CN106673661A - Thick-plate silicon carbide ceramic material and preparation method and application thereof - Google Patents
Thick-plate silicon carbide ceramic material and preparation method and application thereof Download PDFInfo
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- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/63416—Polyvinylalcohols [PVA]; Polyvinylacetates
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F41—WEAPONS
- F41H—ARMOUR; ARMOURED TURRETS; ARMOURED OR ARMED VEHICLES; MEANS OF ATTACK OR DEFENCE, e.g. CAMOUFLAGE, IN GENERAL
- F41H5/00—Armour; Armour plates
- F41H5/02—Plate construction
- F41H5/023—Armour plate, or auxiliary armour plate mounted at a distance of the main armour plate, having cavities at its outer impact surface, or holes, for deflecting the projectile
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- 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
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/422—Carbon
- C04B2235/424—Carbon black
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Abstract
The invention belongs to the field of inorganic nonmetallic materials, relates to a reactive sintering preparation technology of a silicon carbide ceramic material and particularly relates to a thick-plate silicon carbide ceramic material and a preparation method and application thereof. The preparation method of the thick-plate silicon carbide ceramic material comprises the steps of mixing carbon black powder with silicon carbide powder according to mass ratio, adding polyving akohol, ball milling, evenly mixing, spraying and granulating, obtaining a mixed powdery material and die forming to obtain a green body; placing pressed powder made of silicon powder on the surface of the green body, sintering and keeping warm; slowly reducing furnace temperature to 200 DEG C or below after sintering and keeping warm, controlling the cooling speed not to be higher than 5 DEG C/min and obtaining the thick-plate silicon carbide ceramic material. The preparation technology provided by the invention has the advantage of obviously reducing thermal stress generated by ceramic in a reactive sintering process, and the prepared thick-plate silicon carbide ceramic has the advantages of having high density, avoiding defects of crack, large-area residual silicon enrichment or the like and being especially suitable for the field of special vehicle protection.
Description
Technical field
The invention belongs to field of inorganic nonmetallic material, is related to the reaction-sintered preparation technology of thyrite, especially
It is a kind of slab thyrite and its preparation method and application.
Background technology
Silicon carbide ceramics hardness is high, density is less, and high temperature resistant, it is wear-resistant, have certain toughness, low price is new
The ideal material of generation bulletproof ceramic, while preferable ballistic performance is ensured, can keep preferable tactical mobility, in human body
Protection aspect has been obtained for being widely applied.Patent etc. discloses the preparation method of silicon carbide bulletproof spile and its prevents in human body
The application in protector for collar domain.But, in terms of the protection of some special vehicles, need the carborundum plate for being equipped with super thick.Reaction-sintered has
Have the advantages that sintering process is simple, sintering time is short, net-shape-sinter, large-scale commercial Application is easily realized, with wide
Wealthy application prospect.But, often it is difficult to obtain the flawless reaction-sintered carbon of zero defect using method known at present
SiClx ceramics slab.
The content of the invention
It is an object of the invention to overcome the shortcomings of above-mentioned prior art, there is provided one kind prepares flawless, flawless thickness
The process of plate silicon carbide ceramics, and this silicon carbide ceramics is in the application in Vehicle protector field.
In order to realize above technique effect, the present invention is to be achieved by the steps of:
S1. by hydrocarbon black powder and silicon carbide powder in mass ratio 5~12:After 95~88 mixing, addition gross mass 10~
20% polyvinyl alcohol, after ball milling mixing is uniform, mist projection granulating obtains mixed powder;
S2. by the mixed powder die forming in step S1, base substrate is obtained;
S3. the silica flour shape relative to 2.5~4 times of hydrocarbon black powder quality in S1 is placed on the surface of base substrate in step s 2
Into muffin, be sintered insulation;The sintering keeps vacuum to be not less than 5 × 10-1Pa, is to slowly warm up to 1650~1800 DEG C
Afterwards, it is incubated 2h;The slow intensification, when furnace temperature is less than 800 DEG C, programming rate is less than 5 DEG C/min, and protects at 400 DEG C
Warm 1h, after furnace temperature is more than 800 DEG C, programming rate is less than 2 DEG C/min;Using the heating process system of the present invention, Ke Yibao
While card pressed compact sintering quality, the total duration of sintering is shortened as far as possible.Because the present invention only has polyvinyl alcohol as binding agent, can
To adopt comparatively faster programming rate in cold stage.In order to thoroughly remove the polyvinyl alcohol in pressed compact, application claims exist
300 DEG C of insulation 1h.Due to prepared by the present invention being the big silicon carbide articles of thickness, relatively low liter must be kept in hot stage
Warm speed, will otherwise make pressed compact surface produce reaction-sintered prior to pressed compact core, so that molten silicon is difficult to smoothly enter pressed compact
Core, causes to be scrapped because not exclusively sintering.
