CN105385871A - Preparing method of multielement nanometer composite strengthening thermal-resisting aluminum matrix composite - Google Patents

Preparing method of multielement nanometer composite strengthening thermal-resisting aluminum matrix composite Download PDF

Info

Publication number
CN105385871A
CN105385871A CN201510695569.9A CN201510695569A CN105385871A CN 105385871 A CN105385871 A CN 105385871A CN 201510695569 A CN201510695569 A CN 201510695569A CN 105385871 A CN105385871 A CN 105385871A
Authority
CN
China
Prior art keywords
nano
aluminum matrix
carbon
oxide
preparation
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201510695569.9A
Other languages
Chinese (zh)
Other versions
CN105385871B (en
Inventor
李志强
陈马林
谭占秋
范根莲
熊定邦
郭强
张荻
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shanghai Jiaotong University
Original Assignee
Shanghai Jiaotong University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shanghai Jiaotong University filed Critical Shanghai Jiaotong University
Priority to CN201510695569.9A priority Critical patent/CN105385871B/en
Publication of CN105385871A publication Critical patent/CN105385871A/en
Application granted granted Critical
Publication of CN105385871B publication Critical patent/CN105385871B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/05Mixtures of metal powder with non-metallic powder
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/10Alloys containing non-metals
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C21/00Alloys based on aluminium

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention provides a preparing method of a multielement nanometer composite strengthening thermal-resisting aluminum matrix composite. The surface of nanocarbon is coated with a metal ion precursor in advance, the nanocarbon is evenly scattered in aluminum powder, the precursor is converted into oxide through thermal treatment, reactive sintering and densifying treatment are carried out on the obtained composite powder, and the multielement nanometer strengthening aluminum matrix composite is obtained. The nanocarbon has the high specific surface area, the feature size of the nanocarbon is far larger than that of the nanometer oxide, and therefore a proper amount of nanometer oxide can be loaded and evenly led into the aluminum powder, metallic oxide, carbide, an intermetallic compound and other multielement nanometer strengthening phases are generated through the in-situ reaction, and the tissue stability and the thermal resistance of the aluminum matrix composite are improved coordinately. The method achieves the purposes of even leading of high-volume-content multielement nanometer strengthening phases and the space occupation control, and the conventional powder metallurgy technology can be adopted for preparing the multielement nanometer composite strengthening thermal-resisting aluminum matrix composite.

