CN100445235C - Aluminium nitride reinforced sibicon carbide ceramic and its preparation method - Google Patents
Aluminium nitride reinforced sibicon carbide ceramic and its preparation method Download PDFInfo
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- CN100445235C CN100445235C CNB2006101556551A CN200610155655A CN100445235C CN 100445235 C CN100445235 C CN 100445235C CN B2006101556551 A CNB2006101556551 A CN B2006101556551A CN 200610155655 A CN200610155655 A CN 200610155655A CN 100445235 C CN100445235 C CN 100445235C
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- 239000000919 ceramic Substances 0.000 title claims abstract description 42
- 229910017083 AlN Inorganic materials 0.000 title claims description 37
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 title claims description 37
- 238000002360 preparation method Methods 0.000 title description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 68
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 67
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000002002 slurry Substances 0.000 claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 claims abstract description 20
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 239000011230 binding agent Substances 0.000 claims abstract description 10
- 229920003169 water-soluble polymer Polymers 0.000 claims abstract description 10
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 238000009694 cold isostatic pressing Methods 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims description 18
- 238000005245 sintering Methods 0.000 claims description 18
- 235000015895 biscuits Nutrition 0.000 claims description 16
- 238000005516 engineering process Methods 0.000 claims description 12
- 238000003825 pressing Methods 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- 239000006185 dispersion Substances 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 6
- 229920002125 Sokalan® Polymers 0.000 claims description 4
- 229920002401 polyacrylamide Polymers 0.000 claims description 4
- 239000004584 polyacrylic acid Substances 0.000 claims description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 claims description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 3
- 229920000609 methyl cellulose Polymers 0.000 claims description 3
- 239000001923 methylcellulose Substances 0.000 claims description 3
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 3
- -1 polyoxyethylene Polymers 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 claims description 2
- 125000002777 acetyl group Chemical class [H]C([H])([H])C(*)=O 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 7
- 238000005469 granulation Methods 0.000 abstract description 5
- 230000003179 granulation Effects 0.000 abstract description 5
- 239000000843 powder Substances 0.000 abstract description 5
- 238000001694 spray drying Methods 0.000 abstract description 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 abstract 3
- 239000002270 dispersing agent Substances 0.000 abstract 1
- 238000003801 milling Methods 0.000 abstract 1
- 238000001272 pressureless sintering Methods 0.000 abstract 1
- 239000007921 spray Substances 0.000 abstract 1
- 238000000465 moulding Methods 0.000 description 6
- 238000002156 mixing Methods 0.000 description 5
- 239000011324 bead Substances 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000003595 mist Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000003643 water by type Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 150000001241 acetals Chemical class 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000001778 solid-state sintering Methods 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 230000003678 scratch resistant effect Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The invention relates to an aluminum nitride reinforced SiC ceramics, and its weight percentage composition of: SiC 80% ~ 94%, aluminum nitride 5% ~ 19%, yttrium oxide 1% ~ 2%. The invention also open the ceramics production methods, including the following steps : 1) all of the above components as raw added into deionized water, then add the binder, mixture of water-soluble polymer and dispersant, milling 5 ~ 20 hours, then form water-based silicon carbide slurry; 2) use spray granulation process to treat water-based silicon carbide slurry for spray drying, made of SiC powder; 3) using dry-press precompression and cold isostatic pressing final pressure to silicon carbide powder to obtain SiC blank; 4) put the SiC blank into vacuum pressureless sintering furnace, at 1950 ~ 2200 deg for 1 ~ 5 hours, gain enhanced aluminum nitride silicon carbide ceramics. The ceramic made by this method can meet the mechanical seal requirement of special conditions.
Description
Technical field
The present invention relates to a kind of aluminium nitride reinforced sibicon carbide ceramic and production method thereof.
