CN103264542A - Titanium aluminum-ceramic layered material and preparation method thereof - Google Patents
Titanium aluminum-ceramic layered material and preparation method thereof Download PDFInfo
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- CN103264542A CN103264542A CN2013101778449A CN201310177844A CN103264542A CN 103264542 A CN103264542 A CN 103264542A CN 2013101778449 A CN2013101778449 A CN 2013101778449A CN 201310177844 A CN201310177844 A CN 201310177844A CN 103264542 A CN103264542 A CN 103264542A
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Abstract
The invention discloses a titanium aluminum-ceramic layered material and a preparation method thereof, which relate to a layered material and a preparation method thereof, and mainly solve the problem that aluminum fusion loss causes uncontrollable constituents when an element foil reaction annealing method is used for preparing a TiAl base plate material. The titanium aluminum-ceramic layered material is made by an in-situ synthesis technology and prepared from pure Ti foils and an Al base composite foils through alternating lamination, hot-pressing and reaction annealing. The method comprises the following steps of: firstly, preparing an Al base composite material; secondly, carrying out hot extrusion and rolling on the Al base composite material; thirdly, carrying out surface preparation on the rolled Al base composite material foils and the pure Ti foils; fourthly, carrying out alternating lamination and hot-pressing on the foils; fifthly, performing low temperature thermal treatment; sixthly, performing thermal treatment for densifying; and seventhly, performing heat preservation, thus obtaining the titanium aluminum-ceramic layered material. The preparation method provided by the invention is used for preparing the titanium aluminum-ceramic layered material.
Description
Technical field
The present invention relates to a kind of stratified material and preparation method thereof.
Background technology
Titanium aluminium base alloy is a kind of novel light heat resistant structure material, has lightweight, advantage such as high-strength, anti-corrosion, wear-resisting, high temperature resistant, becomes the emphasis material of Aeronautics and Astronautics and military field research and application in the worldwide.Through the effort of decades, titanium aluminium base alloy has entered the practicability developing stage at present.Wherein, the most urgent to the demand of titanium aluminium base alloy sheet material and foil.But single-phase TiAl base intermetallic compound fracture toughness and plasticity is relatively poor to make the TiAl substrate material difficulty that is shaped, and it is quite big to utilize traditional hot rolling method processed to prepare the difficulty of TiAl substrate material, requires very harsh to rolling environment and equipment.Based on this, used new method such as foil element reaction annealing to prepare the crystallized ability that TiAl substrate material has avoided thereby the direct distortion of fragility TiAl phase has been improved TiAl substrate material, introduced the enhancing body simultaneously and improve the problem that single-phase TiAl base intermetallic compound exists elevated temperature strength and croop property deficiency.But the aluminium fusing is run off and is caused the uncontrollable problem of composition in the foil element reaction method for annealing existence reaction annealing.
Summary of the invention
The present invention will solve foil element reaction method for annealing to prepare the aluminium fusing that exists in the TiAl substrate material process and run off and cause the uncontrollable problem of composition, and a kind of titanium aluminium-ceramic laminar material and preparation method thereof is provided.
A kind of titanium aluminium of the present invention-ceramic laminar material is to utilize the in-situ authigenic technology to be made by pure Ti paper tinsel and Al based composites paper tinsel alternative stacked, hot pressing and reaction annealing; TiAl layer and ceramic layer distribute alternately in described titanium aluminium-ceramic laminar material, and the lamination spacing is 5 μ m～100 μ m, and ceramic layer comprises Ti
2AlC phase and Ti
3The AlC phase is lamella γ-TiAl/ α in the TiAl layer
2-Ti
3Al, sheet interlayer spacing are 100nm～500nm; Described Al based composites paper tinsel is by strengthening body and pure Al powder through mixing powder, hot pressed sintering and rolling making.
