CN104761246B - A kind of preparation method of high-performance aluminum oxide/SiC nanocomposites - Google Patents
A kind of preparation method of high-performance aluminum oxide/SiC nanocomposites Download PDFInfo
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Abstract
A kind of preparation method of high-performance aluminum oxide/SiC nanocomposites, it is characterised in that：With bauxite powder and micron-sized SiC particulate as primary raw material, through wet mixed, drying, precalcining, carry out burying burning after being then molded, in 1400~1550 DEG C of sintering, insulation 1 hour, then naturally cools to room temperature, and high-performance aluminum oxide/SiC nanocomposites are obtained.High-performance aluminum oxide/the SiC nanocomposites prepared according to above-mentioned preparation method have the nanometer silicon carbide of growth in situ, form SiO2The particle of nano SiC is coated, and a small amount of mullite parcel being formed at high temperature, the size of carborundum grain is 200~410nm, and the bending strength of material is 306~380MPa, and fracture toughness is 3.3~5.2MPam1/2。
Description
Technical field
The present invention relates to a kind of preparation method of high-performance aluminum oxide/SiC nanocomposites, belong to engineering ceramics
The preparing technical field of material.
Background technology
Aluminium oxide ceramics is considered as " steel " in ceramic material, and in global Ceramic Market, its market share is accounted for
More than 75%.80-90 porcelain refers to the aluminium oxide ceramics that quality of alumina content is 80-90%, the product being made up of 80-90 porcelain because
Its wearability, fracture toughness, bending strength and thermal shock resistance etc. are poor, are often only used as low and middle-grade ceramic product materials.For
This has carried out the enhanced research of toughness reinforcing of aluminium oxide ceramics, main to use Zirconium oxide plasticizing and whisker or nano particle toughened and reinforced
Method.Numerous studies confirm by adding silicon carbide whisker or nano particle, not only can by a relatively large margin improve aluminum oxide and make pottery
The mechanical property of porcelain, while its thermal shock resistance can also be improved, expands its application field.But relevant aluminum oxide/carborundum is multiple
The research of phase ceramics (or nano ceramics) is concentrated mainly on high-purity alumina ceramic system.I.e. in high purity aluminium oxide, (aluminum oxide contains
Amount is often more than 99%) middle addition proper amount of nano SiC particulate or SiC whiskers, by hot pressing, normal pressure gas-protecting sintering
Sintered body is obtained, its sintering temperature is higher, generally more than 1650 DEG C.The performance of the composite diphase material is compared compared with pure alumina, is had
Raising by a relatively large margin, but due to high, it is necessary to atmosphere protection, the property/valency of product is protruded than not, so as to limit to agglomerating plant requirement
The exploitation and application of the material product are made.
The domestic patent at present about aluminum oxide/nanometer (whisker) carbide composite ceramic technology of preparing mainly has CN
1821175A, CN 101555142A and CN 101880163A.Chinese patent CN 1821175A describe a kind of silicon carbide whisker
The preparation method of palpus/aluminium oxide composite ceramic powder body, with natural kaolin and charcoal source as raw material, charcoal source is that graphite or carbon black are inorganic
Carbon or macromolecule organic, are filled with a hydrogen for atmospheric pressure as protective gas, at 1450 DEG C after being vacuumized in atmosphere furnace
~1550 DEG C of calcinings, obtain silicon carbide whisker/aluminium oxide nano level, submicron order composite powder.But do not introduce associated ceramic
Technology of preparing.Patent CN 101555142A describe a kind of preparation method of nanosized silicon carbide toughened aluminum oxide bulletproof ceramic, adopt
With high-purity alumina powder, kaolin and 0.5~1.0% burning talcum that mass fraction is 0.8~1.3%, then additional matter are added
Than being 3~8%, silicon carbide powder of the granularity at 10~30 nanometers, using note solidification forming method, burns amount at 1650~1700 DEG C
