CN109400210A - A kind of Ti3SiC2-Al2O3- SiC-Al composite material and preparation method - Google Patents
A kind of Ti3SiC2-Al2O3- SiC-Al composite material and preparation method Download PDFInfo
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/51—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal
- C04B41/515—Other specific metals
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Abstract
The present invention is a kind of Ti3SiC2‑Al2O3- SiC-Al composite material and preparation method.The composite material outer layer is Ti3SiC2/Al2O3/ SiC conversion zone, inside are SiC/Al composite material；The reaction layer thickness is 100~400 μm.In the composite material outer layer, percent by volume Ti3SiC2: 60~80%, Al2O3: 15%~40%, SiC:5%~20%.This method passes through reaction infiltration method first and obtains Ti3SiC2/ SiC/Al composite material, then the technique handled by a step in-situ oxidation, by controlling oxidation technology parameter (oxidizing temperature and oxidization time), by outer surface Ti3SiC2Al is generated with the Al in-situ oxidation in the gap SiC2O3, surface layer is made to become Ti3SiC2/Al2O3/SiC.Composite material prepared by the present invention has obdurability and good friction and wear behavior.
Description
Technical field
The invention belongs to technology field of ceramic matrix composite material, and in particular to a kind of Ti3SiC2-Al2O3- SiC-Al is compound
Material and preparation method thereof.
Background technique
SiC ceramic because of high-strength light, good heat conductivity, the coefficient of expansion is low, hardness is high, hot property and good mechanical performance etc.
Feature and be widely used in efficient high-speed cutting tool, space technology, engine critical component, seal member, new energy development
Etc. novel industry.However, SiC ceramic material itself has higher coefficient of friction and wear rate as other ceramic materials, it
Belong to fragile material, fracture toughness is low, and in sliding friction, the critical load of ceramic surface fracture is more much lower than under static state.This
Outside, in friction process, friction surface generates the gap stress raisers continuously changed, and then can generate micro-crack.Due to
The blocking of crystal boundary in SiC ceramic, forces micro-crack that can not further expand, and can only assemble and lead to microcell brittle fracture, so
Its application is restricted.Al2O3Ceramics are used as a kind of structural ceramics, and performance has that hardness is high, light-weight, wearability is fabulous etc. one
The advantage of series.Ti3SiC2Be it is a kind of have both ceramics high-melting-point, high chemical stability, it is corrosion-resistant and metal it is thermally conductive, conductive,
The ternary layered ceramic of the advantages that easy processing, self-lubricating.Especially Ti3SiC2Possessed self-lubricating property can play good
Friction reducing effect, reduce coefficient of friction.
With to self-lubricating material Ti3SiC2With wear-resistant material Al2O3Concern, to Al2O3/Ti3SiC2Composite material and list
Pure Ti3SiC2Powder, the preparation research of block are relatively more, and to Ti3SiC2/ SiC and Al2O3/Ti3SiC2/ SiC both answers
The research of condensation material is relatively fewer.So far, Ti3SiC2The preparation method of/SiC ceramic matrix composite material is concentrated mainly on Ti-C-Si body
The powder hot pressed sintering and liquid silicon of system infiltrate two methods.Yin Hongfeng et al. (Yin Hongfeng, Fan Qiang, Ren Yun, etc..SiC content pair
Ti3SiC2The influence [J] of/SiC ceramic matrix composite material performance.Aeronautical material journal, 2008,6 (28) 78-81.) use TiH2、TiC、C
Powder is prepared for Ti by hot pressed sintering3SiC2/ SiC ceramic matrix composite material is not readily available fine and close Ceramic Composite due to powder sintered
Material, therefore performance improvement and little.Tsinghua University Zan blueness peak et al. (Zan Qingfeng, Wang Changan, Huang Yong, Li Cuiwei, Zhao Shike,
Al2O3/Ti3SiC2The preparation of laminar composite and performance [J].Material engineering, 2003,09,15-21.) use two methods
Prepare Al2O3/Ti3SiC2Laminar composite, first is that original position-pressure sintering at 1600 DEG C, i.e. Ti3SiC2It is the system in stratified material
It is synthesized simultaneously during standby；First is that the method for fractional steps, i.e. preparation process are carried out in two steps, Ti is prepared first3SiC2High-purity powder,
It is sintered again using pressure sintering and prepares stratified material.The Al of two methods preparation2O3/Ti3SiC2The micro- knot of laminar composite
There are notable differences for structure, this also results in the difference in mechanical property, and the strength of materials of original position-pressure sintering preparation is higher and is broken
Function is lower, and the intensity of method of fractional steps preparation is lower and work to break is higher.And high-temperature and high-pressure conditions are needed, preparation condition is harsh, because
The meaning of this both methods is not very big.
