CN103757452B - A kind of Ti 2alC/TiAl based composites and low temperature preparation method thereof - Google Patents
A kind of Ti 2alC/TiAl based composites and low temperature preparation method thereof Download PDFInfo
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Abstract
A kind of Ti
2alC/TiAl based composites and low temperature preparation method thereof, by Ti powder, Al powder and Ti
3alC
2after powder ball milling is even, first coldmoulding, then at 950 ~ 1050 DEG C of vacuum heating-press sinterings, obtain Ti
2alC/TiAl based composites.This material is by matrix phase TiAl, Ti
3al and wild phase Ti
2alC two portions form, phase TiC free from foreign meter.The present invention utilizes the original position thermopositive reaction between Ti-Al to form matrix phase, and makes Ti
3alC
2there is self-decomposition reaction and obtain Ti
2alC wild phase, reduces Ti
2the synthesis temperature of AlC/TiAl based composites, technique is simple, controllability is strong, sintering temperature is low, preparation cost is low, product purity is high, foreign matter content is low, highly malleablized successful, obtained material maximum deflection intensity is 651MPa, and maximum fracture toughness property is 10.89MPam
1/2.
Description
Technical field
The invention belongs to Materials Science and Engineering field, be specifically related to a kind of Ti
2alC/TiAl based composites and low temperature preparation method thereof.
Background technology
TiAl intermetallic compound coexists due to the long-range order of its atom and interatomic metallic bond and covalent linkage, makes the hot strength of its plasticity simultaneously may taking into account metal and pottery.Namely there is the performance such as common metal and the unexistent high specific tenacity of 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 the wing, housing etc. of high temperature resistant component for the aerospace such as jet engine and turbine, automotive industry and super speed vehicle, be considered to the lightening fire resistant structured material of new generation having application potential.Especially TiAl intermetallic compound, is applied to aerospace and motor car engine will improve engine operating efficiency by structure loss of weight, has important promoting technology effect.
But TiAl intermetallic compound temperature-room type plasticity and poor toughness, be difficult to formed machining, use temperature becomes higher than problems such as antioxidant property when 800 DEG C reduce rapidly the major obstacle limiting its application process.Research shows, Composite means improve TiAl intermetallic compound toughness and hot strength, improve high-temperature behavior and promote one of its practical most effective means.Relative to long fiber reinforcement type, particle-reinforced TiAl-based intermetallic compound to the thermal expansivity mismatch of matrix and wild phase and chemosensitivity little, and particle reinforce has isotropy, preparation technology is simple, secondary processing is simple, relative low price, thus has larger application prospect.But most of ceramic enhancement phase is as SiC, Al
2o
3, TiC, TiB
2belong to brittlement phase, prepared TiAl base intermetallic compound can be made to become more crisp.The ternary layered compound M of one class
n+1aX
n(M represents transition metal, and A represents the IIIth or the IVth main group, and X is C or N, is called for short MAX), has the dual property of metal and pottery concurrently, receives extensive concern.Typical Representative compound has Ti
2alC and Ti
3alC
2, and Ti
2alC and Ti
3alC
2close with the thermal expansivity of TiAl, be the desirable 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 with Ti powder, Al powder, Nb powder, B powder for raw material, thermal expousure is adopted 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 obtain Ti
2alC/TiAl matrix material, and multi-step heat treatment is carried out to it, thermal treatment temp reaches 1390 DEG C.Northwestern Polytechnical University once reached the clouds (once reached the clouds, spontaneous Ti
2the tissue of AlC/TiAl matrix material and reaction process, Rare Metals Materials and engineering, 42(4 in 2013): method 785-788) adopting Self-propagating Sintering Synthetic and vacuum arc melting, 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 prepares 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 DEG C, Ti
2alC starts to occur, but containing a large amount of TiC dephasign; When sintering temperature is 1150 DEG C, matrix material is by TiAl, Ti
3al and Ti
2alC forms, and has carried out subsequent heat treatment technique.Shaanxi Tech Univ Wang Fen (Wang Fen etc., fabricated in situ Ti
2the microstructure variation of AlC/TiAl matrix material, Special Processes of Metal Castings and non-ferrous alloy, 28(2 in 2008): 145-147) adopt simple substance Ti powder, Al powder, C powder to be raw material, adopt in-situ hot pressing technology to prepare Ti in 1200 DEG C
2alC/TiAl matrix material.Aforesaid method generates Ti mainly through the chemosynthesis reaction between component each in starting material
2alC, and much technique usually needs the operations such as subsequent high temperature thermal treatment, and the cycle is long, complex process, equipment requirements is high, the high (> 1100 DEG C of sintering temperature, if the low TiC impurity phase that has of temperature exists), generate required energy consumption large, add preparation cost.