A kind of titanium aluminium-ceramic laminar preparation methods, carry out according to the following steps:
One, will strengthen body and pure Al powder and carry out the mixed powder of ball milling, mixing the powder time is 6h～20h, ratio of grinding media to material is (10～20): 1, drum's speed of rotation is 150r/min～250r/min, the powder that obtains mixing, and the graphite jig that the powder that mixes will be housed then carries out sintering in vacuum hotpressing stove, sintering temperature is 500 ℃～620 ℃, temperature retention time is 1h～2h, and pressure is 20MPa～30MPa, obtains the Al based composites; The volume fraction of pure Al powder is 85%～99.9% in the wherein said Al based composites, and the volume fraction that strengthens body in the described Al based composites is 0.1%～15%;
Two, the Al based composites that step 1 is obtained carries out hot extrusion and rolling, the control extrusion temperature is 400 ℃～500 ℃, extrusion ratio is (10～20): 1, the controlled rolling temperature is 20 ℃～500 ℃, rolling 10 times～50 times, each drafts is 5%～30%, and the Al based composites thickness after rolling is 100 μ m～500 μ m;
Three, the Al based composites after rolling to step 2 is polished, obtain Al based composites paper tinsel, adopting mass concentration then is that 5%～30% NaOH solution cleans Al based composites paper tinsel, adopting volumetric concentration is that 5%～30% HF solution cleans pure Ti paper tinsel, pure Ti paper tinsel after Al based composites paper tinsel after will cleaning again and the cleaning places acetone, be ultrasonic cleaning 3min～10min under the condition of 20KHz～30KHz in frequency, then in 20 ℃～70 ℃ following dry 1min～5min, the pure Ti paper tinsel after the Al based composites paper tinsel after obtaining handling and the processing;
Four, the pure Ti paper tinsel alternative stacked after the Al based composites paper tinsel after the processing that step 3 is obtained and the processing, outermost layer is the pure Ti paper tinsel after the processing, in the titanium alloy mould, carry out hot pressing then, the control hot pressing temperature is 400 ℃～550 ℃, temperature retention time is 1h～2h, pressure is 20MPa～30MPa, obtains the forming laminated sheet material of Ti-Al based composites; Pure Ti paper tinsel thickness in monolayer after the processing that wherein said step 3 obtains is 50 μ m～200 μ m, the pure Ti paper tinsel after the processing that described step 3 obtains with handle after the thickness in monolayer of Al based composites paper tinsel than being (1.04～1.14): 1;
The forming laminated sheet material of the Ti-Al based composites that five, step 4 is obtained is put into vacuum hotpressing stove and is carried out Low Temperature Heat Treatment, after temperature is 650 ℃～670 ℃ insulation 4h～6h, be cooled to 400 ℃～500 ℃ pressurization 20MPa～30MPa and be incubated 0.5h～3h, be warming up to 700 ℃～800 ℃ insulation 2h～3h again, be cooled to 400 ℃～500 ℃ pressurization 20MPa～30MPa at last and be incubated 0.5h～3h, obtain Ti-TiAl
3Stratified material;
Six, the Ti-TiAl that step 5 is obtained
3Stratified material is put into vacuum hotpressing stove and is carried out densified heat treatment, and the control densification temperature is 1000 ℃～1300 ℃, and temperature retention time is 0.5h～2h, and pressure is 20MPa～100MPa, obtains the stratified material after densified;
Seven, step 6 is obtained densified after stratified material place the insulation of 1100 ℃～1300 ℃ environment to be 3h～10h, namely obtain TiAl-(Ti
2AlC+Ti
3AlC) titanium aluminium-ceramic laminar material.
Advantage of the present invention: one, to utilize the titanium aluminium-ceramic laminar material of in-situ authigenic technology preparation be the stratified material of ceramic layer and titanium aluminium lamination alternative stacked in the present invention, the enhancing body of in-situ authigenic is evenly distributed in the TiAl matrix, not only can improve elevated temperature strength and the croop property of TiAl matrix, can also give full play to the effect that the stratified material structure is toughness reinforcing and strengthen; Two, unique layer structure can compensate the deficiency of monolayer material internal performance in the titanium aluminium-ceramic laminar material of the present invention preparation, obtain the material of obdurability best fit, the lamination spacing is 5 μ m～100 μ m, less lamination spacing has limited the movement of dislocation and the size of defective, thereby improves the performance of titanium aluminium-ceramic laminar material; Three, the titanium aluminium-ceramic laminar material structure of the present invention's preparation is tiny; Four, preparation process of the present invention is pollution-free, the material densification; Five, the present invention is simple for process, and cost is low; Six, kind and the relative thickness of content, primitive element paper tinsel etc. of the present invention by change strengthening body can be realized the controlled design organized, and then can satisfy the different service condition of this stratified material and environment.Seven, the present invention adopts the reaction annealing process of " liquid phase is handled; the solid phase pressurization ", successfully having solved in the reaction annealing process aluminium fusing runs off and causes the uncontrollable problem of composition, the perfection that has realized experimental design and result of the test coincide, and makes the controlled TiAl substrate material of suitability for industrialized production large scale and composition height become possibility.