Background technology
The pottery that the mechanical seal industry is required requires material to have high strength, high tenacity, low creep properties, wear-resisting scouring damage, erosion resistance and good oxidation-resistance.Silicon carbide ceramics has excellent mechanical property, lower thermal expansivity and high heat-conduction coefficient, make silicon carbide ceramics present excellent thermal shock resistance, but also have high thermal stability, good corrosion-resistant, scratch-resistant performance, therefore can be applied in the mechanical seal ring field widely.
Because silicon carbide chemistry key characteristic, its ceramic post sintering condition is comparatively harsh.Normal pressure-sintered appearance makes the silicon carbide ceramics suitability for industrialized production obtain extensive realization.Normal pressure-sinteredly comprise solid state sintering and liquid phase sintering, solid state sintering needs higher sintering temperature (＞2100 ℃), makes that the silicon carbide whisker particle size is bigger, and ceramic fracture mode also mostly is transgranular fracture, causes fracture toughness property lower.Sintering aid is generally commonly used B-C, Al-B-C, Al
2O
3, Al
2O
3-Re
2O
3Deng, wherein Re represents one or more of rare earth element; But these sintering aids are in the time of high temperature and silicon carbide reacts or volatile ratio is more serious, make that the Sintered Quality loss is serious, are unfavorable for densified sintering product.Similar on atomic size, molecular weight, density and crystalline structure of silicon carbide and aluminium nitride material it is found that in recent years, owing to can form sosoloid in 1800～2100 ℃ temperature range; Along with the formation of sosoloid, the sintering activity of material, microstructure, mechanical property and oxidation-resistance are all improved largely.But because aluminium nitride and water can react under churned mechanically situation, adopting at present aluminium nitride is that mostly to adopt ethanol be that solvent carries out ball mill mixing for technology that sintering aid prepares silicon carbide ceramics, but the ceramic cost that this explained hereafter goes out is higher, blasts easily during mist projection granulating.Therefore being necessary to develop novel process prepares water base silicon carbide slurry, introduces the reaction that properties-correcting agent reduces aluminium nitride and water, can satisfy spray-dired requirement again; Thereby prepare high quality silicon carbide powder and high-performance silicon carbide pottery, produce the mechanical seal ring that is used for high-end market.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of aluminium nitride reinforced sibicon carbide ceramic and production method thereof, production method process safety of the present invention, cost are low, made aluminium nitride reinforced sibicon carbide ceramic has high fine and close, high-strength, high tenacity, characteristic such as anti-oxidant, can satisfy the mechanical seal requirement of special operation condition.
In order to solve the problems of the technologies described above, the invention provides a kind of production method of aluminium nitride reinforced sibicon carbide ceramic, with weight percent be the yttrium oxide of 80%～94% silicon carbide, 5%～19% aluminium nitride and 1%～2% as raw material, may further comprise the steps:
1), above-mentioned raw materials is put into deionized water, add binding agent, mixture of water-soluble polymer colloidal sol and dispersion agent again, ball milling mixes and forms water base silicon carbide slurry after 5～20 hours; The weight of described binding agent is 0.5%～3% of raw material gross weight, the weight of mixture of water-soluble polymer colloidal sol is 0.5%～2% of raw material gross weight, the weight of dispersion agent is 0.5%～1.5% of raw material gross weight, and the weight ratio of described raw material and deionized water is 3: 7～3: 2;
2), adopt atomizing granulating technology above-mentioned water base silicon carbide slurry to be carried out spraying drying, 300～400 ℃ of hot blast inlet temperatures, 80～90 ℃ of temperature outs, 100～200 kilograms/hour of slurry flow; Prepare the silicon carbide amyloplastid;
3), above-mentioned silicon carbide amyloplastid is adopted 100～150MPa dry-pressing precompressed and 200～300MPa cold isostatic pressing end pressing successively, acquisition silicon carbide biscuit;
4), above-mentioned silicon carbide biscuit is put into vacuum non-pressure sintering furnace, after being incubated 1～5 hour under 1950～2200 ℃ of temperature, be prepared into aluminium nitride reinforced sibicon carbide ceramic.