Summary of the invention
The object of the present invention is to provide a kind of Ti
2alC/TiAl based composites and low temperature preparation method thereof, the method sintering temperature is low, obtained Ti
2flexural strength and the fracture toughness property of AlC/TiAl based composites are high.
In order to achieve the above object, the technical solution used in the present invention is:
A kind of Ti
2the low temperature preparation method of AlC/TiAl based composites, comprises the following steps:
Step one, by massfraction, by the Ti powder of 55.91% ~ 65.78%, the Al powder of 29.09 ~ 34.22% and 2 ~ 15% Ti
3alC
2powder loads 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, mixed powder is dried after load in mould, coldmoulding under the forming pressure of 3 ~ 5MPa, then load in vacuum hotpressing stove and carry out vacuum heating-press sintering, with the sintering temperature of the temperature rise rate of 5 ~ 10 DEG C/min from room temperature to 950 ~ 1050 DEG C, with stove naturally cooling after being incubated 1 ~ 2 hour at a sintering temperature, obtain Ti
2alC/TiAl based composites.
Described Ti
3alC
2ti in powder
3alC
2massfraction is 92 ~ 99.42%, TiC massfraction is 0.58 ~ 8%.
Described Ti
3alC
2raw powder's production technology is: by massfraction, the TiC powder of the Ti powder of 23.94 ~ 25.38%, the Al and 59.87 ~ 61.53% of 13.87 ~ 16.19% is loaded in ball grinder, add dehydrated alcohol as ball-milling medium, under the rotating speed of 500 ~ 750 revs/min, ball milling obtains powder in 1 ~ 2 hour, load in crucible after powder is dried and carry out vacuum non-pressure sintering, 1300 ~ 1400 DEG C are risen to from room temperature with the temperature rise rate of 5 ~ 10 DEG C/min, then 1 ~ 2 hour is incubated, naturally cool to room temperature with stove 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, adopts Stainless Steel Ball as abrading-ball; Described ball grinder is stainless steel jar mill; The bake out temperature of described powder is 30 ~ 50 DEG C; Described crucible is corundum crucible.
Ratio of grinding media to material in described step one 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 DEG C; Mould in described step 2 is graphite jig.
Vacuum heating-press sintering process in described step 2 takes sectional type to apply pressure, pressurizing device is opened when temperature is raised to 200 ~ 300 DEG C, regulate pressure to 6 ~ 8MPa, maintain pressure constant until temperature reaches 700 ~ 800 DEG C, pressure 1.5 ~ 2.5MPa is increased when temperature often raises 15 ~ 30 DEG C afterwards, when temperature reaches sintering temperature, regulate pressure to being 20 ~ 40MPa to the maximum, and in insulating process, maintain pressure constant.
Described Ti
2the Ti that the low temperature preparation method of AlC/TiAl based composites is obtained
2alC/TiAl based composites, by massfraction, it is made up of 85 ~ 98% matrix phases and 2 ~ 15% wild phase two portions, phase free from foreign meter, and wherein matrix phase is TiAl and Ti
3al, wild phase is Ti
2alC.
Described wild phase Ti
2alC is primarily of Ti in raw material
3alC
2ti in powder
3alC
2decompose in preparation process and obtain, simultaneously Ti in raw material
3alC
2tiC in powder and matrix phase TiAl reacts and also forms wild phase Ti
2alC.
Its flexural strength is 414 ~ 651MPa, and fracture toughness property is 6.52 ~ 10.89MPam
1/2.
Relative to prior art, beneficial effect of the present invention is:
The invention provides a kind of 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, namely obtain Ti
2alC/TiAl based composites.The method utilizes the original position thermopositive reaction between Ti-Al to form matrix phase, and makes full use of the amount of heat of the original position thermopositive reaction release between Ti-Al system, simultaneously by modulation process, makes Ti
3alC
2generation self-decomposition is reacted, thus obtains Ti
2alC wild phase, greatly reduces Ti
2the synthesis temperature of AlC/TiAl based composites, the self-decomposition reaction method that the present invention adopts and reaction in－situ hot-pressing technique, technique are simple, sintering temperature (950 ~ 1050 DEG C) lower than preparation temperature of the prior art, process controllability is strong, preparation cost is low, product purity is high, foreign matter content is low, product property is excellent, highly malleablized successful.
