CN105669204A - Preparation method of Ti2AlC ceramic powder material - Google Patents

Preparation method of Ti2AlC ceramic powder material Download PDF

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Publication number
CN105669204A
CN105669204A CN201610060019.4A CN201610060019A CN105669204A CN 105669204 A CN105669204 A CN 105669204A CN 201610060019 A CN201610060019 A CN 201610060019A CN 105669204 A CN105669204 A CN 105669204A
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Prior art keywords
preparation
polishing
alc
block
sintering
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Inventor
张建峰
王晓帆
李改叶
王红兵
曹慧杨
刘芸伊
周华思
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Hohai University HHU
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Hohai University HHU
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/5607Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides
    • C04B35/5611Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides based on titanium carbides
    • C04B35/5618Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides based on titanium carbides based on titanium aluminium carbides
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products

Abstract

The invention discloses a preparation method of a Ti2AlC ceramic powder material. Firstly, titanium powder, aluminum powder and carbon powder are mixed in proportion, and the mixture is subjected to wet grinding in an absolute ethyl alcohol medium and placed in a produced mold for prepressing after being dried; then the mold is placed in an SPS (spark plasma sintering) furnace, argon is introduced for shielding, pressureless sintering is performed, and the mold is taken out after heat preservation; then the sintered Ti2AlC block is polished; finally, the Ti2AlC block is mashed, ground and screened with a sieve of 200 meshes, and the layered Ti2AlC ceramic powder material is obtained. The preparation process is simple to operate, the reproducibility is high, during preparation, the heating speed is high, the sintering temperature is low, crystal grains are uniform, besides, the method is simple to operate, high in reproducibility, safe and reliable, the space and energy are saved, and the cost is low. The prepared Ti2AlC is high in purity, and the layer gap of the layered structure is large.

