CN108411154A - A kind of fire-retardant graphene titanium-aluminium matrix composites and preparation method - Google Patents
A kind of fire-retardant graphene titanium-aluminium matrix composites and preparation method Download PDFInfo
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- CN108411154A CN108411154A CN201810164334.0A CN201810164334A CN108411154A CN 108411154 A CN108411154 A CN 108411154A CN 201810164334 A CN201810164334 A CN 201810164334A CN 108411154 A CN108411154 A CN 108411154A
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- C22C14/00—Alloys based on titanium
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Abstract
The invention belongs to titanium materials technology field, it is related to a kind of fire-retardant graphene titanium-aluminium matrix composites and preparation method.The composite material, which includes group by mass percentage, to be become：The graphene oxide and titanium aluminium based compound of 0.01~1wt%.The method being combined using temperature control mechanical agitation, vacuumize process and hot isostatic pressing etc., improve the interface binding characteristic of graphene oxide and titanium aluminium based compound mixed-powder, improve the apparent density and subsequent forming of mixed-powder, and graphene oxide is made substantially to be decomposed to form graphene and evenly dispersed, the very good mechanical properties and physical and chemical performance of graphene are given full play to, obtain the flame retardant property 2 times or more higher than common high-temperature titanium alloy of composite material, and heat resistance is more preferable, and completely new technical solution is provided to solve aero-engine titanium fire.The present invention is new material concept, and preparation process flow is short, state modulator is accurate, and batch is suitble to prepare.
Description
Technical field
The invention belongs to titanium materials technology field, it is related to a kind of titanium matrix composite and preparation method, especially relates to
And a kind of fire-retardant graphene titanium-aluminium matrix composites and preparation method.
Background technology
Demand of the high-performance advanced aero engine to titanium dosage is improved is highlighted with the increased sharp contradiction of titanium fire tendentiousness,
Cause titanium fire Frequent Accidents.Effective pre- titanium fire preventing, the titanium dosage of raising compressor are the current and following advanced aero engine skills
One of the great difficult problem that art faces.
Titanium aluminium based compound material becomes advanced aero engine height with advantages such as its high creep resistance, high flame resistances
Warm structure is using one of most potential material, for key components and parts such as the blades of high-pressure compressor and low-pressure turbine.However,
The performances such as temperature-room type plasticity, the wearability of titanium aluminium based compound are poor, and it is pre- cannot to meet the following high-performance/new concept aero-engine
The active demand of titanium fire preventing.
Graphene rapidly becomes and structure-integrated material because having the function of excellent mechanical performance and physical and chemical performance
The ideal Nano filling of material provides new thinking for the titanium-aluminium matrix composites development with flame retarding function.However, graphene
Itself is easy the problems such as reuniting and will being chemically reacted at quite low temperatures with titanium, constrains it in titanium aluminium base alloy
It widely applies.In presently disclosed document report, using " ball milling of elemental mixing method+discharge plasma sintering " or " dry mixed+
Graphene uniform cannot be mixed into titanium aluminium base alloy by the technologies such as discharge plasma sintering ".
Invention content
The present invention exactly for the above-mentioned prior art the problem of and design and propose a kind of fire-retardant graphene titanium aluminium base
Composite material and preparation method.
The technical scheme is that
A kind of fire-retardant graphene titanium-aluminium matrix composites include following compositions by mass percentage：Graphene oxide is
0.01~1wt%, remaining is titanium aluminium based compound.
The composition of the titanium aluminium based compound is calculated as by atomic percent：Al：45~47at%, Cr：1~2at%, Nb：2
~5at%, Ta：0~2at%, W：0~2at%, Mo：0~2at%, Zr：0~2at%, Hf：0~2at%, B：0~
0.2at%, Si：0~0.2at%, O：0~0.25at%, remaining is Ti.
Preferably, the composition of the titanium aluminium based compound is calculated as by atomic percent：Al：45~47at%, Cr：1~
2at%, Nb：3~5at%, Ta：0.1~0.3at%, B：0~0.1at%, Si：0~0.1at%, remaining is Ti.
