CN103757453A - Ti3AlC2-Ti2AlC/TiAl-based composite material and preparation method thereof - Google Patents

Ti3AlC2-Ti2AlC/TiAl-based composite material and preparation method thereof Download PDF

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CN103757453A
CN103757453A CN201310711330.7A CN201310711330A CN103757453A CN 103757453 A CN103757453 A CN 103757453A CN 201310711330 A CN201310711330 A CN 201310711330A CN 103757453 A CN103757453 A CN 103757453A
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tial
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CN103757453B (en
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艾桃桃
冯小明
阮苗苗
徐峰
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Shaanxi University of Technology
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Abstract

The invention discloses a Ti3AlC2-Ti2AlC/TiAl-based composite material and a preparation method thereof. The preparation method comprises the steps of: carrying out uniform ball milling on Ti powder, Al powder and Ti3AlC2 powder, then, carrying out cold press molding; and finally, carrying out vacuum hot pressed sintering at the temperature of 850-950 DEG C to obtain the Ti3AlC2-Ti2AlC/TiAl-based composite material. The material comprises matrix phases TiAl and Ti3Al and reinforced phases Ti3AlC2 and Ti2AlC and contains no impurity phase TiC. According to the invention, the matrix phases are obtained through the in-situ exothermic reaction between Ti and Al, and the reinforced phase Ti2AlC is obtained through the self-decomposition reaction of part of the Ti3AlC2; the preparation method is simple in process, strong in controllability, low in sintering temperature and low in preparation cost; the Ti3AlC2-Ti2AlC/TiAl-based composite material is high in purity, low in impurity content and remarkable in strengthening and toughening effects and has the maximum bending strength of 316MPa and the maximum fracture toughness of 7.28MPa.ml/2.

Description

A kind of Ti 3alC 2-Ti 2alC/TiAl based composites and preparation method thereof
Technical field
The invention belongs to Materials Science and Engineering field, be specifically related to a kind of Ti 3alC 2-Ti 2alC/TiAl based composites and preparation method thereof.
Background technology
Research, Application and Development and the Aeronautics and Astronautics industrial expansion of high-temperature structural material are closely bound up, be also 21 century spacecraft propulsion system realize the key factor of revolutionary change and development.For aircraft engine, improving working temperature is two major measure improving the performance of available engine, study high thrust-weight ratio new work engine with the weight that alleviates engine parts.Therefore, the selection of aerospace device engine should possess " gentlier, more just, stronger and more heat-resisting " four specific characters.
Intermetallic compound, due to the long-range order arrangement of its atom and coexisting of interatomic metallic bond and covalent linkage, makes it may take into account the plasticity of metal and ceramic hot strength simultaneously.There is the performances such as the unexistent high specific tenacity of common metal and alloy, specific rigidity, specific modulus and good resistance to high temperature oxidation, creep resistance and anti-hydrogen embrittlement.Integrated performance index is better than cobalt-based, the superalloy such as Ni-based, and toughness is again higher than common pottery, be expected to, for the high temperature resistant component of the aerospace such as jet engine and turbine, automotive industry and the wing of super speed vehicle, housing etc., be considered to have the lightening fire resistant structured material of new generation of application potential.Especially TiAl intermetallic compound, being applied to aerospace and motor car engine will improve engine operation efficiency by Structure weight reduce, have important promoting technology effect.
