CN105385871B - A kind of preparation method of polynary nanometer complex intensifying heat resisting aluminium base composite material - Google Patents
A kind of preparation method of polynary nanometer complex intensifying heat resisting aluminium base composite material Download PDFInfo
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- CN105385871B CN105385871B CN201510695569.9A CN201510695569A CN105385871B CN 105385871 B CN105385871 B CN 105385871B CN 201510695569 A CN201510695569 A CN 201510695569A CN 105385871 B CN105385871 B CN 105385871B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
Abstract
The present invention provides a kind of preparation method of polynary nanometer complex intensifying heat resisting aluminium base composite material, in advance in nano-sized carbon surface clad ion predecessor, then nano-sized carbon is dispersed in aluminium powder and predecessor is converted into oxide by heat treatment, and then reaction-sintered and densification are carried out to gained composite powder, obtain polynary nanometer reinforced aluminum matrix composites.Nano-sized carbon has high-specific surface area, its characteristic size is much larger than nano-oxide, thus appropriate nano-oxide can be loaded and be homogeneously introduced among aluminium powder, the polynary nanometer hardening constituents such as metal oxide, carbide, intermetallic compound are generated via reaction in-situ again, collaboration improves the structure stability and heat resistance of aluminum matrix composite.The method of the invention solves high volume content, the uniform introducing of polynary nanometer hardening constituent and space occupy-place control problem, so as to prepare polynary nanometer complex intensifying heat resisting aluminium base composite material using conventional powder metallurgical technique.
Description
Technical field
The present invention relates to a kind of preparation method of heat resisting aluminium base field of material technology, has more particularly to one kind more
The preparation method of first nanometer phase reinforced aluminum matrix composites.
Background technology
Aluminium alloy is due to being widely used in Aero-Space and traffic fortune with the characteristic such as lightweight, high-strength, anti-corrosion, easy processing
Defeated field, wherein available for the referred to as heat resisting aluminium base material for preparing the part being on active service under high temperature, such as tank armored vehicle engine
Piston, cylinder sleeve, connecting rod, casing, cylinder cap, missile case, empennage, aero-engine cylinder, blade, aircraft skin etc., adopt
With heat resisting aluminium base material.Developing rapidly for Aeronautics and Astronautics and auto industry, is proposed more to the heat resistance of heat resisting aluminium base material
Carry out higher requirement.Control roughening theoretical based on diffusion, the main method for improving alumina-base material heat resistance is into aluminum substrate
Low solid solubility, the alloying element of low diffusion coefficient are introduced, forms that heat endurance is strong, is not easy the disperse phase that is roughened in aluminum substrate.
High-Temperature Strengthening effect depends on volume fraction, size, heat endurance and the intensity of disperse phase.Especially, Al-Fe systems are quickly solidified
Aluminium alloy can more than Effective Regulation several influence factor factors, so as to become presently the most successful alumite system.
It is stranded however, the low solid solubility of alloying element, the characteristic of low diffusion coefficient also result in introduce it in aluminum substrate
Difficulty, its solid solubility is mainly improved by flash set technology at present, so as to improve the volume fraction of disperse phase, but the technology pair
The requirement of the collocation of alloying element, technology controlling and process and equipment is all high, it is difficult to grasps and control, thus while external passed through
The technology volume production has gone out the heat-resisting aluminium alloy of excellent performance, and domestic heat-resisting aluminium alloy development is still in falling behind situation, homology
Row alloy is difficult to reach external quality level.
