CN106399872B - A kind of preparation method of the whisker carbon nanotubes-aluminum composites semi-solid blank of coating alumina - Google Patents
A kind of preparation method of the whisker carbon nanotubes-aluminum composites semi-solid blank of coating alumina Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
- C22C47/02—Pretreatment of the fibres or filaments
- C22C47/04—Pretreatment of the fibres or filaments by coating, e.g. with a protective or activated covering
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
- C22C47/14—Making alloys containing metallic or non-metallic fibres or filaments by powder metallurgy, i.e. by processing mixtures of metal powder and fibres or filaments
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
- C22C49/02—Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
- C22C49/04—Light metals
- C22C49/06—Aluminium
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
- C22C49/14—Alloys containing metallic or non-metallic fibres or filaments characterised by the fibres or filaments
Abstract
A kind of preparation method of the whisker carbon nanotubes-aluminum composites semi-solid blank of coating alumina; first prepare the whisker CNT of coating alumina; then the whisker carbon nano-tube material of Al alloy powder and coating alumina is imported in ball milling crucible, the lower ball milling of argon gas protection；Mixed-powder is put into crucible afterwards; after 10~20 DEG C of subsolidus being heated to common muffle furnace; it is transferred to and continues to heat in ultrasonic magnetic agitation stove and control its solid rate in certain limit; ultrasound and the lower stirring at low speed of magnetic force devices synergy are disperseed, and are passed through argon gas and are protected and mixing time is controlled；Gained slurry is poured into corresponding mould cooling, obtains semi-solid blank.The present invention has the advantages that simple, safety, low cost are easily operated and controllable.
Description
Technical field
The invention belongs to technical field of material.
Background technology
In recent years, composite strengthening is carried out to aluminium alloy using fiber or particle, the aluminum matrix composite of preparation is due to its height
Specific strength, the advantages that good electrical and thermal conductivity performance and low thermal coefficient of expansion, attracted very big to pay close attention to and be widely used in navigating
The fields such as its aviation, automobile making, electronic instrument.
CNT is the tube formed by the curling of graphite hexagonal network, has unique hollow nano structure, envelope
The topology configuration and helical structure closed, so as to a large amount of special excellent properties, as high intensity, high resiliency, high-specific surface area,
Heat-resisting, corrosion-resistant, heat conduction and electric conductivity etc., imply CNT has huge application space in materials application research.Carbon
The modulus of nanotube is identical with diamond, and theoretical strength has reached 106MPa, it is 100 times of steel, and density is only steel
1/6, while it has both extremely excellent toughness and structural stability again, is the ideal chose as composite enhancing phase.Right CNT's
Defect is also apparent.Carbon pipe is due to its stable SP2Structure, show the wetability of extreme difference simultaneously, CNT is in founding
During easily reunite and wrapping phenomena causes not strong with metallic matrix interfacial bonding property, be unfavorable for the increasing of composite property
By force.Therefore, agglomeration of the CNT in Metal Forming Process how is reduced, and improve itself and the wetability of matrix to turn into
The key of the excellent carbon nano-tube reinforced metal-matrix composite material of processability.
For crystal whisker-shaped carbon nanotube as a kind of new structure CNT, being compared to original carbon nanotubes has surface more
Add smooth, highly polished, the features such as diameter change is little and curvature is low, outside dimension is distributed between 50~200nm, length point
Cloth is between 2~20 μm.Mixed and disorderly degree of aggregation is low, can promote the dispersing technology of CNT to a certain extent, be CNT
Industrialization with providing greatly possibility.
CNT, which improves wetability method, at present overlay coating etc., and such as chemical nickel plating, this method mainly will complete base
The CNT of change is through sensitization plays, after activation, is put into plating in chemical plating fluid, can be in carbon nano tube surface with the progress of reaction
Continuous, uniform coating is obtained, but it is expensive, and toxic reagent is commonly used, not environmentally and production cost is high, is not suitable for big rule
Mould produces.Sol method is also popular research coating direction, adds organic compound in the solution and stirs, reaction a period of time,
Then CNT is added, acid group metallic compound is added and is kept stirring for state until generation colloidal sol, sky is exposed to by this colloid
Aging in gas, product grind into powder is dried after a few days, be heat-treated in last certain temperature inert gas flow and obtain for a period of time
To nano-complex particle.But the proportioning difficulty of amount is big, and the reaction time is long.