But TiAl intermetallic compound exists several key scientific problems urgently to be resolved hurrily: (1) intrinsic fragility, processing performance is poor, is difficult to moulding; (2) high-temperature oxidation resistance deficiency, when its use temperature is during higher than 800 ℃, its antioxidant property reduces rapidly, has seriously hindered its application process.Research shows, Composite is to overcome TiAl intermetallic compound performance deficiency, improve high-temperature behavior and promote its most effective practical approach.With ceramic phase, strengthen TiAl base intermetallic compound and have isotropic character, wild phase preparation technology is simple and convenient in addition, secondary processing simple, relative low price, thereby has larger application prospect.But most of ceramic enhancement phase are as SiC, Al 2o 3, TiC, TiB 2belong to fragility phase, can make prepared TiAl base intermetallic compound become more crisp.The ternary layered compound M of one class n+1aX n(M represents transition metal, and A represents III or IV main group, and X is C or N, is called for short MAX), has metal and ceramic dual excellent properties concurrently, has been subject to extensive concern.Typical Representative has Ti 2alC and Ti 3alC 2, the thermal expansivity of they and TiAl intermetallic compound approaches, and is considered to the optimal wild phase of TiAl intermetallic compound.Yunlong, University Of Ji'nan high mountain (Yue Yunlong etc., Ti 2the refinement of AlC/TiAl matrix material heat-treated sturcture, Rare Metals Materials and engineering, 2007,36(2): 189-193) first take Ti powder, Al powder, Nb powder, B powder as raw material, adopt thermal explosion reaction to synthesize Ti-47.66Al-2.22Nb and Ti-47.66-2.22Nb-1.34B powdered alloy, then powdered alloy is mixed with TiC, adopt discharge plasma sintering technique to make Ti 2alC/TiAl matrix material, and it is carried out to multistep thermal treatment, thermal treatment temp reaches 1390 ℃.Northwestern Polytechnical University once reached the clouds (once reach the clouds etc., spontaneous Ti 2the tissue of AlC/TiAl matrix material and reaction process, Rare Metals Materials and engineering,, 42(4 in 2013): 785-788) adopt the method for the synthetic and vacuum arc melting of self-propagating combustion, with carbon fiber (C f), titanium valve and aluminium powder be raw material, synthesized Ti 2alC/TiAl matrix material.Wuhan University of Technology plum is bright, and just (plum is bright elementary, and discharge plasma sintering is prepared dense TiAl/Ti 2alC matrix material, Materials Science and Engineering journal,, 21(3 in 2003): 356-359) take Ti/Al/TiC as raw material, adopt discharge plasma sintering process to prepare dense TiAl/Ti 2alC matrix material, when sintering temperature is 900 ℃, Ti 2alC starts to occur, but contains a large amount of TiC dephasigns; When sintering temperature is 1150 ℃, matrix material is by TiAl, Ti 3al and Ti 2alC composition, and carried out subsequent heat treatment technique.(Wang Fen etc., original position is synthesized Ti to the Wang Fen of Shaanxi Tech Univ 2the microstructure of AlC/TiAl matrix material and performance, Special Processes of Metal Castings and non-ferrous alloy,, 28 (2): 145-147 in 2008) to adopt simple substance Ti powder, Al powder, C powder be raw material, adopts in-situ hot pressing technology to prepare Ti in 1200 ℃ 2alC/TiAl matrix material.Aforesaid method mainly generates Ti by the chemosynthesis reaction between each component in raw material 2alC, and much technique usually needs the operations such as follow-up high-temperature heat treatment, and the cycle is long, complex process, equipment requirements is high, high (1100 ℃ of the > of sintering temperature, if the low TiC impurity phase that has of temperature exists), generate required energy consumption large, increased preparation cost.
Summary of the invention
The object of the present invention is to provide a kind of Ti 3alC 2-Ti 2alC/TiAl based composites and preparation method thereof, the method sintering temperature is low, the Ti making 3alC 2-Ti 2alC/TiAl based composites has Double substrate micro phase (TiAl+Ti 3al) and two wild phase (Ti 3alC 2+ Ti 2alC).
In order to achieve the above object, the technical solution used in the present invention is:
A kind of Ti 3alC 2-Ti 2the preparation method of AlC/TiAl based composites, comprises the following steps:
Step 1, by massfraction, by 55.91%～65.78% Ti powder, 29.09～34.22% Al powder and 5～15% Ti 3alC 2powder packs in ball grinder, and take dehydrated alcohol as ball-milling medium, under the rotating speed of 500～750 revs/min, ball milling 1～2 hour, obtains mixed powder;
Step 2, pack in mould after will mixed powder drying, coldmoulding under the forming pressure of 3～5MPa, then pack into and in vacuum hotpressing stove, carry out vacuum heating-press sintering, with the temperature rise rates of 5～10 ℃/min, from room temperature, be warming up to the sintering temperature of 850～950 ℃, be incubated 1～2 hour under sintering temperature after, with stove naturally cooling, obtain Ti 3alC 2-Ti 2alC/TiAl based composites.
Described Ti 3alC 2ti in powder 3alC 2massfraction is that 92～99.42%, TiC massfraction is 0.58～8%.