Description of drawings
The Ti-TiAl that Fig. 1 obtains for test one step 5
3TiAl in the stratified material
3The microscopic appearance figure of layer;
The Ti-TiAl that Fig. 2 obtains for test one step 5
3TiAl in the stratified material
3The XRD figure of layer;
Fig. 3 is the TiAl-(Ti of test one preparation
2AlC+Ti
3AlC) the microscopic appearance figure of titanium aluminium-ceramic laminar material;
Fig. 4 is the TiAl-(Ti of test one preparation
2AlC+Ti
3AlC) lamella γ-TiAl/ α in titanium aluminium-ceramic laminar material
2-Ti
3The microscopic appearance figure of Al;
Fig. 5 is the TiAl-(Ti of test one preparation
2AlC+Ti
3AlC) lamella γ-TiAl/ α in titanium aluminium-ceramic laminar material
2-Ti
3The diffraction spot point diagram of Al;
Fig. 6 is the TiAl-(Ti of test one preparation
2AlC+Ti
3AlC) the microscopic appearance figure of carbide lamella in titanium aluminium-ceramic laminar material, Fig. 7 is Ti in the carbide lamella
2The diffraction spot point diagram of AlC phase, Fig. 8 are Ti in the carbide lamella
3The diffraction spot point diagram of AlC phase.
The specific embodiment
The specific embodiment one: a kind of titanium aluminium of present embodiment-ceramic laminar material is to utilize the in-situ authigenic technology to be made by pure Ti paper tinsel and Al based composites paper tinsel alternative stacked, hot pressing and reaction annealing; TiAl layer and ceramic layer distribute alternately in described titanium aluminium-ceramic laminar material, and the lamination spacing is 5 μ m～100 μ m, and ceramic layer comprises Ti
2AlC phase and Ti
3The AlC phase is lamella γ-TiAl/ α in the TiAl layer
2-Ti
3Al, sheet interlayer spacing are 100nm～500nm; Described Al based composites paper tinsel is by strengthening body and pure Al powder through mixing powder, hot pressed sintering and rolling making.
The described lamination spacing of present embodiment refers to the distance of TiAl interlayer or the distance between ceramic layer; Described sheet interlayer spacing refers to distance or the α of γ in the TiAl layer-TiAl sheet interlayer
2-Ti
3The distance of Al sheet interlayer.
The enhancing body of selecting for use in the present embodiment can with titanium, reactive aluminum.
It is the stratified material of ceramic layer and titanium aluminium lamination alternative stacked that present embodiment is utilized the titanium aluminium-ceramic laminar material of in-situ authigenic method preparation, the enhancing body of in-situ authigenic is evenly distributed in the TiAl matrix, not only can improve elevated temperature strength and the croop property of TiAl matrix, can also give full play to the effect that the stratified material structure is toughness reinforcing and strengthen.
Unique layer structure can compensate the deficiency of monolayer material internal performance in the described titanium aluminium of present embodiment-ceramic laminar material, obtain the material of obdurability best fit, the lamination spacing is 5 μ m～100 μ m, less lamination spacing has limited the movement of dislocation and the size of defective, thereby improves the performance of titanium aluminium-ceramic laminar material.
Described titanium aluminium-the ceramic laminar material structure is tiny and controlled for present embodiment, can satisfy the different Service Environment of stratified material by the thickness that changes ceramic layer and TiAl layer.
Present embodiment can be adjusted the relative thickness of ceramic layer by adjusting the content that strengthens body in the Al based composites paper tinsel.
Present embodiment can change lamination spacing and the mechanical property of final titanium aluminium-ceramic laminar material by the thickness of adjusting Ti paper tinsel and Al based composites paper tinsel.
The specific embodiment two: what present embodiment and the specific embodiment one were different is: the thickness in monolayer of described pure Ti paper tinsel is 50 μ m～200 μ m, and the thickness in monolayer of described pure Ti paper tinsel and Al based composites paper tinsel is than being (1.04～1.14): 1.Other is identical with the specific embodiment one.
The specific embodiment three: what present embodiment was different with the specific embodiment one or two is: the volume fraction of pure Al powder is 85%～99.9% in the described Al based composites paper tinsel, and the volume fraction that strengthens body in the described Al based composites paper tinsel is 0.1%～15%.Other is identical with the specific embodiment one or two.
The specific embodiment four: what present embodiment was different with one of specific embodiment one to three is: the particle diameter of described pure Al powder is 10～100 μ m, and strengthening the body particle diameter is 40nm～10 μ m.Other is identical with one of specific embodiment one to three.
