CN106904985A - A kind of titanium silicon-carbon enhanced oxidation aluminium base heterogeneous composite material and preparation method thereof - Google Patents
A kind of titanium silicon-carbon enhanced oxidation aluminium base heterogeneous composite material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of titanium silicon-carbon enhanced oxidation aluminium base heterogeneous composite material and preparation method thereof.Titanium valve, alumina powder and carborundum powder are weighed according to a certain volume, with alcohol as decentralized medium, alumina balls are ball-milling medium, and mixed powder is dried to obtain after being sufficiently mixed；Mixed powder is placed in vacuum hotpressing stove carries out hot pressed sintering with certain pressure, heating rate, sintering temperature, soaking time.In view of the Al under hot pressing condition in alumina base heterogeneous composite material2O3There is strong interfacial reaction at high temperature with Ti, generate Intermatallic Ti-Al compound, especially TiAl and Ti3Al, can reduce the performance of material.The present invention is reacted by filling SiC particulate with Ti, generates new compound TiC, Ti3SiC2Deng activeness and quietness material, while the Si of semi-molten is filled in the part hole of material, so that obtaining, relative density is high, the big alumina base heterogeneous composite material of hardness, toughness, intensity.
Description
Technical field
The invention belongs to the preparing technical field that carbide fills ceramic base metallic composite, it is related to a kind of titanium-silico-carbo
Enhanced oxidation aluminium base heterogeneous composite material and preparation method thereof.
Background technology
In recent years, the research of ceramic-metal composite receives much concern, wherein Al2O3Ceramics are most widely used ceramics
One of material.The features such as alumina ceramic composite material has wear-resistant, corrosion-resistant, high temperature resistant, high rigidity, and possess superior
Inoxidizability and chemical stability, cheap, aboundresources.It has been widely used in Aero-Space, medical treatment, automobile hair at present
The fields such as motivation, electronic component, mechanical material.But the toughness of aluminium oxide ceramics is relatively low, its production application is limited.
At present, the carbide and nitride ceramics of ternary contain excellent property because of itself special layer structure
Can, only ceramic characteristics, while also including metallic character, do not improve the fragility of ceramics, improve toughness, and Ti3SiC2It is three
One of ceramic material for attracting most attention in first carbide, ternary Ti3SiC2The mechanical performance of material is superior, has at high temperature
Good inoxidizability.But Ti3SiC2The heterogeneous composite material for strengthening aluminum oxide has that hardness, relative density are relatively low.
The content of the invention
The present invention is directed to the above-mentioned problems in the prior art, there is provided a kind of titanium-carbon enhanced oxidation aluminium base multiphase is answered
Condensation material, it is high with relative density, the advantages of hardness, toughness, big intensity.
Meanwhile, present invention also offers the preparation method of above-mentioned titanium-silico-carbo enhanced oxidation aluminium base heterogeneous composite material.
Technical solution of the present invention is as follows：
A kind of preparation method of titanium-silico-carbo enhanced oxidation aluminium base heterogeneous composite material, comprises the following steps：
1）The preparation of mixed powder：Will by volume 40：40~50：10~20 measure titanium valve, alumina powder and carborundum powder, with
Alcohol is decentralized medium, and powder is 1 with alcohol by volume ratio：6, alumina balls are ball-milling medium, and ball milling 4h, the slurry after ball milling is put
24h is dried in 70 DEG C, is fully dried after powder, to cross 50 mesh sieves, obtain mixed powder；
2）Vacuum heating-press sintering：Mixed powder is placed in vacuum hotpressing stove, under 20~60MPa pressure, 1400~1800 DEG C
1~5h of hot pressed sintering, obtains titanium-silico-carbo enhanced oxidation aluminium base heterogeneous composite material.
Step 1）In, it is 10 ~ 20% that described carborundum powder accounts for powder cumulative volume ratio used；
Step 1）In, described titanium valve, alumina powder and carborundum powder volume ratio preferably 40:40:20；
Step 1）In, the particle diameter of described titanium valve is 0.5~2 μm, and the particle diameter of alumina powder is 0.5~3 μm, the grain of carborundum powder
Footpath is 0.5~2 μm.