Knot, can obtain nanometer silicon carbide/aluminum oxide composite ceramics；Nanometer silicon carbide is to introduce alumina substrate by outer add mode
In, therefore be difficult to be uniformly dispersed.External Patents include：Korean Patent KR9710308, world patent WO0078690, Japan
Patent JP8208318, European patent EP 0419150, United States Patent (USP) 4,657,877,4,746,635,4,749,667 and 5,455,
212.It is 0.1-30vol.%SiC particles that Japan Patent JP8208318 is described and volume fraction is added in aluminum oxide, by gas
Atmosphere sintering prepares Al2O3The method of/SiC complex phase ceramics.Its feature：By Al2O3/ SiC composite powders are pressed into base substrate, in base substrate
Surrounding places the Al that average grain diameter is 3.0 μm2O3Powder and/or average grain diameter are 5.0 μm of SiO2With C powder, base substrate in Ar or
N2Pass through under normal pressure or higher pressure under protective atmosphere, in high temperature sintering.European EP0419150 is with oxide or non-oxidized substance
It is matrix, is separately added into volume fraction for 3~50%, particle diameter is 5~20 μm of SiC particulate, or sheet (tabular) SiC, and it is put down
Equal particle diameter is 5~50 μm, 1/3 of thickness less than or equal to particle diameter.Composite powder mix grinding after 120 DEG C of dryings 24 hours, by powder
Sieving, shaping, it is normal pressure-sintered in 1400~1900 DEG C, Ar atmosphere.The fracture toughness of material compared with host oxide ceramics by compared with
Increase substantially.European patent 0310342A2 is the Al more than 99% with purity2O3It is matrix, is separately added into diameter less than 0.5 μ
The SiC particulate or length of m are 1.0~5 μm, SiC whisker of the length less than 3.Formed body is quiet through heat etc. at 1400~1800 DEG C
Pressure, hot pressing or normal pressure atmosphere sintering, can obtain dense sintering body.United States Patent (USP) 4,657,877,4,746,635,4,749,667
With aluminum oxide or mullite as matrix, zirconium oxide and SiC whiskers or particle are added, prepared using pressure or atmosphere sintering
Al2O3/ZrO2/ SiC composite diphase materials.Above-mentioned preparation method adds SiC with high purity aluminium oxide as matrix by mechanical mixing
Whisker or nano particle, formed body are obtained using normal pressure, atmosphere protection or pressure (hot pressing, high temperature insostatic pressing (HIP) and air pressure etc.) sintering
Dense sintering body.
The content of the invention
It is an object of the invention to provide a kind of preparation method of high-performance aluminum oxide/SiC nanocomposites, with
Complex phase ceramic prepared by the method is dispersed with nano SiC granule in alumina substrate situ, and with the presence of a small amount of mullite,
The method preparation process is simple, obtained complex phase ceramic has cost performance higher.
To reach above-mentioned purpose, the present invention is realized by the following technical scheme：A kind of high-performance aluminum oxide/receive
The preparation method of rice carborundum composite-phase ceramic, it is characterised in that：With bauxite powder and micron-sized SiC particulate as main former
Material, through wet mixed, drying, precalcining, carries out burying burning after being then molded, and in 1400~1550 DEG C of sintering, is incubated 1 hour, and
After naturally cool to room temperature, high-performance aluminum oxide/SiC nanocomposites are obtained.
Raw material：Quality of alumina content is that 80~90% bauxite powder peace particle diameter is 1.5~5.0 μm of micron
Level SiC；The two mass ratio：SiC is the 5~10% of bauxite powder；
Preparation process：Added water after above-mentioned raw materials powder is mixed in proportion, the ball milling in Ball-stirring mill is well mixed；Dry
Mixed powder precalcining afterwards, 900~1050 DEG C of precalcining temperature is incubated 2~6 hours；It is put into crucible after powder is molded
Burning is buried, it is 600-1200 μm of α-SiC to bury feed powder body and use particle size range, and the crucible equipped with molding blank is with the intensification of 350 DEG C/h
Speed is rapidly heated to 1200 DEG C, and then rising to 1400~1550 DEG C again with the programming rate of 200 DEG C/h is sintered, insulation 1
Hour, room temperature is then naturally cooled to, high-performance aluminum oxide/SiC nanocomposites are obtained.