With the development of aluminium alloy and aluminum matrix composite, nanocrystalline intermetallics and nanometer reinforcement answering in aluminium
With gradually attracting attention.The intermediate compound and Al of the elements such as Fe, Ni, Ti, Zr, Sc, Co, La, Y, Er and aluminium2O3、La2O3
Not only there is very high modulus and hardness etc. nanometer reinforcement, it is possible to increase the modulus and intensity of alumina-base material, moreover it is possible to higher
The stabilization of itself and aluminium grain is kept during the thermal history of temperature, these nanometers are mutually ideal heat resisting aluminium base materials
Reinforcement, its addition, size be all easy to be controlled by reacting synthesis, thus in high-modulus, high intensity, heat-resisting aluminium
It is of great interest in exploitation.Wherein the element such as Ti, Zr, Sc, Er can generate with aluminium base precursor reactant has L12Structure
Three aluminide Al3(M includes following 9 kinds of elements to M：Ti, Zr, Sc, Er, Lu, Tm, Yb, Np, U), because of the aluminium with face-centred cubic structure
Matrix has coherent boundary and is provided with extremely strong heat endurance, and is considered as the enhancing of ideal heat resisting aluminium base material
Body.
But when being introduced by the outer adding method such as stirring casting, ball milling, because nanometer is mutually held in the presence of Van der Waals force
Easily reunite, especially when volume fraction is higher, the nanometer being introduced into is mutually scattered uneven in aluminium, is unfavorable for playing its performance advantage
To obtain high combination property composite
Found by the literature search to prior art, " the Elevated temperature aluminum- of document 1
titanium alloy by powder metallurgy process”(William E.Frazier,Michael
J.Koczak, the patent No. US4834942 A) using quick solidification Al-Ti powder (Al3Ti contents reach 20vol.%) and it is appropriate
CNT prepares the heat resisting aluminium base composite material of Al-Ti-C-O systems after ball milling, densification, but its dispersing technology makes carbon
Nanotube reacts generation Al completely4C3And be distributed in crystal boundary completely, make material mechanical property lifted it is limited, high temperature elongation percentage is bright
It is aobvious to decline；" Mechanically alloyed nanocomposites " (the Progress in Materials of document 2
Science.2013 (58) 383-502) described in technical scheme, by high-energy ball milling machinery alloying, a variety of receive can be prepared
The aluminum matrix composite that rice mutually strengthens, but this method usually requires prolonged high-energy ball milling, and be not easy scattered high volume and contain
Amount, it is tiny (<Nanometer phase 20nm)." Al-the Al of document 33Ti nanocomposites produced in situ by
Technical scheme described in friction stir processing " (Acta Materialia.2006 (54) 5241-5249), will
After aluminium powder and titanium valve mixing pressed compact, then by way of high-speed stirred friction, aluminium and titanium reaction in-situ is set to generate intermediate compound
Al3Ti, simultaneously because under plastic deformation effect strong in agitating friction technique, make Al3Ti is in reaction generation and peeled off scattered
Dynamic process, it is thus possible in aluminium generate volume fraction reach as high as 50vol.%, finely dispersed nanometer Al3Ti.But
It is that agitating friction can be only applied in thin plate, and complex process, its extensive use are severely limited.
Therefore, in summary, improve metal-base composites heat endurance and the key of heat resistance is：1) enhancing is mutually high
Temperature is stable, is difficult to grow up；2) it is small to strengthen phase particle size, is typically in nanoscale, and volume content is higher；3) strengthen mutually necessary
Even dispersion is distributed in the base.However, main deficiency present in above-mentioned existing technical scheme is：1) it is based on fast rapid hardening
Gu heat-resisting aluminium alloy prepared by method requires very high to technical process and manufacturing equipment, it is not easy to grasp, technology controlling and process is led accidentally
Enhancing is caused mutually to reunite or grow up at high temperature；2) time-consuming, high energy consumption for the method for high-energy ball milling machinery alloying, and nanometer is increased
The dispersibility of strong phase is very limited；3) agitating friction welding method is prepared suitable for thin plate, it is difficult to the block materials larger for thickness.
The content of the invention
In view of the deficiencies of the prior art, the present invention provides one kind prepared by nano-sized carbon supported nano-gold category oxide it is polynary
The method of nano crystalline compounding heat resisting aluminium base composite material, because polynary nanometer mutually has preferable chemical stability and different
Space occupy-place, there is efficient stabilization to aluminum substrate crystal grain, so that the aluminum matrix composite prepared is with heat-resisting well
Property.
