CN109231989A - A kind of alloy with high activity intercalation Ti3AlMC2The preparation method of ceramic material - Google Patents
A kind of alloy with high activity intercalation Ti3AlMC2The preparation method of ceramic material Download PDFInfo
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- CN109231989A CN109231989A CN201811294438.XA CN201811294438A CN109231989A CN 109231989 A CN109231989 A CN 109231989A CN 201811294438 A CN201811294438 A CN 201811294438A CN 109231989 A CN109231989 A CN 109231989A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped 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
- C04B35/56—Shaped 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
- C04B35/5607—Shaped 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
- C04B35/5611—Shaped 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
- C04B35/5618—Shaped 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
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Abstract
The present invention relates to a kind of alloy with high activity intercalation Ti3AlMC2The preparation method of ceramic material, with TiH2, AlM alloy, TiC be raw material, synthesize Ti under high-temperature and high-pressure conditions3AlMC2Ceramic material, any one of the AlM alloy in AlLi alloy, AlNa alloy and AlK alloy.Alloy with high activity intercalation Ti of the invention3AlMC2The preparation method novel formula of ceramic material, simple process, time-consuming is few, obtained Ti3AlMC2Ceramic material purity is high, impurity are few, and Product Activity is high, can react with low concentration acid, also it can be reacted with alkali, this greatly reduces ceramic material subsequent processing difficulty, and greatly improve the application range of ceramic material, make it have very high application value.
Description
Technical field
The present invention relates to field of ceramic material preparation, more particularly to a kind of alloy with high activity intercalation Ti3AlMC2Ceramic material
The preparation method of material.
Background technique
Ceramic material has many advantages, such as that fusing point is high, anti-oxidant, corrosion-resistant, has in fields such as the energy, metallurgy, machinery, chemical industry
Wide application prospect.The disadvantages of high, fracture toughness is low, processing difficulties but ceramic material also enbrittles simultaneously.How
The performance for improving ceramic material, increases operation rate, is a problem to be solved.Currently, a kind of novel three with layer structure
First ceramics Mn+1AXnMaterial causes the extensive concern of people.Wherein, M is transiting group metal elements, and A is III or IV race's element, X
It is C or N, n=1,2 or 3.And most representative is Ti3AlC2Ceramic material.
Ternary layered ceramic Ti3AlC2Integrate the excellent performance of metal and ceramics, high temperature resistant, elasticity modulus is high, in height
Temperature is lower to have good plasticity, is the ideal candidates material of high-temperature engine, heat exchanger.Meanwhile Ti3AlC2Resistance to thermal shock has
Good conductive, thermal conductivity, easy processing, and have good self-lubricating property, but also as the conductive component of high-speed slide contact,
Alternating current generator brush etc..In addition, Ti3AlC2Ceramic material also has good machining property, inoxidizability and corrosion resistance,
Blender bearing etc. suitable for chemical reaction kettle.
Zhu Li is intelligent et al. using traditional Ti, Al, C simple substance as raw material, is prepared for mechanical alloying plus annealing
Ti3AlC2Powder body material, but the Ti of inventive method preparation3AlC2In material, TiC content is higher, and the very low (China of activity
Patent CN200510110176.3), limit the application range of product.Guo Jun is bright et al. to use self-propagating high-temperature synthesis
(SHS), using Ti, Al, C as raw material, Ti is synthetically prepared by 3:1:2 molar ratio3AlC2Powder body material, but this method preparation condition
Harsher, product purity is not high enough, and activity is very low, is difficult to be post-processed (Chinese patent CN200910094336.8).King
Sweet smell et al. prepares Ti using the method for mechanical alloying and vacuum thermal sintering3AlC2Ceramic powder, but this method preparation
Ti3AlC2Middle TiC impurity phase is more, and purity is not high, and the activity (Chinese patent not shown
CN201310497696.9).In short, Ti3AlC2Preparation method there are many kinds of, but most methods hardly result in purity compared with
High Ti3AlC2Material, often with some impurity phases in product, such as TiC, Ti3AlC etc. affects the performance of material;This
Outside, it is often more important that, the lytic activity that traditional raw material is formulated is relatively low, hardly reacted with low concentration acid or alkali, after
Continuous application is undesirable, is difficult to meet application demand.
Summary of the invention
Based on this, it is necessary to be directed to current Ti3AlC2Preparation process in the impurity that occurs is more, lytic activity is more low
Problem provides a kind of alloy with high activity intercalation Ti3AlMC2The preparation method of ceramic material.
A kind of alloy with high activity intercalation Ti3AlMC2The preparation method of ceramic material, with TiH2Powder, AlM alloyed powder, TiC powder
For raw material, Ti is synthesized under high-temperature and high-pressure conditions3AlMC2Ceramic material, the AlM alloy be selected from AlLi alloy, AlNa alloy,
With any one in AlK alloy.
Above-mentioned alloy with high activity intercalation Ti3AlMC2The preparation method of ceramic material, novel formula, simple process are time-consuming
It is few.Obtained Ti3AlMC2Ceramic material purity is high, impurity are few, and Product Activity is high, has a good application prospect.