A method of fire-retardant graphene titanium-aluminium matrix composites of the present invention are prepared, are included the following steps：
(1) the stannic oxide/graphene nano piece of 0.01~1wt% of titanium aluminium based compound powder quality is added to anhydrous second
In alcohol, decentralized processing 30min or more then is carried out using ultrasonic cell disrupte machine, working frequency is vibration 2s, gap 3s, is prepared
Go out graphene oxide solution；
(2) be 30~150 μm by grain size, oxygen content is less than the spherical or subsphaeroidal titanium aluminium based compound powder of 1000ppm
It is stirred and mixes in temperature control mechanical agitator with the graphene oxide solution of step (1), prepare graphene oxide and titanium
Aluminium based compound mixed-powder slurry, mixing speed are 500~1200r/min, and mixing time is 50~120min, whipping temp
It is 50~70 DEG C；
(3) baking oven by the slurry of the graphene oxide of step (2) and titanium aluminium based compound mixed-powder at 50~60 DEG C
5~10h of interior drying process obtains graphene oxide and titanium aluminium based compound mixed-powder；
(4) graphene oxide of step (3) and titanium aluminium based compound mixed-powder are fitted into stainless steel capsule, it is then right
Jacket carries out vacuumize process, and room temperature vacuumizes 1.5~3.5h, until vacuum degree≤5Pa, with the rate of heat addition liter of 1~5 DEG C/min
Temperature starts to keep the temperature to 200~300 DEG C, until vacuum degree≤1 × 10-21.5~2.5h is kept the temperature after Pa, continues adding with 1~5 DEG C/min
Hot rate is warming up to 500~700 DEG C and starts to keep the temperature, until vacuum degree≤1 × 10-38~20h is kept the temperature after Pa, then welds jacket
Sealing；
(5) the sealing jacket of step (4) is subjected to hot isostatic pressing, obtains fine and close fire-retardant graphene titanium aluminum-base composite material
Material, heating temperature are 900~1300 DEG C, and heat preservation pressure is 120~150MPa, and soaking time is 2~4h；
(6) the fire-retardant graphene titanium-aluminium matrix composites of step (5) are subjected to Canned Hot molding, prepare fire-retardant stone
Black alkene titanium-aluminium matrix composites bar stock, extrusion ratio are 5~10, and heating temperature is 1200~1300 DEG C, mold preheating temperature 300
~500 DEG C, extrusion speed is 10~30mm/s.
The titanium aluminium based compound powder is prepared using gas atomization.
The stainless steel capsule is substituted by pure titanium or titanium alloy jacket.
The Canned Hot molding is substituted by jacket heat rolling-forming, prepares fire-retardant graphene titanium-aluminium matrix composites
Slab.
The present invention has the following advantages and high-lighting effect：
1) flame retardant property of fire-retardant graphene titanium-aluminium matrix composites is more excellent, 2 times higher than common high-temperature titanium alloy with
On, and heat resistance is more preferable, and completely new technical solution is provided to solve aero-engine titanium fire.
2) use graphene oxide as nanometer reinforcement, in conjunction with processes such as temperature control mechanical agitation, vacuumize processs,
The interface binding characteristic for not only improving graphene oxide and titanium aluminium based compound mixed-powder, substantially increases mixed-powder
Apparent density, the mouldability for improving follow-up powder metallurgy, and graphene oxide can be made substantially to be decomposed to form graphene
And it is evenly dispersed, play graphene very good mechanical properties and physical and chemical performance.
3) by jacket hot isostatic pressing and thermal deformation (extruding, rolling etc.) technique, it is multiple to realize fire-retardant graphene titanium aluminium base
The high densification of condensation material is molded, and even tissue, mechanical performance is also significantly improved.For example, compared with alloy substrate, it is multiple
The density of condensation material is lower；While room temperature tensile intensity slightly improves, plasticity improves 20% or more；Friction coefficient reduces about
10%, wear rate reduces by 20% or more.
4) present invention is new material concept, and preparation process flow is short, state modulator is accurate, is suitble to fire-retardant graphene titanium aluminium
Prepared by the batch of based composites, have a extensive future.
Specific implementation mode
The fire-retardant graphene titanium-aluminium matrix composites and preparation method of the present invention are obtained by following steps.
