CN106350695B - A kind of preparation method of simple substance copper clad multi-walled carbon nanotube/aluminum matrix composite semi-solid blank - Google Patents
A kind of preparation method of simple substance copper clad multi-walled carbon nanotube/aluminum matrix composite semi-solid blank Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/12—Making non-ferrous alloys by processing in a semi-solid state, e.g. holding the alloy in the solid-liquid phase
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- C22C1/101—Pretreatment of the non-metallic additives by coating
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- C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
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- C22C49/06—Aluminium
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Abstract
A kind of preparation method of simple substance copper clad multi-walled carbon nanotube/aluminum matrix composite semi-solid blank; first prepare the multi-walled carbon nanotube of cladding elemental copper; then Al alloy powder and simple substance copper clad multi-walled carbon nanotube are imported in ball milling crucible, the lower ball-milling treatment of argon gas protection.Mixed-powder is put into crucible afterwards, after being heated to 20~40 DEG C of subsolidus with muffle furnace, ultrasonic magnetic agitation stove is transferred to and continues to heat and control its solid rate in a certain range, low speed concussion stirs and is passed through argon gas protection and mixing time is controlled.Gained slurry is poured into corresponding mould cooling, obtains semi-solid blank.Technology of preparing disclosed in this 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, using fiber or particle to aluminium alloy enhancing for composite, 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.
Carbon nanotubes 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 that with 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 carbon nanotubes has huge application space in materials application research.Carbon
The modulus of nanotube is identical with diamond, and theoretical strength has reached 106Megapascal, 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 material enhancing phase.Right CNT's
Defect is also apparent.Carbon pipe is due to its stable SP2Structure, shows very poor wetability at the same time, carbon nanotubes 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 carbon nanotubes in Metal Forming Process how is reduced, and improve itself and the wetability of matrix to become
The key of the excellent carbon nano-tube reinforced metal-matrix composite material of processability.
Carbon nanotubes, which improves wetability method, at present overlay coating etc., and such as chemical nickel plating, this method mainly will complete base
The carbon nanotubes 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 carbon nanotubes is added, acid group metallic compound is added and is kept stirring state until generation colloidal sol, sky is exposed to by this colloid
Aging in gas, after a few days dries product grind into powder, is heat-treated in last certain temperature inert gas flow and obtains 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 number CN101966449A：" for a kind of system of multiwall carbon nanotube-supported titanium dioxide catalyst
In Preparation Method ".Solvent heat and hydro-thermal method are combined, adsorb colloid in a solvent, it is dry in carbon nano tube surface, hydro-thermal point
Its colloid is solved, obtains oxidation applicator.Right this method step is complicated, time length, and cannot coat simple substance in carbon nanotubes table
Face, has certain limitation.
On the other hand, the control to carbon nanotubes dispersiveness is usually embodied in made of metal for during.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 carbon nanotubes.But these types side
The defects of method is also it is clear that for carbon nanotubes as the flowing of melt is reunited seriously, enhancing distributed mutually is uneven under casting condition
Even, powder metallurgy is popular research direction, but interface cohesion and fine and close sex chromosome mosaicism fail effectively to be solved.In-situ synthesis
There are the short slab such as technique is excessively complicated and process is difficult to control.
In publication number CN103614672A, entitled " preparation method of carbon nanotube enhanced aluminium-based composite material ", adopt
Carbon nano tube enhanced aluminium base is prepared for the conventional powder metallurgical method such as batch mixing, drying, ball milling, cold pressing, sintering and extruding to answer
The problems such as condensation material, right interfacial bonding property is poor, material compactness in itself is more prominent.
In publication number CN103911566A, a kind of entitled " powder metallurgy of carbon nano tube reinforced aluminum alloy composite material
It is more uniform by carbon nanotubes using powder metallurgy process processing flake aluminum in preparation method ", but conventional powder metallurgical side
The defects of the defects of method does not melt such as, and compactness is not good enough does not solve.
In publication number CN101376932, entitled " carbon nanotubes enhancing magnesium, aluminum matrix composite and preparation method thereof "
In, reho-forming method is mixed after being heated using powder and prepares carbon nanotubes enhancing aluminium, magnesium-based composite material.Though densification can be improved
Sex chromosome mosaicism, but carbon nanotubes is easily reunited under rheological condition, and the performance raising to composite material is unfavorable.
Therefore, still lack a kind of cost-effective carbon nanotube enhanced aluminium-based composite material at present to prepare and shaping skill
Art.