The specific embodiment five: what present embodiment was different with one of specific embodiment one to four is: described enhancing body is SiC, B
4C, TiB
2, Al
2O
3, TiC and Ti
5Si
3In one or more mixture.Other is identical with one of specific embodiment one to four.
When the described enhancing body of present embodiment is mixture, press between each component arbitrarily than mixing.
The specific embodiment six: a kind of titanium aluminium of present embodiment-ceramic laminar preparation methods, carry out according to the following steps:
One, will strengthen body and pure Al powder and carry out the mixed powder of ball milling, mixing the powder time is 6h～20h, ratio of grinding media to material is (10～20): 1, drum's speed of rotation is 150r/min～250r/min, the powder that obtains mixing, and the graphite jig that the powder that mixes will be housed then carries out sintering in vacuum hotpressing stove, sintering temperature is 500 ℃～620 ℃, temperature retention time is 1h～2h, and pressure is 20MPa～30MPa, obtains the Al based composites; The volume fraction of pure Al powder is 85%～99.9% in the wherein said Al based composites, and the volume fraction that strengthens body in the described Al based composites is 0.1%～15%;
Two, the Al based composites that step 1 is obtained carries out hot extrusion and rolling, the control extrusion temperature is 400 ℃～500 ℃, extrusion ratio is (10～20): 1, the controlled rolling temperature is 20 ℃～500 ℃, rolling 10 times～50 times, each drafts is 5%～30%, and the Al based composites thickness after rolling is 100 μ m～500 μ m;
Three, the Al based composites after rolling to step 2 is polished, obtain Al based composites paper tinsel, adopting mass concentration then is that 5%～30% NaOH solution cleans Al based composites paper tinsel, adopting volumetric concentration is that 5%～30% HF solution cleans pure Ti paper tinsel, pure Ti paper tinsel after Al based composites paper tinsel after will cleaning again and the cleaning places acetone, be ultrasonic cleaning 3min～10min under the condition of 20KHz～30KHz in frequency, then in 20 ℃～70 ℃ following dry 1min～5min, the pure Ti paper tinsel after the Al based composites paper tinsel after obtaining handling and the processing;
Four, the pure Ti paper tinsel alternative stacked after the Al based composites paper tinsel after the processing that step 3 is obtained and the processing, outermost layer is the pure Ti paper tinsel after the processing, in the titanium alloy mould, carry out hot pressing then, the control hot pressing temperature is 400 ℃～550 ℃, temperature retention time is 1h～2h, pressure is 20MPa～30MPa, obtains the forming laminated sheet material of Ti-Al based composites; Pure Ti paper tinsel thickness in monolayer after the processing that wherein said step 3 obtains is 50 μ m～200 μ m, the pure Ti paper tinsel after the processing that described step 3 obtains with handle after the thickness in monolayer of Al based composites paper tinsel than being (1.04～1.14): 1;
The forming laminated sheet material of the Ti-Al based composites that five, step 4 is obtained is put into vacuum hotpressing stove and is carried out Low Temperature Heat Treatment, after temperature is 650 ℃～670 ℃ insulation 4h～6h, be cooled to 400 ℃～500 ℃ pressurization 20MPa～30MPa and be incubated 0.5h～3h, be warming up to 700 ℃～800 ℃ insulation 2h～3h again, be cooled to 400 ℃～500 ℃ pressurization 20MPa～30MPa at last and be incubated 0.5h～3h, obtain Ti-TiAl
3Stratified material;
Six, the Ti-TiAl that step 5 is obtained
3Stratified material is put into vacuum hotpressing stove and is carried out densified heat treatment, and the control densification temperature is 1000 ℃～1300 ℃, and temperature retention time is 0.5h～2h, and pressure is 20MPa～100MPa, obtains the stratified material after densified;
Seven, step 6 is obtained densified after stratified material place the insulation of 1100 ℃～1300 ℃ environment to be 3h～10h, namely obtain TiAl-(Ti
2AlC+Ti
3AlC) titanium aluminium-ceramic laminar material.
Enhancing body described in the present embodiment step 1 can with titanium, reactive aluminum; Need be coated with one deck BN at the contact surface of mould and powder during described graphite jig sintering, to prevent the reaction of powder and graphite jig.
Ratio of grinding media to material described in the present embodiment step 1 is the ratio of quality with the gross mass of the mixture that strengthens body and pure Al powder of abrasive body in the ball grinder.