Description

A kind of preparation method of polynary nanometer composite heat-resisting enhance aluminum matrix composite
Technical field
That the present invention relates to is a kind of preparation method of heat resisting aluminium base field of material technology, particularly relates to a kind of preparation method with polynary nanometer phase reinforced aluminum matrix composites.
Background technology
Aluminium alloy is owing to having the characteristics such as lightweight, high-strength, anti-corrosion, easy processing and being widely used in aerospace and traffic and transport field, the parts of being on active service under wherein can be used for preparing high temperature be called heat resisting aluminium base material, as piston, cylinder sleeve, connecting rod, casing, the cylinder cap of tank armored vehicle engine, missile case, empennage, aircraft engine cylinder, blade, aircraft skin etc., all adopt heat resisting aluminium base material.Developing rapidly of Aeronautics and Astronautics and automotive industry, proposes more and more higher requirement to the resistance toheat of heat resisting aluminium base material.Theoretical based on diffusion control alligatoring, the main method improving alumina-base material resistance toheat is in aluminum substrate, introduce the alloying element of low solid solubility, low spread coefficient, formed in aluminum substrate thermostability by force, the disperse phase of not easily alligatoring.High-Temperature Strengthening effect depends on the volume fraction of disperse phase, size, thermostability and intensity.Especially, rapid solidification Al-Fe line aluminium alloy can more than Effective Regulation several influence factor factor, thus becomes the most successful alumite system at present.
But, the low solid solubility of alloying element, the characteristic of low spread coefficient result also in introduces difficulty by it in aluminum substrate, its solid solubility is improved at present mainly through flash set technology, thus improve the volume fraction of disperse phase, but the requirement of the collocation of this technology alloy element, technology controlling and process and equipment is all high, be difficult to grasp and control, although therefore gone out the heat-resisting aluminium alloy of excellent performance by this technology volume production abroad, domestic heat-resisting aluminium alloy development is still in backward situation, and homologous series alloy is difficult to reach external quality level.
Along with the development of aluminium alloy and aluminum matrix composite, nanocrystalline intermetallics and the application of nanometer reinforcement in aluminium receive publicity gradually.The intermediate compound of the elements such as Fe, Ni, Ti, Zr, Sc, Co, La, Y, Er and aluminium and Al 2o 3, La 2o 3etc. nanometer reinforcement, not only there is very high modulus and hardness, modulus and the intensity of alumina-base material can be improved, the stable of self and aluminium grain can also be kept in the thermal history process of comparatively high temps, these nanophases are reinforcements of ideal heat resisting aluminium base material, its addition, size all control easily through Reactive Synthesis, thus receive in the exploitation of high-modulus, high strength, heat-resisting aluminium and pay close attention to widely.Wherein the element such as Ti, Zr, Sc, Er can react generation with aluminum substrate and has L1 2three aluminide Al of structure 3m (M comprises following 9 kinds of elements: Ti, Zr, Sc, Er, Lu, Tm, Yb, Np, U), be provided with extremely strong thermostability because there is coherent interface with the aluminum substrate of face-centred cubic structure, and be considered to the reinforcement of ideal heat resisting aluminium base material.
But when being introduced by the outer adding method such as stirring casting, ball milling, because nanophase is easily reunited under the effect of Van der Waals force, especially when volume fraction is higher, the nanophase of introducing disperses uneven in aluminium, is unfavorable for playing its performance advantage to obtain high combination property matrix material
Through finding the literature search of prior art, document 1 " Elevatedtemperaturealuminum-titaniumalloybypowdermetallu rgyprocess " (WilliamE.Frazier, MichaelJ.Koczak, patent No. US4834942A) adopt rapid solidification Al-Ti powder (Al 3ti content reaches 20vol.%) after ball milling, densification, prepare the heat resisting aluminium base composite material of Al-Ti-C-O system with appropriate carbon nanotube, but its dispersing technology makes carbon nanotube complete reaction generate Al 4c 3and be distributed in crystal boundary completely, make the mechanical property of material promote limited, high temperature unit elongation and obviously decline; Technical scheme described in document 2 " Mechanicallyalloyednanocomposites " (ProgressinMaterialsScience.2013 (58) 383 – 502), by high-energy ball milling machinery alloying, the aluminum matrix composite that multiple nanophase strengthens can be prepared, but this method needs long high-energy ball milling usually, and not easily disperse the nanophase of high volume content, tiny (<20nm).Document 3 " Al – Al 3tinanocompositesproducedinsitubyfrictionstirprocessing " technical scheme described in (ActaMaterialia.2006 (54) 5241 – 5249); after aluminium powder and titanium valve mixing pressed compact; again by the mode that high-speed stirring rubs, make aluminium and titanium reaction in-situ generate intermediate compound Al 3ti, simultaneously due under viscous deformation effect strong in agitating friction technique, makes Al 3ti is in the dynamic process that reaction generates and peels off dispersion, thus can generate volume fraction and reach as high as 50vol.%, finely dispersed nanometer Al in aluminium 3ti.But agitating friction can only be applied in thin plate, and complex process, its widespread use is severely limited.