The Ti that the present invention obtains
2alC/TiAl based composites is made up of 85 ~ 98% matrix phases and 2 ~ 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.This Ti
2alC/TiAl based composites have high-strength, high tenacity, high temperature resistant, the feature such as can to process, performance is greatly improved, and its maximum deflection intensity can reach 651MPa, and maximum fracture toughness property can reach 10.89MPam
1/2, significantly improve flexural strength and the fracture toughness property of TiAl base intermetallic compound, improve Ti
2the mechanical property of AlC/TiAl based composites, can expand the range of application of TiAl base intermetallic compound.
Further, the raw material Ti of the present invention's employing
3alC
2ti in powder
3alC
2massfraction is 92 ~ 99.42%, TiC massfraction is 0.58 ~ 8%, namely containing a small amount of impurity TiC, but at Ti
2in the preparation process of AlC/TiAl based composites, TiC impurity phase can react with matrix phase TiAl and generate wild phase Ti
2alC, the Ti therefore finally prepared
2phase TiC free from foreign meter in AlC/TiAl based composites, reaches the effect of material from purifying.
Accompanying drawing explanation
Fig. 1 is Ti prepared by the present invention
2the XRD figure of AlC/TiAl based composites, wherein (a) Ti of preparing for the present invention
3alC
2the XRD figure of powder, (b) is the XRD figure before not sintering after being mixed by the raw material of embodiment 3, and (c) be not for add Ti
3alC
2time sinter the XRD figure of material prepared, (d) ~ (g) is respectively the obtained Ti of embodiment 1 ~ 4
2the XRD figure of AlC/TiAl based composites.
Fig. 2 is Ti prepared by the present invention
2the fracture SEM figure of AlC/TiAl based composites, wherein (a) be not for add Ti
3alC
2time sinter the fracture SEM figure of material prepared, (b) ~ (e) is respectively the obtained Ti of embodiment 1 ~ 4
2the fracture SEM figure of AlC/TiAl based composites.
Fig. 3 is Ti prepared by the present invention
2the flexural strength of AlC/TiAl based composites and fracture toughness property change curve.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.
The invention provides Ti
2the low temperature preparation method of AlC/TiAl based composites is at preparation Ti
2mainly there occurs the reaction of building-up reactions Sum decomposition in the process of AlC/TiAl based composites, 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 one, by massfraction, by the Ti powder of 23.94%, the TiC powder of the Al and 59.87% of 16.19% loads 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 after 2 hours and is dried, bake out temperature is 50 DEG C, then dried mixed powder is loaded in corundum crucible, carry out vacuum non-pressure sintering, sintering temperature is risen to from room temperature with the temperature rise rate of 10 DEG C/min, sintering temperature is 1350 DEG C, 1350 DEG C of insulations 2 hours, then room temperature is naturally cooled to stove, obtain Ti
3alC
2powder.
Step 2, by massfraction, by the Ti powder of 64.46%, the Al powder of 33.54% and 2% the Ti for preparing of step one
3alC
2powder loads in stainless steel jar mill, and planetary ball mill carries out ball milling, 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, load in graphite jig after mixed powder is dried at 50 DEG C, pie is cold-pressed under the forming pressure of 5MPa, then load in vacuum hotpressing stove and carry out vacuum heating-press sintering, heat up from room temperature with the temperature rise rate of 10 DEG C/min, pressurizing device is opened when temperature is raised to 200 DEG C, regulate pressure to 6MPa, maintain pressure constant until temperature reaches 700 DEG C, pressure 2MPa is increased when temperature often raises 25 DEG C afterwards, when temperature reaches sintering temperature 1000 DEG C, regulate pressure to being 30MPa to the maximum, maintenance pressure is constant, with stove naturally cooling after being incubated 2 hours at a sintering temperature, obtain Ti
2alC/TiAl based composites.
The Ti that Fig. 1 (a) is prepared for the present embodiment step one
3alC
2the XRD figure of powder, as seen from the figure, this Ti
3alC
2ti in powder
3alC
2purity is very high, Ti
3alC
2content is about 99.42wt%, and also containing a small amount of TiC, its content is about 0.58wt%.