The TiH in one of the embodiments,2, AlM alloy, TiC molar ratio be 1:(1~2): (1.5~2).
In one of the embodiments, the AlM alloy the preparation method comprises the following steps: by aluminum shot and lithium grain/sodium grain/potassium grain
Any one is mixed according to the molar ratio of 1:1, is then used arc-melting furnace melt back under the electric current of 100~200A, is obtained
AlM alloy.
Ti is synthesized under high-temperature and high-pressure conditions in one of the embodiments,3AlMC2By the TiH before ceramic material2Powder,
AlM alloyed powder, TiC powder carry out ball-milling treatment.
The ratio of grinding media to material of the ball-milling treatment is 10:1 in one of the embodiments, and rotational speed of ball-mill is 400~600r/
Min, Ball-milling Time are 4~8h.
It is described in one of the embodiments, to synthesize alloy intercalation Ti at high temperature under high pressure3AlMC2The condition of ceramic material
Are as follows: 10~30min is kept the temperature at 3~4GPa of pressure, 1250~1400 DEG C of temperature to get Ti3AlMC2Ceramic material.
After the completion of keeping the temperature in one of the embodiments, cooling 10min, then slow release, obtains Ti3AlMC2Ceramics
Material.
Above-mentioned alloy with high activity intercalation Ti3AlMC2Ceramic material, due in high temperature and pressure synthesis process, TiH2Deviate from hydrogen
Gas generates stomata, and material is made to generate a large amount of vacancy defects.Importantly, due to the special adsorption of AlM reactive alloys, so that
The Ti arrived3AlMC2With very high activity, it can react, can also be reacted with alkali, this greatly reduces after ceramic material with acid
Continuous processing difficulty, and the application range of ceramic material is greatly improved, make it have very high application value.
Detailed description of the invention
Fig. 1 is the Ti that the embodiment of the present invention 1 obtains3AlLiC2The scanning electron microscope (SEM) photograph of ceramic material;
Fig. 2 is the Ti that the embodiment of the present invention 2 obtains3AlNaC2The scanning electron microscope (SEM) photograph of ceramic material;
Fig. 3 is the Ti that the embodiment of the present invention 3 obtains3AlKC2The scanning electron microscope (SEM) photograph of ceramic material;
Fig. 4 is the Ti that the embodiment of the present invention 1 obtains3AlLiC2Ceramic material passes through 5wt.% hydrofluoric acid treatment, obtains product
Scanning electron microscope (SEM) photograph;
Fig. 5 is the Ti that the embodiment of the present invention 1 obtains3AlLiC2Ceramic material passes through 10wt.% naoh treatment, obtains
The scanning electron microscope (SEM) photograph of product.
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, with reference to the accompanying drawing to the present invention
Specific embodiment be described in detail.Many details are explained in the following description in order to fully understand this hair
It is bright.But the invention can be embodied in many other ways as described herein, those skilled in the art can be not
Similar improvement is done in the case where violating intension of the present invention, therefore the present invention is not limited by the specific embodiments disclosed below.
It is of the invention the preparation method is as follows:
(1) any one in high-purity aluminum shot and lithium grain/sodium grain/potassium grain is mixed according to the molar ratio of 1:1, then electricity consumption
The melt back under the electric current of 100~200A of arc smelting furnace obtains AlM alloy, spare after pulverizing;
(2) by high-purity Ti H2Powder, AlM alloyed powder, TiC powder press 1:(1~2): the molar ratio weighing ingredient of (1.5~2), so
Ratio of grinding media to material 10:1 4~8h of high-energy ball milling under the revolving speed of 400~600r/min is pressed afterwards;
(3) mixed material after ball milling is pressed into the cylindrical body of diameter 10mm, high 15mm in advance at 50MPa, uses cubic apparatus
Press keeps the temperature 10~30min under the conditions of 3~4GPa, 1250~1400 DEG C and carries out high-pressure synthesis;
(4) after the completion of keeping the temperature, cooling 10min, then slow release obtains the alloy with high activity intercalation of high-purity
Ti3AlMC2Ceramic material.
The invention has the following advantages over the prior art:
1, alloy with high activity intercalation Ti of the invention3AlMC2The preparation method simple process of ceramic material, time-consuming few, gained
Product purity is high, impurity is few;
2, alloy with high activity intercalation Ti of the invention3AlMC2The preparation method of ceramic material is due to the M metal in AlM alloy
Fusing point is low, volatile, plays the role of activation, intercalation, so that the material of synthesis has very high activity, keeps it anti-with acid
It answers, can also be reacted with alkali;
3, alloy with high activity intercalation Ti of the invention3AlMC2The preparation method of ceramic material is due to high temperature and pressure synthesis process
In, TiH2Deviate from hydrogen, generate stomata, material is made to generate a large amount of vacancy defects, performance is good.