Therefore, in sum, the key improving metal-base composites thermostability and heat resistance is: 1) wild phase high-temperature stable, be difficult to grow up; 2) wild phase particle size is little, is generally in nano level, and volume content is higher; 3) wild phase must even dispersion distribution in the base.But, the main deficiency existed in above-mentioned existing technical scheme is: the heat-resisting aluminium alloy 1) prepared based on rapid solidification method requires very high to technological process and producing apparatus, not easily grasp, namely technology controlling and process causes wild phase at high temperature reunite or grow up accidentally; 2) the high-energy ball milling machinery method length consuming time of alloying, energy consumption are high, and very limited to the dispersive ability of nanometer reinforcing phase; 3) agitating friction welding method is applicable to thin plate preparation, is difficult to use in the block materials that thickness is larger.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of method by nano-sized carbon loaded with nano metal Preparation polynary nanometer composite heat-resisting enhance aluminum matrix composite is provided, because polynary nanometer has good chemical stability and different space occupy-places mutually, to aluminum substrate crystal grain, there is efficient stabilization, thus the aluminum matrix composite of preparation has good thermotolerance.
The present invention is achieved by the following technical solutions:
The invention provides a kind of preparation method of polynary nanometer composite heat-resisting enhance aluminum matrix composite, comprise the following steps:
1) adopt nano-sized carbon as carrier, with the precursor solution containing metal ion, Surface coating is carried out to nano-sized carbon, obtain precursor coating nano carbon;
2) by step 1) the precursor coating nano carbon that obtains is dispersed in aluminium powder, make the precursor in precursor coating nano carbon be transformed into nano-oxide by thermal response process, thus obtain (nano-sized carbon+nano-oxide)/aluminium composite powder;
3) to step 2) (nano-sized carbon+nano-oxide)/aluminium composite powder of obtaining carries out reaction sintering and densification, thermal treatment, generate the polynary nanometer strengthening phase of metal oxide, carbide, intermetallic compound and residue nano-sized carbon via reaction in-situ, thus obtain polynary nanometer composite heat-resisting enhance aluminum matrix composite.
Preferably, step 1) in, described nano-sized carbon comprises one in carbon nano fiber, carbon nanotube, Graphene, graphene oxide or combination, and at least can form stable rare dispersion liquid with a kind of solvent.
More preferably, the interpolation total amount of described nano-sized carbon is 0.01 ~ 5wt.% of the quality of matrix material, and preferred interpolation total amount is 0.5 ~ 3wt.%.
Preferably, step 1) in, described precursor solution comprises solvent, metal ion compound, can further include reagent and/or linking agent composition.
More preferably, described solvent comprises one in water, methyl alcohol, ethanol, ethylene glycol, toluene, DMF, tween or combination;
Described metal ion compound is one in the oxide compound of Fe, Ni, Ti, Zr, Sc, Co, La, Y, Er, oxyhydroxide, halogenide, nitrate, vitriol, metallocene compound, carbonyl compound or its combination, and the final metal oxide generated is 0.1 ~ 20wt.% of matrix material quality;
Described reagent uses citric acid, glucose, oxalic acid, tartrate, dextrin, EDTA, quadrol, one in hydrazine hydrate or combination; Reagent also can not use;
Described linking agent makes one in spent glycol, polyoxyethylene glycol, polyvinyl alcohol, POLYPROPYLENE GLYCOL, polyvinylpyrrolidone, polypyrrole or combination; Linking agent also can not use.
Preferably, step 1) in, described surface coating method carries out mechanical stirring or ultrasonic for nano-sized carbon being joined in precursor solution, then carries out suction filtration, centrifugal or evaporate to dryness.
Preferably, step 2) in, the described precursor coating nano carbon method be dispersed in aluminium powder comprises that ball milling, slip are blended, one or more in surface adsorption.
More preferably, described aluminium powder comprises fine aluminium and Al alloy powder.
Preferably, step 3) in, described polynary nanometer strengthening phase comprise various can under used technique and service condition in aluminium stable existence, size in a direction is not more than the metallide particle of 100nm, the total amount of polynary nanometer strengthening phase is 0.1 ~ 20wt.%, and preferred total amount is 5 ~ 15wt.%.
Preferably, step 3) in, described reaction in-situ generate metal oxide, carbide, intermetallic compound mode be water-bath, oil bath, hydro-thermal, solvent thermal, atmosphere adds one or more that hanker, reactive mode determines according to selected precursor; Wherein need to add reductive agent (not needing to add reductive agent when generating other materials) when generating metal oxide particle, described reductive agent is the reagent in precursor solution, or solvent, reducing gas or aluminum substrate itself, particularly, reductive agent is one or more in citric acid, glucose, oxalic acid, quadrol, hydrazine hydrate, ethylene glycol, sodium borohydride, hydrogen, aluminium.
Preferably, step 3) in, described densification comprises: cold pressing, isostatic cool pressing, temperature and pressure, pressureless sintering, hot pressed sintering, hot isostatic pressing, and follow-up extruding, forging, jumping-up, one or more in rolling technology.
Preferably, step 3) in, described heat treated object is to make to carry out with the sufficient reacting of the nano metal of reactive aluminum or nano-metal-oxide particle, and generate intermetallic compound or alumina nanoparticles, mode is mainly annealing.
Refractory alloy (high temperature titanium base alloy, high-temperature nickel-base alloy, high temperature aluminum base alloy) research show, the high temperature deformation of alloy is controlled by flooding mechanism, according to High-Temperature Strengthening principle, suitable alloying element alloying need be selected to make in alloy, to produce high temperature not easily decomposition and inversion, the not easily thermally-stabilised wild phase of alligatoring, evenly tiny and Dispersed precipitate is in alloy matrix aluminum, and have enough volume contents, can effectively pin dislocation, stablize substructure, stop Grain Boundary Sliding, the diffusion of matrix recrystallize and solid solution element is suppressed while strengthening crystal boundary, improve matrix recrystallization temperature, hinder recrystallization softening, thus improve alloy high-temp performance.Therefore the high-temperature behavior of metallic substance depends on the thermally-stabilised wild phase in matrix, the thermostability of thermally-stabilised wild phase, size, distribution and the content final decision high-temperature behavior of alloy.The thermostability of precipitated phase is stronger, size is less, distribution high-temperature behavior that is more even, the higher then alloy of content is more excellent.