The Ti that Fig. 1 (d) is prepared for the present embodiment
2alC/TiAl based composites (Ti
3alC
2doping is 2wt%) XRD figure, this Ti can be found out
2main containing TiAl, Ti in AlC/TiAl based composites
3al and Ti
2alC phase, without other impurity phase.
The massfraction that Fig. 1 (c) is 65.78%, Al powder for the massfraction of Ti powder in raw material is 34.22%, does not add Ti
3alC
2, through the XRD analysis result of the material prepared after 2 hours of 1000 DEG C of sintered heat insulatings, can find out in this material main containing TiAl and Ti
3al.
With reference to Fig. 3, employing three-point bending method measures Ti prepared by the present embodiment
2the flexural strength of AlC/TiAl based composites is 571MPa, adopts three-point bending Single edge notch beam (SENB) to measure this Ti
2the fracture toughness property of AlC/TiAl based composites is 8.8MPam
1/2.
Embodiment 2
Step one, by massfraction, by the Ti powder of 23.94%, the TiC powder of the Al and 59.87% of 16.19% loads 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 after 2 hours and is dried, bake out temperature is 50 DEG C, then dried mixed powder is loaded in corundum crucible, carry out vacuum non-pressure sintering, sintering temperature is risen to from room temperature with the temperature rise rate of 10 DEG C/min, sintering temperature is 1350 DEG C, 1350 DEG C of insulations 2 hours, then room temperature is naturally cooled to stove, obtain Ti
3alC
2powder.
Step 2, by massfraction, by the Ti powder of 62.49%, the Al powder of 32.51% and 5% the Ti for preparing of step one
3alC
2powder loads in stainless steel jar mill, and planetary ball mill carries out ball milling, 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, load in graphite jig after mixed powder is dried at 50 DEG C, pie is cold-pressed under the forming pressure of 5MPa, then load in vacuum hotpressing stove and carry out vacuum heating-press sintering, heat up from room temperature with the temperature rise rate of 10 DEG C/min, pressurizing device is opened when temperature is raised to 200 DEG C, regulate pressure to 6MPa, maintain pressure constant until temperature reaches 700 DEG C, pressure 2MPa is increased when temperature often raises 25 DEG C afterwards, when temperature reaches sintering temperature 1000 DEG C, regulate pressure to being 30MPa to the maximum, maintenance pressure is constant, with stove naturally cooling after being incubated 2 hours at a sintering temperature, obtain Ti
2alC/TiAl based composites.
The Ti that Fig. 1 (e) is prepared for the present embodiment
2alC/TiAl based composites (Ti
3alC
2doping is 5wt%) XRD figure, this Ti can be found out
2main containing TiAl, Ti in AlC/TiAl based composites
3al and Ti
2alC phase, without other impurity phase.With reference to Fig. 3, employing three-point bending method measures Ti prepared by the present embodiment
2the flexural strength of AlC/TiAl based composites is 651MPa, adopts three-point bending Single edge notch beam (SENB) to measure this Ti
2the fracture toughness property of AlC/TiAl based composites is 10.89MPam
1/2.
Embodiment 3
Step one, by massfraction, by the Ti powder of 23.94%, the TiC powder of the Al and 59.87% of 16.19% loads 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 after 2 hours and is dried, bake out temperature is 50 DEG C, then dried mixed powder is loaded in corundum crucible, carry out vacuum non-pressure sintering, sintering temperature is risen to from room temperature with the temperature rise rate of 10 DEG C/min, sintering temperature is 1350 DEG C, 1350 DEG C of insulations 2 hours, then room temperature is naturally cooled to stove, obtain Ti
3alC
2powder.
Step 2, by massfraction, by the Ti powder of 59.2%, the Al powder of 30.8% and 10% the Ti for preparing of step one
3alC
2powder loads in stainless steel jar mill, and planetary ball mill carries out ball milling, 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, load in graphite jig after mixed powder is dried at 50 DEG C, pie is cold-pressed under the forming pressure of 5MPa, then load in vacuum hotpressing stove and carry out vacuum heating-press sintering, heat up from room temperature with the temperature rise rate of 10 DEG C/min, pressurizing device is opened when temperature is raised to 200 DEG C, regulate pressure to 6MPa, maintain pressure constant until temperature reaches 700 DEG C, pressure 2MPa is increased when temperature often raises 25 DEG C afterwards, when temperature reaches sintering temperature 1000 DEG C, regulate pressure to being 30MPa to the maximum, maintenance pressure is constant, with stove naturally cooling after being incubated 2 hours at a sintering temperature, obtain Ti
2alC/TiAl based composites.