The present invention is achieved by the following technical solutions：
The present invention provides a kind of preparation method of polynary nanometer complex intensifying heat resisting aluminium base composite material, including following step
Suddenly：
1) Surface coating is carried out as carrier to nano-sized carbon with the precursor solution containing metal ion using nano-sized carbon,
Obtain predecessor coating nano carbon；
2) the predecessor coating nano carbon that step 1) obtains is dispersed in aluminium powder, being handled by thermal response makes forerunner
Predecessor in thing coating nano carbon is transformed into nano-oxide, so as to obtain (nano-sized carbon+nano-oxide)/aluminium composite powder
End；
3) (nano-sized carbon+nano-oxide)/aluminium composite powder that step 2) obtains is carried out at reaction-sintered and densification
Reason, heat treatment, generate metal oxide, carbide, intermetallic compound and the polynary of remaining nano-sized carbon via reaction in-situ and receive
Rice hardening constituent, so as to obtain polynary nanometer complex intensifying heat resisting aluminium base composite material.
Preferably, in step 1), described nano-sized carbon includes carbon nano-fiber, CNT, graphene, graphene oxide
In one kind or combination, and stable dilute dispersion liquid can be at least formed with a kind of solvent.
It is highly preferred that 0.01~5wt.% of the total amount of adding of described nano-sized carbon for the quality of composite, preferably
Total amount of adding is 0.5~3wt.%.
Preferably, in step 1), described precursor solution includes solvent, metal ion compound, can also be further
Formed including reactant and/or crosslinking agent.
It is highly preferred that described solvent includes water, methanol, ethanol, ethylene glycol, toluene, DMF, one kind or group in tween
Close；
Described metal ion compound is Fe, Ni, Ti, Zr, Sc, Co, La, Y, Er oxide, hydroxide, halogenation
One kind or its combination in thing, nitrate, sulfate, metallocene compound, carbonyls, the metal oxide ultimately generated
For 0.1~20wt.% of composite quality；
Described reactant is using in citric acid, glucose, oxalic acid, tartaric acid, dextrin, EDTA, ethylenediamine, hydrazine hydrate
One kind or combination；Reactant can also be without using；
Described crosslinking agent is to use ethylene glycol, polyethylene glycol, polyvinyl alcohol, POLYPROPYLENE GLYCOL, polyvinylpyrrolidone, poly-
One kind or combination in pyrroles；Crosslinking agent can also be without using.
Preferably, in step 1), described surface coating method is that nano-sized carbon is added in precursor solution into the machine that carries out
Tool stirs or ultrasound, is then filtered, centrifuged or is evaporated.
Preferably, in step 2), described predecessor coating nano carbon be dispersed in method in aluminium powder include ball milling,
One or more in slurry blending, adsorption.
It is highly preferred that described aluminium powder includes fine aluminium and Al alloy powder.
Preferably, in step 3), described polynary nanometer hardening constituent include it is various can be in used technique and military service
Under the conditions of be stabilized in aluminium, size in a direction be not more than 100nm metal and metallic compound particle, it is polynary
The total amount of nano-strengthening phase is 0.1~20wt.%, and preferable total amount is 5~15wt.%.
Preferably, in step 3), described reaction in-situ generation metal oxide, carbide, the side of intermetallic compound
Formula is the one or more in water-bath, oil bath, hydro-thermal, solvent heat, atmosphere heating, and reactive mode is determined according to selected predecessor
It is fixed；Wherein need to add reducing agent (reducing agent need not be added when generating other materials) when generating metal oxide particle,
The reducing agent is the reactant in precursor solution, or solvent, reducibility gas or aluminum substrate are in itself, specifically, also
Former agent is the one or more in citric acid, glucose, oxalic acid, ethylenediamine, hydrazine hydrate, ethylene glycol, sodium borohydride, hydrogen, aluminium.