Description

The preparation method of a kind of titanium two aluminium ceramic powder material
Technical field
The invention belongs to field of ceramic material preparation, specifically relate to a kind of titanium two aluminium carbon (Ti2AlC) preparation method of ceramic layered powder body material.
Background technology
Ti2AlC, as the one of MAX phase ternary layered ceramic, is a kind of novel processable ceramics material received much concern. MAX phase is the general designation of the novel ternary compound with microcosmic laminate structure of a class, and chemical formula can represent for Mn+1AXn, M represents transition metal; A represents main group element; X represents carbon or nitrogen. Owing to crystalline structure and the bonding mode of its uniqueness makes it possess metal and the premium properties of pottery simultaneously. Both as pottery, there are high elastic coefficient, low density, good thermostability and antioxidant property; Again as metal, standby excellent heat conduction and conductivity, and lower hardness, it is possible to carry out mechanical workout, and at high temperature have good plasticity, self-lubricating property. Both there is the feature of Graphene high-specific surface area, high conductivity, possesses again component adjustable flexibly, the advantage such as minimum nanometer of thickness is controlled, show huge potentiality in fields such as energy storage, absorption, sensor, conductive fillers, can be used as Novel cathode material for lithium ion battery, advanced composite material reinforcement, high-temperature lubricating material etc.
At Ti2During AlC is ceramic layered, Ti-C key mainly combines with strong covalent bond and ionic linkage so that material has the performances such as high-melting-point, high-modulus, high strength; And Ti-Al key has obviously metallic bond feature so that material is provided with good electroconductibility, thermal conductivity; Again owing to combining to be similar to the Fan Dehua weak bond of graphite layers between Ti atom and Al atomic plane layer so that material has laminate structure and self-lubricating property. Ti2These performances of AlC make it have broad application prospects.
But it is current to Ti2The preparation of AlC mainly utilizes hot pressing, hot isostatic pressing and first prepares corresponding ternary layered ceramic powder body by mechanical alloying method, then carries out the methods such as hot pressed sintering acquisition block materials. These existing preparation methods not only need long-time high temperature, high pressure, and condition is harsh, and the ternary layered structural sheet gap of preparation powder delivery body is little, and there is the problems such as Preparation equipment is huge, cost height, program complicated, the waste energy.And the ternary layered structural sheet gap that the method that we adopt prepares powder delivery body is big, it is easy to be stripped into two-dimensional sheet structure, realize other effect.
Therefore, develop one and prepare ternary layered Ti2The preparation method of AlC ceramic powder material is very necessary, for promoting Ti further2AlC new diseases has significance.
Summary of the invention
Goal of the invention: for problems of the prior art, the ternary layered titanium two aluminium carbon (Ti that the technical problem to be solved in the present invention is to provide a kind of purity height, crystal grain is even, cost is low, preparation method is simple2AlC) ceramic powder material.
The technical problem that the present invention also to be solved is to provide above-mentioned ternary layered Ti2The preparation method of AlC ceramic powder material.
For solving the problems of the technologies described above, the present invention takes following technical scheme: a kind of Ti2The preparation method of AlC ceramic powder material, comprises the steps:
(1) taking titanium valve, aluminium powder, carbon dust as reaction raw materials, according to 2: 1~1.5: 0.7~1 mixing, wet-milling 6~8 hours, fully dry sealing after grinding, obtains mixed powder;
(2) mixed powder step (1) obtained loads in mould, carries out precompressed with the pressure of 5~15MPa;
(3) mould is put into sintering oven under applying argon gas protective condition, carry out high temperature pressure-free sintering, take out after insulation, obtain Ti2AlC block;
(4) by Ti2AlC block is first with polishing machine polishing, and sanding and polishing is for subsequent use to the centre portions of block, is ground by the block after polishing and sieves, obtains Ti2AlC ceramic powder.
Preferably, in step (1), the mean particle size of titanium valve, aluminium powder, carbon dust is 200~400 orders.
In step (1), described wet-milling is entered in organic solvent medium, and described organic solvent medium is dehydrated alcohol.
In step (2), described mould is graphite jig. For ease of follow-up pressureless sintering, described mould can be designed as the drift with card groove so that upper lower punch is stuck on the sleeve of mould, in sintering process, powder body can not be applied pressure. The Ti sintered out like this2AlC block is comparatively loose, and the lamellar spacing of its ternary layered structure is big.
Preferably, in step (2), described mixed powder is loading before mould at mould inner sleeve one layer of carbon paper.
In step (2), precompressed is operating as: for ensureing pre-compressed effect, and in the process of charging, layering loads mixed powder, often adds one layer and just carries out a precompressed.
In step (3), described sintering oven is SPS sintering oven, and heat-up rate during sintering is 90~120 DEG C/min, and sintering temperature is 1000~1400 DEG C, is incubated 10~15min after sintering.
In step (4), when polishing, after the borax of polishing disk upper berth, continue polishing after being polished off by carbon paper to block core position.
In step (4), by the Ti after polishing2It is cleaned by AlC Ultrasonic Cleaners, then, dry with air dry oven.
In step (4), by the Ti of bulk2AlC puts into mortar, smashs to pieces and then crosses 200 object sieves under the environment of drying after grinding