Step 2）In, described sintering, heating rate is 5~20 DEG C/min.
Step 2）In, in vacuum hotpressing stove, preferably under 30MPa pressure, 1600 DEG C of hot pressed sintering 2h.
Titanium-silico-carbo enhanced oxidation aluminium base heterogeneous composite material prepared by a kind of above method.
Described titanium-silico-carbo enhanced oxidation aluminium base heterogeneous composite material, by following weight/mass percentage composition into packet
Into：Titanium 45~47%, silicon 5~12%, carbon 3~5%, the % of oxygen 17~36, balance of aluminium；
Described titanium, carbon and part element silicon are with TiC, Ti5Si3、Ti3SiC2The form of compound particles is embedded in alumina base
In body, remaining element silicon is solid-solution in the hole of composite with atomic form, and the ratio of two parts element silicon is 70~75：25
~30.
Described titanium-silico-carbo enhanced oxidation aluminium base heterogeneous composite material is tabular or column, and has layer structure, chi
Very little is 3~5 μm.
Described titanium-silico-carbo enhanced oxidation aluminium base heterogeneous composite material relative density is 90~99%；Microhardness is
10~25GPa, bending strength is 200~600MPa, and fracture toughness is 3~15 MPa m1/2。
Heterogeneous composite material of the present invention, new compound is generated by the carborundum powder and the titanium that fill, wherein TiC,
Ti3SiC2Activeness and quietness effect is played, the Si of semi-molten is filled in the part hole of material, so as to obtain phase under hot pressing condition
It is high to density, the big alumina base heterogeneous composite material of hardness, toughness, intensity.SiC is used as being only second to diamond and B4The of C
Three hardened materials, with excellent mechanical performance and chemical stability, SiC particulate is added in alumina base heterogeneous composite material,
Advantageously reduce metallic compound TiAl, Ti3The generation of Al.Material is sheet-like particle before the non-plus silicon carbide of the present invention, is existed
A certain amount of stomata, with the addition of carborundum, the crystal grain of material gradually increases, and stomata is gradually reduced, and with part holes
Disappear.Above all SiC and Ti reacts, and forms TiC, Ti5Si3、Ti3SiC2Etc. new compound, wherein TiC, Ti3SiC2
Activeness and quietness effect is played, while the generation of TiC substantially increases the intensity of material, the Si of semi-molten phase is filled in part hole
In, promote the densification of material, so as to obtain the superior alumina base heterogeneous composite material of combination property under hot pressing condition.
Preparation method of the present invention is advantageous in that compared to existing technology：
（1）, compared to non-impurity-doped titanium/alumina composite material, the Si of semi-molten phase is filled out ceramic matric composite prepared by the present invention
Fill in hole, relative density is further improved, one is provided to hot pressed sintering alumina ceramic composite material
Plant more excellent sintering aid；
（2）The carborundum of present invention admixture, can make titanium produce new material with silicon carbide reactor, it is suppressed that chemical combination between titanium-aluminium alloy category
The generation of thing, forms new compound, wherein cenotype TiC, Ti3SiC2Activeness and quietness effect is played, makes its intensity, fracture toughness
It is greatly improved；
（3）Operating process of the present invention is fairly simple, and cost of material is relatively low, and properties of product are superior, and practical application is produced
Important in inhibiting.
Brief description of the drawings
Fig. 1 is the XRD spectrum of the alumina base heterogeneous composite material of admixture carborundum in embodiment 1；
Fig. 2 is the section SEM figures of the alumina base heterogeneous composite material of admixture carborundum in embodiment 1；
Fig. 3 is the XRD spectrum of alumina base heterogeneous composite material in comparative example 1；
Fig. 4 is the section SEM figures of alumina base heterogeneous composite material in comparative example 1.
Specific embodiment
The present invention is described in conjunction with specific embodiments, without departing from the idea case in the present invention described above, according to this area
Various replacements or change that ordinary technical knowledge and customary means are made, are included within the scope of the present invention.