It is entitled in publication CN101966449A：" for a kind of multiwall carbon nanotube-supported titanium dioxide catalyst
Preparation method " in.Solvent heat and hydro-thermal method are combined, adsorb colloid in a solvent, is dried in CNT surface, hydro-thermal point
Its colloid is solved, obtains aoxidizing applicator.Right this method step is complicated, time length, and can not coat simple substance in CNT surface, tool
There is certain limitation.
On the other hand, the control to CNT dispersiveness is generally embodied in metal preparation process.At present, stirring is passed through
It is relatively conventional that casting, in-situ synthesis and powder metallurgic method prepare the strong aluminum matrix composite of CNT.But this several side
The defects of method is also that enhancing distributed mutually is uneven, powder it is clear that CNT is as the flowing of melt is reunited seriously under casting condition
Last metallurgy is popular research direction, but interface cohesion and fine and close sex chromosome mosaicism fail effectively to be solved.In-situ synthesis is present
The short slabs such as technique is excessively complicated and process is difficult to control.
In publication CN103614672A, entitled " preparation method of carbon nanotube enhanced aluminium-based composite material "
In, employ the conventional powder metallurgical method such as batch mixing, drying, ball milling, cold pressing, sintering and extruding and be prepared for CNT enhancing aluminium
Based composites, right interfacial bonding property is poor, more prominent the problems such as material compactness in itself.
In publication number CN103911566A, a kind of entitled " powder metallurgy of carbon nano tube reinforced aluminum alloy composite material
It is more uniform by CNT using powder metallurgy process processing flake aluminum in preparation method ", but conventional powder metallurgical method
The defects of defect does not melt such as, and compactness is not good enough does not solve.
In publication CN101376932, entitled " CNT enhancing magnesium, aluminum matrix composite and its preparation side
Reho-forming method is mixed in method ", after being heated using powder and prepares CNT enhancing aluminium, magnesium-based composite material.Though it can improve
Fine and close sex chromosome mosaicism, but CNT easily reunites under rheological condition, and the performance raising to composite is unfavorable.
Therefore, a kind of cost-effective carbon nanotube enhanced aluminium-based composite material technology of preparing is still lacked at present.
It is a kind of new the invention is intended to provide to overcome traditional carbon nano tube compound material to be prepared into the technological difficulties of shape
CNT alumina-base material semi-solid blank technologies of preparing.Semisolid prepares forming technique and come across in the 1970s, the technique conduct
A kind of efficient, energy-conservation modern metallurgical technology, achieves develop rapidly in the past 40 years, application constantly expands.It relative to
The forming technology such as conventional cast and forging has several obvious advantages：Reduce gross segregation and the cavity of finished product, less shaping
Pressure, and relatively low mold temperature etc..Just because of the technology has a series of particular advantages so as to by catching people's attention, also must
This century most potential material forming techniques will be turned into.
Semisolid, which prepares forming technique, includes 3 semi-solid blank preparation, the reheating of blank and thixotropic forming passes
Prepared by key link, wherein semi-solid blank is core the most.It directly influences subsequent technique and final product quality.
The content of the invention
The purpose of the present invention is to propose to a kind of whisker carbon nanotubes-aluminum composites semi-solid blank of coating alumina
Preparation method.
The present invention is achieved by the following technical solutions.
A kind of preparation of the whisker carbon nanotubes-aluminum composites semi-solid blank of coating alumina of the present invention
Method, comprise the following steps.
（1）By whisker nanotube in the pure salpeter solution pre-dispersed 6 ~ 8h of ultrasound, temperature is 60 ~ 80 DEG C, after being cooled to room temperature,
Cleaned with deionized water, centrifuge to neutrality, then dried in vacuum drying chamber, it is standby.
（2）By aluminum nitrate and through step（1）The whisker CNT of pretreatment is added in methanol solution, and ultrasound 40~
60min, obtain whisker carbon nanotube suspension, wherein whisker CNT and nitric acid al mole ratio 1:0.4~1:1.
（3）Through step（2）The whisker carbon nanotube suspension of processing is imported in hydrothermal reaction kettle, wherein suspension volume
Account for the molten product 25%~40% of reactor.Place into reacting furnace and heat, 100~120 DEG C are warming up to 1~5 DEG C/min, insulation 1~
2h, then after being warming up to 150 DEG C with 1~3 DEG C/min, it is incubated 8~12h；It is cooled to 5 ~ 10 DEG C/min after room temperature and filters low temperature baking
It is dry.