S4. after sintered heat insulating in step s3 terminates, in an inert atmosphere, pressure is kept to be not less than 0.5MPa,
Slowly furnace temperature is reduced to into less than 200 DEG C, cooling rate is not higher than 5 DEG C/min, that is, makes fine and close and flawless slab carbonization
Silicon ceramic material.Because base substrate thickness is larger, usually because thermal stress is excessive pressed compact can be caused crackle occur in temperature-fall period
Etc. defect.The technical scheme provided using the present invention, under pressure, and Slow cooling, you can this problem is solved, is made
Fine and close and flawless slab thyrite.
Preferably, the silicon carbide powder in the mixed powder in step S1 is made up of two kinds of silicon carbide powders of thickness,
The average particle size particle size of coarse powder is 30~50 μm, and the average particle size particle size of fine powder is 2~5 μm, and fine powder is with the mass ratio of coarse powder
1:1.5~2.5.Using the coarse powder and the ratio of fine powder of the present invention, fine powder can be substantially filled to coarse powder particles in mechanical milling process
In piling up the hole for being formed, so that the apparent density of mixed-powder is improved, and high density is obtained in follow-up mold process
Pressed compact, prevent from forming the residual silicon of bulk in follow-up infiltration process.
Preferably, the pressure condition of the die forming of step S2 is 200~250MPa.Too low pressing pressure is by nothing
Method obtains the pressed compact of sufficient density, and pressure is excessive, is easily caused pressed compact and produces the defects such as layering.
Wherein, the sintered heat insulating of step S3 is carried out in a vacuum furnace.
Wherein, the noble gases of step S4 are argon.
Slab thyrite prepared by above-mentioned preparation method.
The thickness of the slab thyrite is 80~300mm.
Above-mentioned slab thyrite is used to make armour.
The invention has the beneficial effects as follows:
1st, the preparation technology that the present invention is provided can significantly reduce the thermal stress that ceramics are produced during reaction-sintered;
2nd, slab silicon carbide ceramics consistency height, no crackle or the enrichment of large area residual silicon that prepared by the present invention etc. lack
Fall into, be particularly well-suited to the protection field of special vehicle.
Specific embodiment
With reference to embodiment, the invention will be further described:
Embodiment 1
A kind of preparation method of slab thyrite, preparation technology is comprised the following steps:
Step one, is 8 by mass ratio:After 92 hydrocarbon black powder mixes with silicon carbide powder, the poly- of gross mass 15% is added
Vinyl alcohol, after ball milling mixing is uniform, mist projection granulating obtains powder.Silicon carbide powder in above-mentioned mixed-powder is by particle mean size
Fine powder and particle mean size for 2 μm is 45 μm of coarse powder with mass ratio 1:2 compoundings are obtained;
Step 2, by above-mentioned powder under 250MPa pressure die forming, obtain thickness be 150mm base substrate;
Step 3, the muffin that the silica flour of 3 times of carbon black mass is formed in billet surface is placed relative to base substrate is positioned over true
In empty stove, reaction-sintered is carried out:Vacuum is kept to be not less than 5 × 10-1Pa, then 1750 DEG C are to slowly warm up to, and it is incubated 2h.In stove
When temperature is less than 800 DEG C, programming rate is less than 5 DEG C/min, and is incubated 1h at 400 DEG C;After furnace temperature is more than 800 DEG C, heat up
Speed is less than 2 DEG C/min;
Step 4, after sintered heat insulating terminates, turns off vacuum system, and argon is filled with stove, keeps argon pressure to be not less than
0.5MPa, and slowly furnace temperature is reduced to into less than 200 DEG C, cooling rate is not higher than 5 DEG C/min, that is, make fine and close and flawless
Slab thyrite.
Above-mentioned slab thyrite is tested, density is 3.13g/cm3, Rockwell hardness HRA is 94~95, and Vickers is hard
Degree HV0.5For 2650~2700, bending strength is 320~380MPa, and porosity is less than 0.09%.
Step 5, using diamond-impregnated wheel the residual silicon on carborundum plate surface that reaction-sintered is obtained is removed, then by these
Carborundum plate is fixed in box made by armour steel material according to certain form marshalling, be can be used for
The silicon carbide ceramics bulletproof armour of Vehicle protector.