It is a kind of new the invention is intended to provide in order to overcome traditional carbon nano tube compound material to be prepared into the technological difficulties of type
Carbon nanotubes/alumina-base material semi-solid blank prepares forming technique.Semi-solid forming technology comes across in the 1970s, the work
Skill achieves develop rapidly in the past 40 years, application range constantly expands as a kind of efficient, energy saving modern metallurgical technology.It
There are several obvious advantages relative to the forming technology such as conventional cast and forging：Gross segregation and the cavity of finished product are reduced, it is smaller
Forming pressure, and relatively low mold temperature etc..Just because of there are the technology a series of particular advantages to be looked steadily by common people
Mesh, will also become this century most potential material forming techniques.
Semi-solid forming technology includes the preparation of semi-solid blank, the reheating of blank and the crucial ring of thixotropic forming 3
Prepared by section, 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 simple substance copper clad multi-walled carbon nanotube/aluminum matrix composite semi-solid blank
Preparation method.
The present invention is achieved by the following technical solutions.
A kind of preparation side of simple substance copper clad multi-walled carbon nanotube/aluminum matrix composite semi-solid blank of the present invention
Method, comprises the following steps.
（1）By multi-walled carbon nanotube in the pure salpeter solution pre-dispersed 6 ~ 8h of ultrasound, temperature is 60 ~ 80 DEG C, is cooled to room temperature
Afterwards, cleaned with deionized water, centrifuge to neutrality, then dried in vacuum drying chamber, it is spare.
（2）By copper nitrate and through step（1）The multi-walled carbon nanotube of pretreatment is added in ethanol solution, and ultrasound 40~
60min, obtains carbon nanotube suspension, wherein multi-walled carbon nanotube and copper nitrate molar ratio 1:0.4~1:1.
（3）Through step（2）Multi-walled carbon nanotube suspension import hydrothermal reaction kettle in, wherein suspension volume accounts for
The molten product 25%~50% of reaction kettle.Place into reacting furnace and heat, 180~200 DEG C are warming up to 1~5 DEG C/s, keep the temperature 1~2h, then
After being warming up to 300 DEG C with 1~5 DEG C/s, 8~12h is kept the temperature；Take out, reaction kettle sealing is air-cooled, is dried, obtained prefabricated with vacuum drying oven
Material.
（4）Through step（3）Gained mixing material is put into vacuum tube furnace, 300 ~ 500 DEG C of height after being put into corundum crucible
When temperature roasting 3 is small, many walls nanotube material of simple substance copper clad is obtained.
（5）Step（4）The many walls nanotube material of obtained simple substance copper clad is mixed with Al alloy powder, is put into ball milling earthenware
Crucible carries out ball milling, and time control accounts for Al alloy powder in 30 ~ 60min, many walls nanotube quality of materials of wherein simple substance copper clad
2% ~ 4%, which is passed through argon gas and is protected.
（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, it is transferred to and continues to heat with 1 ~ 3 DEG C/min in ultrasonic magnetic agitation stove 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 corresponding mould cooling, obtains simple substance copper clad multi-wall carbon nano-tube
Pipe/aluminum matrix composite semi-solid blank.
Step of the present invention（3）The hydrothermal reaction kettle liner is polytetrafluoroethylene (PTFE).
In the present invention, acted synergistically using ultrasound and magnetic stirring equipment, it is mixed under concussion stirring semi-molten state
Powder is closed, can not only promote disperseing for CNT, while the reunion of CNT, agglomerating and rising phenomenon can be reduced.
The present invention concrete principle be：
2Cu(NO3)2=2CuO+4NO2+O2（1）
CH3CH2OH + CuO = CH3CHO + Cu + H2O （2）
Copper nitrate decomposes under high temperature, recycles the further reduction treatment of catalytic activity of cupric oxide, obtains copper simple substance cladding
Carbon nano-tube material.Pretreated carbon nanotubes is mixed with alloyed powder, and stirring at low speed, control are carried out in semi-solid temperature section
Solid rate simultaneously keeps the temperature special time length, obtains required semi-solid blank.
The present invention has following uniqueness：（1）It the method reduce the rising phenomenon of CNT in common process.（2）Utilize this
The further catalysis of oxide that body copper nitrate decomposes in a heated condition is reduced into elemental copper and is deposited directly on whisker.（3）
This method reaction temperature is relatively low, and danger coefficient is low.（4）Multi-walled carbon nanotube is combined under the conditions of aluminium alloy semi-solid with matrix,
While with more preferable interface, the reunion probability of carbon nanotubes under founding state is further reduced.
Brief description of the drawings
Attached drawing 1 is the semi-solid blank microscopic structure prepared in embodiment 1.