Preferably, in step 3), described densification includes：Cold pressing, isostatic cool pressing, temperature and pressure, pressureless sintering, hot pressing
One or more in sintering, high temperature insostatic pressing (HIP), and follow-up extruding, forging, jumping-up, rolling mill practice.
Preferably, in step 3), the purpose of described heat treatment is to make can be with the nano metal or nanometer of reactive aluminum
The reaction of metal oxide particle is fully carried out, and generates intermetallic compound or alumina nanoparticles, and mode is predominantly annealed.
Heat-resisting alloy (high temperature titanium-base alloy, high-temperature nickel-base alloy, high temperature acieral), which is studied, to be shown, the high temperature shape of alloy
Change is controlled by flooding mechanism, according to High-Temperature Strengthening principle, appropriate alloying element alloying need to be selected to make that height can be produced in alloy
The thermostabilization enhancing phase that temperature is not easily decomposed conversion, is not easy to be roughened, uniform tiny and Dispersed precipitate have foot in alloy matrix aluminum
Enough volume contents, can effectively pin dislocation, stable substructure, prevent Grain Boundary Sliding, suppress base while crystal boundary is strengthened
Body recrystallizes and the diffusion of solid solution element, improves matrix recrystallization temperature, recrystallization softening is hindered, so as to improve alloy high-temp
Energy.Therefore the thermostabilization enhancing phase that the high-temperature behavior of metal material is depended in matrix, the heat endurance of thermostabilization enhancing phase, chi
Very little, distribution and content finally determine the high-temperature behavior of alloy.The heat endurance of precipitated phase is stronger, size is smaller, distribution is more equal
The high-temperature behavior of the more high then alloy of even, content is more excellent.
Design is optimized for some above-mentioned enhancing key element emphatically in technical solution of the present invention：
1) the enhancing phase of good thermal stability is introduced：With L12Three aluminide Al of structure3(M includes following 9 kinds of elements to M：
Ti, Zr, Sc, Er, Lu, Tm, Yb, Np, U), because the aluminum substrate with face-centred cubic structure has coherent boundary be provided with it is extremely strong
Heat endurance, it is considered to be preferable thermostabilization enhancing phase；Meanwhile metal oxide and graphene and carbon with ceramic structure
The nano-sized carbons such as nanotube equally have extremely strong heat endurance.
2) reinforcement size is controlled in nanoscale：The easily controllable Al for introducing nanometer of reaction in-situ3M, aluminum oxide, metal
Oxide and nano-sized carbon etc..
3) the high volume content of nanometer phase is ensured：In view of metal or metal oxide nanoparticles and aluminium powder specific surface area
Differ huge, easy reunion, and nano-sized carbon equally has very high specific surface area, can uniform load cumulative volume be more than the gold of itself
Category or oxide nano-particles, and can are dispersed in aluminium powder by powder treatment process such as ball milling, slurry blending, adsorptions
In, so as to realize that metal or metal oxide nanoparticles are dispersed in aluminium as intermediate；The technique side of the present invention
Method introduces the excellent reinforcement of a variety of thermal stabilities by nano-sized carbon load, while realizes uniformly dividing for polynary nanometer phase
Dissipate, because the space occupy-place of variety classes nanometer phase is different, the mutually easy agglomeration of nanometer caused by avoiding high volume content.Cause
This, the introducing of the thermostabilization disperse phase of high content nano-scale, makes alumina-base material Good Heat-resistance, and uses nano-sized carbon to load
Technology makes preparation process simple and easy, low for equipment requirements and be easy to grasp.