Described Ti 3alC 2the preparation method of powder is: by massfraction, 23.94～25.38% Ti powder, 13.87～16.19% Al and 59.87～61.53% TiC powder are packed in ball grinder, add dehydrated alcohol as ball-milling medium, under the rotating speed of 500～750 revs/min, ball milling obtains powder for 1～2 hour, after being dried, powder packs in crucible, carry out vacuum non-pressure sintering, temperature rise rate with 5～10 ℃/min rises to 1300～1400 ℃ from room temperature, then be incubated 1～2 hour, with stove, naturally cool to room temperature again, obtain Ti 3alC 2powder.
Described Ti 3alC 2ratio of grinding media to material in the preparation process of powder during ball milling is (5～7): 1, and adopt Stainless Steel Ball as abrading-ball; Described ball grinder is stainless steel jar mill; The bake out temperature of described powder is 30～50 ℃; Described crucible is corundum crucible.
Ratio of grinding media to material in described step 1 during ball milling is (5～7): 1, and adopt Stainless Steel Ball as abrading-ball, described ball grinder is stainless steel jar mill.
In described step 2, the bake out temperature of mixed powder is 30～50 ℃; Mould in described step 2 is graphite jig.
Vacuum heating-press sintering process in described step 2 takes sectional type to exert pressure, when being raised to 200～300 ℃, temperature opens pressurizing device, regulate pressure to 6～8MPa, maintain that pressure is constant until temperature reaches 550～750 ℃, during 15～30 ℃ of every risings of temperature afterwards, increase pressure 1.5～2MPa, when temperature reaches sintering temperature, regulate pressure to being 20～40MPa to the maximum, and it is constant in insulating process, to maintain pressure.
Described Ti 3alC 2-Ti 2the Ti that the low temperature preparation method of AlC/TiAl based composites makes 3alC 2-Ti 2alC/TiAl based composites, by massfraction, it is comprised of 85～95% matrix phases and 5～15% wild phase two portions, phase free from foreign meter, wherein matrix phase is TiAl and Ti 3al, wild phase is Ti 2alC and Ti 3alC 2.
Described wild phase Ti 2alC is mainly by Ti in raw material 3alC 2part Ti in powder 3alC 2in preparation process, decompose and obtain, simultaneously Ti in raw material 3alC 2tiC in powder reacts and also forms wild phase Ti with matrix phase TiAl 2alC.
Its flexural strength is 148～316MP a, fracture toughness property is 3.88～7.28MPam 1/2.
With respect to prior art, beneficial effect of the present invention is:
The invention provides a kind of Ti 3alC 2-Ti 2the low temperature preparation method of AlC/TiAl based composites, by Ti powder, Al powder and Ti 3alC 2after powder ball milling is even, first carries out coldmoulding, then carry out vacuum heating-press sintering, obtain Ti 3alC 2-Ti 2alC/TiAl based composites.The method utilizes the original position thermopositive reaction between Ti-Al to form matrix phase TiAl and Ti 3al, and make full use of the amount of heat that the original position thermopositive reaction between Ti-Al system discharges, by modulation process, make part Ti simultaneously 3alC 2generation self-decomposition reaction, obtains wild phase Ti 2alC, and undecomposed Ti 3alC 2form wild phase Ti 3alC 2thereby, form Ti 2alC and Ti 3alC 2two kinds of states that wild phase coexists, self-decomposition reaction method and reaction in－situ hot-pressing technique that the present invention adopts, technique is simple, sintering temperature is low (850～950 ℃), process controllability is strong, preparation cost is low, prepare and have Double substrate micro phase (TiAl+Ti 3al) and two wild phase (Ti 3alC 2+ Ti 2alC) Ti 3alC 2-Ti 2alC/TiAl based composites, this matrix material purity is high, foreign matter content is low, highly malleablized successful, has overcome that the cost that prior art exists when preparing particle-reinforced TiAl-based composite material is high, complex process, sintering temperature is high, wild phase is single and the problem such as skewness.
The Ti that the present invention makes 3alC 2-Ti 2alC/TiAl based composites is comprised of 85～95% matrix phases and 5～15% wild phase two portions, phase TiC free from foreign meter, and wherein matrix phase is TiAl and Ti 3al, wild phase is Ti 2alC and Ti 3alC 2.This Ti 3alC 2-Ti 2that AlC/TiAl based composites has is high-strength, high tenacity, high temperature resistant, the feature such as can process, and its maximum deflection intensity can reach 316MPa, maximum fracture toughness property can reach 7.28MPam 1/2, can expand the range of application of TiAl base intermetallic compound.