Application No. is 201310314549.3 Chinese patents to disclose a kind of Ti3Si(Al)C2Modified SiC based composites
Preparation method, this method first pre-processes the multisteps such as SiC precast body, then precast body is carried out infiltration in vacuum and pressure infiltration,
It is taped against precast body surface with Al-Si alloy again, under vacuum conditions high-temperature calcination, to prepare Ti3Si(Al)C2Modified SiC base
Composite material, reduces the damage to SiC fiber and residual thermal stress, composite material strength obtained be improved significantly.But
Its technique preparation condition is harsh, needs to complete under vacuum high-temperature, higher cost is not suitable for large-scale industrial production.
Application No. is a kind of 201711365973.5 Chinese patent " Ti3SiC2The preparation side of/SiC/Al composite material
Ti has been made in method "3SiC2/ SiC/Al, but have residual aluminum at surface gap, after aluminium alloy infiltration SiC matrix, generation
After composite material surface polishing treatment, specimen surface Ti3SiC2With SiC gap location there are still a certain amount of aluminium, Al belongs to soft phase,
Hardness is low, and properties of antifriction and wear resistance is poor, in spite of lubrication phase Ti3SiC2It generates, but since surface layer integral hardness is lower, it is average to tie up
Family name's hardness about 580Hv, composite material surface wearability is very poor, seriously affects its wear-resisting property.
Summary of the invention
It is an object of the present invention in view of the deficiencies of the prior art, provide a kind of Ti3SiC2-Al2O3- SiC-Al self-lubricating is multiple
The preparation method of condensation material.This method passes through infiltration method first and obtains Ti3SiC2/ SiC/Al composite material, then it is in situ by a step
The technique of oxidation processes, by controlling oxidation technology parameter (oxidizing temperature and oxidization time), by outer surface Ti3SiC2Between SiC
Al in-situ oxidation in gap generates Al2O3, surface layer is made to become Ti3SiC2/Al2O3/SiC.Composite material prepared by the present invention, has
Obdurability and good friction and wear behavior.
The present invention solves technical solution used by the technical problem:
A kind of Ti3SiC2-Al2O3- SiC-Al composite material, the composite material outer layer are Ti3SiC2/Al2O3/ SiC reaction
Layer, inside are SiC/Al composite material；The reaction layer thickness is 100~400 μm.
In the composite material outer layer, percent by volume Ti3SiC2: 60~80%, Al2O3: 15%~40%, SiC:
5%~20%
The Ti3SiC2-Al2O3The preparation method of-SiC-Al composite material, this method comprises the following steps:
(1) preparation of aluminium alloy acieral: each element mass percent in aluminium alloy are as follows: Al, 45-90wt.%；
Ti, 3-25wt.%；Mg, 1-6wt.%；Si, 5-30wt.%；
Corresponding raw material is weighed according to the mass percent of above-mentioned each element, fine aluminium ingot is put into NaOH solution and submerges 1-3
Hour, after surface scale removal completely, it is placed in graphite crucible, titanium ingot, magnesium powder, silico briquette is then placed in graphite together
It in crucible, is warming up to 700-1100 DEG C and is melted, stir lower heat preservation 0.5-4h, the acieral that molten condition can be obtained is molten
Liquid；
(2) pretreatment of SiC ceramic: SiC ceramic is cut into required corresponding size, is dried after polishing, ultrasonic cleaning；
(3) it reacts infiltration process: the silicon carbide ceramics handled well in step 2) is immersed into prepared in step (1) melt
Melt in the acieral melt of state, infiltration 0.5-9h, then takes out at 700-1000 DEG C, is cooled to room temperature, and obtains after polishing
Ti3SiC2/ SiC/Al composite material；
(4) oxidation processing technique: by Ti polished in step (3)3SiC2/ SiC/Al composite material is put into porcelain boat, so
After be put into batch-type furnace progress in-situ oxidation processing, 800-1100 DEG C of oxidizing temperature, oxidization time 4-14h then takes out, cooling
To room temperature, Ti is obtained3SiC2-Al2O3- SiC-Al composite material.
The concentration of NaOH solution in the step (1) is 0.3mol/L~0.6mol/L.
The present invention protects a kind of Ti prepared by the above method3SiC2-Al2O3- SiC-Al composite material, the composite wood
Material outer layer is Ti3SiC2/Al2O3/ SiC conversion zone, inside are densification SiC/Al composite material.