Improvement as production method of the present invention: binding agent is polyvinyl alcohol, polyvinyl butyral acetal or methylcellulose gum, and mixture of water-soluble polymer colloidal sol is polyacrylamide or polyoxyethylene glycol, and dispersion agent is polyacrylic acid or aluminum phosphate.
The present invention also provides the aluminium nitride reinforced sibicon carbide ceramic that makes according to above-mentioned any one production method simultaneously.
In production method of the present invention, with aluminium nitride and yttrium oxide as sintering aid, the employing deionized water is a solvent, with the silicon carbide bead as grinding medium, add binding agent, mixture of water-soluble polymer colloidal sol and dispersion agent ball milling again and mix, solid load is 30%～60% in the formed water base silicon carbide slurry.Adopt atomizing granulating technology that above-mentioned slurry is carried out spraying drying, by regulating hot blast inlet temperature and slurry flow, water ratio, flowability and the intensity of control granulation ball are prepared and are flowed and the good silicon carbide granulating powder of processability.With of the two steps mode moulding of above-mentioned silicon carbide granulating powder, obtain highdensity biscuit of ceramics again through dry-pressing precompressed and cold isostatic pressing end pressing.The one-tenth aluminium nitride reinforced sibicon carbide ceramic that finally makes in actual use, through cleaning, mill processing, polished finish, just can be prepared the aluminium nitride reinforced sibicon carbide mechanical seal ring.
The present invention compared with prior art has following advantage:
1, in this ceramic preparation process, spray drying granulation technology is that the slurry that will mix directly is sprayed in the warm air, at very short time inner drying, has avoided the reunion again of each component and settlement separate, has kept the original homogeneity of slurry; Make the slurry atomizing simultaneously evenly, the even particle size distribution that obtains, good fluidity, being fit to continuous automatic moulding spheroidal particle (is the silicon carbide amyloplastid, as shown in Figure 1).(be the silicon carbide biscuit, as shown in Figure 2) section is even, and the granulation ball is all broken, does not stay any big macroscopic defects in biscuit for the biscuit of ceramics of gained.
2, the granulation powder fluidity can be good, is suitable for automatic moulding.This not only improves homogeneity, density and the sintering character of ceramics biscuits of carbonized bricks, but also can improve the Air quality of fitting room, and the protection workman is healthy, reduces workman's labor capacity, improves the quality of production and efficient.Molten and the dispersion agent of binding agent, water-soluble polymer that is added in the mist projection granulating slurry even can guarantee water base silicon carbide slurry under the solid load condition with higher, still keeps less viscosity, good flowing property and stability.
3, introducing aluminium nitride and yttrium oxide is sintering aid, compare with other auxiliary agent, suppressed the growth of carborundum grain in the sintering process, can prepare high densification, high strength, high tenacity aluminium nitride reinforced sibicon carbide ceramic, among its profile scanning Electronic Speculum figure (Fig. 3) as can be seen, columns such as grain morphology is, grain-size is between 0.5-2 μ m, original powder mean sizes then is 0.74 μ m, the relative density of pottery is 98%-99%, folding strength is between 400～600MPa, and fracture toughness property is 4～6MPam
1/2Between.
4, the present invention adopts deionized water to carry out ball mill mixing as solvent, not only can reduce production costs, and can also guarantee the safety of production process; Be suitable for producing in batches.In the mist projection granulating process, deionized water is evaporated, and in sintering process subsequently, binding agent, mixture of water-soluble polymer colloidal sol and dispersion agent are all volatilized to be fallen, the aluminium nitride reinforced sibicon carbide ceramic of therefore final gained is made up of these 3 kinds of compositions of silicon carbide, aluminium nitride and yttrium oxide or its sosoloid.