Embodiment 1
A kind of preparation method of titanium-silico-carbo enhanced oxidation aluminium base heterogeneous composite material, step is：
1）By titanium valve, alumina powder, carborundum powder by volume 40：40：20 mixing, with alcohol as decentralized medium, powder and wine
Smart discrete volume ratio is 1:6, alumina balls are ball-milling medium, the ball milling 4h in polytetrafluoroethyltank tank；Slurry after ball milling is placed in
In drying box, 24h is dried under the conditions of 70 DEG C；Fully dry and obtain mixed powder after powder, to cross 50 mesh sieves；
2）30g mixed powders are taken in vacuum hotpressing stove, is placed in 1500 DEG C in the graphite jig of diameter 45mm, under the conditions of 30MPa
Sintering 2h, 10 DEG C/min of heating rate, obtain titanium-silico-carbo enhanced oxidation aluminium base heterogeneous composite material.
After measured, 1 titanium of embodiment-silico-carbo enhanced oxidation aluminium base heterogeneous composite material is 3~5 μm of long column shape or plate
Shape, and have layer structure, by following weight/mass percentage composition into being grouped into：The % of titanium 46.1, the % of silicon 11.4, carbon 4.9%, oxygen
17.7 %, balance of aluminium；Described titanium, carbon and part element silicon are with TiC, Ti5Si3、Ti3SiC2The form edge of compound particles
It is embedded in alumina substrate, remaining element silicon is solid-solution in the hole of composite with atomic form, the ratio of two parts silicon is
3:1.Relative density is 97.76%, bending strength 437.26MPa, and microhardness is 19.61 GPa, and fracture toughness is 9.95MPa
·m1/2.X-ray diffraction analysis show（Image is as shown in Figure 1）, after addition carborundum, new chemical combination is formd between Ti and SiC
Thing, product includes TiC, Ti5Si3、Ti3SiC2, product Ti now3SiC2Content increases, and the performance of material is further carried
It is high.Meanwhile, by scanning electron microscope analysis（Image is as shown in Figure 2）, it is seen that the combination of its contact layer is more tight, further lifting
The intensity of composite.
Embodiment 2
A kind of preparation method of titanium-silico-carbo enhanced oxidation aluminium base heterogeneous composite material, step is：
1）By titanium valve（1μm）, alumina powder（1μm）, carborundum powder（800nm）By volume 40：45：15 mixing, be with alcohol
Decentralized medium, discrete volume ratio is 1:6, alumina balls are ball-milling medium, the ball milling 4h in polytetrafluoroethyltank tank；Material after ball milling
Slurry is placed in drying box, and 24h is dried under the conditions of 70 DEG C；Fully dry and obtain mixed powder after powder, to cross 50 mesh sieves；
2）30g mixed powders are taken in vacuum hotpressing stove, is placed in 1500 DEG C in the graphite jig of diameter 45mm, under the conditions of 30MPa
Sintering 2h, 10 DEG C/min of heating rate, obtain titanium-silico-carbo enhanced oxidation aluminium base heterogeneous composite material.
After measured, 2 titaniums of embodiment-silico-carbo enhanced oxidation aluminium base heterogeneous composite material is 3~5 μm of long column shape or plate
Shape, and have layer structure, by following weight/mass percentage composition into being grouped into：The % of titanium 45.8, silicon 8.5%, the % of carbon 3.6, oxygen 19.8
%, balance of aluminium；Described titanium, carbon and part element silicon are with TiC, Ti5Si3、Ti3SiC2The form of compound particles is embedded in oxygen
Change in aluminum substrate, remaining element silicon is solid-solution in the hole of composite with atomic form, the ratio of two parts silicon is 37:14.
Relative density is 98.47%, bending strength 431.23MPa, and microhardness is 19.52GPa, and fracture toughness is 7.83MPa m1 /2, the performance of material is significantly improved.X-ray diffraction analysis show that after addition carborundum, Ti and SiC forms new
Compound, Ti is consumed, and product includes TiC, Ti5Si3、Ti3SiC2, wherein TiC, Ti3SiC2Play activeness and quietness, improve material
The intensity and toughness of material, the Si of wherein semi-molten are filled in the hole of part, and this has important meaning to the density for improving material
Justice, finds, the combination of contact layer is more tight, and the intensity of composite is further lifted by scanning electron microscope analysis.