It is the stratified material of ceramic layer and titanium aluminium lamination alternative stacked that present embodiment is utilized the titanium aluminium-ceramic laminar material of in-situ authigenic technology preparation, the enhancing body of in-situ authigenic is evenly distributed in the TiAl matrix, not only can improve elevated temperature strength and the croop property of TiAl matrix, can also give full play to the effect that the stratified material structure is toughness reinforcing and strengthen.
Unique layer structure can compensate the deficiency of monolayer material internal performance in the titanium aluminium-ceramic laminar material of present embodiment preparation, obtain the material of obdurability best fit, the lamination spacing is 5 μ m～100 μ m, less lamination spacing has limited the movement of dislocation and the size of defective, thereby improves the performance of titanium aluminium-ceramic laminar material.
Titanium aluminium-ceramic laminar the material structure of present embodiment preparation is tiny and controlled, can satisfy the different Service Environment of stratified material by the thickness that changes ceramic layer and TiAl layer.
The present embodiment preparation process is pollution-free, the material densification.
Present embodiment is simple for process, and cost is low.
Kind and the relative thickness of content, primitive element paper tinsel etc. of present embodiment by change strengthening body can be realized the controlled design organized, and then can satisfy the different service condition of this stratified material and environment.
Present embodiment adopts the reaction annealing process of " liquid phase is handled; the solid phase pressurization ", having solved in the reaction annealing process aluminium fusing runs off and causes the uncontrollable problem of composition, the perfection that has realized experimental design and result of the test coincide, and makes the controlled TiAl substrate material of suitability for industrialized production large scale and composition height become possibility.
Present embodiment can be adjusted the relative thickness of ceramic layer by adjusting the content that strengthens body in the Al based composites paper tinsel.
Present embodiment can change lamination spacing and the mechanical property of final titanium aluminium-ceramic laminar material by the thickness of adjusting Ti paper tinsel and Al based composites paper tinsel.
The specific embodiment seven: what present embodiment and the specific embodiment six were different is: the enhancing body described in the step 1 is SiC, B
4C, TiB
2, Al
2O
3, TiC and Ti
5Si
3In one or more mixture.Other is identical with the specific embodiment six.
When the described enhancing body of present embodiment is mixture, press between each component arbitrarily than mixing.
The specific embodiment eight: what present embodiment was different with the specific embodiment six or seven is: the particle diameter of the pure Al powder described in the step 1 is 10 μ m～100 μ m, and strengthening the body particle diameter is 40nm～10 μ m.Other is identical with the specific embodiment six or seven.
The specific embodiment nine: what present embodiment was different with one of specific embodiment six to eight is: the forming laminated sheet material of the Ti-Al based composites that in the step 5 step 4 is obtained is put into vacuum hotpressing stove and is carried out Low Temperature Heat Treatment, after temperature is 660 ℃～670 ℃ insulation 5h～6h, be cooled to 450 ℃～500 ℃ pressurization 25MPa～30MPa and be incubated 1h～3h, be warming up to 750 ℃～800 ℃ insulation 2h～3h again, be cooled to 450 ℃～500 ℃ pressurization 25MPa～30MPa at last and be incubated 1h～3h, obtain Ti-TiAl
3Stratified material.Other is identical with one of specific embodiment six to eight.
The specific embodiment ten: what present embodiment was different with one of specific embodiment six to nine is: the Ti-TiAl that in the step 6 step 5 is obtained
3Stratified material is put into vacuum hotpressing stove and is carried out densified heat treatment, and the control densification temperature is 1100 ℃～1250 ℃, and temperature retention time is 1h～2h, and pressure is 30MPa～100MPa, obtains the stratified material after densified.Other is identical with one of specific embodiment six to nine.