Compared with prior art, the present invention has advantages below：
1) metal of chemical method fabricated in situ and metal oxide nanoparticles content, size, morphology controllable；
2) by the carrier function of nano-sized carbon, it can realize that a large amount of heterogeneous nanometers are mutually dispersed in alumina-base material,
Violent plastic deformation need not be carried out；
3), can be gentleer by the reaction of additional reducing agent or aluminum substrate and metal and metal oxide nanoparticles
Under conditions of realize the introducing of nanometer phase；
4) conventional chemical processes and PM technique are used, is easy to carry out industrialized production.
In summary, the nanometer phase volume fraction of present invention gained is high, species is extensive, is evenly distributed, and technical scheme is easy
It is easy, mutually strengthen heat resisting aluminium base material suitable for being prepared on a large scale nanometer.
Brief description of the drawings
The detailed description made by reading with reference to the following drawings to non-limiting example, further feature of the invention,
Objects and advantages will become more apparent upon：
Fig. 1 is the preparation technology flow chart of the embodiment of the present invention.
Embodiment
Embodiments of the invention are elaborated below, the present embodiment is carried out lower premised on technical solution of the present invention
Implement, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following implementation
Example.
The present embodiment provides one kind, and by nano-sized carbon supported nano-gold category oxide to prepare polynary nanometer complex intensifying heat-resisting
The method of aluminum matrix composite, this method in nano-sized carbon surface clad ion precursor solution, obtain predecessor bag in advance
Cover nano-sized carbon；Then predecessor coating nano carbon is dispersed in aluminium powder and to turn to it nano oxidized by heat treatment
Thing, obtain (nano-sized carbon+nano-oxide)/aluminium composite powder；And then reaction-sintered and densification are carried out to gained composite powder
Processing, heat treatment, so as to obtain polynary nanometer reinforced aluminum matrix composites.
In following embodiments, all substrates use for different Al alloy powders, wherein：Embodiment 1 is 325 mesh
6061 Al alloy powders；Embodiment 2 is 10 μm of pure aluminium powders of diameter；Embodiment 3 is the aluminium powder of 300 mesh 2024.
Contrast test of the comparative example 1 as embodiment 1, it is same as Example 1 spherical using CNT, 325 mesh
6061 Al alloy powders prepare aluminum matrix composite as initial raw material, and reaction-sintered and densified conditions are also identical, different
It is directly to use the spherical TiO of diameter 30nm2Powder and its directly directly carry out ball milling mixing with CNT, aluminium powder.Embodiment 1
Nanometer mutually for CNT, nanometer Al3Ti and nanometer Al2O3, the nanometer of embodiment 2 is mutually CNT and nanometer La2O3, it is real
The nanometer for applying example 3 is mutually graphene and nanometer Al3Ni.The nanometer carbon carrier of embodiment 1,2 is CNT, and embodiment 3 is received
Rice carbon carrier is graphene oxide, and the design component of each embodiment is listed in table 1.The room temperature mechanical property of material in all embodiments
Can equal reference《GB/T228.1-2010》Carry out, rate of extension 0.5mm/min, the high-temperature mechanics of material in all embodiments
Can equal reference《GB/T 4338-2006》Carry out, rate of extension 0.5mm/min.
Embodiment 1：
By 6mlTiCl4, 12g citric acids and 10ml ethylene glycol be dissolved in 40ml alcohol, magnetic agitation is allowed to fully dissolve
To precursor solution；By 3g CNTs, ultrasonic 1h forms dispersing Nano carbon tubes dispersion liquid in 400ml alcohol.Predecessor is molten
Drop is added in carbon nano tube dispersion liquid, and continuing ultrasonic 1h makes predecessor be coated to carbon nano tube surface, is added into dispersion liquid
Enter 93g aluminium powders, filtered after magnetic agitation 0.5h and be dried to obtain predecessor-CNT-aluminium composite powder.Again by predecessor-carbon
Nanotube-aluminium composite powder is put into N2230 DEG C of reaction 1h are heated in tube furnace under atmosphere protection, are heated to 600 DEG C of guarantors
Warm 0.5h removes the organic matter of surface residual, obtains nano-titanium oxide -- CNT-aluminium composite powder.By nano-titanium oxide --
CNT-aluminium composite powder is cold-pressed into after diameter 40mm ingot blank in punching block in 600 DEG C, N22h is sintered under atmosphere.Then
By sintered blank in 550 DEG C, N2Anneal 6h under atmosphere, nano-titanium oxide and aluminium base precursor reactant in annealing, forms nanometer Al3Ti, receive
Rice Al2O3, nanometer Al4C3The alumina-base material mutually strengthened with quaternary nanometers such as CNTs, the room temperature mechanics of the material finally prepared
Performance and mechanical behavior under high temperature are listed in table 2 and table 3 respectively.
