CN104761246A - Method for manufacturing high-performance aluminum oxide/nano silicon carbide composite ceramic - Google Patents
Method for manufacturing high-performance aluminum oxide/nano silicon carbide composite ceramic Download PDFInfo
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Abstract
A method for manufacturing high-performance aluminum oxide/nano silicon carbide composite ceramic is characterized in that bauxite powder and nano SiC particles are adopted as main raw materials, wet mixing, drying and precalcination are carried out, then bury-burning is carried out after forming, sintering is carried out at the temperature of 1,400 DEG C to 1,550 DEG C, heat preservation is carried out for one hour, then natural cooling is carried out to room temperature, and the high-performance aluminum oxide/nano silicon carbide composite ceramic is manufactured. According to the manufactured composite ceramic, the nano SiC particles are distributed in an aluminum oxide base in situ, a little mullite exists, the method is simple in manufacturing process, and the manufactured composite ceramic has the high cost performance.
Description
Technical field
The present invention relates to the preparation method of a kind of high-performance aluminum oxide/SiC nanocomposites, belong to the preparing technical field of engineering ceramic material.
Background technology
Alumina-ceramic is considered to " steel " in stupalith, and in global Ceramic Market, its market share accounts for more than 75%.80-90 porcelain refers to that quality of alumina content is the alumina-ceramic of 80-90%, the product be made up of 80-90 porcelain because of its wear resistance, fracture toughness property, flexural strength and heat-shock resistance etc. all poor, often only as low and middle-grade ceramic product material.Carried out the research of the toughen and intensify of alumina-ceramic, the main method adopting Zirconium oxide plasticizing and whisker or nano particle toughened and reinforced for this reason.Large quantity research confirms, by adding silicon carbide whisker or nano particle, not only to improve the mechanical property of alumina-ceramic by a relatively large margin, can also improve its thermal shock resistance simultaneously, expand its Application Areas.But about the research of aluminum oxide/carborundum composite-phase ceramic (or nano ceramics) mainly concentrates on high-purity alumina ceramic system.Namely in high purity aluminium oxide (alumina content is often more than 99%), add proper amount of nano SiC particle or SiC whisker, obtain sintered compact by hot pressing, normal pressure gas-protecting sintering, its sintering temperature is higher, usually more than 1650 DEG C.The performance of this composite diphase material comparatively pure alumina is compared, and has raising by a relatively large margin, but owing to requiring high to agglomerating plant, need atmosphere protection, the property/valency of product is given prominence to than not, thus limits the development & application of this material product.
Domestic at present about the patent of aluminum oxide/nanometer (whisker) carbide composite ceramic technology of preparing mainly contains CN 1821175A, CN 101555142A and CN 101880163 A.Chinese patent CN 1821175A describes the preparation method of a kind of silicon carbide whisker/aluminium oxide composite ceramic powder body; with natural kaolin and charcoal source for raw material; charcoal source is graphite or carbon black inorganic carbon or macromolecule organic; an atmospheric hydrogen is filled with as shielding gas after vacuumizing in atmosphere furnace; 1450 DEG C ~ 1550 DEG C calcinings, obtain silicon carbide whisker/aluminium oxide nano level, submicron order composite powder.But do not introduce the technology of preparing of associated ceramic.Patent CN 101555142A describes a kind of preparation method of nanosized silicon carbide toughened aluminum oxide bulletproof ceramic, adopt high-purity alumina powder, adding massfraction is the kaolin of 0.8 ~ 1.3% and the burning talcum of 0.5 ~ 1.0%, additional mass ratio is 3 ~ 8% again, granularity is at the silicon carbide powder of 10 ~ 30 nanometers, adopt Inject & congeal shaping method, at 1650 ~ 1700 DEG C of sintering, nanometer silicon carbide/aluminum oxide composite ceramics can be obtained; Nanometer silicon carbide is introduced in alumina substrate by outer add mode, is therefore difficult to be uniformly dispersed.External Patents comprises: Korean Patent KR9710308, world patent WO0078690, Japanese Patent JP8208318, European patent EP 0419150, United States Patent (USP) 4,657,877,4,746,635,4,749,667 and 5,455,212.Japanese Patent JP8208318 describes that in aluminum oxide, add volume fraction be 0.1-30vol.%SiC particle, prepares Al by atmosphere sintering