Useful effect: compared with prior art, the present invention provides a kind of simple to operate, preparation Ti that reproducibility is high2The method of AlC powder body, heat-up rate is fast in the preparation, sintering temperature is low, crystal grain is even, and simple to operate, reproducibility height, safe and reliable, save space, the energy and low cost and other advantages; The Ti of preparation2AlC purity height, is easy to realize the solution strengthening of multicomponent. Ti prepared by the present invention2AlC powder body can be used as Novel cathode material for lithium ion battery, advanced composite material reinforcement, high-temperature lubricating material etc.
Accompanying drawing explanation
Fig. 1 is that in embodiment 3, sintering temperature is the Ti at 1200 DEG C2The XRD figure spectrum of AlC powder body;
Fig. 2 is the Ti of embodiment 3 under 1200 DEG C of sintering temperatures2The SEM surface topography map of AlC powder body.
Embodiment
Embodiment 1
It is averaged granularity 200 object titanium valve, aluminium powder, carbon dust, according to 2: 1: 0.7 mixing. With mortar wet-milling 6 hours in dehydrated alcohol, fully dry after grinding. After graphite jig inner sleeve one layer of carbon paper, get appropriate mixed powder, join in graphite jig in batches, with the pressure layering precompressed successively of 5MPa in the process loading graphite jig. Mould being put into SPS sintering oven, carries out pressureless sintering at 1000 DEG C, heat-up rate is 90 DEG C/min, and applying argon gas is protected, and takes out, obtain Ti after insulation 10min2AlC block. After the borax of polishing disk upper berth, by Ti2AlC block sanding and polishing, after being removed by the carbon paper being wrapped on block, continues the centre portions of sanding and polishing to block. Then, with Ultrasonic Cleaners, it is cleaned, then with air dry oven, it is dry. Dried block is put into mortar, smashs ground 200 mesh sieve to pieces, be prepared into Ti2The ceramic layered powder body material of AlC.
Embodiment 2
It is averaged granularity 250 object titanium valve, aluminium powder, carbon dust, according to 2: 1.2: 0.75 mixing. With mortar wet-milling 6.5 hours in dehydrated alcohol, fully dry after grinding. After graphite jig inner sleeve one layer of carbon paper, get appropriate mixed powder, join in graphite jig in batches, with the pressure layering precompressed successively of 10MPa in the process loading graphite jig. Mould being put into SPS sintering oven, carries out pressureless sintering at 1150 DEG C, heat-up rate is 100 DEG C/min, and applying argon gas is protected, and takes out, obtain Ti after insulation 10min2AlC block; After the borax of polishing disk upper berth, by Ti2AlC block sanding and polishing, after being removed by the carbon paper being wrapped on block, continues the centre portions of sanding and polishing to block. Then, with Ultrasonic Cleaners, it is cleaned, then with air dry oven, it is dry. Dried block is put into mortar, smashs ground 200 mesh sieve to pieces, be prepared into Ti2The ceramic layered powder body material of AlC.
Embodiment 3
Get granularity 300 object titanium valve, aluminium powder, carbon dust, according to 2: 1.3: 0.8 mixing. With mortar wet-milling 7 hours in dehydrated alcohol, fully dry after grinding. After graphite jig inner sleeve one layer of carbon paper, get appropriate mixed powder, join in graphite jig in batches, with the pressure layering precompressed successively of 15MPa in the process loading graphite jig. Mould being put into SPS sintering oven, carries out pressureless sintering at 1200 DEG C, heat-up rate is 100 DEG C/min, and applying argon gas is protected, and takes out, obtain Ti after insulation 10min2AlC block; After the borax of polishing disk upper berth, by Ti2AlC block sanding and polishing, after being removed by the carbon paper being wrapped on block, continues the centre portions of sanding and polishing to block. Then, with Ultrasonic Cleaners, it is cleaned, then with air dry oven, it is dry. Dried block is put into mortar, smashs ground 200 mesh sieve to pieces, be prepared into Ti2The ceramic layered powder body material of AlC. To ternary layered Ti2AlC powder body carries out XRD sign, and as shown in Figure 1, Fig. 1 is sintering temperature is the Ti at 1200 DEG C2The XRD figure spectrum of AlC powder body. As can be seen from the figure Ti is prepared2AlC powder purity is very high, only containing minute quantity SiC impurity.
Embodiment 4
Get granularity 350 object titanium valve, aluminium powder, carbon dust, according to 2: 1.4: 0.9 mixing.With mortar wet-milling 7.5 hours in dehydrated alcohol, fully dry after grinding. After graphite jig inner sleeve one layer of carbon paper, get appropriate mixed powder, join in graphite jig in batches, with the pressure layering precompressed successively of 10MPa in the process loading graphite jig. Mould being put into SPS sintering oven, carries out pressureless sintering at 1250 DEG C, heat-up rate is 100 DEG C/min, and applying argon gas is protected, and takes out, obtain Ti after insulation 10min2AlC block; After the borax of polishing disk upper berth, by Ti2AlC block sanding and polishing, after being removed by the carbon paper being wrapped on block, continues the centre portions of sanding and polishing to block. Then, with Ultrasonic Cleaners, it is cleaned, then with air dry oven, it is dry. Dried block is put into mortar, smashs ground 200 mesh sieve to pieces, be prepared into Ti2The ceramic layered powder body material of AlC.
Embodiment 5
Get granularity 400 object titanium valve, aluminium powder, carbon dust, according to 2: 1.5: 1 mixing. With mortar wet-milling 8 hours in dehydrated alcohol, fully dry after grinding. After graphite jig inner sleeve one layer of carbon paper, get appropriate mixed powder, join in graphite jig in batches, with the pressure layering precompressed successively of 15MPa in the process loading graphite jig. Mould being put into SPS sintering oven, carries out pressureless sintering at 1300 DEG C, heat-up rate is 120 DEG C/min, and applying argon gas is protected, and takes out, obtain Ti after insulation 10min2AlC block; After the borax of polishing disk upper berth, by Ti2AlC block sanding and polishing, after being removed by the carbon paper being wrapped on block, continues the centre portions of sanding and polishing to block. Then, with Ultrasonic Cleaners, it is cleaned, then with air dry oven, it is dry. Dried block is put into mortar, smashs ground 200 mesh sieve to pieces, be prepared into Ti2The ceramic layered powder body material of AlC.