The method of the present invention be further characterized by by adjust aluminium alloy in Ti content, infiltrating temperature, soaking time,
Oxidizing temperature and oxidization time can effectively control Ti3SiC2/Al2O3In the in-situ preparation process of surface of SiC；By adjusting aluminium
Ti in alloy, Si, Mg content can effectively control the fusing point and alloy flowability and aluminium alloy and SiC ceramic of aluminium alloy
Wetability.
SiC ceramic used in the method for the present invention, aluminium, titanium, silicon, magnesium etc. can be commercially available.The raw material of aluminium is pure
Aluminium ingot, the raw material of titanium are pure titanium ingot, titanium valve or stud, and the raw material of silicon is silico briquette, and the raw material of magnesium is magnesium powder.
Substantive distinguishing features of the invention are as follows:
The present invention passes through the technique that a step in-situ oxidation is handled, by outer surface Ti3SiC2With the Al situ oxygen in the gap SiC
Metaplasia is at Al2O3, surface layer is made to become Ti3SiC2/Al2O3The conversion zone of/SiC is found, temperature mistake by numerous studies and experiment
Low, the oxidation reaction of aluminium is insufficient, and anti-friction wear-resistant effect is poor, and temperature is excessively high, easily by newly-generated lubrication phase Ti3SiC2With SiC base
Body Oxidative demage is prepared for antifriction so optimal infiltration process parameter and in-situ oxidation technological parameter have been arrived in present invention exploration
The best Ti of abrasion resistant effect3SiC2-Al2O3- SiC-Al composite material.
The beneficial effects of the present invention are:
What forefathers proposed contains Ti3SiC2And Al2O3SiC based self lubricated composite material remain in powder hot pressed sintering and
On ceramics/ceramic composite, powder associativity is poor, and the raising of obdurability is limited, and hardness is lower, and wearability raising is smaller, and
And embodiment is more complex, the period is long, and energy consumption is high, higher cost.Preparation method of the present invention by adjust auxiliary element Ti, Si,
It is low that Mg content prepares fusing point, good fluidity, the Al based alloy good with SiC ceramic wetability.After the completion of infiltration, sample is polished
Processing, tentatively obtains Ti3SiC2/ SiC/Al composite material, then the heat treatment process of in-situ oxidation is used, it will be existing for gap location
Aluminium carries out in-situ oxidation processing, by adjusting oxidizing temperature and oxidization time, tests repeatedly, exploring can be only gap location
Aluminium is fully oxidized, and newly-generated Ti3SiC2Lubricate the optimum treatment process parameter of mutually not oxidized decomposition, the Parameter Conditions
Under, obtained composite material extexine is by Ti3SiC2-Al2O3- SiC composition, it is internal to be made of fine and close SiC/Al.The invention system
Standby composite material has obdurability and good friction and wear behavior.By embodiment 6 it is found that by control the infiltration time and
Infiltrating temperature can make the complete osmotic ceramic of alloy, and by control oxidizing temperature and oxidization time, can control reaction layer thickness,
Conversion zone maximum gauge is 400 μm, and the fracture toughness of composite material that the preparation method obtains is 5.9MPam1/2, compared to
Original SiC ceramics (2.2MPam1/2) improve 3.7MPam1/2, fracture toughness maximum improves nearly 168%.Under equal conditions into
The test of row friction and wear behavior, the average friction coefficient for measuring material is 0.30, and average wear rate is 3.2 × 10-3mm3/ min,
Compared to original SiC ceramic (coefficient of friction 0.55, wear rate 5 × 10-3mm3/ min), coefficient of friction reduces 0.25, close to drop
Low 45%, the wear rate relative to original SiC ceramics reduces 1.8 × 10-3mm3/ min, close to reduce 36%, the oxidation
Process method step is simple, at low cost, can effectively improve the obdurability and properties of antifriction and wear resistance of SiC ceramic, is suitble to push away on a large scale
Extensively.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples.
Fig. 1 is Ti of the present invention3SiC2-Al2O3Gained Ti in the preparation method embodiment 6 of-SiC-Al composite material3SiC2-
Al2O3- SiC-Al composite material surface SEM figure.
Fig. 2 is Ti of the present invention3SiC2-Al2O3Gained Ti in the preparation method embodiment 6 of-SiC-Al composite material3SiC2-
Al2O3- SiC-Al composite material surface XRD diagram.
Fig. 3 is Ti of the present invention3SiC2-Al2O3Gained Ti in the preparation method embodiment 6 of-SiC-Al composite material3SiC2-
Al2O3- SiC-Al composite material surface EDS figure.