2o
3the method of/SiC complex phase ceramic.Its feature: by Al
2o
3/ SiC composite powder is pressed into base substrate, places the Al that median size is 3.0 μm around base substrate
2o
3powder and/or median size are the SiO of 5.0 μm
2with C powder, base substrate is at Ar or N
2by normal pressure or more under high pressure under protective atmosphere, in high temperature sintering.Europe EP0419150 is that adding volume fraction is respectively 3 ~ 50%, and particle diameter is the SiC particle of 5 ~ 20 μm, or sheet (tabular) SiC, and its median size is 5 ~ 50 μm, and thickness is less than or equal to 1/3 of particle diameter with oxide compound or non-oxidized substance for matrix.In 120 DEG C of dryings 24 hours after composite powder mix grinding, powder to be sieved, shaping, 1400 ~ 1900 DEG C, normal pressure-sintered in Ar atmosphere.Comparatively host oxide is ceramic by improving by a relatively large margin for the fracture toughness property of material.European patent 0310342A2 be greater than with purity 99% Al
2o
3for matrix, add respectively diameter be less than the SiC particle of 0.5 μm or length be 1.0 ~ 5 μm, the length SiC whisker that is less than 3.Formed body through hot isostatic pressing, hot pressing or normal pressure atmosphere sintering, can obtain dense sintering body at 1400 ~ 1800 DEG C.United States Patent (USP) 4,657,877,4,746,635,4,749,667 all with aluminum oxide or mullite for matrix, add zirconium white and SiC whisker or particle, adopt pressure or atmosphere sintering to prepare Al
2o
3/ ZrO
2/ SiC composite diphase material.Above-mentioned preparation method take all high purity aluminium oxide as matrix, adds SiC whisker or nano particle by mechanical mixing, and formed body adopts normal pressure, atmosphere protection or pressure (hot pressing, hot isostatic pressing and air pressure etc.) sintering, obtained dense sintering body.
Summary of the invention
The object of the present invention is to provide the preparation method of a kind of high-performance aluminum oxide/SiC nanocomposites, the complex phase ceramic prepared in this approach is dispersed with nano SiC granule at alumina substrate situ, and have a small amount of mullite to exist, this method preparation technology is simple, and obtained complex phase ceramic has higher cost performance.
For achieving the above object, the present invention is realized by following technical proposals: a kind of preparation method of high-performance aluminum oxide/SiC nanocomposites, it is characterized in that: with bauxitic clay powder and micron-sized SiC particle for main raw material, through wet mixing, drying, precalcining, then carry out burying burning after shaping, at 1400 ~ 1550 DEG C of sintering, be incubated 1 hour, then naturally cool to room temperature, obtained high-performance aluminum oxide/SiC nanocomposites.
Raw material: quality of alumina content be 80 ~ 90% bauxitic clay powder peace all particle diameter be the micron order SiC of 1.5 ~ 5.0 μm; The two mass ratio: SiC is 5 ~ 10% of bauxitic clay powder;
Preparation process: add water after being mixed in proportion by above-mentioned raw materials powder, ball milling in Ball-stirring mill, mixes; Dried mixed powder precalcining, precalcining temperature 900 ~ 1050 DEG C, is incubated 2 ~ 6 hours; Put into crucible after powder is shaping and bury burning, burying material powder adopts particle size range to be 600-1200 μm of α-SiC, the crucible that molding blank is housed is rapidly heated to 1200 DEG C with the heat-up rate of 350 DEG C/h, then rise to 1400 ~ 1550 DEG C again with the heat-up rate of 200 DEG C/h to sinter, be incubated 1 hour, then naturally cool to room temperature, obtained high-performance aluminum oxide/SiC nanocomposites.
For making raw material mix in preparation process, can add when material powder is mixed in proportion and accounting for the dispersion agent methacrylic acid amino that bauxite powder body mass ratio is 0.08%.
High-performance aluminum oxide/the SiC nanocomposites prepared according to above-mentioned preparation method has the nanometer silicon carbide of growth in situ, forms SiO
2the particle of clad nano SiC, and a small amount of mullite parcel be at high temperature formed, carborundum grain is of a size of 200 ~ 410nm, and the flexural strength of material is 306 ~ 380MPa, and fracture toughness property is 3.3 ~ 5.2MPam
1/2.