To be well mixed raw material in preparation process, can be added when material powder mixes in proportion and account for bauxite powder
Mass ratio is 0.08% dispersant methacrylic acid amino.
High-performance aluminum oxide/the SiC nanocomposites prepared according to above-mentioned preparation method have receiving for growth in situ
Rice carborundum, forms SiO2The particle of nano SiC is coated, and a small amount of mullite parcel being formed at high temperature, silicon carbide whisker
The size of grain is 200~410nm, and the bending strength of material is 306~380MPa, and fracture toughness is 3.3~5.2MPam1/2。
The advantage of the invention is that using A12O3Mass content is that the bauxite and micron-sized SiC powder of 80-90% are
Raw material, then carries out pre-burning to mixed composite powder, forms SiO2The particle of nano SiC is coated, is formed at high temperature
Mullite parcel.Coarse granule buried powder α-SiC and nano SiC are aoxidized because a small amount of air enters crucible in sintering process, on the one hand
Nano SiC granule is set further to refine, while forming reducing atmosphere in crucible, whole sintering process is protected without additional atmosphere
Shield.According to said method obtained aluminum oxide/SiC nanocomposites, with intensity and toughness is higher, low cost the characteristics of.
Brief description of the drawings
Fig. 1 is the present invention in 1500 DEG C of sintering, insulation 1 hour, the XRD of obtained aluminum oxide/nano silicon carbide ceramic
Spectrum.
Fig. 2 is the present invention in 1500 DEG C of sintering, insulation 1 hour, the Electronic Speculum photograph of obtained aluminum oxide/nano silicon carbide ceramic
Piece.
Specific embodiment
With bauxite that quality of alumina content is 80~90% as primary raw material, addition mass content is 5~10%, is put down
Equal particle diameter is 1.5~5.0 μm of micron order SiC particulate；By powder wet mixed, drying, in 900~1050 DEG C of precalcinings 2~6
Hour, by powder shaping, burning is buried, the particle size range of feed powder body α-SiC is buried for 600-1200 μm, will be equipped with the sealed crucible of base substrate
It is rapidly heated to 1200 DEG C, programming rate is advisable more than 350 DEG C/h, continues to be warmed up to 1400~1550 DEG C, programming rate is
200 DEG C/h, it is incubated 1 hour.The enhanced Toughened Alumina Ceramics of nanometer silicon carbide with growth in situ can be obtained.Material
Bending strength be 306~380MPa, fracture toughness be 3.3~5.2MPam1/2.α-SiC are claimed to bury material matter after burning 5~10 stoves
Amount, when material weightening is buried more than 10%, need to change or replace part α-SiC and bury material, it is ensured that the uniformity of product quality.
Embodiment 1：
L kilograms of the bauxite that mass content is 80% accurately is weighed, it is 5% that mass ratio is added in bauxite powder, is put down
Equal particle diameter is 1.5 μm of 50 grams of SiC powder.1700ml distilled water is added, while addition accounts for powder quality than being 0.08%
Methacrylic acid amine dispersant.By compound in Ball-stirring mill ball milling 4 hours, in 1050 DEG C of precalcinings 4 hours after drying, then
Granulation, shaping.Molding blank is put into crucible, is buried with α-SiC powder that particle size range is 600-1200 μm and is covered base substrate, covered tightly
Crucible cover；It is rapidly heated to 1200 DEG C with the speed of 350 DEG C/h, continues to be heated up 1500 DEG C with the speed of 200 DEG C/h, insulation 1 is small
When.Room temperature is then naturally cooled to, has a small amount of mullite in obtained aluminum oxide/SiC nanocomposites (such as Fig. 1 institutes
Show), the size of carborundum grain is about 200nm (as shown in the figure), and the average bending strength of material is 310 ± 26MPa, average disconnected
Toughness is split for 3.3 ± 0.48MPam1/2。
Embodiment 2：
L kilograms of the bauxite that mass content is 80% accurately is weighed, it is 8% that mass ratio is added in bauxite powder, is put down
Equal particle diameter is 2.5 μm of 80 grams of SiC powder.1700ml distilled water is added, while addition accounts for powder quality than being 0.08%
Methacrylic acid amine dispersant.By compound in Ball-stirring mill ball milling 4 hours, in 1050 DEG C of precalcinings 6 hours after drying, then