Embodiment 2
A kind of preparation method of slab thyrite, preparation technology is comprised the following steps:
Step one, is 12 by mass ratio:After 88 hydrocarbon black powder mixes with silicon carbide powder, the poly- of gross mass 20% is added
Vinyl alcohol, after ball milling mixing is uniform, mist projection granulating obtains powder.Silicon carbide powder in above-mentioned mixed-powder is by particle mean size
Fine powder and particle mean size for 3 μm is 40 μm of coarse powder with mass ratio 1:2.5 compoundings are obtained;
Step 2, by above-mentioned powder under 220MPa pressure die forming, obtain thickness be 200mm base substrate;
Step 3, the muffin that the silica flour of 3.5 times of carbon black mass is formed in billet surface is placed relative to base substrate, is positioned over
In vacuum drying oven, reaction-sintered is carried out:Vacuum is kept to be not less than 5 × 10-1Pa, then 1800 DEG C are to slowly warm up to, and 2h is incubated,
When furnace temperature is less than 800 DEG C, programming rate is less than 5 DEG C/min, and is incubated 1h at 400 DEG C, after furnace temperature is more than 800 DEG C, rises
Warm speed is less than 2 DEG C/min;
Step 4, after sintered heat insulating terminates, turns off vacuum system, and argon is filled with stove, keeps argon pressure to be not less than
0.5MPa, and slowly furnace temperature is reduced to into less than 200 DEG C, cooling rate is not higher than 5 DEG C/min, that is, make fine and close and flawless
Slab thyrite.
Above-mentioned slab thyrite is tested, density is 3.10g/cm3, Rockwell hardness HRA is 94~95, and Vickers is hard
Degree HV0.5For 2650~2700, bending strength is 310~370MPa, and porosity is less than 0.1%.
The above is presently preferred embodiments of the present invention, but the present invention should not be limited to disclosed in the embodiment
Content.So it is every without departing from the equivalent or modification completed under spirit disclosed in this invention, both fall within the model of present invention protection
Enclose.
Claims (8)
1. a kind of preparation method of slab thyrite, it is characterised in that comprise the following steps:
S1. by hydrocarbon black powder and silicon carbide powder in mass ratio 5~12:After 95~88 mixing, gross mass 10~20% is added
Polyvinyl alcohol, after ball milling mixing is uniform, mist projection granulating obtains mixed powder;
S2. by the mixed powder die forming in step S1, base substrate is obtained;
S3. what is formed relative to the silica flour of 2.5~4 times of hydrocarbon black powder quality in S1 placed in the surface of base substrate in step s 2
Muffin, is sintered insulation;The sintering keeps vacuum to be not less than 5 × 10-1Pa, after being to slowly warm up to 1650~1800 DEG C,
Insulation 2h;The slow intensification, when furnace temperature is less than 800 DEG C, programming rate is less than 5 DEG C/min, and is incubated at 400 DEG C
1h, after furnace temperature is more than 800 DEG C, programming rate is less than 2 DEG C/min;
S4. after sintered heat insulating in step s3 terminates, in an inert atmosphere, pressure is kept to be not less than 0.5MPa, slowly
Furnace temperature is reduced to into less than 200 DEG C, cooling rate is not higher than 5 DEG C/min, that is, makes fine and close and flawless slab carborundum pottery
Ceramic material.
2. the preparation method of slab thyrite as described in the appended claim 1, it is characterised in that:In step S1
Silicon carbide powder in mixed powder is made up of two kinds of silicon carbide powders of thickness, and the average particle size particle size of coarse powder is 30~50 μm,
The average particle size particle size of fine powder is 2~5 μm, and fine powder is 1 with the mass ratio of coarse powder:1.5~2.5.
3. the preparation method of slab thyrite as described in the appended claim 1, it is characterised in that:The mould of step S2
The pressure condition of pressing formation is 200~250MPa.
4. the preparation method of slab thyrite as described in the appended claim 1, it is characterised in that:The burning of step S3
Knot insulation is carried out in a vacuum furnace.
5. the preparation method of slab thyrite as described in the appended claim 1, it is characterised in that:Step S4 it is lazy
Property gas be argon.
6. such as the slab thyrite of any preparation method preparation described in claim 1-5.
7. slab thyrite as described in claim 6, it is characterised in that:The slab thyrite
Thickness be 80~300mm.
8. slab thyrite as described in claim 6 is used to make armour.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107673761A (en) * | 2017-10-27 | 2018-02-09 | 潍坊华美精细技术陶瓷股份有限公司 | A kind of preparation method of big specification compact silicon carbide ceramic plate |
CN116023148A (en) * | 2021-10-25 | 2023-04-28 | 中国科学院上海硅酸盐研究所 | Preparation method of silicon carbide ceramic and silicon carbide ceramic material prepared by preparation method |
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