（4）Through step（3）Gained mixing material is put into corundum crucible, 480 ~ 700 DEG C of high-temperature roastings 3 hours, whole
Argon gas protection is imported, obtains the whisker carbon nano-tube material of coating alumina.
（5）Step（4）The whisker carbon nano-tube material of obtained coating alumina mixes with Al alloy powder, is put into ball milling
Crucible carries out ball milling, and the wherein whisker carbon nano-tube material quality of coating alumina is the 2% ~ 4% of corresponding Al alloy powder amount, the time
Control is passed through argon gas and protected in 30 ~ 60min, the process.
（6）Step（5）Gained mixed-powder is put into crucible, with muffle furnace with 5 ~ 10 DEG C/min heating rates extremely
After 10 ~ 20 DEG C of subsolidus, be transferred to ultrasonic magnetic agitation stove continue to heat with 1 ~ 3 DEG C/min and control its solid rate in 20 ~
40% scope, ultrasound should be indirect ultrasound, and power is passed to by crucible bottom.And Power Control is in 1.0 ~ 2.0Kw, frequency
20KHz, stirring at low speed are simultaneously passed through argon gas protection, and ultrasonic magnetic agitation time control is in 1 ~ 3min.
（7）Step（6）Gained semi solid slurry pours into mould cooling, obtains the whisker CNT material of coating alumina
Material/aluminum matrix composite semi-solid blank.
In the present invention, the mixed-powder under semi-molten state is stirred using ultrasound and magnetic stirring equipment collaboration concussion,
CNT reunion, agglomerating and rising phenomenon can be reduced.Compared with traditional material technology of preparing, the low solid rate semi-solid blank
Preparing this technology of preparing has following features：（1）Semi-solid-state shaping belongs to near-net forming, easily reaches configuration design requirement.（2）
At low shear rates, slurry behaves like solidliquid mixture, only slight flow to semi solid slurry blank, viscosity compared with
Height, enhancing are mutually not easy to reunite.（3）The oxide decomposed in a heated condition using nitric acid metal carbonyl compound is deposited directly to crystalline substance
On palpus.（4）CNT is combined under the conditions of aluminium alloy semi-solid with matrix, is had more preferable interface simultaneously, is avoided founding
Under the conditions of CNT reunion.（5）Prepared using more straight and short carbon nano-tube material, further reduce carbon nanometer
The probability that pipe is reunited.
Brief description of the drawings
Accompanying drawing 1 is the semi-solid blank microstructure picture prepared by embodiment 1.
Embodiment
The present invention will be described further by following examples.
Embodiment 1.
By whisker CNT in the pure salpeter solution pre-dispersed 8h of ultrasound, temperature is 60 DEG C, after being cooled to room temperature, spend from
Sub- water cleaning, centrifuge to neutrality, be then dried for standby in vacuum drying chamber.With aluminum nitrate and the whisker CNT of above-mentioned drying
As raw material, ultrasonic 40min in methanol solution is added；Wherein whisker CNT, aluminum nitrate and methanol molar ratio are 1:0.4:
182, obtain whisker carbon nanotube suspension；The suspension is imported in hydrothermal reaction kettle, wherein suspension volume accounts for reactor
Molten product 25%.Place into reacting furnace and heat, be warming up to 100 DEG C with 5 DEG C/min, be incubated 1h, then 150 DEG C are warming up to 3 DEG C/min
Afterwards, it is incubated 8h；Be cooled to 5 DEG C/min after room temperature filter be put into corundum crucible after low temperature drying it is small with 500 DEG C of high-temperature roastings 3
When, the whisker carbon nano-tube material of coating alumina is obtained, the process is whole to import argon gas protection.
Whisker carbon nano-tube material and corresponding mass by mass fraction for 2% coating alumina of Al alloy powder
7075 Al alloy powders are put into ball milling crucible and carry out ball milling, the protection of whole argon gas, time control in 30min, after by mixed-powder
Crucible is poured into, with 10 DEG C/min heating rates to 455 DEG C.Afterwards by crucible move in magnetic agitation stove with 1 DEG C/min after
It is continuous to heat and control its solid rate in 20% scope.Ultrasonic power is controlled in 1.0Kw, magnetic force devices collaboration under stirring at low speed simultaneously
Be passed through argon gas protection, ultrasonic magnetic agitation time control in 3min, after pour into corresponding mould and be cooled to room temperature, obtain coating oxidation
The aluminium-based semisolid-state blank of the whisker CNT of aluminium/7075.