Description of drawings
Fig. 1 is the pattern synoptic diagram of the silicon carbide amyloplastid of gained behind the atomizing granulating technology;
Fig. 2 is the pattern synoptic diagram of the silicon carbide biscuit section of gained after the two one-step forming technologies;
Fig. 3 is that the crystalline substance of aluminium nitride reinforced sibicon carbide ceramic section of final gained is as synoptic diagram.
Embodiment
Below among the used embodiment, " part " all represents weight part.
The production method of embodiment 1, a kind of aluminium nitride reinforced sibicon carbide ceramic selects for use 94 parts of silicon carbide, 5 parts of aluminium nitride and 1 part of yttrium oxide as raw material, carries out following steps successively:
1), above-mentioned raw materials is put into 70 parts of deionized waters, the silicon carbide bead is as grinding medium; Add 0.5 part of polyvinyl alcohol, 2 parts of polyacrylamides and 1 part of polyacrylic acid again, the ball milling mixing was configured to water base silicon carbide slurry after 10 hours;
2), adopt atomizing granulating technology that above-mentioned water base silicon carbide slurry is carried out spraying drying, require 300～400 ℃ of hot blast inlet temperatures, 80～90 ℃ of temperature outs, 100 kilograms/hour of slurry flow; Prepare the silicon carbide amyloplastid;
3), above-mentioned silicon carbide amyloplastid is carried out two step mode moulding, promptly adopt 100～150MPa dry-pressing precompressed and 200～300MPa cold isostatic pressing end pressing successively, obtain highdensity silicon carbide biscuit;
4), above-mentioned silicon carbide biscuit is put into vacuum non-pressure sintering furnace, be prepared into aluminium nitride reinforced sibicon carbide ceramic after 2 hours in insulation under 1950～2200 ℃ of temperature.
This ceramic relative density is 98%-99%, and folding strength is between 400～600MPa, and fracture toughness property is 4～6MPam
1/2Between.
The production method of embodiment 2, a kind of aluminium nitride reinforced sibicon carbide ceramic selects for use 81 parts of silicon carbide, 17 parts of aluminium nitride and 2 parts of yttrium oxide as raw material, carries out following steps successively:
1), above-mentioned raw materials is put into 230 parts of deionized waters, the silicon carbide bead is as grinding medium; Add 2 parts of polyvinyl butyral acetals, 0.5 part of polyoxyethylene glycol and 1.5 parts of aluminum phosphates again, the ball milling mixing was configured to water base silicon carbide slurry after 20 hours;
2), adopt atomizing granulating technology that above-mentioned water base silicon carbide slurry is carried out spraying drying, 300～350 ℃ of hot blast inlet temperatures, 80～90 ℃ of temperature outs, 200 kilograms/hour of slurry flow prepare the silicon carbide amyloplastid;
3), above-mentioned silicon carbide amyloplastid is carried out two step mode moulding, promptly adopt 100～150MPa dry-pressing precompressed and 200～300MPa cold isostatic pressing end pressing successively, obtain highdensity silicon carbide biscuit;
4), above-mentioned silicon carbide biscuit is put into vacuum non-pressure sintering furnace, be prepared into aluminium nitride reinforced sibicon carbide ceramic after 5 hours in insulation under 1950～2200 ℃ of temperature.
This ceramic relative density is 98%-99%, and folding strength is between 400～600MPa, and fracture toughness property is 4～6MPam
1/2Between.