Technical solution of the present invention is optimized design for some enhancing key element above-mentioned emphatically:
1) wild phase of good thermal stability is introduced: there is L1 2three aluminide Al of structure 3m (M comprises following 9 kinds of elements: Ti, Zr, Sc, Er, Lu, Tm, Yb, Np, U), being provided with extremely strong thermostability because having coherent interface with the aluminum substrate of face-centred cubic structure, being considered to desirable thermally-stabilised wild phase; Meanwhile, metal oxide and the nano-sized carbon such as Graphene and carbon nanotube with ceramic structure have extremely strong thermostability equally.
2) reinforcement size is controlled at nanoscale: reaction in-situ is easy to the Al controlling to introduce nanometer 3m, aluminum oxide, metal oxide and nano-sized carbon etc.
3) the high volume content of nanophase is ensured: consider that metal or metal oxide nanoparticles differ huge with aluminium powder specific surface area, easily reunite, and nano-sized carbon has very high specific surface area equally, self metal or oxide nano-particles can be greater than by uniform loading cumulative volume, the powder treatment process such as, surface adsorption blended by ball milling, slurry is dispersed in aluminium powder again, thus realizes dispersed in aluminium of metal or metal oxide nanoparticles as intermediate; Processing method of the present invention introduces the reinforcement of multiple thermal stability excellence by nano-sized carbon load, realize the dispersed of polynary nanometer phase simultaneously, because the space occupy-place of different sorts nanophase is different, the easy agglomeration of the nanophase avoiding high volume content to cause.Therefore, the introducing of the thermally-stabilised disperse phase of high-content nano-scale, makes alumina-base material Good Heat-resistance, and adopts nano-sized carbon load technology to make preparation process simple, low for equipment requirements and be easy to grasp.
Compared with prior art, the present invention has the following advantages:
1) metal of chemical process fabricated in situ and metal oxide nanoparticles content, size, morphology controllable;
2) by the carrier function of nano-sized carbon, dispersed in alumina-base material of a large amount of heterogeneous nanophase can be realized, do not need to carry out violent viscous deformation;
3) by the reaction of additional reducing agent or aluminum substrate and metal and metal oxide nanoparticles, the introducing of nanophase can be realized under relatively mild condition;
4) use conventional chemical processes and powder metallurgy technology, be easy to carry out suitability for industrialized production.
In sum, the nanophase volume fraction of gained of the present invention is high, kind extensively, be evenly distributed, technical scheme is simple and easy to do, is suitable for preparing nanophase in enormous quantities and strengthens heat resisting aluminium base material.
Accompanying drawing explanation
By reading the detailed description done non-limiting example with reference to the following drawings, other features, objects and advantages of the present invention will become more obvious:
Fig. 1 is preparation technology's schema of the embodiment of the present invention.
Embodiment
Elaborate to embodiments of the invention below, the present embodiment is implemented under premised on technical solution of the present invention, give detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
The present embodiment provides a kind of method by nano-sized carbon loaded with nano metal Preparation polynary nanometer composite heat-resisting enhance aluminum matrix composite, and the method at nano-sized carbon surface clad ion precursor solution, obtains precursor coating nano carbon in advance; Then precursor coating nano carbon to be dispersed in aluminium powder and to make it turn to nano-oxide by thermal treatment, obtaining (nano-sized carbon+nano-oxide)/aluminium composite powder; And then reaction sintering and densification, thermal treatment are carried out to gained composite powder, thus obtain polynary nanometer reinforced aluminum matrix composites.
In following embodiment, what all substrates adopted is different Al alloy powders, wherein: embodiment 1 is 325 order 6061 Al alloy powders; Embodiment 2 is diameter 10 μm of pure aluminium powder; Embodiment 3 is 300 order 2024 aluminium powders.
Comparative example 1 is as the simultaneous test of embodiment 1, spherical 6061 Al alloy powders of employing carbon nanotube identical with embodiment 1,325 orders prepare aluminum matrix composite as initial raw material, reaction sintering and densified conditions are also identical, unlike directly adopting the spherical TiO of diameter 30nm 2powder and its directly directly carry out ball milling with carbon nanotube, aluminium powder and mix.The nanophase of embodiment 1 is carbon nanotube, nanometer Al 3ti and nanometer Al 2o 3, the nanophase of embodiment 2 is carbon nanotube and nanometer La 2o 3, the nanophase of embodiment 3 is Graphene and nanometer Al 3ni.The nano-sized carbon carrier of embodiment 1,2 is carbon nanotube, and the nano-sized carbon carrier of embodiment 3 is graphene oxide, and the design component of each embodiment lists in table 1.In all embodiments, the room-temperature mechanical property of material all carries out with reference to " GB/T228.1-2010 ", and rate of extension is 0.5mm/min, and in all embodiments, the mechanical behavior under high temperature of material is all carried out with reference to " GB/T4338-2006 ", and rate of extension is 0.5mm/min.
Embodiment 1:
