CN100363303C - Silicon carbide base multiphase composite ceramic and its preparation method - Google Patents
Silicon carbide base multiphase composite ceramic and its preparation method Download PDFInfo
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- CN100363303C CN100363303C CNB2005100613035A CN200510061303A CN100363303C CN 100363303 C CN100363303 C CN 100363303C CN B2005100613035 A CNB2005100613035 A CN B2005100613035A CN 200510061303 A CN200510061303 A CN 200510061303A CN 100363303 C CN100363303 C CN 100363303C
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 80
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 239000002131 composite material Substances 0.000 title claims abstract description 55
- 239000000919 ceramic Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910017083 AlN Inorganic materials 0.000 claims abstract description 9
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 7
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 7
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 claims abstract description 5
- 238000005245 sintering Methods 0.000 claims description 25
- 238000005554 pickling Methods 0.000 claims description 14
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 13
- 235000015895 biscuits Nutrition 0.000 claims description 13
- 239000008187 granular material Substances 0.000 claims description 13
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 13
- 239000011812 mixed powder Substances 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- 238000003825 pressing Methods 0.000 claims description 12
- 238000010792 warming Methods 0.000 claims description 12
- 239000000084 colloidal system Substances 0.000 claims description 11
- 238000009413 insulation Methods 0.000 claims description 10
- 239000011230 binding agent Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 238000007704 wet chemistry method Methods 0.000 claims description 7
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 6
- 238000009694 cold isostatic pressing Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000007669 thermal treatment Methods 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 10
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000470 constituent Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 15
- 239000011159 matrix material Substances 0.000 description 14
- 238000005516 engineering process Methods 0.000 description 11
- 239000000835 fiber Substances 0.000 description 11
- 239000013078 crystal Substances 0.000 description 10
- 239000002245 particle Substances 0.000 description 10
- 230000002787 reinforcement Effects 0.000 description 10
- 230000003014 reinforcing effect Effects 0.000 description 9
- 229910010293 ceramic material Inorganic materials 0.000 description 8
- 230000002708 enhancing effect Effects 0.000 description 8
- 239000000654 additive Substances 0.000 description 7
- 208000037656 Respiratory Sounds Diseases 0.000 description 6
- 238000005452 bending Methods 0.000 description 6
- 238000009740 moulding (composite fabrication) Methods 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 230000000996 additive effect Effects 0.000 description 4
- 229910021431 alpha silicon carbide Inorganic materials 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000012010 growth Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000007773 growth pattern Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- -1 silicon carbide compound Chemical class 0.000 description 1
- 229960001866 silicon dioxide Drugs 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
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Abstract
The present invention discloses silicon carbide base multiphase composite ceramics. The present invention has the constituents (wt%): 72-to 90% of silicon carbide with more than 99.5% purity, 0 to 18% of aluminium nitride or silicon nitride, and 8 to 10% of yttrium aluminum garnet / aluminum oxide. The present invention also discloses a preparation method of the silicon carbide base multiphase composite ceramics. The preparation method has the advantages of compact technique and easy operation. The silicon carbide base multiphase composite ceramics prepared by the method have the advantages of good hardness, good flexural strength, good fracture toughness, etc.
Description
Technical field
The present invention relates to a kind of preparation method of silicon carbide ceramics, specifically, is a kind of preparation method of silicon carbide base multiphase composite ceramic.
Background technology
As a kind of high-temperature structural material, silicon carbide ceramics has the unrivaled performance of other material, and is good or the like as high high-temp stability, wear-resisting acid-alkali-corrosive-resisting, good thermal shock, low-expansion coefficient, high thermal conductivity, creep resistance and antioxidant property.Thyrite has been widely used in industrial circle and national defense industry such as machinery, electronics, petrochemical complex, metallurgy.As machinery sealing material of new generation, silicon carbide has been confirmed as the 4th kind of basic material since metal, aluminum oxide, Wimet in the world.Though silicon carbide ceramics has many performances, also be applied in a lot of fields; But its room temperature strength is low, and toughness is not enough, and moulding is difficulty relatively, has also limited its application.Meanwhile, various fields such as the national defence in the high speed development, space technology, automobile, the energy constantly propose new requirement to structured material.Therefore have only the toughness reinforcing means of the various enhancings of employing to prepare carborundum based material, improve its intensity and toughness, could satisfy the requirement that silicon carbide ceramics is used in leading-edge fields such as national defence, space technologies better.Preparation integrates the composite silicon carbide ceramic material of the excellent performance of high-strength, high-ductility, high multifrequency nature such as hard, corrosion-resistant, high temperature resistant, wear-resisting, becomes the main flow of thyrite research and development.