Further, the raw material Ti that the present invention adopts 3alC 2ti in powder 3alC 2massfraction is that 92～99.42%, TiC massfraction is 0.58～8%, contains a small amount of impurity TiC, but at Ti 3alC 2-Ti 2in the preparation process of AlC/TiAl based composites, TiC impurity phase can generate wild phase Ti with matrix phase TiAl reaction 2alC, the Ti therefore finally preparing 3alC 2-Ti 2phase TiC free from foreign meter in AlC/TiAl based composites, has reached the effect of material from purifying.
Accompanying drawing explanation
Fig. 1 is the Ti of preparation 3alC 2the XRD figure of powder.
Fig. 2 is Ti prepared by the present invention 3alC 2-Ti 2the XRD figure of AlC/TiAl based composites, wherein (a) do not add Ti 3alC 2time the sintering powder prepared XRD figure, (b)～(d) be respectively the Ti of embodiment 1～3 preparation 3alC 2-Ti 2the XRD figure of AlC/TiAl based composites.
Fig. 3 is Ti prepared by the present invention 3alC 2-Ti 2the fracture SEM figure of AlC/TiAl based composites, wherein (a) do not add Ti 3alC 2time the sintering powder prepared fracture SEM figure, (b)～(d) be respectively the Ti of embodiment 1～3 preparation 3alC 2-Ti 2the fracture SEM figure of AlC/TiAl based composites.
Fig. 4 is Ti prepared by the present invention 3alC 2-Ti 2the bending strength of AlC/TiAl based composites and Fracture Toughness.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.
The invention provides Ti 3alC 2-Ti 2the low temperature preparation method of AlC/TiAl based composites is at preparation Ti 3alC 2-Ti 2building-up reactions and decomposition reaction have mainly occurred in the process of AlC/TiAl based composites, and concrete reaction is as follows:
Ti+Al → TiAl(building-up reactions)
3Ti+Al → Ti 3al(building-up reactions)
Ti 3alC 2→ Ti 2alC+TiC(decomposition reaction)
TiC+TiAl → Ti 2alC(building-up reactions)
Embodiment 1
Step 1, by massfraction, by 23.94% Ti powder, 16.19% Al and 59.87% TiC powder pack in stainless steel jar mill, add 400mL dehydrated alcohol as ball-milling medium, Stainless Steel Ball is as abrading-ball, drum's speed of rotation is 750 revs/min, ratio of grinding media to material is 7:1, ball milling obtains uniform powder and is dried after 2 hours, bake out temperature is 50 ℃, then dried mixed powder is packed in corundum crucible, carry out vacuum non-pressure sintering, temperature rise rate with 10 ℃/min rises to sintering temperature from room temperature, sintering temperature is 1350 ℃, 1350 ℃ of insulations 2 hours, then with stove, naturally cool to room temperature, obtain Ti 3alC 2powder.
Step 2, by massfraction, Ti prepared by the step 1 of 62.49% Ti powder, 32.51% Al powder and 5% 3alC 2powder packs in stainless steel jar mill, carries out ball milling on planetary ball mill, and adding 200mL dehydrated alcohol is ball-milling medium, and Stainless Steel Ball is abrading-ball, and ratio of grinding media to material is 7:1, and under the rotating speed of 750 revs/min, ball milling 2 hours, obtains mixed powder;
Step 3, mixed powder is packed in graphite jig after 50 ℃ of oven dry, under the forming pressure of 5MPa, be cold-pressed into pie, then pack into and in vacuum hotpressing stove, carry out vacuum heating-press sintering, with the temperature rise rates of 10 ℃/min, from room temperature, start to heat up, when being raised to 200 ℃, temperature opens pressurizing device, regulate pressure to 6MPa, maintain that pressure is constant until temperature reaches 600 ℃, during 25 ℃ of every risings of temperature afterwards, increase pressure 2MPa, when temperature reaches 900 ℃ of sintering temperatures, regulate pressure to being 30MPa to the maximum, maintain pressure constant, be incubated 2 hours under sintering temperature after with stove naturally cooling, obtain Ti 3alC 2-Ti 2alC/TiAl based composites.