(1) by titanium aluminium based compound, (composition is calculated as by atomic percent, Al：45~47at%, Cr：1~2at%, Nb：
3~5at%, Ta：0.1~0.3at%, B：0~0.1at%, Si：0~0.1at%, remaining is Ti) it is used as fire-retardant graphene titanium
The matrix of aluminum matrix composite, spherical or subsphaeroidal pre-alloyed powder is prepared using gas atomization, and grain size is 30~150 μ
M, oxygen content is less than 1000ppm.
(2) 3g stannic oxide/graphene nano pieces are added in 500~1000ml absolute ethyl alcohols, then utilize ultrasonic cell powder
Broken machine carries out decentralized processing 30min or more, and working frequency is vibration 2s, gap 3s, obtains monodispersed graphene oxide solution；
(3) the above-mentioned titanium aluminium based compound powder of 997g is stirred with graphene oxide solution in temperature control mechanical agitator
Mixing is mixed, the slurry of the good graphene oxide of interface cohesion and titanium aluminium based compound mixed-powder is prepared, mixing speed is
500~1200r/min, mixing time are 50~120min, and whipping temp is 50~70 DEG C；Then by the slurry of mixed-powder
5~10h of processing is dried in 50~60 DEG C of baking oven, obtains graphene oxide and titanium aluminium based compound mixed-powder；
(4) graphene oxide and titanium aluminium based compound mixed-powder are fitted into stainless steel capsule, are changed by constantly shaking
It has been apt to the apparent density of mixed-powder, vacuumize process then has been carried out to jacket, room temperature vacuumizes 1.5~3.5h, until vacuum degree
≤ 5Pa is warming up to 200~300 DEG C with the rate of heat addition of 1~5 DEG C/min and starts to keep the temperature, until vacuum degree≤1 × 10-2It is kept the temperature after Pa
1.5~2.5h, continuation are warming up to 500~700 DEG C with the rate of heat addition of 1~5 DEG C/min and start to keep the temperature, until vacuum degree≤1 ×
10-38~20h is kept the temperature after Pa obtains the graphene oxide that graphene oxide content is about 0.3% then by jacket welded seal
With titanium aluminium based compound mixed-powder；
(5) jacket after encapsulation is subjected to hot isostatic pressing, obtains fine and close fire-retardant graphene titanium-aluminium matrix composites, heating
Temperature is 900~1300 DEG C, and heat preservation pressure is 120~150MPa, and soaking time is 2~4h, by composite sample and
Initial powder carries out Raman spectrum analysis before hot isostatic pressing, show that the characteristic peak of graphene oxide disappears substantially, and stone occurs
The characteristic peak of black alkene illustrates that graphene oxide has substantially been decomposed to form graphene in composite material after hot isostatic pressing.
(6) fire-retardant graphene titanium-aluminium matrix composites are subjected to Canned Hot molding, prepare fire-retardant graphene titanium aluminium
Based composites bar stock sample, extrusion ratio be 5~10, heating temperature be 1200~1300 DEG C, mold preheating temperature be 300~
500 DEG C, extrusion speed is 10~30mm/s.
The present invention is further explained in the light of specific embodiments, but the present invention is not limited to following embodiments.