Adopt following verification experimental verification effect of the present invention:
Test one: a kind of titanium aluminium-ceramic laminar preparation methods, carry out according to the following steps:
One, will strengthen body SiC and pure Al powder and carry out the mixed powder of ball milling, mixing the powder time is 15h, ratio of grinding media to material is 15:1, drum's speed of rotation is 200r/min, the powder that obtains mixing, and the graphite jig that the powder that mixes will be housed then carries out sintering in vacuum hotpressing stove, sintering temperature is 600 ℃, temperature retention time is 1h, and pressure is 25MPa, obtains the Al based composites; The volume fraction of pure Al powder is 98% in the wherein said Al based composites, and the volume fraction that strengthens body in the described Al based composites is 2%;
Two, the Al based composites that step 1 is obtained carries out hot extrusion and rolling, and the control extrusion temperature is 450 ℃, and extrusion ratio is 16:1, the controlled rolling temperature is 500 ℃, rolling 22 times, each drafts is 10%, and the Al based composites thickness after rolling is 320 μ m;
Three, the Al based composites after rolling to step 2 is polished, obtain Al based composites paper tinsel, adopting mass concentration then is that 10% NaOH solution cleans Al based composites paper tinsel, adopting volumetric concentration is that 10% HF solution cleans pure Ti paper tinsel, pure Ti paper tinsel after Al based composites paper tinsel after will cleaning again and the cleaning places acetone, be ultrasonic cleaning 5min under the condition of 25KHz in frequency, then in 50 ℃ of dry 3min down, the Al based composites paper tinsel after obtaining handling and handle after pure Ti paper tinsel;
Four, with 11 layers, be of a size of 30 * 30 * 0.092mm
3Processing after Al based composites paper tinsel and 12 layers, be of a size of 30 * 30 * 0.1mm
3Pure Ti paper tinsel alternative stacked after the processing, outermost layer is the pure Ti paper tinsel after the processing, carries out hot pressing then in the titanium alloy mould, and the control hot pressing temperature is 520 ℃, and temperature retention time is 1h, and pressure is 30MPa, obtains the forming laminated sheet material of Ti-Al based composites;
The forming laminated sheet material of the Ti-Al based composites that five, step 4 is obtained is put into vacuum hotpressing stove and is carried out Low Temperature Heat Treatment, after temperature is 660 ℃ of insulation 5h, be cooled to 500 ℃ of pressurization 30MPa and be incubated 1h, be warming up to 800 ℃ of insulation 3h again, be cooled to 500 ℃ of pressurization 30MPa at last and be incubated 1h, obtain Ti-TiAl
3Stratified material;
Six, the Ti-TiAl that step 5 is obtained
3Stratified material is put into vacuum hotpressing stove and is carried out densified heat treatment, and the control densification temperature is 1225 ℃, and temperature retention time is 1h, and pressure is 40MPa, obtains the stratified material after densified;
Seven, step 6 is obtained densified after stratified material place the insulation of 1200 ℃ of environment to be 10h, namely obtain TiAl-(Ti
2AlC+Ti
3AlC) titanium aluminium-ceramic laminar material.
Need be coated with one deck BN at the contact surface of mould and powder during graphite jig sintering described in this test procedure one, to prevent the reaction of powder and graphite jig.
Ratio of grinding media to material described in this test procedure one is the ratio of quality with the gross mass of the mixture that strengthens body SiC and pure Al powder of abrasive body in the ball grinder.
Adopt ESEM and X-ray diffractometer to detect the Ti-TiAl that this test procedure five obtains
3Stratified material, the result as depicted in figs. 1 and 2, the Ti-TiAl that Fig. 1 obtains for this test procedure five
3TiAl in the stratified material
3The microscopic appearance figure of layer, the Ti-TiAl that Fig. 2 obtains for this test procedure five
3TiAl in the stratified material
3The XRD figure of layer has only TiAl in the XRD collection of illustrative plates
3Diffraction maximum, illustrate through aluminium after the step 5 heat treatment all to be converted into TiAl
3
Adopt ESEM to detect the TiAl-(Ti of this test preparation
2AlC+Ti
3AlC) titanium aluminium-ceramic laminar material, the result as shown in Figure 3, Fig. 3 is the TiAl-(Ti of this test preparation
2AlC+Ti
3AlC) the microscopic appearance figure of titanium aluminium-ceramic laminar material, the white particle among Fig. 3 is generated in-situ Ti
5Si
3Phase can be improved the problem of TiAl matrix elevated temperature strength and croop property deficiency; The a place is carbide lamella, and the b place is for having lamella γ-TiAl/ α
2-Ti
3The TiAl layer of Al structure.As shown in Figure 3, utilize the in-situ authigenic technology successfully to prepare titanium aluminium-ceramic laminar material, utilize the reaction annealing process of " liquid phase is handled; the solid phase pressurization " successfully to solve the problem that the aluminium fusing is run off in the reaction annealing process, the controlled stratified material of composition height that obtains makes the controlled TiAl substrate material of suitability for industrialized production large scale and composition become possibility.
Adopt transmission electron microscope to detect the TiAl-(Ti of this test preparation
2AlC+Ti
3AlC) titanium aluminium-ceramic laminar material, the result as shown in Figure 4 and Figure 5, Fig. 4 is the TiAl-(Ti of this test preparation
2AlC+Ti
3AlC) lamella γ-TiAl/ α in titanium aluminium-ceramic laminar material
2-Ti
3The microscopic appearance figure of Al, wherein black is organized as α
2-Ti
3Al, white is organized as γ-TiAl, and sheet interlayer spacing is 100nm～500nm.γ-TiAl/ α
2-Ti
3The generation of Al lamellar structure has illustrated that aluminium does not run off in the reaction annealing process, the aluminium content approximately equal of the aluminium content of this tissue and the Ti-Al based composites that step 4 obtains, and compare with single-phase TiAl and to have better intensity and plasticity; Fig. 5 is the TiAl-(Ti of this test preparation
2AlC+Ti
3AlC) lamella γ-TiAl/ α in titanium aluminium-ceramic laminar material
2-Ti
3The diffraction spot point diagram of Al, γ-TiAl and α
2-Ti
3Al has less sheet interlayer spacing, certain orientation relationship and good interface combination, all will play good malleableize effect to titanium aluminium-ceramic laminar material.
Adopt transmission electron microscope to detect the TiAl-(Ti of this test preparation
2AlC+Ti
3AlC) titanium aluminium-ceramic laminar material, result such as Fig. 6, Fig. 7 and shown in Figure 8, Fig. 6 is the TiAl-(Ti of this test preparation
2AlC+Ti
3AlC) the microscopic appearance figure of carbide lamella in titanium aluminium-ceramic laminar material, wherein a place is Ti
2AlC, b place are Ti
3AlC, its symbiosis explanation two-phase good interface combination; Fig. 7 is Ti in the carbide lamella
2The diffraction spot point diagram of AlC phase, Fig. 8 are Ti in the carbide lamella
3The diffraction spot point diagram of AlC phase, by Fig. 6, Fig. 7 and Fig. 8 as can be known, carbide lamella is mainly by Ti
2AlC and Ti
3AlC forms, and carbide lamella and TiAl layer that in-situ authigenic generates distribute alternately, and unique layer structure can compensate the deficiency of monolayer material internal performance, obtains the material of obdurability best fit.
Claims (10)
1. titanium aluminium-ceramic laminar material is characterized in that titanium aluminium-ceramic laminar material is to utilize the in-situ authigenic technology to be made by pure Ti paper tinsel and Al based composites paper tinsel alternative stacked, hot pressing and reaction annealing; TiAl layer and ceramic layer distribute alternately in described titanium aluminium-ceramic laminar material, and the lamination spacing is 5 μ m～100 μ m, and ceramic layer comprises Ti
2AlC phase and Ti
3The AlC phase is lamella γ-TiAl/ α in the TiAl layer
2-Ti
3Al, sheet interlayer spacing are 100nm～500nm; Described Al based composites paper tinsel is by strengthening body and pure Al powder through mixing powder, hot pressed sintering and rolling making.
2. a kind of titanium aluminium according to claim 1-ceramic laminar material, the thickness in monolayer that it is characterized in that described pure Ti paper tinsel is 50 μ m～200 μ m, the thickness in monolayer of described pure Ti paper tinsel and Al based composites paper tinsel is than being (1.04～1.14): 1.
3. a kind of titanium aluminium according to claim 1-ceramic laminar material is characterized in that the volume fraction of pure Al powder in the described Al based composites paper tinsel is 85%～99.9%, and the volume fraction that strengthens body in the described Al based composites paper tinsel is 0.1%～15%.
4. a kind of titanium aluminium according to claim 1-ceramic laminar material, the particle diameter that it is characterized in that described pure Al powder is 10～100 μ m, strengthening the body particle diameter is 40nm～10 μ m.
5. a kind of titanium aluminium according to claim 1-ceramic laminar material is characterized in that described enhancing body is SiC, B
4C, TiB
2, Al
2O
3, TiC and Ti
5Si
3In one or more mixture.