By domestic and international material supplier author unremitting effort for many years, develop the toughness reinforcing means of multiple enhancing such as to comprise original position enhancing, particle enhancing, whisker (fiber) reinforcement, and proposed crackle deviation, crackle bending, crackle bridging and a series of toughness reinforcing enhancings such as extracted theoretical.According to the difference of its reinforcing and toughening principle, the silicon carbide base multiphase composite ceramic material can be divided into whisker (or fiber) reinforcement composite ceramics, particle strengthen composite ceramics, from reinforcement composite ceramics and gradient composite ceramic.The crystal whisker excess weld metal carborundum based material is that whisker is dispersed in the SiC matrix, and when matrix material was subjected to extraneous stress, crackle deflected because the effect of whisker makes, crackle bridging, whisker are extracted, and strengthened toughness reinforcing purpose thereby reach; The crystal whisker excess weld metal carborundum based material mainly is SiC (w)/SiC matrix material.The mechanical property of fibrous reinforcement carborundum based material depends on the performance and the distribution situation of fiber in matrix at fiber, matrix and interface.Interface performance has determined the effect that fiber is introduced, and influences the fracture mode of matrix material to a great extent, and the enhancing toughening effect of fiber is fiber unsticking, the bridging that produces therefrom and extracts homenergic consume mechanism.Fortifying fibre mainly adopts Nextell, Nicalon, continuous carbon fibre, SiC fiber or the like at present.Particle reinforcement carborundum based material is to introduce second phase or the third phase particle in the SiC matrix, because thermal expansivity between particle and the matrix and the difference on the Young's modulus, cause the interface of matrix and particle to form the stressed zone, this stress and applied stress interact, crackle is advanced to be obstructed, take place deviation, around to and branch, thereby improve the intensity and the toughness of silicon carbide.At present, the heterogeneous composite material that has developed has: SiC-TiC, SiC-TiB
2, SiC-TiC-TiB
2, SiC-TiC-Al
2O
3, SiC-AlN, SiC-Mullite, SiC-YAG, SiC-Si
3N
4Or the like.Mainly concentrate on growth in situ column and needle-like β-Si from the reinforcement composite material of silicon carbide
3N
4, make SiC crystal grain generation refinement, Si
3N
4Cause material surface to form compressive stress layer with the difference of SiC layer on the coefficient of expansion, thereby make the intensity and toughness will double of matrix material than pure SiC material.The original position reinforced composite mainly is meant SiC particulate crystal conversion, be that β-SiC transforms to α-SiC, at α-SiC parent crystal surface growth-layer α-SiC settled layer, make the particle growth anisotropy, form " nuclear/shell " structure, crystal grain has good length-to-diameter ratio, reaches the enhanced purpose by the crystal grain bridging.
Though, the exploitation of silicon-carbide-based composite ceramic material and strengthen toughness reinforcing theory and method is well developed, but still have following problem:
1) no matter be crystal whisker excess weld metal, fibrous reinforcement,, still particle reinforcement, maximum difficult point is owing to structural form, difference of specific gravity on technology, makes to strengthen between unit and the matrix to be difficult to accomplish homodisperse, thereby make reinforcing effect not good, even influence the silicon carbide self performance; Therefore take measures to make the composite components homogenizing to seem particularly important;
2), crystal whisker excess weld metal and fiber reinforced complicated process of preparation, the cost height is difficult to realize industrialization production; Realize that the particle of introducing is to the use properties of composite material of silicon carbide, and is unfavorable as oxidation-resistance, erosion resistance and hot strength though particle enhanced technology is relatively easy; Must adopt advanced fabricating technology to realize from reinforcement or original position enhancement techniques; Therefore it is necessary adopting reinforcement measure easy, that cost is low in actual production.
Summary of the invention
At the deficiencies in the prior art part, the invention provides that a kind of technology is succinct, the preparation method of the silicon carbide base multiphase composite ceramic of easy handling, and the silicon carbide base multiphase composite ceramic of good combination properties such as this kind method hardness of producing, bending strength, fracture toughness property.