Embodiment 3
A kind of preparation method of titanium-silico-carbo enhanced oxidation aluminium base heterogeneous composite material, step is：
1）By titanium valve（1μm）, alumina powder（1μm）, carborundum powder（800nm）By volume 40：50：10 mixing, be with alcohol
Decentralized medium, discrete volume ratio is 1:6, alumina balls are ball-milling medium, the ball milling 4h in polytetrafluoroethyltank tank；Material after ball milling
Slurry is placed in drying box, and 24h is dried under the conditions of 70 DEG C；Fully dry and obtain mixed powder after powder, to cross 50 mesh sieves；
2）30g mixed powders are taken in vacuum hotpressing stove, is placed in 1500 DEG C in the graphite jig of diameter 45mm, under the conditions of 30MPa
Sintering 2h, 10 DEG C/min of heating rate, obtain titanium-silico-carbo enhanced oxidation aluminium base heterogeneous composite material.
After measured, 2 titaniums of embodiment-silico-carbo enhanced oxidation aluminium base heterogeneous composite material is 3~5 μm of long column shape or plate
Shape, and have layer structure, by following weight/mass percentage composition into being grouped into：The % of titanium 45.6, the % of silicon 5.6, the % of carbon 2.4, oxygen
21.8 %, balance of aluminium；Described titanium, carbon and part element silicon are with TiC, Ti5Si3、Ti3SiC2The form edge of compound particles
It is embedded in alumina substrate, remaining element silicon is solid-solution in the hole of composite with atomic form, the ratio of two parts silicon is
7:3.Relative density is 96.48%, bending strength 392.39MPa, and microhardness is 17.61GPa, and fracture toughness is 6.87MPa
·m1/2, the performance of material is significantly improved.X-ray diffraction analysis show that after addition carborundum, Ti is formd with SiC
New compound, Ti is consumed, and product includes TiC, Ti5Si3、Ti3SiC2, wherein TiC, Ti3SiC2Play activeness and quietness, carry
The intensity and toughness of material high, the Si of wherein semi-molten are filled in the hole of part, and this has important to the density for improving material
Meaning, find that the combination of contact layer is more tight by scanning electron microscope analysis, the intensity of composite can be lifted.
Comparative example 1
By titanium valve（1μm）, alumina powder（1μm）By 40：60 volume ratio is prepared, with alcohol as decentralized medium, dispersion
Product is than being 1:6, alumina balls are ball-milling medium, the ball milling 4h in polytetrafluoroethyltank tank；Slurry after ball milling is placed in drying box
24h is dried under the conditions of 70 DEG C；Dried powder is crossed into 50 mesh sieves and obtains mixed powder；Take 30g mixed powders and be placed in diameter
2h, 10 DEG C/min of heating rate are sintered 1500 DEG C in the graphite jig of 45mm, under the conditions of 30MPa；Sample is obtained.
After measured, the relative density of sample is 94.52%, and bending strength is 324.46MPa, and microhardness is
15.48GPa, fracture toughness is 4.63MPa m1/2.X-ray diffraction analysis show（Image is as shown in Figure 3）, there is big in sample
The TiAl and Ti of amount3The generation of Al intermetallic compounds, these materials have stronger brittleness at room temperature, can substantially reduce composite wood
Expect overall intensity and toughness.Meanwhile, by scanning electron microscope analysis we have found that titanium is obvious with the crystal boundary of aluminium（Image is as schemed
Shown in 4）, adhesion is weaker between the two.
Claims (10)
1. the preparation method of a kind of titanium-silico-carbo enhanced oxidation aluminium base heterogeneous composite material, it is characterised in that including following step
Suddenly：
1）The preparation of mixed powder：Will by volume 40：40~50：10~20 measure titanium valve, alumina powder and carborundum powder, with
Alcohol is decentralized medium, and powder is 1 with alcohol by volume ratio：6, alumina balls are ball-milling medium, and ball milling 4h, the slurry after ball milling is put
24h is dried in 70 DEG C, is fully dried after powder, to cross 50 mesh sieves, obtain mixed powder；
2）Vacuum heating-press sintering：Mixed powder is placed in vacuum hotpressing stove, under 20~60MPa pressure, 1400~1800 DEG C
1~5h of hot pressed sintering, obtains titanium-silico-carbo enhanced oxidation aluminium base heterogeneous composite material.