By 6mlTiCl 4, 12g citric acid and 10ml ethylene glycol is dissolved in 40ml alcohol, magnetic agitation makes it fully to dissolve to obtain precursor solution; 3g carbon nanotube ultrasonic 1h in 400ml alcohol is formed dispersing Nano carbon tubes dispersion liquid.Be added drop-wise in carbon nano tube dispersion liquid by precursor solution, and continue ultrasonic 1h and make precursor be coated to carbon nano tube surface, in dispersion liquid, add 93g aluminium powder, after magnetic agitation 0.5h, suction filtration drying obtains precursor-carbon nanotube-aluminium composite powder.Again precursor-carbon nanotube-aluminium composite powder is put into N 2be heated to 230 DEG C of reaction 1h in tube furnace under atmosphere protection, reheat the organism that 600 DEG C of insulation 0.5h remove surface residual, obtain nano-titanium oxide--carbon nanotube-aluminium composite powder.By nano-titanium oxide--carbon nanotube-aluminium composite powder is cold-pressed into after the ingot blank of diameter 40mm at 600 DEG C, N in punching block 22h is sintered under atmosphere.Then by sintered blank at 550 DEG C, N 2anneal under atmosphere 6h, and in annealing, nano-titanium oxide and aluminum substrate reaction, form nanometer Al 3ti, nanometer Al 2o 3, nanometer Al 4c 3with the alumina-base material that the quaternary nanophase such as carbon nanotube strengthens, room-temperature mechanical property and the mechanical behavior under high temperature of the material of final preparation list in table 2 and table 3 respectively.
Embodiment 2:
By 9gLa 2cl 35H 2o and 5g polyvinylpyrrolidone is dissolved in 20ml water, and magnetic agitation makes it fully to dissolve to obtain precursor solution; By 1g carbon nanotube and 1g Graphene, ultrasonic 1h in 200ml water forms dispersing Nano carbon tubes dispersion liquid respectively.Be added drop-wise to respectively getting half quality precursor solution respectively in carbon nano tube dispersion liquid and graphene dispersing solution, and continue ultrasonic 1h and make precursor be coated to carbon nano tube surface and graphenic surface, suction filtration drying subsequently obtains precursor-carbon nano-tube composite powder end.N is put at precursor-carbon nano-tube composite powder end 2be heated to 600 DEG C of insulation 2h in tube furnace under atmosphere protection, obtain nano lanthanum oxide-carbon nano-tube composite powder end.After being mixed with 93g aluminium powder at nano lanthanum oxide-carbon nano-tube composite powder end, with 20:1 ratio of grinding media to material, 425rpm rotating speed ball milling 8h in planetary ball mill, obtain nano lanthanum oxide-carbon nanotube-aluminium composite powder.By nano lanthanum oxide-carbon nanotube-aluminium composite powder in diameter 40mm punching block, 500 DEG C, 400MPa pressure, hot pressed sintering 2h under vacuum condition, obtain nanometer La 2o 3, nanometer Al 3c 4with the alumina-base material that carbon nanometer pipe ternary nanophase strengthens.Room-temperature mechanical property and the mechanical behavior under high temperature of the material of final preparation list in table 2 and table 3 respectively.
Embodiment 3:
By 12gNiCl 26H 2o and 20g glucose is dissolved in 20ml water, and magnetic agitation makes it fully to dissolve to obtain precursor solution; 0.5g graphene oxide ultrasonic 1h in 200ml water is formed graphene oxide dispersion.Precursor solution is added drop-wise in graphene oxide dispersion, and continues ultrasonic 1h and make precursor be coated to surface of graphene oxide.96.5g2024 Al alloy powder is placed in 200ml water magnetic agitation, slowly drip graphene oxide dispersion, vigorous stirring solution subsequently, adds 8g sodium borohydride, then carries out suction filtration drying, obtains nano nickel-graphene oxide-aluminium composite powder simultaneously.Nano nickel-graphene oxide-aluminium composite powder is cold-pressed in punching block after the ingot blank of diameter 40mm at 600 DEG C, N 22h is sintered under atmosphere.In sintering process, nano nickel and aluminum substrate reaction, form nanometer Al 3ni, nanometer Al 3c 4and the alumina-base material that Graphene strengthens.Room-temperature mechanical property and the mechanical behavior under high temperature of the material of final preparation list in table 2 and table 3 respectively.
Comparative example 1:
Be, after the TiO2 powder of 30nm, 3g carbon nanotube and 93g fine aluminium powder carry out ball milling mixing, powder is being put into N by 4g diameter 2be heated to 230 DEG C of reaction 1h in tube furnace under atmosphere protection, reheat the organism that 600 DEG C of insulation 0.5h remove surface residual, obtain nano-titanium oxide--carbon nanotube-aluminium composite powder.By nano-titanium oxide--carbon nanotube-aluminium powder form is cold-pressed into after the ingot blank of diameter 40mm at 600 DEG C, N in punching block 22h is sintered under atmosphere.Then by sintered blank at 550 DEG C, N 2anneal under atmosphere 6h, obtained final matrix material, and its room-temperature mechanical property and mechanical behavior under high temperature list in table 2 and table 3 respectively, obviously due to the difference of its reinforcement dispersiveness, cause its over-all properties comparatively embodiment 1 have obvious decline.
The composition of table 1 matrix material
The room-temperature mechanical property of table 2 matrix material
The high-temperature behavior of table 3 matrix material
The metal of chemical process fabricated in situ of the present invention and metal oxide nanoparticles content, size, morphology controllable; By the carrier function of nano-sized carbon, dispersed in alumina-base material of a large amount of heterogeneous nanophase can be realized, do not need to carry out violent viscous deformation; By the reaction of additional reducing agent or aluminum substrate and metal and metal oxide nanoparticles, the introducing of nanophase can be realized under relatively mild condition; Use conventional chemical processes and powder metallurgy technology, be easy to carry out suitability for industrialized production.The nanophase volume fraction of gained of the present invention is high, kind extensively, be evenly distributed, technical scheme is simple and easy to do, is suitable for preparing nanophase in enormous quantities and strengthens heat resisting aluminium base material.
Above specific embodiments of the invention are described.It is to be appreciated that the present invention is not limited to above-mentioned particular implementation, those skilled in the art can make various distortion or amendment within the scope of the claims, and this does not affect flesh and blood of the present invention.