The present invention is for reaching above purpose, be to realize by such technical scheme: a kind of silicon carbide base multiphase composite ceramic is provided, and this ceramic weight percent consists of: purity reaches SiC (silicon carbide) 72～90%, AlN (aluminium nitride) or the Si more than 99.5%
3N
4(silicon nitride) 0～18% and YAG (yttrium aluminum garnet, are Y
3Al
5O
12) 8～10%.
The present invention also provides the preparation method of above-mentioned silicon carbide base multiphase composite ceramic, may further comprise the steps successively:
1), powder shaped silicon carbide is carried out pickling, the silicon carbide purity after the pickling is reached more than 99.5%;
2), in above-mentioned silicon carbide, add the aluminium nitride or the silicon nitride of powder shaped, make mixed powder after the mixing;
3), adopting wet chemistry method, preparation yttrium aluminum garnet and deionized water weight ratio is 15: 85 colloid; In this colloid, add above-mentioned mixed powder then and as the PVA (polyvinyl alcohol) of binding agent, stir, dry, 920～950 ℃ of thermal treatments 4～6 hours, make heterogeneous composite granule, the consumption of described polyvinyl alcohol is 3～5% of a mixed powder gross weight;
4), above-mentioned heterogeneous composite granule is adopted the dry-pressing precompressed of 70～100MPa earlier, carry out the cold isostatic pressing end pressing of 200～400MPa again, obtain biscuit;
5), above-mentioned biscuit is placed the vacuum sintering furnace sintering that heats up, insulation is 0.5～1 hour when being warming up to 1600～1700 ℃, continues to be warming up to 1750～2000 ℃ of insulations 1～2 hour then, and sintering finishes.
A kind of improvement as the preparation method of silicon carbide base multiphase composite ceramic of the present invention: step 5) is warming up to 1600～1700 ℃ with the heat-up rate of 5～20 ℃/min.
Further improvement as the preparation method of silicon carbide base multiphase composite ceramic of the present invention: adopt HF (hydrofluoric acid) and HNO in the step 1)
3The mix acid liquor of (nitric acid) carries out pickling, described HF and HNO
3Mol ratio be 1: 2.
Silicon carbide base multiphase composite ceramic of the present invention and preparation method thereof obtains through long term studies, experiment back the contriver.The present invention by the design of material design and processes, at first adopts the method purification silicon carbide powder that mixes pickling according to the heterogeneous composite material technology on the broad sense, selects aluminium nitride (AlN) or silicon nitride (Si then
3N
4) as the second phase body material, adopt wet chemistry method to introduce additive again, additive is YAG or YAG-Al
2O
3(YAG is Y
3Al
5O
12), realized the thorough mixing and the uniform distribution of the second phase matrix, additive and SiC matrix.The present invention adopts two one-step formings and two-step sintering technology, realized the low-temperature sintering of composite ceramic material, the grain-size of the second phase matrix and growth pattern, structure, size and the failure mode etc. of SiC crystal grain have been controlled, the collaborative enhancing that has realized silicon carbide base multiphase composite ceramic is toughness reinforcing, thereby obtains high performance silicon carbide base multiphase composite ceramic.Among the present invention employed as one of colloid composition water and as the PVA of binding agent, volatilizedly in sintering process fall.According to the silicon carbide base multiphase composite ceramic that method of the present invention makes, its body is close to be 3.05～3.18g/min
3, hardness is 22～28GPa, bending strength is 420～1100MPa, fracture toughness property 3.1～6.8MPa.m
1/2
The present invention compared with prior art has the following advantages:
(1), removes free silicon-dioxide in the silicon carbide powder to silicon carbide powder mixing pickling as far as possible; Thereby reduce Al
2O
3-Y
2O
3With SiO
2Eutectic reaction and vaporization at high temperature loss;
(2) introduce aluminium nitride (AlN) or silicon nitride (Si
3N
4) as the second phase body material, the YAG additive both can be used as sintering aid, also can be used as wild phase, thereby form the toughness reinforcing silicon-carbide-based composite ceramic of heterogeneous enhancing;
(3) adopt wet chemistry method to introduce YAG or YAG-Al
2O
3Additive overcomes problems such as distribution of additives inequality that present employing mechanical mixing brings, sintering temperature height, sintered density difference;
(4) adopt two one-step formings and two-step sintering technology, overcome low, the problems such as sintering volatilization loss big, sintered density difference of biscuit relative density that present existing one-step moulding, sintering technology bring.
The silicon carbide base multiphase composite ceramic material and the goods of the present invention's preparation can be used for components and parts such as processing machinery wear ring, bearing housing, also can be used for preparing electronic substrates; Application prospect in industries such as space flight, national defence, electronics is very wide.