Fig. 1 (b) is the XRD analysis result after the raw material mixing in the present embodiment step 2 before not sintering, as seen from the figure, main containing Ti, Al and Ti in this mixed powder
3alC
2phase, because TiC dephasign content is too low, can't detect the existence of TiC dephasign.
The Ti that Fig. 1 (f) is prepared for the present embodiment
2alC/TiAl based composites (Ti
3alC
2doping is 10wt%) XRD figure, this Ti can be found out
2main containing TiAl, Ti in AlC/TiAl based composites
3al and Ti
2alC phase, without other impurity phase.With reference to Fig. 3, employing three-point bending method measures Ti prepared by the present embodiment
2the flexural strength of AlC/TiAl based composites is 600MPa, adopts three-point bending Single edge notch beam (SENB) to measure this Ti
2the fracture toughness property of AlC/TiAl based composites is 7.37MPam
1/2.
Embodiment 4
Step one, by massfraction, by the Ti powder of 23.94%, the TiC powder of the Al and 59.87% of 16.19% loads 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 after 2 hours and is dried, bake out temperature is 50 DEG C, then dried mixed powder is loaded in corundum crucible, carry out vacuum non-pressure sintering, sintering temperature is risen to from room temperature with the temperature rise rate of 10 DEG C/min, sintering temperature is 1350 DEG C, 1350 DEG C of insulations 2 hours, then room temperature is naturally cooled to stove, obtain Ti
3alC
2powder.
Step 2, by massfraction, by the Ti powder of 55.91%, the Al powder of 29.09% and 15% the Ti for preparing of step one
3alC
2powder loads in stainless steel jar mill, and planetary ball mill carries out ball milling, 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, load in graphite jig after mixed powder is dried at 50 DEG C, pie is cold-pressed under the forming pressure of 5MPa, then load in vacuum hotpressing stove and carry out vacuum heating-press sintering, heat up from room temperature with the temperature rise rate of 10 DEG C/min, pressurizing device is opened when temperature is raised to 200 DEG C, regulate pressure to 6MPa, maintain pressure constant until temperature reaches 700 DEG C, pressure 2MPa is increased when temperature often raises 25 DEG C afterwards, when temperature reaches sintering temperature 1000 DEG C, regulate pressure to being 30MPa to the maximum, maintenance pressure is constant, with stove naturally cooling after being incubated 2 hours at a sintering temperature, obtain Ti
2alC/TiAl based composites.
The Ti that Fig. 1 (g) is prepared for the present embodiment
2alC/TiAl based composites (Ti
3alC
2doping is 15wt%) XRD figure, this Ti can be found out
2main containing TiAl, Ti in AlC/TiAl based composites
3al and Ti
2alC phase, without other impurity phase.And as can be seen from Figure 1, along with Ti
3alC
2the increase of doping, the Ti of preparation
2ti in AlC/TiAl based composites
2alC content is increasing gradually.With reference to Fig. 3, employing three-point bending method measures Ti prepared by the present embodiment
2the flexural strength of AlC/TiAl based composites is 414MPa, adopts three-point bending Single edge notch beam (SENB) to measure this Ti
2the fracture toughness property of AlC/TiAl based composites is 6.52MPam
1/2.
Fig. 2 is Ti prepared by the present invention
2the fracture SEM figure of AlC/TiAl based composites, wherein (a) be not for add Ti
3alC
2time sinter the fracture SEM figure of material prepared, (b) ~ (e) is respectively the obtained Ti of embodiment 1 ~ 4
2the fracture SEM figure of AlC/TiAl based composites.As seen from the figure, along with Ti
3alC
2the increase of doping, matrix phase crystal grain reduces gradually, and wild phase is mainly distributed in crystal boundary, Ti
2the density of AlC/TiAl based composites is deteriorated.