The invention has the advantages that and adopt A1
2o
3mass content is the bauxitic clay of 80-90% and micron-sized SiC powder is raw material, then carries out pre-burning to mixed composite powder, forms SiO
2the particle of clad nano SiC, the mullite be at high temperature formed wraps up.Enter crucible oxidation coarse particles buried powder α-SiC and nano SiC at sintering process because of a small amount of air, make the further refinement of nano SiC granule on the one hand, in crucible, form reducing atmosphere, whole sintering process is without the need to additional atmosphere protection simultaneously.According to said method obtained aluminum oxide/SiC nanocomposites, has intensity and toughness is higher, cost is low feature.
Accompanying drawing explanation
Fig. 1 is the present invention in 1500 DEG C of sintering, insulation 1 hour, the XRD figure spectrum of obtained aluminum oxide/nano silicon carbide ceramic.
Fig. 2 is the present invention in 1500 DEG C of sintering, insulation 1 hour, the electromicroscopic photograph of obtained aluminum oxide/nano silicon carbide ceramic.
Embodiment
Take quality of alumina content as the bauxitic clay of 80 ~ 90% be main raw material, adding mass content is 5 ~ 10%, and median size is the micron order SiC particle of 1.5 ~ 5.0 μm; By powder wet mixing, drying, 900 ~ 1050 DEG C of precalcinings 2 ~ 6 hours, powder is shaping, bury burning, the particle size range of burying material powder α-SiC is 600-1200 μm, be rapidly heated by the sealed crucible that base substrate is housed to 1200 DEG C, heat-up rate is greater than 350 DEG C/h and is advisable, and continues to be warmed up to 1400 ~ 1550 DEG C, heat-up rate is 200 DEG C/h, is incubated 1 hour.The Toughened Alumina Ceramics of the nanometer silicon carbide enhancing with growth in situ can be obtained.The flexural strength of material is 306 ~ 380MPa, and fracture toughness property is 3.3 ~ 5.2MPam
1/2.Claim α-SiC to bury material quality after burning 5 ~ 10 stoves, when burying material weightening finish more than 10%, need change or replace part α-SiC and burying material, the consistence of quality product can be ensured.
Embodiment 1:
Accurately take the bauxitic clay l kilogram that mass content is 80%, in bauxitic clay powder, add mass ratio is 5%, and median size is the SiC powder 50 grams of 1.5 μm.Add 1700ml distilled water again, add simultaneously and account for powder quality than the methacrylic acid amino dispersion agent being 0.08%.By compound ball milling 4 hours in Ball-stirring mill, 1050 DEG C of precalcinings 4 hours after drying, then granulation, shaping.Molding blank is put into crucible, buries with the α-SiC powder that particle size range is 600-1200 μm and cover base substrate, cover tightly crucible cover; Be rapidly heated to 1200 DEG C with the speed of 350 DEG C/h, continue to heat up 1500 DEG C with the speed of 200 DEG C/h, be incubated 1 hour.Then naturally cool to room temperature, a small amount of mullite (as shown in Figure 1) is had in obtained aluminum oxide/SiC nanocomposites, the size of carborundum grain is about 200nm (as shown in the figure), and the average bending strength of material is 310 ± 26MPa, and average fracture toughness property is
3.3±0.48MPa·m
1/2。
Embodiment 2:
Accurately take the bauxitic clay l kilogram that mass content is 80%, in bauxitic clay powder, add mass ratio is 8%, and median size is the SiC powder 80 grams of 2.5 μm.Add 1700ml distilled water again, add simultaneously and account for powder quality than the methacrylic acid amino dispersion agent being 0.08%.By compound ball milling 4 hours in Ball-stirring mill, 1050 DEG C of precalcinings 6 hours after drying, then granulation, shaping.Molding blank is put into crucible, buries with the α-SiC powder that particle size range is 600-1200 μm and cover base substrate, cover tightly crucible cover; Be rapidly heated to 1200 DEG C with the speed of 350 DEG C/h, continue to heat up 1530 DEG C with the speed of 200 DEG C/h, be incubated 1 hour.Then naturally cool to room temperature, have a small amount of mullite in obtained aluminum oxide/SiC nanocomposites, the size of carborundum grain is about 220nm, and the average bending strength of material is 360 ± 33MPa, and average fracture toughness property is 5.2 ± 0.53MPam
1/2.