Embodiment 2：
By 9g La2Cl3·5H2O and 5g polyvinylpyrrolidones are dissolved in 20ml water, and magnetic agitation is allowed to fully dissolve
To precursor solution；By 1g CNTs and 1g graphenes, ultrasonic 1h formation dispersing Nano carbon tubes disperse in 200ml water respectively
Liquid.It will respectively take half quality precursor solution to be added drop-wise to respectively in carbon nano tube dispersion liquid and graphene dispersing solution, and continue to surpass
Sound 1h makes predecessor be coated to carbon nano tube surface and graphenic surface, and then it is multiple to be dried to obtain predecessor-CNT for suction filtration
Close powder.Predecessor-carbon nano-tube composite powder end is put into N2600 DEG C of insulation 2h are heated in tube furnace under atmosphere protection,
Obtain nano lanthanum oxide-carbon nano-tube composite powder end.After nano lanthanum oxide-carbon nano-tube composite powder end is mixed with 93g aluminium powders,
With 20:1 ratio of grinding media to material, 425rpm rotating speeds ball milling 8h in planetary ball mill, obtain nano lanthanum oxide-CNT-aluminium composite powder
End.By nano lanthanum oxide-CNT-aluminium composite powder in diameter 40mm punching blocks, 500 DEG C, 400MPa pressure, vacuum bar
Hot pressed sintering 2h under part, obtain a nanometer La2O3, nanometer Al3C4The alumina-base material mutually strengthened with carbon nanometer pipe ternary nanometer.Finally
The room-temperature mechanical property and mechanical behavior under high temperature of the material of preparation are listed in table 2 and table 3 respectively.
Embodiment 3：
By 12g NiCl2·6H2O and 20g glucose is dissolved in 20ml water, and magnetic agitation is allowed to fully dissolving and obtains forerunner
Thing solution；By 0.5g graphene oxides, ultrasonic 1h forms graphene oxide dispersion in 200ml water.Precursor solution is added dropwise
Into graphene oxide dispersion, and continuing ultrasonic 1h makes predecessor be coated to surface of graphene oxide.96.5g2024 aluminium is closed
Bronze is placed in magnetic agitation in 200ml water, while graphene oxide dispersion is slowly added dropwise, and is then stirred vigorously solution, adds
8g sodium borohydrides, then suction filtration drying is carried out, obtain nano nickel-graphene oxide-aluminium composite powder.By nano nickel-graphite oxide
Alkene-aluminium composite powder is cold-pressed into after diameter 40mm ingot blank in punching block in 600 DEG C, N22h is sintered under atmosphere.In sintering process
In, nano nickel and aluminium base precursor reactant, form nanometer Al3Ni, nanometer Al3C4And the alumina-base material of graphene enhancing.It is final to prepare
Material room-temperature mechanical property and mechanical behavior under high temperature be listed in table 2 and table 3 respectively.