Granulation, shaping.Molding blank is put into crucible, is buried with α-SiC powder that particle size range is 600-1200 μm and is covered base substrate, covered tightly
Crucible cover；It is rapidly heated to 1200 DEG C with the speed of 350 DEG C/h, continues to be heated up 1530 DEG C with the speed of 200 DEG C/h, insulation 1 is small
When.Room temperature is then naturally cooled to, has a small amount of mullite, silicon carbide whisker in obtained aluminum oxide/SiC nanocomposites
The size of grain is about 220nm, and the average bending strength of material is 360 ± 33MPa, and average fracture toughness is 5.2 ± 0.53MPa
m1/2。
Embodiment 3：
L kilograms of the bauxite that mass content is 90% accurately is weighed, it is 10% that mass ratio is added in bauxite powder, is put down
Equal particle diameter is 5.0 μm of 100 grams of SiC powder.1700ml distilled water is added, while addition accounts for powder quality than being 0.08%
Methacrylic acid amine dispersant.By compound in Ball-stirring mill ball milling 4 hours, in 900 DEG C of precalcinings 2 hours after drying, then
Granulation, shaping.Molding blank is put into crucible, is buried with α-SiC powder that particle size range is 600-1200 μm and is covered base substrate, covered tightly
Crucible cover；It is rapidly heated to 1200 DEG C with the speed of 350 DEG C/h, continues to be heated up 1550 DEG C with the speed of 200 DEG C/h, insulation 1 is small
When.Room temperature is then naturally cooled to, has a small amount of mullite, silicon carbide whisker in obtained aluminum oxide/SiC nanocomposites
The size of grain is about 410nm, and the average bending strength of material is 420 ± 23MPa, and average fracture toughness is 3.8 ± 0.50MPa
m1/2。
Embodiment 4：
L kilograms of the bauxite that mass content is 90% accurately is weighed, it is 10% that mass ratio is added in bauxite powder, is put down
Equal particle diameter is 2.5 μm of 100 grams of SiC powder.1700ml distilled water is added, while addition accounts for powder quality than being 0.08%
Methacrylic acid amine dispersant.By compound in Ball-stirring mill ball milling 4 hours, in 1050 DEG C of precalcinings 6 hours after drying, then
Granulation, shaping.Molding blank is put into crucible, is buried with α-SiC powder that particle size range is 600-1200 μm and is covered base substrate, covered tightly
Crucible cover；It is rapidly heated to 1200 DEG C with the speed of 350 DEG C/h, continues to be heated up 1530 DEG C with the speed of 200 DEG C/h, insulation 1 is small
When.Room temperature is then naturally cooled to, has a small amount of mullite, silicon carbide whisker in obtained aluminum oxide/SiC nanocomposites
The size of grain is about 240nm, and the average bending strength of material is 440 ± 26MPa, and average fracture toughness is 4.6 ± 0.49MPa
m1/2。
Claims (7)
1. a kind of preparation method of high-performance aluminum oxide/SiC nanocomposites, it is characterised in that：
Raw material：Quality of alumina content is that 80~90% bauxite powder peace particle diameter is 1.5~5.0 μm of micron order
SiC；The two mass ratio：SiC is the 5~10% of bauxite powder；
Preparation process：Added water after above-mentioned raw materials powder is mixed in proportion, the ball milling in Ball-stirring mill is well mixed；It is dried
Mixed powder precalcining, 900~1050 DEG C of precalcining temperature is incubated 2~6 hours；It is put into after powder is molded in crucible and buries burning,
It is 600-1200 μm of α-SiC to bury feed powder body and use particle size range, and the crucible equipped with molding blank is fast with the programming rate of 350 DEG C/h
Speed is warming up to 1200 DEG C, and then rising to 1400~1550 DEG C again with the programming rate of 200 DEG C/h is sintered, and is incubated 1 hour, and
After naturally cool to room temperature, high-performance aluminum oxide/SiC nanocomposites are obtained；
Described high-performance aluminum oxide/SiC nanocomposites have the nanometer silicon carbide of growth in situ, form SiO2Cladding
The particle of nano SiC, and a small amount of mullite parcel being formed at high temperature, the size of carborundum grain is 200~410nm,
The bending strength of material is 306~380MPa, and fracture toughness is 3.3~5.2MPam1/2。
2. the preparation method of high-performance aluminum oxide/SiC nanocomposites according to claim 1, its feature exists
In：Added when material powder mixes in proportion and account for the dispersant methacrylic acid amino that bauxite powder body mass ratio is 0.08%.