Fig. 4 is Ti of the present invention3SiC2-Al2O3Gained Ti in the preparation method embodiment 6 of-SiC-Al composite material3SiC2-
Al2O3SEM schemes at-SiC-Al composite material center.
Fig. 5 is Ti of the present invention3SiC2-Al2O3Gained Ti in the preparation method embodiment 6 of-SiC-Al composite material3SiC2-
Al2O3EDS schemes at-SiC-Al composite material center.
Specific embodiment
It is further discussed below the present invention below with reference to examples and drawings, but is not protected in this, as to the claim of this application
Protect the restriction of range.
Ti of the present invention3SiC2-Al2O3The preparation method of-SiC-Al composite material, this method comprises the following steps:
1) preparation of Al based alloy: each element mass percent of Al based alloy are as follows: Al, 45-90wt.%；Ti, 3-
25wt.%；Mg, 1-6wt.%；Si, 5-30wt.%；
Corresponding raw material is weighed by above-mentioned each element mass percent, fine aluminium ingot is put into the NaOH solution of 0.5mol/L,
After 1-3 hours, after surface scale removal completely, it is placed in graphite crucible, is then placed in titanium ingot, magnesium powder, silico briquette together
In graphite crucible, then graphite crucible is placed in the energy saving chamber type electric resistance furnace of model SX-G04132 and is warming up to 700-1100
DEG C, it is melted, and keep the temperature 0.5-4h, is stirred to being completely dissolved to get the Al based alloy liquid of molten condition is arrived；
2) SiC ceramic raw material the processing of SiC ceramic: is cut into required size with diamond custting machine；Respectively with 800 mesh,
1500 mesh, 3000 mesh diamond disk polish surface of SiC, be polishing to that surface is smooth and non-oxidation layer, be placed in third
Ultrasonic cleaning is clean in ketone and dehydrated alcohol；After circulation 4 times, finally it is dried for standby；
3) SiC ceramic handled well in step 2) Infiltration Technics: is immersed in the molten condition prepared in step 1)
It in Al based alloy liquid, is put into batch-type furnace and keeps the temperature, infiltrating temperature is 700-1000 DEG C, and the infiltration time is 0.5-9h, takes out sample
It is cooled to room temperature, then surface is processed by shot blasting, tentatively obtain Ti3SiC2/ SiC/Al composite material.
4) in-situ oxidation treatment process: by Ti polished in step 3)3SiC2/ SiC/Al composite material is put into ceramic boat
In, it is then placed in progress in-situ oxidation processing in batch-type furnace, 800-1100 DEG C of oxidizing temperature, oxidization time 4-14h, oxidation is completed
Afterwards, it takes out sample to be cooled to room temperature, Ti can be obtained3SiC2-Al2O3- SiC-Al composite material.
The present invention protects a kind of Ti prepared by the above method3SiC2-Al2O3- SiC-Al composite material, the composite wood
Expect that outer layer is containing Ti3SiC2/Al2O3The conversion zone of/SiC, inside are SiC/Al composite material.
Preparation method of the present invention be further characterized by by adjust aluminium alloy in Ti, Al surplus, infiltrating temperature and when
Between and in-situ oxidation temperature and time, Ti can be effectively controlled3SiC2And Al2O3Process is formed in situ on the surface layer SiC, at this
Under part, the outer layer Ti of composite material3SiC2And Al2O3Conversion zone dense uniform, fracture toughness and properties of antifriction and wear resistance are preferable.It is logical
Overregulate the wetting of the fusing point, mobility and Al based alloy and SiC of the controllable Al based alloy of content of Si, Mg in Al based alloy
Property.
SiC ceramic used (uses the density of the magnificent fine ceramics Co., Ltd production in Shandong Province for 3.02g/ in the present invention
cm3, SiC ceramic that voidage is 1.48%), Al, Ti, Si, Mg etc. it is commercially available, the raw material of metallic aluminium selects aluminium ingot,
The raw material of silicon is silico briquette, and the raw material of Mg is pure magnesium powder, and the raw material of titanium is titanium valve or titanium ingot.
Embodiment 1
The present embodiment Ti3SiC2-Al2O3The preparation method following steps of-SiC-Al composite material:
1) preparation of acieral: each element mass percentage composition of acieral are as follows: Al, 78wt%；Ti,
10wt%；Mg, 2wt%；Si, 10wt%；
Corresponding raw material is weighed by above-mentioned each element mass percent, each raw material is respectively Al ingot (purity 99.9%), Ti ingot
Fine aluminium ingot, is put into the NaOH solution of 0.5mol/L by (purity 99.9%), Mg powder (purity 99.9%), Si block (purity 99.5%)
In, after 2 hours, after surface scale removal completely, 156gAl ingot is taken to be placed in graphite crucible, then by 20gTi, 20g Si,
4gMg is placed in graphite crucible together, and graphite crucible is placed in the energy saving chamber type electric resistance furnace of model SX-G04132, is warming up to
800 DEG C, heating rate is 20 DEG C/min, keeps the temperature 45min at such a temperature, and stirring arrives molten condition to being completely dissolved
Al based alloy liquid.