Claims (10)

1. the preparation method of a titanium two aluminium ceramic powder material, it is characterised in that, comprise the steps:
(1) taking titanium valve, aluminium powder, carbon dust as reaction raw materials, according to 2: 1~1.5: 0.7~1 mixing, wet-milling 6~8 hours, fully dry after grinding, obtain mixed powder;
(2) mixed powder step (1) obtained loads in mould, carries out precompressed with the pressure of 5~15MPa;
(3) mould is put into sintering oven under applying argon gas protective condition, carry out high temperature pressure-free sintering, take out after insulation, obtain Ti2AlC block;
(4) by Ti2AlC block is first with polishing machine polishing, and sanding and polishing is for subsequent use to the centre portions of block, is ground by the block after polishing and sieves, obtains Ti2AlC ceramic powder.
2. preparation method according to claim 1, it is characterised in that, in step (1), the mean particle size of titanium valve, aluminium powder, carbon dust is 200~400 orders.
3. preparation method according to claim 1, it is characterised in that, in step (1), described wet-milling is entered in organic solvent medium, and described organic solvent medium is dehydrated alcohol.
4. preparation method according to claim 1, it is characterised in that, in step (2), described mould is graphite jig.
5. preparation method according to claim 1, it is characterised in that, in step (2), described mixed powder is loading before mould at mould inner sleeve one layer of carbon paper.
6. preparation method according to claim 1, it is characterised in that, in step (2), precompressed is operating as: for ensureing pre-compressed effect, and in the process of charging, layering loads mixed powder, often adds one layer and just carries out a precompressed.
7. preparation method according to claim 1, it is characterised in that, in step (3), described sintering oven is SPS sintering oven, and heat-up rate during sintering is 90~120 DEG C/min, and sintering temperature is 1000~1400 DEG C, pressure is 30~60MPa, is incubated 10~15min after sintering.
8. preparation method according to claim 4, it is characterised in that, in step (4), when polishing, after the borax of polishing disk upper berth, continue polishing after being polished off by carbon paper to block core position, the rotating speed of sanding and polishing is 100~120rad/min.
9. preparation method according to claim 1, it is characterised in that, in step (4), by the Ti after polishing2It is cleaned by AlC Ultrasonic Cleaners, then, dry with air dry oven.
10. preparation method according to claim 1, it is characterised in that, in step (4), by the Ti of bulk2AlC puts into mortar, smashs to pieces and then crosses 200 object sieves under the environment of drying after grinding.
CN201610060019.4A 2016-01-28 2016-01-28 Preparation method of Ti2AlC ceramic powder material Pending CN105669204A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106830971A (en) * 2017-04-05 2017-06-13 河海大学 A kind of preparation method of MAX phases porous ceramics
CN109553418A (en) * 2018-12-05 2019-04-02 武汉轻工大学 A kind of Ti2AlC porous material and preparation method thereof
CN110357633A (en) * 2019-07-11 2019-10-22 上海交通大学 A kind of method that room temperature quickly prepares titanium aluminium-carbon ceramic
CN113121236A (en) * 2021-03-02 2021-07-16 西安交通大学 Micron-sized three-dimensional lamellar Ti2AlC ceramic powder and preparation method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106830971A (en) * 2017-04-05 2017-06-13 河海大学 A kind of preparation method of MAX phases porous ceramics
CN109553418A (en) * 2018-12-05 2019-04-02 武汉轻工大学 A kind of Ti2AlC porous material and preparation method thereof
CN109553418B (en) * 2018-12-05 2021-08-13 武汉轻工大学 Ti2AlC porous material and preparation method thereof
CN110357633A (en) * 2019-07-11 2019-10-22 上海交通大学 A kind of method that room temperature quickly prepares titanium aluminium-carbon ceramic
CN113121236A (en) * 2021-03-02 2021-07-16 西安交通大学 Micron-sized three-dimensional lamellar Ti2AlC ceramic powder and preparation method thereof

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