The production method of embodiment 3, a kind of aluminium nitride reinforced sibicon carbide ceramic selects for use 90 parts of silicon carbide, 8.5 parts of aluminium nitride and 1.5 parts of yttrium oxide as raw material, carries out following steps successively:
1), above-mentioned raw materials is put into 150 parts of deionized waters, the silicon carbide bead is as grinding medium; Add 3 parts of methylcellulose gum, 1 part of polyacrylamide and 0.5 part of polyacrylic acid again, the ball milling mixing was configured to water base silicon carbide slurry after 5 hours;
2), adopt atomizing granulating technology that above-mentioned water base silicon carbide slurry is carried out spraying drying, 350 ℃ of hot blast inlet temperatures, 80～90 ℃ of temperature outs, 150 kilograms/hour of slip flows prepare the silicon carbide amyloplastid;
3), above-mentioned silicon carbide amyloplastid is carried out two step mode moulding, promptly adopt 100～150MPa dry-pressing precompressed and 200～300MPa cold isostatic pressing end pressing successively, obtain highdensity silicon carbide biscuit;
4), above-mentioned silicon carbide biscuit is put into vacuum non-pressure sintering furnace, be prepared into aluminium nitride reinforced sibicon carbide ceramic after 4 hours in insulation under 1950～2200 ℃ of temperature.
This ceramic relative density is 98%-99%, and folding strength is between 400～600MPa, and fracture toughness property is 4～6MPam
1/2Between.
At last, it is also to be noted that what more than enumerate only is several specific embodiments of the present invention.Obviously, the invention is not restricted to above embodiment, many distortion can also be arranged.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.
Claims (5)
1, a kind of production method of aluminium nitride reinforced sibicon carbide ceramic is characterized in that: with weight percent be the yttrium oxide of 80%～94% silicon carbide, 5%～19% aluminium nitride and 1%～2% as raw material, may further comprise the steps:
1), above-mentioned raw materials is put into deionized water, add binding agent, mixture of water-soluble polymer colloidal sol and dispersion agent again, ball milling mixes and forms water base silicon carbide slurry after 5～20 hours; The weight of described binding agent is 0.5%～3% of raw material gross weight, the weight of mixture of water-soluble polymer colloidal sol is 0.5%～2% of raw material gross weight, the weight of dispersion agent is 0.5%～1.5% of raw material gross weight, and the weight ratio of described raw material and deionized water is 3: 7～3: 2;
2), adopt atomizing granulating technology above-mentioned water base silicon carbide slurry to be carried out spraying drying, 300～400 ℃ of hot blast inlet temperatures, 80～90 ℃ of temperature outs, 100～200 kilograms/hour of slurry flow; Prepare the silicon carbide amyloplastid;
3), above-mentioned silicon carbide amyloplastid is adopted 100～150MPa dry-pressing precompressed and 200～300MPa cold isostatic pressing end pressing successively, acquisition silicon carbide biscuit;
4), above-mentioned silicon carbide biscuit is put into vacuum non-pressure sintering furnace, after being incubated 1～5 hour under 1950～2200 ℃ of temperature, be prepared into aluminium nitride reinforced sibicon carbide ceramic.
2, the production method of aluminium nitride reinforced sibicon carbide ceramic according to claim 1 is characterized in that: described binding agent is polyvinyl alcohol, polyvinyl butyral acetal or methylcellulose gum.
3, the production method of aluminium nitride reinforced sibicon carbide ceramic according to claim 2 is characterized in that: described mixture of water-soluble polymer colloidal sol is polyacrylamide or polyoxyethylene glycol.
4, the production method of aluminium nitride reinforced sibicon carbide ceramic according to claim 3 is characterized in that: described dispersion agent is polyacrylic acid or aluminum phosphate.
5, the aluminium nitride reinforced sibicon carbide ceramic that makes according to any one production method in the claim 1～4.
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| CN101555143B (en) * | 2009-05-12 | 2012-06-06 | 宁波欧翔精细陶瓷技术有限公司 | Preparation method of normal pressure-sintered silicon carbide ceramics |
| CN101653964B (en) * | 2009-09-10 | 2011-05-18 | 浙江立泰复合材料有限公司 | Cold isostatic pressing method of large-size cylindrical thin silicon carbide ceramic biscuit |
| CN102030533B (en) * | 2010-11-09 | 2012-09-19 | 浙江大学 | Low-friction-factor silicon carbide ceramic sealing element and preparation method thereof |
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