Embodiment 2.
By whisker CNT in the pure salpeter solution pre-dispersed 8h of ultrasound, temperature is 60 DEG C, after being cooled to room temperature, spend from
Sub- water cleaning, centrifuge to neutrality, be then dried for standby in vacuum drying chamber.With aluminum nitrate and the whisker CNT of above-mentioned drying
As raw material, ultrasonic 40min in methanol solution is added；Wherein whisker CNT, aluminum nitrate and methanol molar ratio are 1:0.7:
182, obtain whisker carbon nanotube suspension；The suspension is imported in hydrothermal reaction kettle, wherein suspension volume accounts for reactor
Molten product 30%.Place into reacting furnace and heat, be warming up to 120 DEG C with 3 DEG C/min, be incubated 1h, then 150 DEG C are warming up to 1 DEG C/min
Afterwards, it is incubated 10h；It is cooled to after filtering low temperature drying after room temperature and is put into corundum crucible with 600 DEG C of high-temperature roastings 3 with 7 DEG C/min
Hour, the whisker carbon nano-tube material of coating alumina is obtained, the process is whole to import argon gas protection.
Whisker carbon nano-tube material and 6061 aluminium alloys by mass fraction for 3% coating alumina of Al alloy powder
Powder is put into ball milling crucible and carries out ball milling, and whole argon gas protection, time control is in 30min.Mixed-powder is poured into crucible simultaneously afterwards
With 10 DEG C/min heating rates to 550 DEG C.After be transferred to and continue to heat with 3 DEG C/min in magnetic agitation stove and control its solid phase
For rate in 30% or so, ultrasonic power is controlled in 1.5Kw, and stirring at low speed and argon gas protection, ultrasonic magnetic are passed through under magnetic force devices collaboration
The control of power mixing time in 2min, after pour into corresponding mould and be cooled to room temperature, obtain the whisker CNT of coating alumina/
6061 aluminium-based semisolid-state blanks.
Embodiment 3.
By whisker CNT in the pure salpeter solution pre-dispersed 8h of ultrasound, temperature is 60 DEG C, after being cooled to room temperature, spend from
Sub- water cleaning, centrifuge to neutrality, be then dried for standby in vacuum drying chamber.With aluminum nitrate and the whisker CNT of above-mentioned drying
As raw material, ultrasonic 60min in methanol solution is added；Wherein whisker CNT, aluminum nitrate and methanol molar ratio are 1:1:
182, obtain whisker carbon nanotube suspension；The suspension is imported in hydrothermal reaction kettle, wherein suspension volume accounts for reactor
Molten product 40%.Place into reacting furnace and heat, be warming up to 120 DEG C with 3 DEG C/min, be incubated 1h, then 150 DEG C are warming up to 1 DEG C/min
Afterwards, it is incubated 12h；It is cooled to after filtering low temperature drying after room temperature and is put into corundum crucible with 700 DEG C of high-temperature roastings 3 with 10 DEG C/min
Hour, the whisker carbon nano-tube material of coating alumina is obtained, the process is whole to import argon gas protection.
Whisker carbon nano-tube material and 2024 aluminium alloys by mass fraction for 4% coating alumina of Al alloy powder
Powder imports ball milling crucible and carries out ball milling, and whole argon gas protection, time control is in 30min.Gained mixed-powder imports corresponding earthenware
Crucible is with 5 DEG C/min heating rates to 480 DEG C.After be transferred to and continue to heat with 5 DEG C/min in magnetic agitation stove and control it solid
For one after another in 40% or so, ultrasonic power is controlled in 2.0Kw, and stirring at low speed and argon gas protection, ultrasound are passed through under magnetic force devices collaboration
Magnetic agitation time control in 1min, after pour into corresponding mould and be cooled to room temperature, obtain the whisker CNT of coating alumina/
2024 aluminium-based semisolid-state blanks.