Embodiment 1
Powder In Argon Atomization is used to prepare the spherical or subsphaeroidal conjunction that grain size is less than 1000ppm for 30~105 μm, oxygen content
Bronze end, nominal composition are Ti-46Al-5Nb-2Cr (atomic percent, at%)；1.5g stannic oxide/graphene nano pieces are added
It adds in 500ml absolute ethyl alcohols, carries out decentralized processing 40min using ultrasonic cell disrupte machine, working frequency is vibration 2s, gap
3s obtains graphene oxide solution, then by the above-mentioned alloy powders of 998.5g and graphene oxide solution in temperature control mechanical agitation
Mixing is stirred in device, mixing speed is 500~600r/min, and mixing time is 50~80min, and whipping temp is 60 DEG C,
The slurry of graphene oxide and titanium aluminium based compound mixed-powder is prepared, and processing is dried in 50~60 DEG C of baking oven
5~10h obtains graphene oxide and titanium aluminium based compound mixed-powder and is fitted into vacuumize process in stainless steel capsule, room temperature
2h is vacuumized, until vacuum degree≤5Pa, is warming up to 200~300 DEG C with the rate of heat addition of 1~5 DEG C/min and starts to keep the temperature, until vacuum
Degree≤1 × 10-22h is kept the temperature after Pa, continuation is warming up to 500~600 DEG C with the rate of heat addition of 1~5 DEG C/min and starts to keep the temperature, until true
Reciprocal of duty cycle≤1 × 10-312h is kept the temperature after Pa, then by jacket welded seal；Jacket after encapsulation is subjected to hot isostatic pressing, heating temperature
Degree is 1200~1300 DEG C, and heat preservation pressure is 120~150MPa, soaking time 3h, obtains fine and close fire-retardant graphene titanium aluminium
Based composites simultaneously carry out Canned Hot molding, and extrusion ratio is 5~10, and heating temperature is 1200~1300 DEG C, mold preheating
Temperature is 400 DEG C, and extrusion speed is 10~30mm/s, to prepare fire-retardant graphene titanium-aluminium matrix composites bar stock.Using
The friction ignition equipment of middle Air China hair Beijing Research Inst. of Aeronautic Material carries out flammability test, obtains in identical flow conditions
Under, the high 2 times or more of titanium alloys such as flame retardant property ratio TA15, TC4 of fire-retardant graphene titanium-aluminium matrix composites.
Embodiment 2
Powder In Argon Atomization is used to prepare the spherical or subsphaeroidal conjunction that grain size is less than 1000ppm for 53~104 μm, oxygen content
Bronze end, nominal composition are Ti-46Al-4Nb-1.6Cr-0.2Ta-0.1B-0.1Si (atomic percent, at%)；By 0.5g
Stannic oxide/graphene nano piece is added in 200ml absolute ethyl alcohols, and decentralized processing 30min, work are carried out using ultrasonic cell disrupte machine
Working frequency is vibration 2s, gap 3s, graphene oxide solution is obtained, then by the above-mentioned alloy powders of 999.5g and graphene oxide
Solution is stirred mixing in temperature control mechanical agitator, and mixing speed is 500~600r/min, and mixing time is 50~
80min, whipping temp are 60 DEG C, prepare the slurry of graphene oxide and titanium aluminium based compound mixed-powder, and 50~60
DEG C baking oven in 5~10h of processing is dried, obtain graphene oxide and titanium aluminium based compound mixed-powder and be packed into stainless steel
Vacuumize process in jacket, room temperature vacuumize 2h, until vacuum degree≤5Pa, 200 are warming up to the rate of heat addition of 1~5 DEG C/min~
300 DEG C start to keep the temperature, until vacuum degree≤1 × 10-22h is kept the temperature after Pa, continues to be warming up to 500 with the rate of heat addition of 1~5 DEG C/min
~600 DEG C start to keep the temperature, until vacuum degree≤1 × 10-312h is kept the temperature after Pa, then by jacket welded seal；By the jacket after encapsulation
Hot isostatic pressing is carried out, heating temperature is 1200~1300 DEG C, and heat preservation pressure is 120~150MPa, and soaking time 3h is caused
Close fire-retardant graphene titanium-aluminium matrix composites simultaneously carry out jacket heat rolling-forming, and initial temperature of rolling is 1200~1300 DEG C,
Pass deformation is 10~20%, to prepare fire-retardant graphene titanium-aluminium matrix composites slab.Air China sends out Beijing in
The graduate friction ignition equipment of aeronautical material carries out flammability test, obtains under identical flow conditions, fire-retardant graphite
The high 2 times or more of titanium alloys such as flame retardant property ratio TA15, TC4 of alkene titanium-aluminium matrix composites.
Claims (7)
1. a kind of fire-retardant graphene titanium-aluminium matrix composites, it is characterised in that：The composite material includes by mass percentage
Following compositions：Graphene oxide is 0.01~1wt%, remaining is titanium aluminium based compound.
2. a kind of fire-retardant graphene titanium-aluminium matrix composites according to claim 1, it is characterised in that：Titanium aluminium system
The composition for closing object is calculated as by atomic percent：Al：45~47at%, Cr：1~2at%, Nb：2~5at%, Ta：0~2at%,
W：0~2at%, Mo：0~2at%, Zr：0~2at%, Hf：0~2at%, B：0~0.2at%, Si：0~0.2at%, O：0
~0.25at%, remaining is Ti.