Claims (12)

1. a preparation method for polynary nanometer composite heat-resisting enhance aluminum matrix composite, is characterized in that, comprises the following steps:
1) adopt nano-sized carbon as carrier, with the precursor solution containing metal ion, Surface coating is carried out to nano-sized carbon, obtain precursor coating nano carbon;
2) by step 1) the precursor coating nano carbon that obtains is dispersed in aluminium powder, make the precursor in precursor coating nano carbon be transformed into nano-oxide by thermal response process, thus obtain (nano-sized carbon+nano-oxide)/aluminium composite powder;
3) to step 2) (nano-sized carbon+nano-oxide)/aluminium composite powder of obtaining carries out reaction sintering and densification, thermal treatment, generate the polynary nanometer strengthening phase of metal oxide, carbide, intermetallic compound and residue nano-sized carbon via reaction in-situ, thus obtain polynary nanometer composite heat-resisting enhance aluminum matrix composite.
2. the preparation method of a kind of polynary nanometer composite heat-resisting enhance aluminum matrix composite according to claim 1, it is characterized in that, step 1) in, described nano-sized carbon be size be not more than in the carbon nanophase of 100nm one or more, and at least can form stable rare dispersion liquid with a kind of solvent, nano-sized carbon adds 0.01 ~ 5wt.% that total amount is final matrix material quality.
3. the preparation method of a kind of polynary nanometer composite heat-resisting enhance aluminum matrix composite according to claim 2, is characterized in that, described nano-sized carbon is one or more in carbon nano fiber, carbon nanotube, Graphene, graphene oxide.
4. the preparation method of a kind of polynary nanometer composite heat-resisting enhance aluminum matrix composite according to claim 2, is characterized in that, described nano-sized carbon adds 0.5 ~ 3wt.% that total amount is final matrix material quality.
5. the preparation method of a kind of polynary nanometer composite heat-resisting enhance aluminum matrix composite according to claim 1, it is characterized in that, step 1) in, described precursor solution is made up of solvent, metal ion compound, or is made up of solvent, metal ion compound, linking agent and/or reagent.
6. the preparation method of a kind of polynary nanometer composite heat-resisting enhance aluminum matrix composite according to claim 5, is characterized in that, described solvent is one in water, methyl alcohol, ethanol, ethylene glycol, toluene, DMF, tween or combination;
Described metal ion compound is one in the oxide compound of Fe, Ni, Ti, Zr, Sc, Co, La, Y, Er, oxyhydroxide, halogenide, nitrate, vitriol, metallocene compound, carbonyl compound or its combination, and the final metal oxide generated is 0.1 ~ 20wt.% of matrix material quality;
Described reagent uses citric acid, glucose, oxalic acid, tartrate, dextrin, EDTA, quadrol, one in hydrazine hydrate or combination, and reagent also can not use;
Described linking agent makes one in spent glycol, polyoxyethylene glycol, polyvinyl alcohol, POLYPROPYLENE GLYCOL, polyvinylpyrrolidone, polypyrrole or combination, and linking agent also can not use.
7. the preparation method of a kind of polynary nanometer composite heat-resisting enhance aluminum matrix composite according to claim 1, it is characterized in that, step 1) in, described surface coating method is: nano-sized carbon joined in precursor solution and carry out mechanical stirring or ultrasonic, then carries out suction filtration, centrifugal or evaporate to dryness.
8. the preparation method of a kind of polynary nanometer composite heat-resisting enhance aluminum matrix composite according to claim 1, it is characterized in that, step 2) in, the described precursor coating nano carbon method be dispersed in aluminium powder is that ball milling, slip are blended, one or more in surface adsorption; Described aluminium powder is fine aluminium and/or Al alloy powder.
9. the preparation method of a kind of polynary nanometer composite heat-resisting enhance aluminum matrix composite according to any one of claim 1-8, it is characterized in that, step 3) in, the polynary nanometer strengthening phase of described metal oxide, carbide, intermetallic compound, characteristic dimension is in one direction not more than 100nm; The total amount of described polynary nanometer strengthening phase is 0.1 ~ 20wt.% of whole matrix material quality.
10. the preparation method of a kind of polynary nanometer composite heat-resisting enhance aluminum matrix composite according to claim 9, is characterized in that, the total amount of described polynary nanometer strengthening phase is 5 ~ 15wt.% of whole matrix material quality.
The preparation method of 11. a kind of polynary nanometer composite heat-resisting enhance aluminum matrix composites according to any one of claim 1-8, it is characterized in that, step 3) in, the mode of described reaction in-situ metal oxide, carbide, intermetallic compound is water-bath, oil bath, hydro-thermal, solvent thermal, atmosphere add one or more that hanker, and reactive mode determines according to selected precursor;
Described needs to add reductive agent by during (nano-sized carbon+nano-oxide)/aluminium composite powder reaction in-situ generation metal oxide; Described reductive agent is the reagent in precursor solution, or solvent, reducing gas or aluminum substrate itself, particularly, reductive agent is one or more in citric acid, glucose, oxalic acid, quadrol, hydrazine hydrate, ethylene glycol, sodium borohydride, hydrogen or aluminium.
The preparation method of 12. a kind of polynary nanometer composite heat-resisting enhance aluminum matrix composites according to any one of claim 1-8, it is characterized in that, step 3) in, described densification comprises: cold pressing, isostatic cool pressing, temperature and pressure, pressureless sintering, hot pressed sintering, hot isostatic pressing, and follow-up extruding, forging, jumping-up, one or more in rolling technology.
CN201510695569.9A 2015-10-22 2015-10-22 A kind of preparation method of polynary nanometer complex intensifying heat resisting aluminium base composite material Active CN105385871B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510695569.9A CN105385871B (en) 2015-10-22 2015-10-22 A kind of preparation method of polynary nanometer complex intensifying heat resisting aluminium base composite material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510695569.9A CN105385871B (en) 2015-10-22 2015-10-22 A kind of preparation method of polynary nanometer complex intensifying heat resisting aluminium base composite material