Fig. 1 is Ti prepared by the present embodiment step 1 3alC 2the XRD figure of powder, as can be seen from Figure, this Ti 3alC 2ti in powder 3alC 2purity is very high, Ti 3alC 2content is about 99.42wt%, also contains a small amount of TiC, and its content is about 0.58wt%.The Ti that Fig. 2 (b) is prepared for the present embodiment 3alC 2-Ti 2alC/TiAl based composites (Ti 3alC 2doping is 5wt%) XRD figure, can find out, in this material except containing matrix phase TiAl and Ti 3outside Al, also contain Ti 2alC and Ti 3alC 2wild phase, illustrates Ti 3alC 2be decomposed into Ti 2alC, shows that this material matrix is TiAl and Ti mutually 3al, wild phase is Ti 2alC and Ti 3alC 2.With reference to Fig. 4, the flexural strength that adopts three-point bending method to measure material is 316MPa, and the fracture toughness property that adopts three-point bending single notched beam method (SENB) to measure material is 7.28MPam 1/2.
Embodiment 2
Step 1, by massfraction, by 23.94% Ti powder, 16.19% Al and 59.87% TiC powder pack in stainless steel jar mill, add 400mL dehydrated alcohol as ball-milling medium, Stainless Steel Ball is as abrading-ball, drum's speed of rotation is 750 revs/min, ratio of grinding media to material is 7:1, ball milling obtains uniform powder and is dried after 2 hours, bake out temperature is 50 ℃, then dried mixed powder is packed in corundum crucible, carry out vacuum non-pressure sintering, temperature rise rate with 10 ℃/min rises to sintering temperature from room temperature, sintering temperature is 1350 ℃, 1350 ℃ of insulations 2 hours, then with stove, naturally cool to room temperature, obtain Ti 3alC 2powder.
Step 2, by massfraction, Ti prepared by the step 1 of 59.2% Ti powder, 30.8% Al powder and 10% 3alC 2powder packs in stainless steel jar mill, carries out ball milling on planetary ball mill, and adding 200mL dehydrated alcohol is ball-milling medium, and Stainless Steel Ball is abrading-ball, and ratio of grinding media to material is 7:1, and under the rotating speed of 750 revs/min, ball milling 2 hours, obtains mixed powder;
Step 3, mixed powder is packed in graphite jig after 50 ℃ of oven dry, under the forming pressure of 5MPa, be cold-pressed into pie, then pack into and in vacuum hotpressing stove, carry out vacuum heating-press sintering, with the temperature rise rates of 10 ℃/min, from room temperature, start to heat up, when being raised to 200 ℃, temperature opens pressurizing device, regulate pressure to 6MPa, maintain that pressure is constant until temperature reaches 600 ℃, during 25 ℃ of every risings of temperature afterwards, increase pressure 2MPa, when temperature reaches 900 ℃ of sintering temperatures, regulate pressure to being 30MPa to the maximum, maintain pressure constant, be incubated 2 hours under sintering temperature after with stove naturally cooling, obtain Ti 3alC 2-Ti 2alC/TiAl based composites.
The Ti that Fig. 2 (c) is prepared for the present embodiment 3alC 2-Ti 2alC/TiAl based composites (Ti 3alC 2doping is 10wt%) XRD figure, can find out, in this material except containing matrix phase TiAl and Ti 3outside Al, also contain Ti 2alC and Ti 3alC 2wild phase, illustrates Ti 3alC 2be decomposed into Ti 2alC, shows that this material matrix is TiAl and Ti mutually 3al, wild phase is Ti 2alC and Ti 3alC 2.With reference to Fig. 4, the flexural strength that adopts three-point bending method to measure material is 267MPa, and the fracture toughness property that adopts three-point bending single notched beam method (SENB) to measure material is 5.54MPam 1/2.
Embodiment 3
Step 1, by massfraction, by 23.94% Ti powder, 16.19% Al and 59.87% TiC powder pack in stainless steel jar mill, add 400mL dehydrated alcohol as ball-milling medium, Stainless Steel Ball is as abrading-ball, drum's speed of rotation is 750 revs/min, ratio of grinding media to material is 7:1, ball milling obtains uniform powder and is dried after 2 hours, bake out temperature is 50 ℃, then dried mixed powder is packed in corundum crucible, carry out vacuum non-pressure sintering, temperature rise rate with 10 ℃/min rises to sintering temperature from room temperature, sintering temperature is 1350 ℃, 1350 ℃ of insulations 2 hours, then with stove, naturally cool to room temperature, obtain Ti 3alC 2powder.