Embodiment 1
High purity lithium grain 7g, aluminum shot 27g are weighed, then under an argon atmosphere with arc-melting furnace, with 100A electric current melting 4
It is secondary, AlLi alloy is obtained after cooling, and pulverize;By high-purity Ti H2Powder, AlLi alloyed powder, TiC powder TiH in molar ratio2:
AlLi:TiC=1:1:2 is weighed, i.e. TiH2Powder 5g, AlLi powder 3.4g, TiC powder 12g, is then weighed firmly by ratio of grinding media to material 10:1
Matter alloying pellet 204g, will be filled with argon gas in ball grinder, the high-energy ball milling 4h under 400rpm revolving speed;By the good material of ball milling in 50MPa
It is pressed into the cylindrical body of diameter 10mm, high 15mm in advance down, keeps the temperature 10min under the conditions of 3GPa, 1250 DEG C with cubic hinge press and carry out
High-pressure synthesis;After the completion of heat preservation, cooling 10min, then slow release obtains the high activity AlLi intercalation Ti of high-purity3AlLiC2
Ceramic material.
Embodiment 2
High pure sodium grain 23g, aluminum shot 27g are weighed, then under an argon atmosphere with arc-melting furnace, with 150A electric current melting 4
It is secondary, AlNa alloy is obtained after cooling, and pulverize;By high-purity Ti H2Powder, AlNa alloyed powder, TiC powder TiH in molar ratio2:
AlNa:TiC=1:1.5:2 is weighed, i.e. TiH2Then powder 5g, AlNa alloyed powder 7.5g, TiC powder 12g presses ratio of grinding media to material 10:1
Sintered carbide ball 245g is weighed, argon gas will be filled in ball grinder, the high-energy ball milling 6h under 500rpm revolving speed;The good material of ball milling is existed
The cylindrical body of diameter 10mm, high 15mm are pressed under 50MPa in advance, is kept the temperature under the conditions of 3.5GPa, 1350 DEG C with cubic hinge press
20min carries out high-pressure synthesis;After the completion of heat preservation, 10min, then slow release are cooled down, the high activity AlNa for obtaining high-purity is inserted
Layer Ti3AlNaC2Ceramic material.
Embodiment 3
High-purity potassium grain 39g, aluminum shot 27g are weighed, then under an argon atmosphere with arc-melting furnace, with 200A electric current melting 4
It is secondary, AlK alloy is obtained after cooling, and pulverize;By high-purity Ti H2Powder, AlK alloyed powder, TiC powder TiH in molar ratio2:AlK:
TiC=1:1.5:1.5 is weighed, i.e. TiH2Powder 5g, AlK alloyed powder 9.9g, iC powder 9g, is then weighed firmly by ratio of grinding media to material 10:1
Matter alloying pellet 239g, will be filled with argon gas in ball grinder, the high-energy ball milling 8h under 600rpm revolving speed;By the good material of ball milling in 50MPa
It is pressed into the cylindrical body of diameter 10mm, high 15mm in advance down, keeps the temperature 30min under the conditions of 4GPa, 1400 DEG C with cubic hinge press and carry out
High-pressure synthesis;After the completion of heat preservation, cooling 10min, then slow release obtains the high activity AlK intercalation Ti of high-purity3AlKC2Pottery
Ceramic material.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (6)
1. a kind of alloy with high activity intercalation Ti3AlMC2The preparation method of ceramic material, which is characterized in that with TiH2Powder, AlM alloy
Powder, TiC powder are raw material, synthesize Ti under high-temperature and high-pressure conditions3AlMC2Ceramic material, the AlM alloy be selected from AlLi alloy,
Any one in AlNa alloy and AlK alloy.
2. alloy with high activity intercalation Ti according to claim 13AlMC2The preparation method of ceramic material, which is characterized in that
The TiH2, AlM alloy, TiC molar ratio be 1:(1~2): (1.5~2).
3. alloy with high activity intercalation Ti according to claim 13AlMC2The preparation method of ceramic material, which is characterized in that
The AlM alloy the preparation method comprises the following steps: any one in aluminum shot and lithium grain/sodium grain/potassium grain is mixed according to the molar ratio of 1:1
It closes, then uses arc-melting furnace melt back under the electric current of 100~200A, obtain AlM alloy.
4. alloy with high activity intercalation Ti according to claim 13AlMC2The preparation method of ceramic material, which is characterized in that
Ti is synthesized under high-temperature and high-pressure conditions3AlMC2By the TiH before ceramic material2Powder, AlM alloyed powder, TiC powder carry out at ball milling
Reason.
5. alloy with high activity intercalation Ti according to claim 43AlMC2The preparation method of ceramic material, which is characterized in that
The ratio of grinding media to material of the ball-milling treatment is 10:1, and rotational speed of ball-mill is 400~600r/min, and Ball-milling Time is 4~8h.
6. alloy with high activity intercalation Ti according to claim 13AlMC2The preparation method of ceramic material, which is characterized in that
It is described to synthesize Ti at high temperature under high pressure3AlMC2The condition of ceramic material are as follows: at 3~4GPa of pressure, 1250~1400 DEG C of temperature
10~30min is kept the temperature to get Ti3AlMC2Ceramic material.
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Application publication date: 20190118 |