Publications (2)

Publication Number Publication Date
CN105385871A true CN105385871A (en) 2016-03-09
CN105385871B CN105385871B (en) 2018-01-19

Family

ID=55418643

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510695569.9A Active CN105385871B (en) 2015-10-22 2015-10-22 A kind of preparation method of polynary nanometer complex intensifying heat resisting aluminium base composite material

Country Status (1)

Country Link
CN (1) CN105385871B (en)

Cited By (21)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105798302A (en) * 2016-05-16 2016-07-27 江苏悦达新材料科技有限公司 Preparation method of superconductive plate for refrigerator
CN106025595A (en) * 2016-05-24 2016-10-12 国网江西省电力科学研究院 Preparation method of high-resistance reduction corrosion-resistant and abrasion-resistant grounding body
CN106399873A (en) * 2016-09-09 2017-02-15 南昌大学 Preparation method for whisker nanotube-reinforced magnesium matrix composite coated with aluminum oxide
CN106399880A (en) * 2016-09-09 2017-02-15 南昌大学 Preparation method for whisker carbon nanotube-reinforced aluminum matrix composite coated with aluminum oxide
CN106566942A (en) * 2016-10-24 2017-04-19 上海理工大学 A method of preparing a high-performance graphene reinforced aluminium-based composite material
CN107254644A (en) * 2017-05-26 2017-10-17 贵州全世通精密机械科技有限公司 A kind of high intensity alumina-base material and preparation method thereof
CN108672702A (en) * 2018-05-21 2018-10-19 宁波市奇强精密冲件有限公司 Damper knuckle support
CN109207780A (en) * 2018-09-17 2019-01-15 南昌大学 A kind of milling method enhancing AZ31 magnesium alloy
CN109207781A (en) * 2018-09-17 2019-01-15 南昌大学 A kind of pressing method improving 7075 aluminium alloys
CN109207782A (en) * 2018-09-17 2019-01-15 南昌大学 A kind of coated with titanium oxide/graphene oxide reinforced Si phase method for preparing aluminum-based composite material
CN109439964A (en) * 2018-09-08 2019-03-08 天津大学 Carbon nanotube-graphene collaboration reinforced aluminum matrix composites mechanical property preparation method
CN110744045A (en) * 2019-09-06 2020-02-04 西安交通大学 Method for in-situ synthesis of carbon nano tube on surface of aluminum alloy spherical powder
CN111235436A (en) * 2020-01-16 2020-06-05 上海交通大学 In-situ synthesized aluminum carbide reinforced aluminum-based composite material and preparation method thereof
CN112024896A (en) * 2020-10-16 2020-12-04 湘潭大学 Preparation method of CNTs-ZA27 zinc-aluminum-based composite bar with high C content
CN112542279A (en) * 2020-11-25 2021-03-23 诺正集团股份有限公司 Preparation method of homogeneous graphene aluminum alloy cable
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
CN114523099A (en) * 2022-04-23 2022-05-24 南通瑞升运动休闲用品有限公司 High-performance metal composite material and preparation method thereof
CN114686786A (en) * 2020-12-25 2022-07-01 南京凤源新材料科技有限公司 Graphene oxide and carbon nanotube reinforced aluminum-based composite material and preparation method thereof
CN115896550A (en) * 2021-09-29 2023-04-04 矢崎总业株式会社 Aluminum-based composite member, method for producing same, and electrically connecting member
CN116024447A (en) * 2022-12-30 2023-04-28 中国科学院金属研究所 Preparation method of aluminum alloy material
US11732327B2 (en) 2019-11-29 2023-08-22 Nanjing Tech University Nano-carbon reinforced aluminum matrix composites for conductor and preparation method

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000345254A (en) * 1999-06-03 2000-12-12 Toyota Motor Corp Aluminum base composite material and its production
CN104264000A (en) * 2014-09-03 2015-01-07 上海交通大学 Graphene modified high-heat-conductivity aluminum-based composite material and powder metallurgy preparation method
CN104962841A (en) * 2015-05-26 2015-10-07 上海交通大学 Interface design and preparation method of carbon nanotube metal matrix composite material

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000345254A (en) * 1999-06-03 2000-12-12 Toyota Motor Corp Aluminum base composite material and its production
CN104264000A (en) * 2014-09-03 2015-01-07 上海交通大学 Graphene modified high-heat-conductivity aluminum-based composite material and powder metallurgy preparation method
CN104962841A (en) * 2015-05-26 2015-10-07 上海交通大学 Interface design and preparation method of carbon nanotube metal matrix composite material