Step 2, by massfraction, Ti prepared by the step 1 of 55.91% Ti powder, 29.09% Al powder and 15% 3alC 2powder packs in stainless steel jar mill, carries out ball milling on planetary ball mill, and adding 200mL dehydrated alcohol is ball-milling medium, and Stainless Steel Ball is abrading-ball, and ratio of grinding media to material is 7:1, and under the rotating speed of 750 revs/min, ball milling 2 hours, obtains mixed powder;
Step 3, mixed powder is packed in graphite jig after 50 ℃ of oven dry, under the forming pressure of 5MPa, be cold-pressed into pie, then pack into and in vacuum hotpressing stove, carry out vacuum heating-press sintering, with the temperature rise rates of 10 ℃/min, from room temperature, start to heat up, when being raised to 200 ℃, temperature opens pressurizing device, regulate pressure to 6MPa, maintain that pressure is constant until temperature reaches 600 ℃, during 25 ℃ of every risings of temperature afterwards, increase pressure 2MPa, when temperature reaches 900 ℃ of sintering temperatures, regulate pressure to being 30MPa to the maximum, maintain pressure constant, be incubated 2 hours under sintering temperature after with stove naturally cooling, obtain Ti 3alC 2-Ti 2alC/TiAl based composites.
The Ti that Fig. 2 (d) is prepared for the present embodiment 3alC 2-Ti 2alC/TiAl based composites (Ti 3alC 2doping is 15wt%) XRD figure, can find out, in this material except containing matrix phase TiAl and Ti 3outside Al, also contain Ti 2alC and Ti 3alC 2wild phase, illustrates Ti 3alC 2be decomposed into Ti 2alC, shows that this material matrix is TiAl and Ti mutually 3al, wild phase is Ti 2alC and Ti 3alC 2.With reference to Fig. 4, the flexural strength that adopts three-point bending method to measure material is 148MPa, and the fracture toughness property that adopts three-point bending single notched beam method (SENB) to measure material is 3.88MPam 1/2.
Fig. 2 is Ti prepared by the present invention 3alC 2-Ti 2the XRD analysis result of AlC/TiAl based composites, wherein: be (a) that the massfraction of Ti powder in raw material is that the massfraction of 65.78%, Al powder is 34.22%, do not add Ti 3alC 2, through the XRD analysis result of 900 ℃ of sintered heat insulatings prepared material after 2 hours, as seen from the figure, in this material, only contain TiAl and Ti 3al; (b)～(d) be respectively the Ti of embodiment 1～3 preparation 3alC 2-Ti 2the XRD figure of AlC/TiAl based composites, as seen from the figure, removes and contains matrix phase TiAl and Ti in material 3outside Al, also contain Ti 2alC and Ti 3alC 2wild phase, illustrates Ti 3alC 2be decomposed into Ti 2alC; And along with Ti 3alC 2the increase of doping, Ti 3alC 2-Ti 2ti in AlC/TiAl based composites 2alC content is also increasing gradually.
Fig. 3 is Ti prepared by the present invention 3alC 2-Ti 2the fracture SEM figure of AlC/TiAl based composites, is (a) that the massfraction of Ti powder in raw material is that the massfraction of 65.78%, Al powder is 34.22%, does not add Ti 3alC 2, through the fracture SEM photo of 900 ℃ of sintered heat insulatings prepared material after 2 hours, can find out that this material has formed thick stratiform matrix; (b) be Ti prepared by embodiment 1 3alC 2-Ti 2the fracture SEM photo of AlC/TiAl based composites, has formed sheet tissue, and wild phase is mainly distributed in crystal boundary, and matrix grain diminishes, compact structure; (c) be Ti prepared by embodiment 2 3alC 2-Ti 2the fracture SEM photo of AlC/TiAl based composites, can find out that it has formed sheet tissue, and wild phase is distributed in crystal boundary, and with the increase of wild phase content, matrix grain diminishes gradually; (d) be Ti prepared by embodiment 3 3alC 2-Ti 2the fracture SEM photo of AlC/TiAl based composites, can find out that its weave construction is loose.
Fig. 4 is Ti prepared by the present invention 3alC 2-Ti 2the flexural strength of AlC/TiAl based composites and Fracture Toughness.As seen from Figure 4, at Ti 3alC 2when doping is 5wt%, its fracture toughness property reaches maximum value (7.28MPam 1/2), higher than unadulterated Ti 3alC 2fracture toughness property (7.21MPam 1/2); Along with Ti 3alC 2the increase of doping, its flexural strength reduces gradually, at Ti 3alC 2doping exceedes after 5wt%, and its flexural strength reduces rapidly.