2) processing of SiC ceramic: SiC ceramic raw material is cut out with diamond custting machine having a size of 40mm × 5mm × 5mm
(being used for fracture toughness test) and 25mm × 25mm × 5mm (being used for friction and wear test) testing bar is several；Respectively with 800 mesh,
The diamond disk of 1500 mesh polishes to surface of SiC, is polishing to that surface is smooth and non-oxidation layer, is placed in acetone and anhydrous
Ultrasonic cleaning is clean in ethyl alcohol；After circulation 4 times, finally it is dried for standby；
3) SiC ceramic handled well in step 2) Infiltration Technics: is immersed in the molten condition prepared in step 1)
In Al based alloy liquid, infiltration is carried out in the energy saving chamber type electric resistance furnace of model SX-G04132, infiltrating temperature is 900 DEG C, infiltration
Time is 4h, after the completion of infiltration, takes out sample and is cooled to room temperature, after being processed by shot blasting to surface, tentatively obtain Ti3SiC2/
SiC/Al composite material.
4) in-situ oxidation treatment process: the Ti that will tentatively be obtained in step 3)3SiC2/ SiC/Al composite material is put into ceramics
In boat, it is then placed in progress in-situ oxidation processing in batch-type furnace, 950 DEG C of oxidizing temperature, oxidization time 8h after the completion of oxidation, takes
Sample is cooled to room temperature out, and Ti can be obtained3SiC2-Al2O3- SiC-Al composite material.
To obtained Ti3SiC2-Al2O3- SiC-Al composite material carries out fracture toughness test and friction and wear test, tool
Body process is:
Take Ti obtained3SiC2-Al2O35 of-SiC-Al composite material are having a size of the parallel examination of 40mm × 5mm × 5mm
Sample is first polished off the aluminium alloy of surface adhesion with corundum wheel, successively with 150 mesh, 400 mesh, 1500 mesh sand paper by sample table
Face polishes flat, dehydrated alcohol ultrasonic cleaning 4min, recycles 4 times, then 5 sample diamond custting machines are chosen in drying
In the prefabricated wide 0.2mm in middle position, the precrack that depth is 2mm carries out fracture toughness test, the average fracture of sample
Toughness is 5.1MPam1/2, compared to original SiC ceramics (2.2MPam1/2) improve 2.9MPam1/2；Select again 5 having a size of
25mm × 25mm × 5mm sample carries out friction and wear behavior test to sample with SFT-2M pin disk-type friction abrasion tester, uses
The Si of diameter 4mm3N4Ceramic Balls do friction pair, and 25 DEG C of room temperature, revolving speed 200r/min, load 5N, wearing- in period 20min rub
Wiping radius of turn is 3mm.Under this condition, the average friction coefficient for measuring material is 0.4, average wear rate is 4 × 10-3mm3/
Min, compared to original SiC ceramic (coefficient of friction 0.55, wear rate 5 × 10-3mm3/ min), coefficient of friction reduces 0.15, mill
Loss rate reduces 1 × 10-3mm3/min.Original SiC ceramics herein refer to the SiC ceramic raw material in step 2.
The preparation method of the present embodiment can obtain Ti3SiC2-Al2O3- SiC-Al composite material, and be in the infiltration time
Can Al be made to completely penetrate in SiC ceramic when 4h, and Ti is relatively compact in the aggregation of the surface layer SiC, reaction generation
Ti3SiC2Layer, in-situ oxidation time 8h are oxidized most of Al in gap, form relatively compact Ti on surface layer3SiC2-
Al2O3SiC layer.
Embodiment 2
The present embodiment Ti3SiC2The specific steps are the same as those in embodiment 1 for the preparation method of/SiC/Al composite material, and difference exists
In each element mass percentage composition of acieral are as follows: Al, 83wt%；Ti, 5wt%；Mg, 2wt%；Si, 10wt%.