Cited By (28)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105798302A (en) * 2016-05-16 2016-07-27 江苏悦达新材料科技有限公司 Preparation method of superconductive plate for refrigerator
CN106025595A (en) * 2016-05-24 2016-10-12 国网江西省电力科学研究院 Preparation method of high-resistance reduction corrosion-resistant and abrasion-resistant grounding body
CN106399873A (en) * 2016-09-09 2017-02-15 南昌大学 Preparation method for whisker nanotube-reinforced magnesium matrix composite coated with aluminum oxide
CN106399880A (en) * 2016-09-09 2017-02-15 南昌大学 Preparation method for whisker carbon nanotube-reinforced aluminum matrix composite coated with aluminum oxide
CN106399880B (en) * 2016-09-09 2018-05-25 南昌大学 A kind of preparation method of coating alumina whisker carbon nanotube enhanced aluminium-based composite material
CN106566942A (en) * 2016-10-24 2017-04-19 上海理工大学 A method of preparing a high-performance graphene reinforced aluminium-based composite material
CN106566942B (en) * 2016-10-24 2018-05-22 上海理工大学 A kind of method for preparing High-performance graphene reinforced aluminum matrix composites
CN107254644A (en) * 2017-05-26 2017-10-17 贵州全世通精密机械科技有限公司 A kind of high intensity alumina-base material and preparation method thereof
CN108672702A (en) * 2018-05-21 2018-10-19 宁波市奇强精密冲件有限公司 Damper knuckle support
CN109439964A (en) * 2018-09-08 2019-03-08 天津大学 Carbon nanotube-graphene collaboration reinforced aluminum matrix composites mechanical property preparation method
CN109207780A (en) * 2018-09-17 2019-01-15 南昌大学 A kind of milling method enhancing AZ31 magnesium alloy
CN109207781A (en) * 2018-09-17 2019-01-15 南昌大学 A kind of pressing method improving 7075 aluminium alloys
CN109207782A (en) * 2018-09-17 2019-01-15 南昌大学 A kind of coated with titanium oxide/graphene oxide reinforced Si phase method for preparing aluminum-based composite material
CN109207780B (en) * 2018-09-17 2020-07-14 南昌大学 Rolling method for reinforcing AZ31 magnesium alloy
CN110744045A (en) * 2019-09-06 2020-02-04 西安交通大学 Method for in-situ synthesis of carbon nano tube on surface of aluminum alloy spherical powder
US11732327B2 (en) 2019-11-29 2023-08-22 Nanjing Tech University Nano-carbon reinforced aluminum matrix composites for conductor and preparation method
CN111235436A (en) * 2020-01-16 2020-06-05 上海交通大学 In-situ synthesized aluminum carbide reinforced aluminum-based composite material and preparation method thereof
CN111235436B (en) * 2020-01-16 2021-02-02 上海交通大学 In-situ synthesized aluminum carbide reinforced aluminum-based composite material and preparation method thereof
CN112024896B (en) * 2020-10-16 2023-03-28 湘潭大学 Preparation method of CNTs-ZA27 zinc-aluminum-based composite bar with high C content
CN112024896A (en) * 2020-10-16 2020-12-04 湘潭大学 Preparation method of CNTs-ZA27 zinc-aluminum-based composite bar with high C content
CN112542279A (en) * 2020-11-25 2021-03-23 诺正集团股份有限公司 Preparation method of homogeneous graphene aluminum alloy cable
CN112542279B (en) * 2020-11-25 2021-08-27 诺正集团股份有限公司 Preparation method of homogeneous graphene aluminum alloy cable
CN114686786A (en) * 2020-12-25 2022-07-01 南京凤源新材料科技有限公司 Graphene oxide and carbon nanotube reinforced aluminum-based composite material and preparation method thereof
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
CN115896550A (en) * 2021-09-29 2023-04-04 矢崎总业株式会社 Aluminum-based composite member, method for producing same, and electrically connecting member
CN114523099A (en) * 2022-04-23 2022-05-24 南通瑞升运动休闲用品有限公司 High-performance metal composite material and preparation method thereof
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

Also Published As

Publication number Publication date
CN105385871B (en) 2018-01-19

Similar Documents

Publication Publication Date Title
CN105385871A (en) Preparing method of multielement nanometer composite strengthening thermal-resisting aluminum matrix composite
Hu et al. Microstructure refinement and mechanical properties improvement in the W-Y2O3 alloys via optimized freeze-drying
Ma et al. Research status and development of magnesium matrix composites
Dong et al. The simultaneous improvements of strength and ductility in W–Y2O3 alloy obtained via an alkaline hydrothermal method and subsequent low temperature sintering
Dong et al. The synthesis of composite powder precursors via chemical processes for the sintering of oxide dispersion-strengthened alloys
CN106077695B (en) A kind of preparation method of high-copper tungsten copper nano composite powder
CN106555089B (en) A kind of carbon nanotube and nano-ceramic particle mixing reinforced magnesium-base composite material and preparation method
CN106191494B (en) Carbon nanotube enhances the metallurgical preparation method of titanium matrix composite
CN109554565A (en) A kind of interface optimization method of carbon nanotube enhanced aluminium-based composite material
Li et al. Microstructure and properties of La2O3 doped W composites prepared by a wet chemical process
CN111020333B (en) Method for refining size of yttrium oxide at crystal boundary in yttrium oxide dispersion-strengthened tungsten-based alloy
Zhou et al. Densification and microstructure evolution of W-TiC-Y2O3 during spark plasma sintering
Xiang et al. Synthesis and microstructure of tantalum carbide and carbon composite by liquid precursor route
CN112226639B (en) In-situ ultrafine grain TiC reinforced titanium-based composite material based on cyclohexene ball milling medium and preparation method thereof
Wu et al. Preparation technology of ultra-fine tungsten carbide powders: an overview
CN108531780B (en) Preparation method of graphene reinforced nickel-aluminum alloy based composite material
CN114164367A (en) High-toughness fine-grain molybdenum alloy and preparation method thereof
Zhang et al. Preparation and properties of Al2O3 dispersed fine-grained W-Cu alloy
CN112011703A (en) High-hardness composite oxide dispersion strengthening ODS tungsten alloy and preparation method thereof
Qian et al. Effect of the carbon content on the morphology evolution of the η phase in cemented carbides with the CoNiFeCr high entropy alloy binder
CN112846198A (en) Nanoparticle reinforced metal matrix composite material and preparation method thereof
Wen et al. 2D materials-based metal matrix composites
Xu et al. Properties and microstructure of oxide dispersion strengthened tungsten alloy prepared by liquid-phase method: a review
Wang et al. In-situ manipulation of TiB whisker orientation and investigation of its high-temperature mechanical properties in titanium matrix composites
Li et al. Inhibiting GNPs breakage during ball milling for a balanced strength-ductility match in GNPs/Al composites

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant