CN109940944A - A method of regulation titanium composite material reinforcement layered distribution - Google Patents

A method of regulation titanium composite material reinforcement layered distribution Download PDF

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Publication number
CN109940944A
CN109940944A CN201910307233.9A CN201910307233A CN109940944A CN 109940944 A CN109940944 A CN 109940944A CN 201910307233 A CN201910307233 A CN 201910307233A CN 109940944 A CN109940944 A CN 109940944A
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China
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composite material
reinforcement
titanium composite
foil
pure
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CN201910307233.9A
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Inventor
吴昊
胡海波
张浩天
周港怀
刘阳
张学谦
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University of Jinan
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University of Jinan
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Abstract

A method of regulation titanium composite material reinforcement layered distribution is related to the technical method of metal-base composites reinforcement distribution mode and regulation.The invention solves the problems that reinforcement layered distribution present in metal-base composites industrial production is difficult to control.Method: the one, polishing and surface treatment of titanium composite material foil and pure aluminum foil;Two, hot pressing connects;Three, reaction heat treatment realizes the stratiform controlled distribution of reinforcement using the push effect that elements diffusion generates, and ensures effective connection of reinforcement and basal body interface.The present invention is based on vacuum reaction annealing technology, the material oxygen content of synthesis is low, pollution-free, and material is fine and close, fine microstructures and reinforcement distribution is controllable, and reaction rate is fast, and synthesis cycle is short.The present invention is used for the preparation field of high-performance metal based composites.

Description

A method of regulation titanium composite material reinforcement layered distribution
Technical field
The present invention relates to metal-base composites reinforcement distribution mode and the technical methods of regulation.
Background technique
China is the manufacture big country of engineering mechanical device.Metal material manufacturing industry is the core of mechanical industry, is concerning state Family economic security, the strategic pillar industry of national defense safety.Integrated and development lightweight, high-strength, high-ductility metallic composite are The unremitting pursuit of domestic and international researcher.The research of the past few decades, which is concentrated mainly on, utilizes refined crystalline strengthening, solution strengthening, more It dissipates the modes such as reinforcing and improves the mechanical property of material, but facts have proved only by solely adjusting Fine Texture of Material/structure dimension Traditional material mentality of designing frequently can lead to the strength of materials and the imbalance of modeling/toughness.Chinese Academy of Sciences metal Suo Lu Ke Yuan in 2010 Scholar proposes the multiple dimensioned configuration design theory of metal material, attempts to turn traditional " reinforcement distribution mode as uniform as possible " Become novel " the non-uniform reinforcement distribution mode with specific heterojunction structure (such as layered distribution) ", to obtain performance More excellent metal-base composites.The Research Thinking is tested in the metal/metals laminar composite such as Cu/Al Card, but there are still technical problems for the controllable stratiform regulation that realization reinforcement is distributed in metal-base composites.
Summary of the invention
The invention solves reinforcement layered distributions present in high-performance metal based composites industrial production to be difficult to control The problem of processed, and provide the technical method of a kind of titanium composite material reinforcement distribution mode and regulation.
The method of regulation titanium composite material reinforcement layered distribution of the invention is to sequentially include the following steps:
One, Ti based composites and pure Al plate are polished into Ti based composites foil and pure Al foil, are using volumetric concentration respectively The NaOH solution that 3% ~ 20% HF solution and mass concentration is 3% ~ 20% is surface-treated, then by Ti based composites foil and pure Al foil is successively cleaned by ultrasonic and dries in acetone and ethyl alcohol.Pure Al foil after surface treatment is with a thickness of 50 μm ~ 300 μm, Ti base The thickness ratio of composite material and pure Al plate is 1 ~ 9;
Two, by step 1 treated Ti based composites foil and pure Al foil alternative stacked, jacket is placed in graphite jig, true Hot pressing connects are carried out in empty hot-pressed sintering furnace, control hot pressing temperature is 350 DEG C ~ 600 DEG C, and pressure is 20MPa ~ 100MPa, heat preservation Time is 1h ~ 3h.Jacket used in hot pressing is made of pure titanium;
Three, the Ti-Al based composite material sheet material that step 2 obtains is put into vacuum hotpressing stove and is heat-treated, control heat treatment Temperature is 550 DEG C ~ 800 DEG C, keeps the temperature 1h ~ 10h, then be warming up to 1000 DEG C ~ 1400 DEG C progress high-temperature heat treatments, application 20MPa ~ The pressure and pressure maintaining 1h ~ 5h of 70MPa.Titanium composite material enhancing layered body point is realized using the phase counterdiffusion of Ti and Al element The purpose of cloth.
The beneficial effects of the present invention are: the push effect that (1) present invention is generated using elements diffusion, realizes reinforcement Stratiform controlled distribution, and ensure effective connection of reinforcement and basal body interface;(2) of the invention by multilayer Ti-Al composite plate It is sealed in the jacket of pure titanium, is effectively prevented graphite jig and participates in reacting and polluting;(3) present invention is anti-using vacuum It should anneal, the material oxygen content of synthesis is low, pollution-free, and material is fine and close, fine microstructures and reinforcement distribution is controllable;(4) reaction speed Rate is fast, and synthesis cycle is short.
Detailed description of the invention
Fig. 1 is the microstructure that the reinforcement of embodiment preparation is in the TiB/Ti based composites of layered distribution.
Specific embodiment
Technical solution of the present invention is not limited to the specific embodiment of act set forth below, further include each specific embodiment it Between any combination.
Specific embodiment 1: a kind of method of regulation titanium composite material reinforcement layered distribution of present embodiment is It sequentially includes the following steps:
One, Ti based composites and pure Al plate are polished into Ti based composites foil and pure Al foil, are using volumetric concentration respectively The NaOH solution that 3% ~ 20% HF solution and mass concentration is 3% ~ 20% is surface-treated, then by Ti based composites foil and pure Al foil is successively cleaned by ultrasonic and dries in acetone and ethyl alcohol.Pure Al foil after surface treatment is with a thickness of 50 μm ~ 300 μm, Ti base The thickness ratio of composite material and pure Al plate is 1 ~ 9;
Two, by step 1 treated Ti based composites foil and pure Al foil alternative stacked, jacket is placed in graphite jig, true Hot pressing connects are carried out in empty hot-pressed sintering furnace, control hot pressing temperature is 350 DEG C ~ 600 DEG C, and pressure is 20MPa ~ 100MPa, heat preservation Time is 1h ~ 3h.Jacket used in hot pressing is made of pure titanium;
Three, the Ti-Al based composite material sheet material that step 2 obtains is put into vacuum hotpressing stove and is heat-treated, control heat treatment Temperature is 550 DEG C ~ 800 DEG C, keeps the temperature 1h ~ 10h, then be warming up to 1000 DEG C ~ 1400 DEG C progress high-temperature heat treatments, application 20MPa ~ The pressure and pressure maintaining 1h ~ 5h of 70MPa.Titanium composite material enhancing layered body point is realized using the phase counterdiffusion of Ti and Al element The purpose of cloth.
Specific embodiment 2: the present embodiment is different from the first embodiment in that: titanium-based composite wood in step 1 Material is made of volume fraction of 85% ~ 99% titanium and 1% ~ 15% reinforcement.It is other same as the specific embodiment one.
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that: titanium-based is multiple in step 1 The reinforcement morphology of condensation material is the combination of one or more of whisker, fiber or particle, and reinforcement type is energy and matrix SiC, B of reaction4C、TiB2One or more of combination, can also be and matrix nonreactive TiC, TiB, Ti5Si3In One or more of combinations.It is other the same as one or two specific embodiments.
Specific embodiment 4: unlike one of present embodiment and specific embodiment one to three: titanium in step 1 The average grain diameter of Ti is 5 μm ~ 200 μm in based composites, and the average or equivalent grain size of reinforcement is 10nm ~ 10 μm.It is other with One of specific embodiment one to three is identical.
Specific embodiment 5: unlike one of present embodiment and specific embodiment one to four: in step 1 The mass concentration of NaOH solution is that the volumetric concentration of 10%, HF solution is 10%.Other phases one of with specific embodiment one to four Together.
Specific embodiment 6: unlike one of present embodiment and specific embodiment one to five: Ti in step 1 The thickness ratio of based composites and pure Al plate is 7.6:1.It is other identical as one of specific embodiment one to five.
Specific embodiment 7: unlike one of present embodiment and specific embodiment one to six: Ti in step 2 The number of plies of based composites foil is 13 layers, and the number of plies of pure Al foil is 12 layers.It is other identical as one of specific embodiment one to six.
Specific embodiment 8: unlike one of present embodiment and specific embodiment one to seven: being controlled in step 2 Hot pressing temperature processed is 515 DEG C, pressure 70MPa, soaking time 1.5h.Other phases one of with specific embodiment one to seven Together.
Specific embodiment 9: unlike one of present embodiment and specific embodiment one to eight: being controlled in step 3 Heating treatment temperature is 700 DEG C, keeps the temperature 1h, then be warming up to 1100 DEG C of progress high-temperature heat treatments, applies the pressure of 30MPa and pressure maintaining 4.5h.It is other identical as one of specific embodiment one to eight.
Beneficial effects of the present invention are verified using following embodiment:
A kind of method of regulation titanium composite material reinforcement layered distribution of the present embodiment, is specifically prepared according to the following steps :
One, powder metallurgic method prepares the equally distributed TiB/Ti based composites of reinforcement.The average grain diameter of Ti is 100 μm, is increased The equivalent grain size of strong body is 5 μm.TiB/Ti based composites and pure Al plate are polished into TiB/Ti based composites foil and pure Al The NaOH solution that the HF solution and mass concentration that foil is respectively 10% using volumetric concentration are 10% is surface-treated, then by Ti Based composites foil and pure Al foil are successively cleaned by ultrasonic and dry in acetone and ethyl alcohol.Pure Al foil after surface treatment with a thickness of 100 μm, the thickness ratio of Ti based composites and pure Al plate is 7.6;
Two, by step 1 treated Ti based composites foil and pure Al foil alternative stacked, the number of plies of Ti based composites foil is 13 layers, the number of plies of pure Al foil is 12 layers, and jacket is placed in graphite jig, and hot pressing connects are carried out in vacuum sintering funace, is controlled Hot pressing temperature processed is 515 DEG C, pressure 70MPa, soaking time 1.5h.Jacket used in hot pressing is made of pure titanium;
Three, the Ti-Al based composite material sheet material that step 2 obtains is put into vacuum hotpressing stove and is heat-treated, control heat treatment Temperature is 700 DEG C, keeps the temperature 1h, then be warming up to 1100 DEG C of progress high-temperature heat treatments, applies the pressure and pressure maintaining 4.5h of 30MPa.Benefit The purpose of titanium composite material reinforcement layered distribution is realized with the phase counterdiffusion of Ti and Al element.
The scanning electron microscope (SEM) photograph of TiB/Ti based composites manufactured in the present embodiment is as shown in Figure 1.The composite material of synthesis causes Close no hole, reinforcement TiB are well combined in layered distribution and with matrix.

Claims (9)

1. a kind of method of regulation titanium composite material reinforcement layered distribution, it is characterised in that realize titanium composite material enhancing The layered distribution of body controls, and is specifically prepared according to the following steps:
One, Ti based composites and pure Al plate are polished into Ti based composites foil and pure Al foil, are using volumetric concentration respectively The NaOH solution that 3% ~ 20% HF solution and mass concentration is 3% ~ 20% is surface-treated, then by Ti based composites foil and pure Al foil is successively cleaned by ultrasonic and dries in acetone and ethyl alcohol, and the pure Al foil after surface treatment is with a thickness of 50 μm ~ 300 μm, Ti base The thickness ratio of composite material and pure Al plate is 1 ~ 9;
Two, by step 1 treated Ti based composites foil and pure Al foil alternative stacked, jacket is placed in graphite jig, true Hot pressing connects are carried out in empty hot-pressed sintering furnace, control hot pressing temperature is 350 DEG C ~ 600 DEG C, and pressure is 20MPa ~ 100MPa, heat preservation Time is 1h ~ 3h, and jacket used in hot pressing is made of pure titanium;
Three, the Ti-Al based composite material sheet material that step 2 obtains is put into vacuum hotpressing stove and is heat-treated, control heat treatment Temperature is 550 DEG C ~ 800 DEG C, keeps the temperature 1h ~ 10h, then be warming up to 1000 DEG C ~ 1400 DEG C progress high-temperature heat treatments, application 20MPa ~ The pressure and pressure maintaining 1h ~ 5h of 70MPa realizes titanium composite material enhancing layered body point using the phase counterdiffusion of Ti and Al element The purpose of cloth.
2. the method for regulation titanium composite material reinforcement layered distribution according to claim 1, it is characterised in that step Titanium composite material is made of volume fraction of 85% ~ 99% titanium and 1% ~ 15% reinforcement in one.
3. the method for regulation titanium composite material reinforcement layered distribution according to claim 1, it is characterised in that step The reinforcement morphology of titanium composite material is the combination of one or more of whisker, fiber or particle, reinforcement type in one It is SiC, the B that can be reacted with matrix4C、TiB2One or more of combination, can also be with the nonreactive TiC, TiB of matrix, Ti5Si3One or more of combination.
4. the method for regulation titanium composite material reinforcement layered distribution according to claim 1, it is characterised in that step The average grain diameter of Ti is 5 μm ~ 200 μm in titanium composite material in one, and the average or equivalent grain size of reinforcement is 10nm ~ 10 μm.
5. the method for regulation titanium composite material reinforcement layered distribution according to claim 1, it is characterised in that step It is 10% that the mass concentration of NaOH solution, which is the volumetric concentration of 10%, HF solution, in one.
6. the method for regulation titanium composite material reinforcement layered distribution according to claim 1, it is characterised in that step The thickness ratio of Ti based composites and pure Al plate is 7.6:1 in one.
7. the method for regulation titanium composite material reinforcement layered distribution according to claim 1, it is characterised in that step The number of plies of Ti based composites foil is 13 layers in two, and the number of plies of pure Al foil is 12 layers.
8. the method for regulation titanium composite material reinforcement layered distribution according to claim 1, it is characterised in that step It is 515 DEG C, pressure 70MPa, soaking time 1.5h that hot pressing temperature is controlled in two.
9. the method for regulation titanium composite material reinforcement layered distribution according to claim 1, it is characterised in that step It is 700 DEG C that heat treatment temperature is controlled in three, keeps the temperature 1h, then be warming up to 1100 DEG C of progress high-temperature heat treatments, applies the pressure of 30MPa And pressure maintaining 4.5h.
CN201910307233.9A 2019-04-17 2019-04-17 A method of regulation titanium composite material reinforcement layered distribution Pending CN109940944A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110369690A (en) * 2019-08-19 2019-10-25 西安航空学院 A kind of graphite film block composite material and preparation method thereof of Al and Ti hybrid buildup
CN113511895A (en) * 2021-04-23 2021-10-19 西安航空学院 TiC/graphite film layered composite material and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110369690A (en) * 2019-08-19 2019-10-25 西安航空学院 A kind of graphite film block composite material and preparation method thereof of Al and Ti hybrid buildup
CN113511895A (en) * 2021-04-23 2021-10-19 西安航空学院 TiC/graphite film layered composite material and preparation method thereof

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