Analysis test is carried out to composite material made from the present embodiment according to the test and analytic process of embodiment 1, specifically
The result is that: pass through fracture toughness test, the average fracture toughness of composite material made from the present embodiment is 4.3MPam1/2, compare
In original SiC ceramics (2.2MPam1/2) improve 2.1MPam1/2；Friction and wear behavior test is carried out under equal conditions, measures material
The average friction coefficient of material is 0.45, and average wear rate is 4.2 × 10-3mm3/ min, compared to the ceramic (coefficient of friction of original SiC
0.55, wear rate 5 × 10-3mm3/ min), coefficient of friction reduces 0.1, and wear rate reduces 0.8 × 10-3mm3/min.Herein
In original SiC ceramics refer to the SiC ceramic raw material in step 2.
The preparation method of the present embodiment can obtain Ti3SiC2-Al2O3- SiC-Al composite material, and be in the infiltration time
Can Al be made to completely penetrate in SiC ceramic when 4h, but lower Ti content can not be such that Ti fills on the surface layer SiC in aluminium alloy
Divide aggregation, so textura epidermoidea is not fine and close, is still mingled with the complete SiC of a large amount of unreacteds.
Embodiment 3
Ti in the present embodiment3SiC2-Al2O3The specific preparation method and step of-SiC-Al composite material are with embodiment 1, no
With the mass percent of place each element in aluminium alloy in this present embodiment are as follows: Al, 75wt.%；Ti, 10wt.%；Mg,
5wt%；Si, 10wt%.
Analysis test is carried out to composite material made from the present embodiment according to the test and analytic process of embodiment 1, specifically
The result is that: pass through fracture toughness test, the average fracture toughness of composite material made from the present embodiment is 5.2MPam1/2, compare
In original SiC ceramics (2.2MPam1/2) improve 3.0MPam1/2；Friction and wear behavior test is carried out under equal conditions, measures material
The average friction coefficient of material is 0.42, and average wear rate is 4.0 × 10-3mm3/ min, compared to the ceramic (coefficient of friction of original SiC
0.55, wear rate 5 × 10-3mm3/ min), coefficient of friction reduces 0.13, and wear rate reduces 1.0 × 10-3mm3/min。
The preparation method of the present embodiment can obtain Ti3SiC2-Al2O3- SiC-Al composite material, and be in the infiltration time
Can Al be made to completely penetrate in SiC ceramic when 4h, higher Mg content greatly improves aluminium alloy in aluminium alloy
Mobility promotes Ti to be sufficiently enriched on the surface layer SiC, so textura epidermoidea is finer and close compared to embodiment 3, reaction layer thickness is more
Greatly.
Embodiment 4
The present embodiment Ti3SiC2With embodiment 3, difference exists the specific steps of the preparation method of/SiC/Al composite material
In this present embodiment in aluminium alloy each element mass percent are as follows: Al, 70wt.%；Ti, 15wt.%；Mg, 5wt%；Si,
10wt%.
Analysis test is carried out to composite material made from the present embodiment according to the test and analytic process of embodiment 3, specifically
The result is that: pass through fracture toughness test, the average fracture toughness of composite material made from the present embodiment is 5.4MPam1/2, compare
In original SiC ceramics (2.2MPam1/2) improve 3.2MPam1/2；Friction and wear behavior test is carried out under equal conditions, measures material
The average friction coefficient of material is 0.38, and average wear rate is 3.8 × 10-3mm3/ min, compared to the ceramic (coefficient of friction of original SiC
0.55, wear rate 5 × 10-3mm3/ min), coefficient of friction reduces 0.17, and wear rate reduces 1.2 × 10-3mm3/min。
The preparation method of the present embodiment can obtain Ti3SiC2-Al2O3- SiC-Al composite material, when oxidization time is 8h
The remaining major part Al in surface layer can be made to be oxidized to Al2O3, and enough Ti contents assemble Ti sufficiently on the surface layer SiC, so surface layer
It organizes finer and close.
Embodiment 5
The present embodiment Ti3SiC2With embodiment 3, difference exists the specific steps of the preparation method of/SiC/Al composite material
In the oxidization time of the present embodiment is 6h.
Analysis test is carried out to composite material made from the present embodiment according to the test and analytic process of embodiment 3, specifically
The result is that: pass through fracture toughness test, the average fracture toughness of composite material made from the present embodiment is 4.4MPam1/2, compare
In original SiC ceramics (2.2MPam1/2) improve 2.2MPam1/2；Friction and wear behavior test is carried out under equal conditions, measures material
The average friction coefficient of material is 0.46, and average wear rate is 4.3 × 10-3mm3/ min, compared to the ceramic (coefficient of friction of original SiC
0.55, wear rate 5 × 10-3mm3/ min), coefficient of friction reduces 0.09, and wear rate reduces 0.7 × 10-3mm3/min。
The preparation method of the present embodiment can obtain Ti3SiC2-Al2O3- SiC-Al composite material, although oxidization time is
The remaining Al in surface layer can be made to be oxidized to Al when 6h2O3, but the aluminium in ceramic internal void fails as the aluminium in embodiment 3
Oxidation sufficiently, so textura epidermoidea is not fine and close, is still mingled with the complete Al of unreacted.