Claims (1)
1. a kind of preparation method of the whisker carbon nanotubes-aluminum composites semi-solid blank of coating alumina, it is characterized in that
Comprise the following steps：
（1）By whisker CNT in the pure salpeter solution pre-dispersed 6 ~ 8h of ultrasound, temperature is 60 ~ 80 DEG C, after being cooled to room temperature, is used
Deionized water is cleaned, and is centrifuged to neutrality, is then dried in vacuum drying chamber, standby；
（2）By aluminum nitrate and through step（1）The whisker CNT of pretreatment is added in methanol solution, 40~60min of ultrasound,
Obtain whisker carbon nanotube suspension, wherein whisker CNT and nitric acid al mole ratio 1:0.4~1:1；
（3）Through step（2）The whisker carbon nanotube suspension of processing is imported in hydrothermal reaction kettle, and wherein suspension volume accounts for instead
Answer kettle volume 25%~40%；Place into reacting furnace and heat, 100~120 DEG C are warming up to 1~5 DEG C/min, be incubated 1~2h, then
After being warming up to 150 DEG C with 1~3 DEG C/min, 8~12h is incubated；Low temperature drying is filtered after being cooled to room temperature with 5 ~ 10 DEG C/min；
（4）Through step（3）Gained mixing material is put into corundum crucible, and 480 ~ 700 DEG C of high-temperature roastings 3 hours, whole process imports
Argon gas is protected, and obtains the whisker carbon nano-tube material of coating alumina；
（5）Step（4）The whisker carbon nano-tube material of obtained coating alumina mixes with Al alloy powder, is put into ball milling crucible
Ball milling is carried out, the wherein whisker carbon nano-tube material quality of coating alumina is the 2% ~ 4% of corresponding Al alloy powder amount, time control
In 30 ~ 60min, the process is passed through argon gas and protected；
（6）Step（5）Gained mixed-powder is put into crucible, with muffle furnace with 5 ~ 10 DEG C/min heating rates to solid phase
Below line after 10 ~ 20 DEG C, it is transferred to ultrasonic magnetic agitation stove and continues to heat with 1 ~ 3 DEG C/min and control its solid rate in 20 ~ 40% models
Enclose, ultrasound should be indirect ultrasound, and power is passed to by crucible bottom；And Power Control is in 1.0 ~ 2.0kW, frequency 20KHz is low
Speed stirs and is passed through argon gas protection, and ultrasonic magnetic agitation time control is in 1 ~ 3min；
（7）Step（6）Gained semi solid slurry pours into mould cooling, obtain the whisker carbon nano-tube material of coating alumina/
Aluminum matrix composite semi-solid blank.
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| CN109207782B (en) * | 2018-09-17 | 2020-07-14 | 南昌大学 | Preparation method of titanium oxide/graphene oxide coated reinforced silicon-phase aluminum-based composite material |
| CN110669956A (en) * | 2019-11-21 | 2020-01-10 | 吉林大学 | Preparation method of carbon nano tube reinforced aluminum-based composite material with surface coated with aluminum oxide |
| CN111286634B (en) * | 2020-02-27 | 2021-03-16 | 南昌航空大学 | Preparation method of cerium oxide-coated graphene oxide aluminum material semi-solid blank |
| CN113088744B (en) * | 2021-02-20 | 2022-03-22 | 南昌大学 | Preparation method of modified carbon nanotube reinforced aluminum alloy semi-solid slurry |
| CN113444906B (en) * | 2021-06-10 | 2023-06-16 | 湘潭大学 | Method for preparing carbon nano tube reinforced light aluminum-based alloy |
| CN114172296B (en) * | 2022-02-08 | 2022-05-13 | 爱柯迪股份有限公司 | Sapphire reinforced aluminum alloy motor shell for electric automobile and preparation method |
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| JP2011047029A (en) * | 2009-08-27 | 2011-03-10 | Taisei Kaken:Kk | METHOD FOR PRODUCING ALTERNATIVE RARE METAL BY COMPOSITE NANOMETAL STOCK OF Fe-Cu, Fe-Al OR THE LIKE INCLUDING CARBON NANOTUBE-REINFORCING Fe GROUP, AND PRODUCT THEREBY |
| CN102108455B (en) * | 2009-12-25 | 2013-11-06 | 清华大学 | Preparation method of aluminum-base composite material |
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| CN104549146B (en) * | 2014-12-10 | 2017-10-13 | 湖南大学 | Multi-walled carbon nanotube nano composite material of aluminum oxide modification and its preparation method and application |
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