6. a kind of titanium aluminium as claimed in claim 1-ceramic laminar preparation methods is characterized in that titanium aluminium-ceramic laminar preparation methods is to carry out according to the following steps:
One, will strengthen body and pure Al powder and carry out the mixed powder of ball milling, mixing the powder time is 6h～20h, ratio of grinding media to material is (10～20): 1, drum's speed of rotation is 150r/min～250r/min, the powder that obtains mixing, and the graphite jig that the powder that mixes will be housed then carries out sintering in vacuum hotpressing stove, sintering temperature is 500 ℃～620 ℃, temperature retention time is 1h～2h, and pressure is 20MPa～30MPa, obtains the Al based composites; The volume fraction of pure Al powder is 85%～99.9% in the wherein said Al based composites, and the volume fraction that strengthens body in the described Al based composites is 0.1%～15%;
Two, the Al based composites that step 1 is obtained carries out hot extrusion and rolling, the control extrusion temperature is 400 ℃～500 ℃, extrusion ratio is (10～20): 1, the controlled rolling temperature is 20 ℃～500 ℃, rolling 10 times～50 times, each drafts is 5%～30%, and the Al based composites thickness after rolling is 100 μ m～500 μ m;
Three, the Al based composites after rolling to step 2 is polished, obtain Al based composites paper tinsel, adopting mass concentration then is that 5%～30% NaOH solution cleans Al based composites paper tinsel, adopting volumetric concentration is that 5%～30% HF solution cleans pure Ti paper tinsel, pure Ti paper tinsel after Al based composites paper tinsel after will cleaning again and the cleaning places acetone, be ultrasonic cleaning 3min～10min under the condition of 20KHz～30KHz in frequency, then in 20 ℃～70 ℃ following dry 1min～5min, the pure Ti paper tinsel after the Al based composites paper tinsel after obtaining handling and the processing;
Four, the pure Ti paper tinsel alternative stacked after the Al based composites paper tinsel after the processing that step 3 is obtained and the processing, outermost layer is the pure Ti paper tinsel after the processing, in the titanium alloy mould, carry out hot pressing then, the control hot pressing temperature is 400 ℃～550 ℃, temperature retention time is 1h～2h, pressure is 20MPa～30MPa, obtains the forming laminated sheet material of Ti-Al based composites; Pure Ti paper tinsel thickness in monolayer after the processing that wherein said step 3 obtains is 50 μ m～200 μ m, the pure Ti paper tinsel after the processing that described step 3 obtains with handle after the thickness in monolayer of Al based composites paper tinsel than being (1.04～1.14): 1;
The forming laminated sheet material of the Ti-Al based composites that five, step 4 is obtained is put into vacuum hotpressing stove and is carried out Low Temperature Heat Treatment, after temperature is 650 ℃～670 ℃ insulation 4h～6h, be cooled to 400 ℃～500 ℃ pressurization 20MPa～30MPa and be incubated 0.5h～3h, be warming up to 700 ℃～800 ℃ insulation 2h～3h again, be cooled to 400 ℃～500 ℃ pressurization 20MPa～30MPa at last and be incubated 0.5h～3h, obtain Ti-TiAl
3Stratified material;
Six, the Ti-TiAl that step 5 is obtained
3Stratified material is put into vacuum hotpressing stove and is carried out densified heat treatment, and the control densification temperature is 1000 ℃～1300 ℃, and temperature retention time is 0.5h～2h, and pressure is 20MPa～100MPa, obtains the stratified material after densified;
Seven, step 6 is obtained densified after stratified material place the insulation of 1100 ℃～1300 ℃ environment to be 3h～10h, namely obtain TiAl-(Ti
2AlC+Ti
3AlC) titanium aluminium-ceramic laminar material.
7. a kind of titanium aluminium according to claim 6-ceramic laminar preparation methods is characterized in that the enhancing body described in the step 1 is SiC, B
4C, TiB
2, Al
2O
3, TiC and Ti
5Si
3In one or more mixture.
8. a kind of titanium aluminium according to claim 6-ceramic laminar preparation methods, the particle diameter that it is characterized in that the pure Al powder described in the step 1 is 10 μ m～100 μ m, strengthening the body particle diameter is 40nm～10 μ m.
9. a kind of titanium aluminium according to claim 6-ceramic laminar preparation methods, the forming laminated sheet material that it is characterized in that the Ti-Al based composites that in the step 5 step 4 obtained is put into vacuum hotpressing stove and is carried out Low Temperature Heat Treatment, after temperature is 660 ℃～670 ℃ insulation 5h～6h, be cooled to 450 ℃～500 ℃ pressurization 25MPa～30MPa and be incubated 1h～3h, be warming up to 750 ℃～800 ℃ insulation 2h～3h again, be cooled to 450 ℃～500 ℃ pressurization 25MPa～30MPa at last and be incubated 1h～3h, obtain Ti-TiAl
3Stratified material.
10. a kind of titanium aluminium according to claim 6-ceramic laminar preparation methods is characterized in that the Ti-TiAl that in the step 6 step 5 is obtained
3Stratified material is put into vacuum hotpressing stove and is carried out densified heat treatment, and the control densification temperature is 1100 ℃～1250 ℃, and temperature retention time is 1h～2h, and pressure is 30MPa～100MPa, obtains the stratified material after densified.
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