Comparative example 1：
After a diameter of 30nm of 4g TiO2 powder, 3g CNTs and 93g pure aluminium powders are carried out into ball milling mixing, by powder
End is put into N2230 DEG C of reaction 1h are heated in tube furnace under atmosphere protection, it is residual to be heated to 600 DEG C of insulation 0.5h removals surfaces
Remaining organic matter, obtains nano-titanium oxide -- CNT-aluminium composite powder.By nano-titanium oxide -- CNT-aluminium powder
It is cold-pressed into punching block after diameter 40mm ingot blank in 600 DEG C, N22h is sintered under atmosphere.Then by sintered blank in 550 DEG C, N2Gas
Anneal 6h under atmosphere, and final composite is made, and its room-temperature mechanical property and mechanical behavior under high temperature are listed in table 2 and table 3 respectively, shows
So due to the difference of its reinforcement dispersiveness, its combination property is caused to have obvious decline compared with embodiment 1.
The composition of the composite of table 1
The room-temperature mechanical property of the composite of table 2
The high-temperature behavior of the composite of table 3
The metal and metal oxide nanoparticles content, size, morphology controllable of chemical method fabricated in situ of the present invention；Borrow
The carrier function of nano-sized carbon is helped, can realize that a large amount of heterogeneous nanometers are mutually dispersed in alumina-base material, it is not necessary to carry out acute
Strong plastic deformation；By the reaction of additional reducing agent or aluminum substrate and metal and metal oxide nanoparticles, can compared with
The introducing of nanometer phase is realized under conditions of gentle；Using conventional chemical processes and PM technique, it is easy to carry out industrial metaplasia
Production.The nanometer phase volume fraction height of gained of the invention, species is extensive, is evenly distributed, and technical scheme is simple and easy to do, suitable for high-volume
Preparing nanometer mutually strengthens heat resisting aluminium base material.
The specific embodiment of the present invention is described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring the substantive content of the present invention.
Claims (11)
1. a kind of preparation method of polynary nanometer complex intensifying heat resisting aluminium base composite material, it is characterised in that comprise the following steps：
1) Surface coating is carried out to nano-sized carbon with the precursor solution containing metal ion, obtained as carrier using nano-sized carbon
Predecessor coating nano carbon；Described precursor solution is made up of solvent, metal ion compound, or by solvent, metal from
Sub- compound, crosslinking agent and/or reactant composition；
2) the predecessor coating nano carbon that step 1) obtains is dispersed in aluminium powder, being handled by thermal response makes predecessor bag
The predecessor covered in nano-sized carbon is transformed into nano-oxide, so as to obtain (nano-sized carbon+nano-oxide)/aluminium composite powder；
3) reaction-sintered and densification, heat are carried out to (nano-sized carbon+nano-oxide)/aluminium composite powder that step 2) obtains
Processing, the polynary nanometer that metal oxide, carbide, intermetallic compound and remaining nano-sized carbon are generated via reaction in-situ are strengthened
Phase, so as to obtain polynary nanometer complex intensifying heat resisting aluminium base composite material；
Described metal ion compound be Fe, Ni, Ti, Zr, Sc, Co, La, Y, Er oxide, hydroxide, halide,
One kind or its combination, the metal oxide ultimately generated in nitrate, sulfate, metallocene compound, carbonyls are
0.1~20wt.% of composite quality；
Described solvent is water, methanol, ethanol, ethylene glycol, toluene, DMF, one kind in tween or combination；
Described reactant is using one in citric acid, glucose, oxalic acid, tartaric acid, dextrin, EDTA, ethylenediamine, hydrazine hydrate
Kind or combination；
Described crosslinking agent is using ethylene glycol, polyethylene glycol, polyvinyl alcohol, POLYPROPYLENE GLYCOL, polyvinylpyrrolidone, polypyrrole
In one kind or combination.
2. a kind of preparation method of polynary nanometer complex intensifying heat resisting aluminium base composite material according to claim 1, it is special
Sign is, in step 1), described nano-sized carbon is the one or more in carbon nanometer phase of the size no more than 100nm, and at least
Can form stable dilute dispersion liquid with a kind of solvent, nano-sized carbon total amount of adding for final composite quality 0.01~
5wt.%.