Fig. 3 is Ti prepared by the present invention
2the flexural strength of AlC/TiAl based composites and fracture toughness property change curve.As can be seen from the figure Ti is worked as
3alC
2when doping is 5wt%, flexural strength and fracture toughness property reach maximum value, are respectively 651MPa and 10.89MPam
1/2, far above non-doped Ti
3alC
2the flexural strength of material and fracture toughness property (its value is respectively 484MPa and 7.7MPam
1/2).
Embodiment 5
Step one, by massfraction, by the Ti powder of 25.38%, the TiC powder of the Al and 60.62% of 14.0% loads 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 after 1 hour and is dried, bake out temperature is 30 DEG C, then dried mixed powder is loaded in corundum crucible, carry out vacuum non-pressure sintering, sintering temperature is risen to from room temperature with the temperature rise rate of 8 DEG C/min, sintering temperature is 1400 DEG C, 1400 DEG C of insulations 1.5 hours, then room temperature is naturally cooled to stove, obtain Ti
3alC
2powder, wherein Ti
3alC
2ti in powder
3alC
2massfraction is 92%, TiC massfraction is 8%.
Step 2, by massfraction, by the Ti powder of 65.78%, the Al powder of 30.72% and 3.5% the Ti for preparing of step one
3alC
2powder loads in stainless steel jar mill, and planetary ball mill carries out ball milling, 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, load in graphite jig after mixed powder is dried at 40 DEG C, pie is cold-pressed under the forming pressure of 3MPa, then load in vacuum hotpressing stove and carry out vacuum heating-press sintering, heat up from room temperature with the temperature rise rate of 5 DEG C/min, pressurizing device is opened when temperature is raised to 300 DEG C, regulate pressure to 7MPa, maintain pressure constant until temperature reaches 750 DEG C, pressure 2.5MPa is increased when temperature often raises 15 DEG C afterwards, when temperature reaches sintering temperature 950 DEG C, regulate pressure to being 40MPa to the maximum, maintenance pressure is constant, with stove naturally cooling after being incubated 1 hour at a sintering temperature, obtain Ti
2alC/TiAl based composites.
Embodiment 6
Step one, by massfraction, by the Ti powder of 24.17%, the TiC powder of the Al and 61.53% of 14.3% loads 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 after 1.5 hours and is dried, bake out temperature is 40 DEG C, then dried mixed powder is loaded in corundum crucible, carry out vacuum non-pressure sintering, sintering temperature is risen to from room temperature with the temperature rise rate of 5 DEG C/min, sintering temperature is 1300 DEG C, 1300 DEG C of insulations 1 hour, then room temperature is naturally cooled to stove, obtain Ti
3alC
2powder, Ti
3alC
2ti in powder
3alC
2massfraction is 95.88%, TiC massfraction is 4.12%.
Step 2, by massfraction, by the Ti powder of 57.78%, the Al powder of 34.22% and 8% the Ti for preparing of step one
3alC
2powder loads in stainless steel jar mill, and planetary ball mill carries out ball milling, 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, load in graphite jig after mixed powder is dried at 30 DEG C, pie is cold-pressed under the forming pressure of 4MPa, then load in vacuum hotpressing stove and carry out vacuum heating-press sintering, heat up from room temperature with the temperature rise rate of 7 DEG C/min, pressurizing device is opened when temperature is raised to 250 DEG C, regulate pressure to 8MPa, maintain pressure constant until temperature reaches 800 DEG C, pressure 1.5MPa is increased when temperature often raises 30 DEG C afterwards, when temperature reaches sintering temperature 1050 DEG C, regulate pressure to being 20MPa to the maximum, maintenance pressure is constant, with stove naturally cooling after being incubated 1.5 hours at a sintering temperature, obtain Ti
2alC/TiAl based composites.
Claims (9)
1. a Ti
2the low temperature preparation method of AlC/TiAl based composites, is characterized in that, comprises the following steps:
Step one, by massfraction, by the Ti powder of 55.91% ~ 65.78%, the Al powder of 29.09 ~ 34.22% and 2 ~ 15% Ti
3alC
2powder loads 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, load after mixed powder is dried in mould, coldmoulding under the forming pressure of 3 ~ 5MPa, then load in vacuum hotpressing stove and carry out vacuum heating-press sintering, with the sintering temperature of the temperature rise rate of 5 ~ 10 DEG C/min from room temperature to 950 ~ 1050 DEG C, with stove naturally cooling after being incubated 1 ~ 2 hour at a sintering temperature, wherein vacuum heating-press sintering process takes sectional type to apply pressure, pressurizing device is opened when temperature is raised to 200 ~ 300 DEG C, regulate pressure to 6 ~ 8MPa, maintain pressure constant until temperature reaches 700 ~ 800 DEG C, pressure 1.5 ~ 2.5MPa is increased when temperature often raises 15 ~ 30 DEG C afterwards, when temperature reaches sintering temperature, regulate pressure to being 20 ~ 40MPa to the maximum, and it is constant to maintain pressure in insulating process, namely Ti is obtained after vacuum heating-press sintering completes
2alC/TiAl based composites.