Embodiment 4
Step 1, by massfraction, by 25.38% Ti powder, 14.0% Al and 60.62% TiC powder pack in stainless steel jar mill, add 200mL dehydrated alcohol as ball-milling medium, Stainless Steel Ball is as abrading-ball, drum's speed of rotation is 600 revs/min, ratio of grinding media to material is 5:1, ball milling obtains uniform powder and is dried after 1 hour, bake out temperature is 30 ℃, then dried mixed powder is packed in corundum crucible, carry out vacuum non-pressure sintering, temperature rise rate with 8 ℃/min rises to sintering temperature from room temperature, sintering temperature is 1400 ℃, 1400 ℃ of insulations 1.5 hours, then with stove, naturally cool to room temperature, obtain Ti 3alC 2powder, wherein Ti 3alC 2ti in powder 3alC 2massfraction is that 92%, TiC massfraction is 8%.
Step 2, by massfraction, Ti prepared by the step 1 of 65.78% Ti powder, 30.72% Al powder and 3.5% 3alC 2powder packs in stainless steel jar mill, carries out ball milling on planetary ball mill, and adding 400mL dehydrated alcohol is ball-milling medium, and Stainless Steel Ball is abrading-ball, and ratio of grinding media to material is 6:1, and under the rotating speed of 500 revs/min, ball milling 1 hour, obtains mixed powder;
Step 3, mixed powder is packed in graphite jig after 40 ℃ of oven dry, under the forming pressure of 3MPa, be cold-pressed into pie, then pack into and in vacuum hotpressing stove, carry out vacuum heating-press sintering, with the temperature rise rates of 5 ℃/min, from room temperature, start to heat up, when being raised to 300 ℃, temperature opens pressurizing device, regulate pressure to 8MPa, maintain that pressure is constant until temperature reaches 550 ℃, during 15 ℃ of every risings of temperature afterwards, increase pressure 1.5MPa, when temperature reaches 850 ℃ of sintering temperatures, regulate pressure to being 40MPa to the maximum, maintain pressure constant, be incubated 1 hour under sintering temperature after with stove naturally cooling, obtain Ti 3alC 2-Ti 2alC/TiAl based composites.
Embodiment 5
Step 1, by massfraction, by 24.17% Ti powder, 14.3% Al and 61.53% TiC powder pack in stainless steel jar mill, add 300mL dehydrated alcohol as ball-milling medium, Stainless Steel Ball is as abrading-ball, drum's speed of rotation is 500 revs/min, ratio of grinding media to material is 6:1, ball milling obtains uniform powder and is dried after 1.5 hours, bake out temperature is 40 ℃, then dried mixed powder is packed in corundum crucible, carry out vacuum non-pressure sintering, temperature rise rate with 5 ℃/min rises to sintering temperature from room temperature, sintering temperature is 1300 ℃, 1300 ℃ of insulations 1 hour, then with stove, naturally cool to room temperature, obtain Ti 3alC 2powder, Ti 3alC 2ti in powder 3alC 2massfraction is that 95.88%, TiC massfraction is 4.12%.
Step 2, by massfraction, Ti prepared by the step 1 of 57.78% Ti powder, 34.22% Al powder and 8% 3alC 2powder packs in stainless steel jar mill, carries out ball milling on planetary ball mill, and adding 300mL dehydrated alcohol is ball-milling medium, and Stainless Steel Ball is abrading-ball, and ratio of grinding media to material is 5:1, and under the rotating speed of 650 revs/min, ball milling 1.5 hours, obtains mixed powder;
Step 3, mixed powder is packed in graphite jig after 30 ℃ of oven dry, under the forming pressure of 4MPa, be cold-pressed into pie, then pack into and in vacuum hotpressing stove, carry out vacuum heating-press sintering, with the temperature rise rates of 7 ℃/min, from room temperature, start to heat up, when being raised to 250 ℃, temperature opens pressurizing device, regulate pressure to 7MPa, maintain that pressure is constant until temperature reaches 750 ℃, during 30 ℃ of every risings of temperature afterwards, increase pressure 2MPa, when temperature reaches 950 ℃ of sintering temperatures, regulate pressure to being 20MPa to the maximum, maintain pressure constant, be incubated 1.5 hours under sintering temperature after with stove naturally cooling, obtain Ti 3alC 2-Ti 2alC/TiAl based composites.