Embodiment
Embodiment 1, a kind of silicon carbide base multiphase composite ceramic, this ceramic weight percent consists of: purity reaches SiC 90% and the YAG 10% more than 99.5%.
According to above-mentioned weight ratio, concrete preparation method is as follows:
1) be that 0.78 micron powder shaped SiC adopts HF and HNO with median size,
3Mix acid liquor carry out pickling, the SiC purity after the pickling is reached more than 99.5%;
2), adopt wet chemistry method, preparation YAG and deionized water weight ratio are 15: 85 colloid, in this colloid, add above-mentioned SiC powder then and as the PVA of binding agent, stir, dry, 920～950 ℃ of thermal treatments 4～6 hours, make heterogeneous composite granule, the consumption of PVA is 3% of a SiC powder gross weight; The presoma of YAG is chemical reagent, and purity is greater than 99.9%;
3), above-mentioned heterogeneous composite granule is adopted the dry-pressing precompressed of 70～100MPa earlier, carry out the cold isostatic pressing end pressing of 200～400MPa again, obtain biscuit behind two one-step formings;
4), above-mentioned biscuit is placed the vacuum sintering furnace sintering that heats up, insulation is 0.5～1 hour when being warming up to 1600～1700 ℃ with the heat-up rate of 5～20 ℃/min, continue to be warming up to 1750～2000 ℃ of insulations 1～2 hour then, sintering finishes the silicon carbide base multiphase composite ceramic material that the back obtains, and its body is close to be 3.0～3.15g/min
3, hardness is 20～28GPa, bending strength is 400～1100MPa, fracture toughness property 3.0～7MPam
1/2
Embodiment 2, a kind of silicon carbide base multiphase composite ceramic, this ceramic weight percent consists of: purity reaches SiC82%, AlN 10% and the YAG8% more than 99.5%.
According to above-mentioned weight ratio, concrete preparation method is as follows:
1) be that 0.78 micron powder shaped SiC adopts HF and HNO with median size,
3Mix acid liquor carry out pickling, the SiC purity after the pickling is reached more than 99.5%;
2), in above-mentioned SiC, add the AlN of powder shaped, make mixed powder behind the uniform mixing;
3), adopt wet chemistry method, preparation YAG and deionized water weight ratio are 15: 85 colloid, in this colloid, add above-mentioned mixed powder then and as the PVA of binding agent, stir, dry, 920～950 ℃ of thermal treatments 4～6 hours, make heterogeneous composite granule, the consumption of PVA is 4% of a mixed powder gross weight; The presoma of YAG is chemical reagent, and purity is greater than 99.9%;
4), above-mentioned heterogeneous composite granule is adopted the dry-pressing precompressed of 70～100MPa earlier, carry out the cold isostatic pressing end pressing of 200～400MPa again, obtain biscuit behind two one-step formings;
5), above-mentioned biscuit is placed the vacuum sintering furnace sintering that heats up, insulation is 0.5～1 hour when being warming up to 1600～1700 ℃ with the heat-up rate of 5～20 ℃/min, continue to be warming up to 1750～2000 ℃ of insulations 1～2 hour then, sintering finishes the silicon carbide base multiphase composite ceramic material that the back obtains, and its body is close to be 3.0～3.15g/min
3, hardness is 20～28GPa, bending strength is 400～1100MPa, fracture toughness property 3.0～7MPam
1/2
Embodiment 3, a kind of silicon carbide base multiphase composite ceramic, this ceramic weight percent consists of: purity reaches SiC72%, the Si more than 99.5%
3N
418% and YAG-Al
2O
310%.