3. a kind of fire-retardant graphene titanium-aluminium matrix composites according to claim 1, it is characterised in that：Titanium aluminium system
The composition for closing object is calculated as by atomic percent：Al：45~47at%, Cr：1~2at%, Nb：3~5at%, Ta：0.1~
0.3at%, B：0~0.1at%, Si：0~0.1at%, remaining is Ti.
4. a kind of method preparing fire-retardant graphene titanium-aluminium matrix composites described in claim 1, it is characterised in that：The preparation
Method includes the following steps,
(1) the stannic oxide/graphene nano piece of 0.01~1wt% of titanium aluminium based compound powder quality is added in absolute ethyl alcohol,
Then decentralized processing 30min or more is carried out using ultrasonic cell disrupte machine, working frequency is vibration 2s, gap 3s, prepares oxygen
Graphite alkene solution；
(2) be 30~150 μm by grain size, oxygen content is less than the spherical or subsphaeroidal titanium aluminium based compound powder of 1000ppm and walks
Suddenly the graphene oxide solution of (1) is stirred mixing in temperature control mechanical agitator, prepares graphene oxide and titanium aluminium system
Compound mixed-powder slurry, mixing speed are 500~1200r/min, and mixing time is 50~120min, whipping temp 50
~70 DEG C；
(3) slurry of the graphene oxide of step (2) and titanium aluminium based compound mixed-powder is done in 50~60 DEG C of baking oven
5~10h of dry processing obtains graphene oxide and titanium aluminium based compound mixed-powder；
(4) graphene oxide of step (3) and titanium aluminium based compound mixed-powder are fitted into stainless steel capsule, then to jacket
Vacuumize process is carried out, room temperature vacuumizes 1.5~3.5h, until vacuum degree≤5Pa, is warming up to the rate of heat addition of 1~5 DEG C/min
200~300 DEG C start to keep the temperature, until vacuum degree≤1 × 10-21.5~2.5h is kept the temperature after Pa, continues the heating speed with 1~5 DEG C/min
Rate is warming up to 500~700 DEG C and starts to keep the temperature, until vacuum degree≤1 × 10-38~20h is kept the temperature after Pa, then by jacket welded seal；
(5) the sealing jacket of step (4) is subjected to hot isostatic pressing, obtains fine and close fire-retardant graphene titanium-aluminium matrix composites, adds
Hot temperature is 900~1300 DEG C, and heat preservation pressure is 120~150MPa, and soaking time is 2~4h；
(6) the fire-retardant graphene titanium-aluminium matrix composites of step (5) are subjected to Canned Hot molding, prepare fire-retardant graphene
Titanium-aluminium matrix composites bar stock, extrusion ratio be 5~10, heating temperature be 1200~1300 DEG C, mold preheating temperature be 300~
500 DEG C, extrusion speed is 10~30mm/s.
5. a kind of preparation method of fire-retardant graphene titanium-aluminium matrix composites according to claim 4, it is characterised in that：Institute
Titanium aluminium based compound powder is stated to prepare using gas atomization.
6. a kind of preparation method of fire-retardant graphene titanium-aluminium matrix composites according to claim 4, it is characterised in that：Institute
Stainless steel capsule is stated to be substituted by pure titanium or titanium alloy jacket.
7. a kind of preparation method of fire-retardant graphene titanium-aluminium matrix composites according to claim 4, it is characterised in that：Institute
It states Canned Hot molding to be substituted by jacket heat rolling-forming, prepares fire-retardant graphene titanium-aluminium matrix composites slab.
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Cited By (2)
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| CN112404426A (en) * | 2020-11-24 | 2021-02-26 | 西北工业大学 | Titanium-aluminum alloy die, preparation method of titanium-aluminum alloy outer sheath and method for performing spark plasma sintering by using titanium-aluminum alloy die |
| CN114959359A (en) * | 2022-05-11 | 2022-08-30 | 河南科技大学 | High densification of directionally aligned Ti 2 AlC/TiAl bionic composite material and preparation method thereof |
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