Embodiment 6
The present embodiment Ti3SiC2With embodiment 3, difference exists the specific steps of the preparation method of/SiC/Al composite material
In the oxidization time of the present embodiment is 10h.
Analysis test is carried out to composite material made from the present embodiment according to the test and analytic process of embodiment 3, specifically
The result is that: pass through fracture toughness test, the average fracture toughness of composite material made from the present embodiment is 5.9MPam1/2, compare
In original SiC ceramics (2.2MPam1/2) improve 3.7MPam1/2；Friction and wear behavior test is carried out under equal conditions, measures material
The average friction coefficient of material is 0.30, and average wear rate is 3.2 × 10-3mm3/ min, compared to the ceramic (coefficient of friction of original SiC
0.55, wear rate 5 × 10-3mm3/ min), coefficient of friction reduces 0.25, and wear rate reduces 1.8 × 10-3mm3/min。
The Ti that will be obtained3SiC2-Al2O3- SiC-Al composite material successively use 150 mesh, 400 mesh, 800 mesh, 1500 mesh,
2000 mesh sand paper carry out surface grinding, remove the Al based alloy of surfaces stick, dry after dehydrated alcohol ultrasonic cleaning 4min；
Surface carries out XRD detection and SEM and EDS is analyzed, and concrete outcome is respectively such as Fig. 1, Fig. 2, shown in Fig. 3, the maximum area of area in Fig. 1
Domain represents Ti3SiC2Phase, white area represent Al2O3Phase, the most deep fine grained chippings shape Regional Representative's SiC phase of color.From Fig. 1
As can be seen that the outer layer (interface) of composite material has a large amount of Ti3SiC2And Al2O3It generates, minimal amount of SiC, at this time
Ti3SiC2-Al2O3The Ti of-SiC-Al composite material3SiC2And Al2O3Layer is most fine and close.Pass through model OLMYMPUSDSX510's
Metallographic microscope is surveyed using multiphase content measurement ASTME 1245-2003 software according to the difference of the not gray value of jljl phase
Obtain each component percent by volume Ti in the present embodiment3SiC2: 57%, Al2O3: 35%, SiC:8%.
To Ti3SiC2-Al2O3The coupon of-SiC-Al composite material, respectively with 150 mesh, 400 mesh, 800 mesh, 1500 mesh,
2000 mesh diamond disks carry out section grinding, are polished through 0.5 μm of polishing agent, at pair cross-section center position carry out SEM and
EDS analysis, concrete outcome is respectively such as Fig. 4, shown in Fig. 5.SiC ceramic internal structure is fine and close as can be seen from Figure 4, multiple as shown in Figure 5
It is mainly Si, C, Al element inside condensation material, illustrates that Al permeates inside SiC ceramic completely and forms fine and close knot with SiC particulate
Structure.
The preparation method of the present embodiment can obtain Ti3SiC2-Al2O3- SiC-Al composite material, when oxidization time is 10h
Remaining Al in the gap of surface layer can be made to be completely oxidized to Al2O3, and other objects are not damaged mutually, and Ti is sufficiently poly- on the surface layer SiC
Collection, completely reaction generate a large amount of Ti3SiC2, reaction layer thickness is up to 400 μm, so textura epidermoidea is most fine and close, toughness highest,
Anti-attrition abrasion resistant effect is best.
