic is maximum, is 411MPa.
Claims (10)
1. a kind of preparation method of the nanometer toughening silicon carbide complex phase ceramic of densification, it is characterised in that the method includes walking as follows
It is rapid:
Step 1: mixing: using α-SiC particle as raw material, nanometer β-SiC particle is toughening phase, adds sintering aid and binder,
It is put into aluminum oxide ball grinder after preparing raw material, distilled water is added, investment mill ball is ground, and is obtained component and is uniformly divided
Scattered slurry, in which: the mass ratio of α-SiC particle and toughening phase nanometer β-SiC particle is 1:0.05~1；Sintering aid adds
Dosage is the 1~5% of total mass of raw material；The additive amount that binder is is the 10~15% of total mass of raw material；Raw material, mill ball and steaming
The mass ratio of distilled water is 3:6~9:1；
Step 2: being granulated: being granulated using atomizing granulating technology；
Step 3: molding: pelletizing is dry-pressing formed, obtain biscuit；
Step 4: sintering: biscuit being placed in vacuum sintering furnace and carries out normal pressure-sintered, obtains fine and close nanometer toughening silicon carbide
Complex phase ceramic.
2. the preparation method of the nanometer toughening silicon carbide complex phase ceramic of densification according to claim 1, it is characterised in that institute
State nanometer β-SiC particle the preparation method is as follows: carbon dust, silicon powder and silicon dioxide powder are uniformly mixed, and are sintered, are obtained at high temperature
To nanometer β-SiC particle, in which: the molar ratio of carbon dust, silicon powder and silicon dioxide powder is 1:3~7:1.
3. the preparation method of the nanometer toughening silicon carbide complex phase ceramic of densification according to claim 2, it is characterised in that institute
Stating incorporation time is 30~90min；Sintering temperature is 1200~1900 DEG C, and sintering time is 2~6h.
4. the preparation method of the nanometer toughening silicon carbide complex phase ceramic of densification according to claim 1, it is characterised in that institute
Stating sintering aid is B4C, binder are phenolic resin.
5. the preparation method of the nanometer toughening silicon carbide complex phase ceramic of densification according to claim 1, it is characterised in that institute
The revolving speed for stating grinding is 300~390r/min, and the time is 8~12h.
6. the preparation method of the nanometer toughening silicon carbide complex phase ceramic of densification according to claim 1, it is characterised in that institute
Stating step 3, specific step is as follows: being passed through clear water with peristaltic pump first, after whole system obtains wetting, is passed through uniformly mixed
Slurry, be granulated under certain revolving speed of spray dryer spray head, collect pelletizing.
7. the preparation method of the nanometer toughening silicon carbide complex phase ceramic of densification according to claim 6, it is characterised in that institute
The rotating speed of shower nozzle for stating spray dryer is 20000~24000r/min.
8. the preparation method of the nanometer toughening silicon carbide complex phase ceramic of densification according to claim 1, it is characterised in that institute
Stating briquetting pressure is 100~600MPa.
9. the preparation method of the nanometer toughening silicon carbide complex phase ceramic of densification according to claim 1, it is characterised in that institute
Stating sintering atmosphere is inert gas.
10. the preparation method of the nanometer toughening silicon carbide complex phase ceramic of densification according to claim 1, it is characterised in that institute
Stating sintering temperature is 1900~2100 DEG C, and the time is 0.5~2h.
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Cited By (4)
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| CN112266252A (en) * | 2020-11-04 | 2021-01-26 | 黑龙江冠瓷科技有限公司 | Preparation method of pressureless sintering micro-nano mixed silicon carbide granulation powder |
| CN112321310A (en) * | 2020-11-04 | 2021-02-05 | 黑龙江冠瓷科技有限公司 | Preparation method of nanoparticle toughened high-toughness SiC product |
| CN113072383A (en) * | 2021-05-20 | 2021-07-06 | 郑州海赛高技术陶瓷有限责任公司 | Preparation method and application of corrosion-resistant silicon carbide ceramic |
| CN114591086A (en) * | 2022-03-31 | 2022-06-07 | 中国兵器工业第五二研究所烟台分所有限责任公司 | Nano powder modified silicon carbide-boron carbide composite ceramic and preparation method thereof |
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