2. Ti according to claim 1
2the low temperature preparation method of AlC/TiAl based composites, is characterized in that: described Ti
3alC
2ti in powder
3alC
2massfraction is 92 ~ 99.42%, TiC massfraction is 0.58 ~ 8%.
3. Ti according to claim 2
2the low temperature preparation method of AlC/TiAl based composites, is characterized in that: described Ti
3alC
2raw powder's production technology is: by massfraction, by the Ti powder of 23.94 ~ 25.38%, the Al powder of 13.87 ~ 16.19% and 59.87 ~ 61.53% TiC powder load in ball grinder, add dehydrated alcohol as ball-milling medium, under the rotating speed of 500 ~ 750 revs/min, ball milling obtains powder in 1 ~ 2 hour, load after powder is dried in crucible, carry out vacuum non-pressure sintering, 1300 ~ 1400 DEG C are risen to from room temperature with the temperature rise rate of 5 ~ 10 DEG C/min, then 1 ~ 2 hour is incubated, naturally cool to room temperature with stove again, obtain Ti
3alC
2powder.
4. Ti according to claim 3
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, adopts Stainless Steel Ball as abrading-ball; Described ball grinder is stainless steel jar mill; The bake out temperature of described powder is 30 ~ 50 DEG C; Described crucible is corundum crucible.
5. Ti according to claim 3
2the low temperature preparation method of AlC/TiAl based composites, is characterized in that: the ratio of grinding media to material in described step one 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
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 DEG C; Mould in described step 2 is graphite jig.
7. according to the Ti in claim 2-6 described in any one
2the Ti that the low temperature preparation method of AlC/TiAl based composites is obtained
2alC/TiAl based composites, is characterized in that: by massfraction, and it is made up of 85 ~ 98% matrix phases and 2 ~ 15% wild phase two portions, phase free from foreign meter, and wherein matrix phase is TiAl and Ti
3al, wild phase is Ti
2alC.
8. Ti according to claim 7
2alC/TiAl based composites, is characterized in that: described wild phase Ti
2alC is primarily of Ti in raw material
3alC
2ti in powder
3alC
2decompose in preparation process and obtain, simultaneously Ti in raw material
3alC
2tiC in powder and matrix phase TiAl reacts and also forms wild phase Ti
2alC.
9. the Ti according to claim 7 or 8
2alC/TiAl based composites, is characterized in that: its flexural strength is 414 ~ 651MPa, and fracture toughness property is 6.52 ~ 10.89MPam
1/2.
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| CN104789808A (en) * | 2015-04-29 | 2015-07-22 | 陕西理工学院 | Titanium-aluminum-carbon-ceramic-reinforced Ti3Al-base composite material and preparation method thereof |
| CN104907564B (en) * | 2015-05-25 | 2017-05-03 | 陕西理工学院 | Preparation method for Ti3SiC2-Co based diamond ultra-thin saw blade materials |
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| CN108585879B (en) * | 2018-05-07 | 2020-08-28 | 西安交通大学 | Method for rapidly preparing anisotropic titanium nitride ceramic block material |
| CN109865841B (en) * | 2019-03-19 | 2020-07-28 | 陕西理工大学 | Periodic multilayer alloy plate and preparation method thereof |
| CN112694333A (en) * | 2021-01-15 | 2021-04-23 | 安徽工业大学 | TixAlCy/TiCz/TiaAlb multi-component complex-phase ceramic powder and low-temperature rapid preparation method thereof |
| CN112935250A (en) * | 2021-01-28 | 2021-06-11 | 北京大学 | Cu and Ti for pantograph slide plate3AlC2Functionally graded material and preparation method thereof |
| CN114804888A (en) * | 2022-05-06 | 2022-07-29 | 郑州大学 | Preparation method of ternary diboride solid solution based composite ceramic |
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