3. a kind of preparation method of polynary nanometer complex intensifying heat resisting aluminium base composite material according to claim 2, it is special
Sign is that described nano-sized carbon is the one or more in carbon nano-fiber, CNT, graphene, graphene oxide.
4. a kind of preparation method of polynary nanometer complex intensifying heat resisting aluminium base composite material according to claim 2, it is special
Sign is that the nano-sized carbon total amount of adding is 0.5~3wt.% of final composite quality.
5. a kind of preparation method of polynary nanometer complex intensifying heat resisting aluminium base composite material according to claim 1, it is special
Sign is, in step 1), described surface coating method is：By nano-sized carbon be added in precursor solution carry out mechanical agitation or
Ultrasound, then filtered, centrifuged or be evaporated.
6. a kind of preparation method of polynary nanometer complex intensifying heat resisting aluminium base composite material according to claim 1, it is special
Sign is, in step 2), described predecessor coating nano carbon be dispersed in method in aluminium powder for ball milling, slurry blending,
One or more in adsorption；Described aluminium powder is fine aluminium and/or Al alloy powder.
A kind of 7. preparation side of polynary nanometer complex intensifying heat resisting aluminium base composite material according to claim any one of 1-6
Method, it is characterised in that in step 3), described metal oxide, carbide, the polynary nanometer hardening constituent of intermetallic compound,
Characteristic size in one direction is not more than 100nm；The total amount of described polynary nanometer hardening constituent is whole composite matter
0.1~20wt.% of amount.
8. a kind of preparation method of polynary nanometer complex intensifying heat resisting aluminium base composite material according to claim 7, it is special
Sign is that the total amount of described polynary nanometer hardening constituent is 5~15wt.% of whole composite quality.
A kind of 9. preparation side of polynary nanometer complex intensifying heat resisting aluminium base composite material according to claim any one of 1-6
Method, it is characterised in that in step 3), described reaction in-situ metal oxide, carbide, the mode of intermetallic compound are water
One or more in bath, oil bath, hydro-thermal, solvent heat, atmosphere heating, reactive mode determine according to selected predecessor；
Described needs to add also when generating metal oxide by (nano-sized carbon+nano-oxide)/aluminium composite powder reaction in-situ
Former agent；Described reducing agent is the reactant in precursor solution, or solvent, reducibility gas or aluminum substrate are in itself.
10. a kind of preparation method of polynary nanometer complex intensifying heat resisting aluminium base composite material according to claim 9, it is special
Sign is, described reducing agent be citric acid, glucose, oxalic acid, ethylenediamine, hydrazine hydrate, ethylene glycol, sodium borohydride, hydrogen or
One or more in aluminium.
A kind of 11. preparation of polynary nanometer complex intensifying heat resisting aluminium base composite material according to claim any one of 1-6
Method, it is characterised in that in step 3), described densification includes：Cold pressing, isostatic cool pressing, temperature and pressure, pressureless sintering, heat
One or more in pressure sintering, high temperature insostatic pressing (HIP), and follow-up extruding, forging, jumping-up, rolling mill practice.
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| CN113249633A (en) * | 2021-06-10 | 2021-08-13 | 北京石墨烯技术研究院有限公司 | Dispersion strengthening alloy and preparation method and application thereof |
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| CN114523099B (en) * | 2022-04-23 | 2022-07-01 | 南通瑞升运动休闲用品有限公司 | High-performance metal composite material and preparation method thereof |
| CN116024447A (en) * | 2022-12-30 | 2023-04-28 | 中国科学院金属研究所 | Preparation method of aluminum alloy material |
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| CN104264000B (en) * | 2014-09-03 | 2016-09-07 | 上海交通大学 | The high thermal conductivity aluminum matrix composite of Graphene modification and method for preparing powder metallurgy thereof |
| CN104962841B (en) * | 2015-05-26 | 2017-06-09 | 上海交通大学 | The interface and preparation method of a kind of carbon nanotube metal based composite materials |
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