Embodiment 3:
Accurately take the bauxitic clay l kilogram that mass content is 90%, in bauxitic clay powder, add mass ratio is 10%, and median size is the SiC powder 100 grams of 5.0 μm.Add 1700ml distilled water again, add simultaneously and account for powder quality than the methacrylic acid amino dispersion agent being 0.08%.By compound ball milling 4 hours in Ball-stirring mill, 900 DEG C of precalcinings 2 hours after drying, then granulation, shaping.Molding blank is put into crucible, buries with the α-SiC powder that particle size range is 600-1200 μm and cover base substrate, cover tightly crucible cover; Be rapidly heated to 1200 DEG C with the speed of 350 DEG C/h, continue to heat up 1550 DEG C with the speed of 200 DEG C/h, be incubated 1 hour.Then naturally cool to room temperature, have a small amount of mullite in obtained aluminum oxide/SiC nanocomposites, the size of carborundum grain is about 410nm, and the average bending strength of material is 420 ± 23MPa, and average fracture toughness property is 3.8 ± 0.50MPam
1/2.
Embodiment 4:
Accurately take the bauxitic clay l kilogram that mass content is 90%, in bauxitic clay powder, add mass ratio is 10%, and median size is the SiC powder 100 grams of 2.5 μm.Add 1700ml distilled water again, add simultaneously and account for powder quality than the methacrylic acid amino dispersion agent being 0.08%.By compound ball milling 4 hours in Ball-stirring mill, 1050 DEG C of precalcinings 6 hours after drying, then granulation, shaping.Molding blank is put into crucible, buries with the α-SiC powder that particle size range is 600-1200 μm and cover base substrate, cover tightly crucible cover; Be rapidly heated to 1200 DEG C with the speed of 350 DEG C/h, continue to heat up 1530 DEG C with the speed of 200 DEG C/h, be incubated 1 hour.Then naturally cool to room temperature, have a small amount of mullite in obtained aluminum oxide/SiC nanocomposites, the size of carborundum grain is about 240nm, and the average bending strength of material is 440 ± 26MPa, and average fracture toughness property is 4.6 ± 0.49MPam
1/2.
Claims (8)
1. the preparation method of high-performance aluminum oxide/SiC nanocomposites, it is characterized in that: with bauxitic clay powder and micron-sized SiC particle for main raw material, through wet mixing, drying, precalcining, then carry out burying burning after shaping, at 1400 ~ 1550 DEG C of sintering, be incubated 1 hour, then naturally cool to room temperature, obtained high-performance aluminum oxide/SiC nanocomposites.
2. the preparation method of high-performance aluminum oxide/SiC nanocomposites according to claim 1, is characterized in that:
Raw material: quality of alumina content be 80 ~ 90% bauxitic clay powder peace all particle diameter be the micron order SiC of 1.5 ~ 5.0 μm; The two mass ratio: SiC is 5 ~ 10% of bauxitic clay powder;
Preparation process: add water after being mixed in proportion by above-mentioned raw materials powder, ball milling in Ball-stirring mill, mixes; Dried mixed powder precalcining, precalcining temperature 900 ~ 1050 DEG C, is incubated 2 ~ 6 hours; Put into crucible after powder is shaping and bury burning, burying material powder adopts particle size range to be 600-1200 μm of α-SiC, the crucible that molding blank is housed is rapidly heated to 1200 DEG C with the heat-up rate of 350 DEG C/h, then rise to 1400 ~ 1550 DEG C again with the heat-up rate of 200 DEG C/h to sinter, be incubated 1 hour, then naturally cool to room temperature, obtained high-performance aluminum oxide/SiC nanocomposites.
3. the preparation method of high-performance aluminum oxide/SiC nanocomposites according to claim 2, is characterized in that: add when material powder is mixed in proportion and account for the dispersion agent methacrylic acid amino that bauxite powder body mass ratio is 0.08%.
4. the preparation method of the high-performance aluminum oxide/SiC nanocomposites according to claim 1,2 or 3, is characterized in that: described raw material: quality of alumina content be 80% bauxitic clay powder peace all particle diameter be the micron order SiC of 1.5 μm; The two mass ratio: SiC is 5% of bauxitic clay powder;
Precalcining temperature is 1050 DEG C, is incubated 4 hours; Sintering temperature is 1500 DEG C, is incubated 1 hour.