Claims (10)

1. a Ti 3alC 2-Ti 2the preparation method of AlC/TiAl based composites, is characterized in that, comprises the following steps:
Step 1, by massfraction, by 55.91%～65.78% Ti powder, 29.09～34.22% Al powder and 5～15% Ti 3alC 2powder packs in ball grinder, and take dehydrated alcohol as ball-milling medium, under the rotating speed of 500～750 revs/min, ball milling 1～2 hour, obtains mixed powder;
Step 2, pack in mould after will mixed powder drying, coldmoulding under the forming pressure of 3～5MPa, then pack into and in vacuum hotpressing stove, carry out vacuum heating-press sintering, with the temperature rise rates of 5～10 ℃/min, from room temperature, be warming up to the sintering temperature of 850～950 ℃, be incubated 1～2 hour under sintering temperature after, with stove naturally cooling, obtain Ti 3alC 2-Ti 2alC/TiAl based composites.
2. Ti according to claim 1 3alC 2-Ti 2the low temperature preparation method of AlC/TiAl based composites, is characterized in that: described Ti 3alC 2ti in powder 3alC 2massfraction is that 92～99.42%, TiC massfraction is 0.58～8%.
3. Ti according to claim 2 3alC 2-Ti 2the low temperature preparation method of AlC/TiAl based composites, is characterized in that: described Ti 3alC 2the preparation method of powder is: by massfraction, 23.94～25.38% Ti powder, 13.87～16.19% Al and 59.87～61.53% TiC powder are packed in ball grinder, add dehydrated alcohol as ball-milling medium, under the rotating speed of 500～750 revs/min, ball milling obtains powder for 1～2 hour, after being dried, powder packs in crucible, carry out vacuum non-pressure sintering, temperature rise rate with 5～10 ℃/min rises to 1300～1400 ℃ from room temperature, then be incubated 1～2 hour, with stove, naturally cool to room temperature again, obtain Ti 3alC 2powder.
4. Ti according to claim 3 3alC 2-Ti 2the low temperature preparation method of AlC/TiAl based composites, is characterized in that: described Ti 3alC 2ratio of grinding media to material in the preparation process of powder during ball milling is (5～7): 1, and adopt Stainless Steel Ball as abrading-ball; Described ball grinder is stainless steel jar mill; The bake out temperature of described powder is 30～50 ℃; Described crucible is corundum crucible.
5. Ti according to claim 3 3alC 2-Ti 2the low temperature preparation method of AlC/TiAl based composites, is characterized in that: the ratio of grinding media to material in described step 1 during ball milling is (5～7): 1, and adopt Stainless Steel Ball as abrading-ball, described ball grinder is stainless steel jar mill.
6. Ti according to claim 3 3alC 2-Ti 2the low temperature preparation method of AlC/TiAl based composites, is characterized in that: in described step 2, the bake out temperature of mixed powder is 30～50 ℃; Mould in described step 2 is graphite jig.
7. Ti according to claim 3 3alC 2-Ti 2the low temperature preparation method of AlC/TiAl based composites, it is characterized in that: the vacuum heating-press sintering process in described step 2 takes sectional type to exert pressure, when being raised to 200～300 ℃, temperature opens pressurizing device, regulate pressure to 6～8MPa, maintain that pressure is constant until temperature reaches 550～750 ℃, during 15～30 ℃ of every risings of temperature afterwards, increase pressure 1.5～2MPa, when temperature reaches sintering temperature, regulate pressure to being 20～40MPa to the maximum, and it is constant in insulating process, to maintain pressure.
8. according to the Ti described in any one in claim 2-7 3alC 2-Ti 2the Ti that the low temperature preparation method of AlC/TiAl based composites makes 3alC 2-Ti 2alC/TiAl based composites, is characterized in that: by massfraction, it is comprised of 85～95% matrix phases and 5～15% wild phase two portions, phase free from foreign meter, and wherein matrix phase is TiAl and Ti 3al, wild phase is Ti 2alC and Ti 3alC 2.
9. Ti according to claim 8 3alC 2-Ti 2alC/TiAl based composites, is characterized in that: described wild phase Ti 2alC is mainly by Ti in raw material 3alC 2part Ti in powder 3alC 2in preparation process, decompose and obtain, simultaneously Ti in raw material 3alC 2tiC in powder reacts and also forms wild phase Ti with matrix phase TiAl 2alC.
10. Ti according to claim 8 or claim 9 3alC 2-Ti 2alC/TiAl based composites, is characterized in that: its flexural strength is 148～316MPa, and fracture toughness property is 3.88～7.28MPam 1/2.
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