According to above-mentioned weight ratio, concrete preparation method is as follows:
1) be that 0.78 micron powder shaped SiC adopts HF and HNO with median size,
3Mix acid liquor carry out pickling, the SiC purity after the pickling is reached more than 99.5%;
2) Si that, in above-mentioned SiC, adds powder shaped
3N
4, make mixed powder behind the uniform mixing;
3), adopt wet chemistry method, preparation YAG-Al
2O
3With the deionized water weight ratio be 15: 85 colloid, in this colloid, add above-mentioned mixed powder then and as the PVA of binding agent, stir, dry, 920～950 ℃ of thermal treatments 4～6 hours, make heterogeneous composite granule, the consumption of PVA is 5% of a mixed powder gross weight; The presoma of YAG is chemical reagent, and purity is greater than 99.9%;
4), above-mentioned heterogeneous composite granule is adopted the dry-pressing precompressed of 70～100MPa earlier, carry out the cold isostatic pressing end pressing of 200～400MPa again, obtain biscuit behind two one-step formings;
5), above-mentioned biscuit is placed the vacuum sintering furnace sintering that heats up, insulation is 0.5～1 hour when being warming up to 1600～1700 ℃ with the heat-up rate of 5～20 ℃/min, continue to be warming up to 1750～2000 ℃ of insulations 1～2 hour then, sintering finishes the silicon carbide base multiphase composite ceramic material that the back obtains, and its body is close to be 3.0～3.15g/min
3, hardness is 20～28GPa, bending strength is 400～1100MPa, fracture toughness property 3.0～7MPam
1/2
Comparative Examples: a kind of silicon carbide base multiphase composite ceramic, this ceramic weight percent consists of: SiC90% and Al
2O
3+ Y
2O
310%; The consumption of binding agent PVA is SiC and Al
2O
3+ Y
2O
35% of gross weight; Described Al
2O
3+ Y
2O
3Middle Y
2O
3And Al
2O
3Mol ratio is 3: 5, Al
2O
3And Y
2O
3Generate YAG by pyroreaction.Above-mentioned powder mixes back preparation composite granule, and composite granule is meter dry-pressing precompressed with 100MPa earlier, carries out the cold isostatic pressing end pressing of 250MPa again, obtains biscuit behind two one-step formings; Biscuit prepares the silicon carbide compound pottery at 2000 ℃ of sintering after 2 hours.It is 2.8～3.05g/min
3, the density physical strength is 350MPa, hardness is 20GPa.
Compare YAG of the present invention and YAG-Al with the comparison sample
2O
3Additive adds with colloidal form, form heterogeneous composite granule at 920-950 ℃, and relatively sample need could form more than 1550 ℃.Therefore sintering temperature of the present invention is lower, and sintering character and mechanical property all are better than the comparison sample.
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 (3)
1. the preparation method of a silicon carbide base multiphase composite ceramic, it is characterized in that this ceramic weight percent consists of: purity reaches silicon carbide 72～90%, aluminium nitride or silicon nitride 0～18% and the yttrium aluminum garnet 8～10% more than 99.5%, may further comprise the steps successively:
1), powder shaped silicon carbide is carried out pickling, the silicon carbide purity after the pickling is reached more than 99.5%;
2), in above-mentioned silicon carbide, add the aluminium nitride or the silicon nitride of powder shaped, make mixed powder after the mixing;
3), adopt wet chemistry method, preparation yttrium aluminum garnet and deionized water weight ratio are 15: 85 colloid, in described colloid, add above-mentioned mixed powder then and as the polyvinyl alcohol of binding agent, stir, dry, 920～950 ℃ of thermal treatments 4～6 hours, make heterogeneous composite granule, the consumption of described polyvinyl alcohol is 3～5% of a mixed powder gross weight;
4), above-mentioned heterogeneous composite granule is adopted the dry-pressing precompressed of 70～100MPa earlier, carry out the cold isostatic pressing end pressing of 200～400MPa again, obtain biscuit;
5), above-mentioned biscuit is placed the vacuum sintering furnace sintering that heats up, insulation is 0.5～1 hour when being warming up to 1600～1700 ℃, continues to be warming up to 1750～2000 ℃ of insulations 1～2 hour then, and sintering finishes.
2. the preparation method of silicon carbide base multiphase composite ceramic according to claim 1, it is characterized in that: described step 5) is warming up to 1600～1700 ℃ with the heat-up rate of 5～20 ℃/min.
3. the preparation method of silicon carbide base multiphase composite ceramic according to claim 1 and 2 is characterized in that: adopt the mix acid liquor of hydrofluoric acid and nitric acid to carry out pickling in the described step 1), the mol ratio of described hydrofluoric acid and nitric acid is 1: 2.
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| CN101164989B (en) * | 2006-10-16 | 2011-06-01 | 宁波大学 | Method for preparing silicon carbide ceramic plasticized by rod-like aluminum oxide particle and carbon fibre combination |
| CN101164997B (en) * | 2006-10-16 | 2010-07-28 | 宁波大学 | Method for preparing silicon carbide ceramic plasticized by rod-like aluminum oxide particle and silicon carbide whisker combination |
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