2. preparation method according to claim 1, it is characterised in that：Step 1）In, described carborundum powder accounts for powder used
Material cumulative volume ratio is 10 ~ 20%；Described titanium valve, alumina powder and carborundum powder volume ratio are 40:40:20.
3. preparation method according to claim 1, it is characterised in that：Step 1）In, the particle diameter of described titanium valve for 0.5~
2 μm, the particle diameter of alumina powder is 0.5~3 μm, and the particle diameter of carborundum powder is 0.5~2 μm.
4. preparation method according to claim 1, it is characterised in that：Step 1）In, described sintering, heating rate is 5
~20 DEG C/min.
5. preparation method according to claim 1, it is characterised in that：Step 2）In, in vacuum hotpressing stove, 30MPa pressure
Under, 1600 DEG C of hot pressed sintering 2h.
6. titanium-silico-carbo enhanced oxidation aluminium base heterogeneous composite material that prepared by a kind of any one of Claims 1 to 5 methods described.
7. titanium according to claim 6-silico-carbo enhanced oxidation aluminium base heterogeneous composite material, it is characterised in that by following
Weight/mass percentage composition into being grouped into：Titanium 45~47%, silicon 5~12%, carbon 3~5%, the % of oxygen 17~36, balance of aluminium.
8. titanium according to claim 7-silico-carbo enhanced oxidation aluminium base heterogeneous composite material, it is characterised in that described
Titanium, carbon and part element silicon are with TiC, Ti5Si3、Ti3SiC2The form of compound particles is embedded in alumina substrate, excess silicon
Element is solid-solution in the hole of composite with atomic form, and the ratio of two parts element silicon is 70~75：25~30.
9. titanium according to claim 6-silico-carbo enhanced oxidation aluminium base heterogeneous composite material, it is characterised in that：It is tabular
Or column, and having layer structure, size is 3~5 μm.
10. titanium according to claim 6-silico-carbo enhanced oxidation aluminium base heterogeneous composite material, it is characterised in that described
Titanium-silico-carbo enhanced oxidation aluminium base heterogeneous composite material relative density be 90~99%, microhardness be 10~25GPa, it is curved
Qu Qiangdu is 200~600MPa, and fracture toughness is 3~15 MPa m1/2。
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| CN113264775A (en) * | 2020-01-29 | 2021-08-17 | 日本碍子株式会社 | Dense composite material, method for producing same, joined body, and member for semiconductor manufacturing apparatus |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107805071A (en) * | 2017-10-26 | 2018-03-16 | 西南交通大学 | A kind of preparation method of the low glass wetting aluminium two/mullite composite ceramic of carbon of titanium three |
| CN108101520A (en) * | 2017-12-23 | 2018-06-01 | 深圳万佳互动科技有限公司 | Alundum (Al2O3)-composite material of silicon carbide and preparation method thereof |
| CN113264775A (en) * | 2020-01-29 | 2021-08-17 | 日本碍子株式会社 | Dense composite material, method for producing same, joined body, and member for semiconductor manufacturing apparatus |
| CN113264775B (en) * | 2020-01-29 | 2023-07-04 | 日本碍子株式会社 | Compact composite material, method for producing the same, bonded body, and member for semiconductor manufacturing device |
| CN112571886A (en) * | 2020-12-29 | 2021-03-30 | 瓯锟科技温州有限公司 | Preparation method of silicon metal composite plate |
| CN112571886B (en) * | 2020-12-29 | 2023-01-24 | 瓯锟科技温州有限公司 | Preparation method of silicon metal composite plate |
| CN113582673A (en) * | 2021-08-26 | 2021-11-02 | 济南大学 | Aluminum oxide/titanium silicon carbon layered composite material and in-situ preparation method thereof |
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