3. the preparation method of high-performance aluminum oxide/SiC nanocomposites according to claim 1 and 2, its feature
It is：The raw material：Quality of alumina content is that 80% bauxite powder peace particle diameter is 1.5 μm of micron order SiC；Two
Person's mass ratio：SiC is the 5% of bauxite powder；
Precalcining temperature is 1050 DEG C, is incubated 4 hours；Sintering temperature is 1500 DEG C, is incubated 1 hour.
4. the preparation method of high-performance aluminum oxide/SiC nanocomposites according to claim 1 and 2, its feature
It is：The raw material：Quality of alumina content is that 80% bauxite powder peace particle diameter is 2.5 μm of micron order SiC；Two
Person's mass ratio：SiC is the 8% of bauxite powder；
Precalcining temperature is 1050 DEG C, is incubated 6 hours；Sintering temperature is 1530 DEG C, is incubated 1 hour.
5. the preparation method of high-performance aluminum oxide/SiC nanocomposites according to claim 1 and 2, its feature
It is：The raw material：Quality of alumina content is that 90% bauxite powder peace particle diameter is 5.0 μm of micron order SiC；Two
Person's mass ratio：SiC is the 10% of bauxite powder；
Precalcining temperature is 900 DEG C, is incubated 2 hours；Sintering temperature is 1550 DEG C, is incubated 1 hour.
6. the preparation method of high-performance aluminum oxide/SiC nanocomposites according to claim 1 and 2, its feature
It is：The raw material：Quality of alumina content is that 90% bauxite powder peace particle diameter is 2.5 μm of micron order SiC；Two
Person's mass ratio：SiC is the 10% of bauxite powder；
Precalcining temperature is 1050 DEG C, is incubated 6 hours；Sintering temperature is 1530 DEG C, is incubated 1 hour.
7. high-performance aluminum oxide/SiC nanocomposites that the preparation method described in claim 1 is prepared, its feature exists
In：
Prepared using following methods：Raw material：Quality of alumina content be 80~90% bauxite powder peace particle diameter be 1.5
~5.0 μm of micron order SiC；The two mass ratio：SiC is the 5~10% of bauxite powder；
Preparation process：Added water after above-mentioned raw materials powder is mixed in proportion, the ball milling in Ball-stirring mill is well mixed；It is dried
Mixed powder precalcining, 900~1050 DEG C of precalcining temperature is incubated 2~6 hours；It is put into after powder is molded in crucible and buries burning,
It is 600-1200 μm of α-SiC to bury feed powder body and use particle size range, and the crucible equipped with molding blank is fast with the programming rate of 350 DEG C/h
Speed is warming up to 1200 DEG C, and then rising to 1400~1550 DEG C again with the programming rate of 200 DEG C/h is sintered, and is incubated 1 hour, and
After naturally cool to room temperature, high-performance aluminum oxide/SiC nanocomposites are obtained；
Described high-performance aluminum oxide/SiC nanocomposites have the nanometer silicon carbide of growth in situ, form SiO2Cladding
The particle of nano SiC, and a small amount of mullite parcel being formed at high temperature, the size of carborundum grain is 200~410nm,
The bending strength of material is 306~380MPa, and fracture toughness is 3.3~5.2MPam1/2。
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| 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 |
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