5. the preparation method of the high-performance aluminum oxide/SiC nanocomposites according to claim 1,2 or 3, is characterized in that: described raw material: quality of alumina content be 80% bauxitic clay powder peace all particle diameter be the micron order SiC of 2.5 μm; The two mass ratio: SiC is 8% of bauxitic clay powder;
Precalcining temperature is 1050 DEG C, is incubated 6 hours; Sintering temperature is 1530 DEG C, is incubated 1 hour.
6. the preparation method of the high-performance aluminum oxide/SiC nanocomposites according to claim 1,2 or 3, is characterized in that: described raw material: quality of alumina content be 90% bauxitic clay powder peace all particle diameter be the micron order SiC of 5.0 μm; The two mass ratio: SiC is 10% of bauxitic clay powder;
Precalcining temperature is 900 DEG C, is incubated 2 hours; Sintering temperature is 1550 DEG C, is incubated 1 hour.
7. the preparation method of the high-performance aluminum oxide/SiC nanocomposites according to claim 1,2 or 3, is characterized in that: described raw material: quality of alumina content be 90% bauxitic clay powder peace all particle diameter be the micron order SiC of 2.5 μm; The two mass ratio: SiC is 10% of bauxitic clay powder;
Precalcining temperature is 1050 DEG C, is incubated 6 hours; Sintering temperature is 1530 DEG C, is incubated 1 hour.
8. high-performance aluminum oxide/SiC nanocomposites of preparing of preparation method according to claim 1, is characterized in that:
Prepared by employing following methods: raw material: quality of alumina content be 80 ~ 90% bauxitic clay powder peace all particle diameter be the micron order SiC of 1.5 ~ 5.0 μm; The two mass ratio: SiC is 5 ~ 10% of bauxitic clay powder;
Preparation process: add water after being mixed in proportion by above-mentioned raw materials powder, ball milling in Ball-stirring mill, mixes; Dried mixed powder precalcining, precalcining temperature 900 ~ 1050 DEG C, is incubated 2 ~ 6 hours; Put into crucible after powder is shaping and bury burning, burying material powder adopts particle size range to be 600-1200 μm of α-SiC, the crucible that molding blank is housed is rapidly heated to 1200 DEG C with the heat-up rate of 350 DEG C/h, then rise to 1400 ~ 1550 DEG C again with the heat-up rate of 200 DEG C/h to sinter, be incubated 1 hour, then naturally cool to room temperature, obtained high-performance aluminum oxide/SiC nanocomposites;
Described high-performance aluminum oxide/SiC nanocomposites has the nanometer silicon carbide of growth in situ, forms SiO
2the particle of clad nano SiC, and a small amount of mullite parcel be at high temperature formed, carborundum grain is of a size of 200 ~ 410nm, and the flexural strength of material is 306 ~ 380MPa, and fracture toughness property is 3.3 ~ 5.2MPam
1/2.
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| CN110709367A (en) * | 2017-06-29 | 2020-01-17 | 住友大阪水泥股份有限公司 | Composite sintered body, electrostatic chuck member, and electrostatic chuck device |
| CN111848136A (en) * | 2019-04-29 | 2020-10-30 | 扬州北方三山工业陶瓷有限公司 | Preparation method of high-toughness and high-hardness alumina-based wear-resistant ceramic |
| CN113502407A (en) * | 2021-07-13 | 2021-10-15 | 湖南金天铝业高科技股份有限公司 | Pretreatment method of silicon carbide particles and preparation method of aluminum matrix composite |
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| CN110709367A (en) * | 2017-06-29 | 2020-01-17 | 住友大阪水泥股份有限公司 | Composite sintered body, electrostatic chuck member, and electrostatic chuck device |
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| CN113502407A (en) * | 2021-07-13 | 2021-10-15 | 湖南金天铝业高科技股份有限公司 | Pretreatment method of silicon carbide particles and preparation method of aluminum matrix composite |
| CN113502407B (en) * | 2021-07-13 | 2022-04-26 | 湖南金天铝业高科技股份有限公司 | Pretreatment method of silicon carbide particles and preparation method of aluminum matrix composite |
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