By being compared to embodiment 1-6 it can be concluded that the following conclusions: the raising of Ti content facilitates in surface layer
Ti3SiC2Generation, the addition of Ti, Mg, Si help to improve the mobility of aluminium alloy in Al alloy, increase infiltration depth, excellent
950 DEG C of oxidizing temperature are selected, with the extension (6h-10h) of oxidization time, Ti3SiC2-Al2O3The thickness of-SiC conversion zone increases,
6 effect of embodiment is best, and for conversion zone highest thickness up to 400 μm, fracture toughness reaches as high as 5.9MPam1/2, coefficient of friction subtracts
It is small to 0.30, wear rate is reduced to 3.2 × 10-3mm3/min。
Table 1 is embodiment 6Ti3SiC2-Al2O3Fracture toughness, coefficient of friction, wear rate and the original of-SiC-Al composite material
Beginning ceramics comparison
| Sample | Fracture toughness (MPam1/2) | Coefficient of friction | Wear rate (mm3/min) |
| SiC ceramic | 2.2 | 0.55 | 5×10-3 |
| Embodiment 6 | 5.9 | 0.30 | 3.2×10-3 |
In conclusion wetability of the present invention by element al, Ti, Si, Mg and ceramics, using reaction infiltration method, by Al
Based alloy introduces inside SiC ceramic, and inside forms fine and close SiC/Al structure, while can generate one layer in SiC ceramic outer surface
Contain Ti simultaneously3SiC2, SiC, Al cermet coating be placed on electricity after being then processed by shot blasting the specimen surface after infiltration
It in furnace, is further heat-treated, i.e., carries out the situ oxygen of certain time to the composite material tentatively obtained at a certain temperature
Change processing, by outer surface Ti3SiC2Al is generated with the Al in-situ oxidation in the gap SiC2O3, extexine can be obtained in this way is
Ti3SiC2/Al2O3/ SiC, inside are the Ti of densification SiC/Al3SiC2-Al2O3- SiC-Al composite material, this method significantly improve
The obdurability and properties of antifriction and wear resistance of SiC based composites；And the preparation method can be completed under normal pressure, in-situ preparation, letter
Preparation process is changed, and material interface bond strength is high, compatibility is good, and overcoming in the prior art can only be in high pressure even Gao Zhen
The shortcomings that prepared by the stringent process conditions such as sky, greatly reduces production cost, can be realized size and forms only.System of the present invention
Standby process can be completed under normal pressure, and operating procedure is simple, can be realized size and forms only, is suitable for industrializing implementation and reality
Using being particularly suitable for requiring high-intensitive, high abrasion operating condition field.
Above-mentioned multiple embodiments are relatively intended to be easy to understand preparation method of the present invention properties of product on technical arrangement plan
Trend.So that those skilled in the art can understand the innovation essence for grasping technical solution of the present invention, not only in function or production
Moral character can go up the embodiment for proposing to limit.In addition to the implementation, so the present invention can also have other polynary embodiments.
All technical solutions formed using equivalent substitution or equivalent transformation, are fallen within the scope of protection required by the present invention.
The present invention does not address place and is suitable for the prior art.
Claims (4)
1. a kind of Ti3SiC2-Al2O3- SiC-Al composite material, it is characterized in that the composite material outer layer is Ti3SiC2/Al2O3/SiC
Conversion zone, inside are SiC/Al composite material；The reaction layer thickness is 100 ~ 400 μm.
2. the Ti as described in claim 13SiC2-Al2O3- SiC-Al composite material, it is characterized in that the composite wood
Expect in outer layer, percent by volume Ti3SiC2: 60 ~ 80%, Al2O3: 15% ~ 40%, SiC:5% ~ 20%.
3. Ti as described in claim 13SiC2-Al2O3The preparation method of-SiC-Al composite material, it is characterized in that this method packet
Include following steps:
(1) preparation of aluminium alloy acieral: each element mass percent in aluminium alloy are as follows: Al, 45-90 wt.%；Ti, 3-
25 wt.%；Mg, 1-6 wt.%；Si, 5-30 wt.%；
Corresponding raw material is weighed according to the mass percent of above-mentioned each element, fine aluminium ingot is put into NaOH solution and is submerged 1-3 hours,
Surface scale is removed, is then placed in graphite crucible together with titanium ingot, magnesium powder, silico briquette, be warming up to 700-1100 DEG C into
Row fusing stirs lower heat preservation 0.5-4 h, the acieral melt of molten condition can be obtained；
(2) pretreatment of SiC ceramic: SiC ceramic is cut into required size, is dried after polishing, ultrasonic cleaning；
(3) it reacts infiltration process: the silicon carbide ceramics handled well in step 2 is immersed into molten prepared in step (1)
In the acieral melt of state, infiltration 0.5-9 h, is then taken out at 700-1000 DEG C, is cooled to room temperature, and is obtained after polishing
Ti3SiC2/ SiC/Al composite material；
(4) oxidation processing technique: by Ti polished in step (3)3SiC2/ SiC/Al composite material is put into porcelain boat, is then put
Enter progress in-situ oxidation processing in batch-type furnace, 800-1100 DEG C of oxidizing temperature, oxidization time 4-14 h then takes out, is cooled to
Room temperature obtains Ti3SiC2-Al2O3- SiC-Al composite material.
4. Ti as described in claim 13SiC2-Al2O3The preparation method of-SiC-Al composite material, it is characterized in that the step
Suddenly the concentration of the NaOH solution in (1) is 0.3mol/L ~ 0.6mol/L.
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