Embodiment
The present invention will be described further by following embodiments.
Embodiment 1.
By multi-walled carbon nanotube 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, is then dried for standby in vacuum drying chamber.Copper nitrate and the multi-walled carbon nanotube of above-mentioned drying are made
For raw material, ultrasound 40min in straight alcohol is added；Wherein multi-walled carbon nanotube, copper nitrate and ethanol molar ratio are 1:0.4:127,
Obtain multi-walled carbon nanotube suspension；The suspension is imported in hydrothermal reaction kettle, wherein suspension volume accounts for the molten product of reaction kettle
25%.Place into reacting furnace and heat, be warming up to 200 DEG C with 3 DEG C/min, keep the temperature 2h, then after being warming up to 300 DEG C with 3 DEG C/min,
Keep the temperature 8h；Sealing be cooled to room temperature after filter low temperature drying after be put into corundum crucible with 500 DEG C of high-temperature roastings 3 it is small when, obtain
The many walls nanotube material of simple substance copper clad, the process need to be protected with vacuum tube furnace.
Many walls nanotube material and corresponding mass by mass fraction for 2% simple substance copper clad 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 ultrasonic magnetic agitation stove with 1 DEG C/
Min continues to heat and controls that its solid rate opens ultrasonic device after 20% scope and ultrasonic disperse is simultaneously under electromagnetic equipment collaboration
Mixing time is controlled in 3min, ultrasonic power 1.0Kw, is subsequently poured into corresponding mould and is cooled to room temperature, obtains simple substance copper clad
The aluminium-based semisolid-state blank of many walls nanotube material/7075.
Embodiment 2.
By multi-walled carbon nanotube 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, is then dried for standby in vacuum drying chamber.Copper nitrate and the multi-walled carbon nanotube of above-mentioned drying are made
For raw material, ultrasound 50min in straight alcohol is added；Wherein carbon nanotubes, copper nitrate and ethanol molar ratio are 1:0.6:127, obtain
Multi-walled carbon nanotube suspension；The suspension is imported in hydrothermal reaction kettle, wherein suspension volume accounts for the molten product 25% of reaction kettle.
Place into reacting furnace and heat, be warming up to 200 DEG C with 5 DEG C/min, keep the temperature 1h, then after being warming up to 300 DEG C with 3 DEG C/min, insulation
8h；Sealing be cooled to room temperature after filter low temperature drying after be put into corundum crucible with 400 DEG C of high-temperature roastings 3 it is small when, obtain simple substance
The many walls nanotube material of copper clad, the process need to be protected with vacuum tube furnace.
Many walls nanotube material and 6061 Al alloy powders by mass fraction for 3% simple substance copper clad of Al alloy powder
End is put into ball milling crucible and carries out ball milling, and whole argon gas protection, time control is in 30min.Afterwards by mixed-powder pour into crucible and with
10 DEG C/min heating rates are 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 rate
Ultrasonic device is opened after 30% scope and simultaneously mixing time is controlled in 2min, ultrasonic work(to ultrasonic disperse under electromagnetic equipment collaboration
Rate 1.5Kw, is subsequently poured into corresponding mould and is cooled to room temperature, and obtains the aluminium base half of many walls nanotube material of simple substance copper clad/6061
Solid blank.
Embodiment 3.
By multi-walled carbon nanotube 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, is then dried for standby in vacuum drying chamber.Copper nitrate and the multi-walled carbon nanotube of above-mentioned drying are made
For raw material, ultrasound 60min in straight alcohol is added；Wherein multi-walled carbon nanotube, copper nitrate and ethanol molar ratio are 1:0.8:127,
Obtain multi-walled carbon nanotube suspension；The suspension is imported in hydrothermal reaction kettle, wherein suspension volume accounts for the molten product of reaction kettle
25%.Place into reacting furnace and heat, be warming up to 200 DEG C with 3 DEG C/min, keep the temperature 1h, then after being warming up to 300 DEG C with 3 DEG C/min,
Keep the temperature 10h；Sealing be cooled to room temperature after filter low temperature drying after be put into corundum crucible with 500 DEG C of high-temperature roastings 3 it is small when, obtain
The many walls nanotube material of simple substance copper clad, the process need to be protected with vacuum tube furnace.
Many walls nanotube material and 2024 Al alloy powders by mass fraction for 4% simple substance copper clad of Al alloy powder
End imports ball milling crucible and carries out ball milling, and whole argon gas protection, time control is in 30min.Gained mixed powder imports corresponding crucible
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 its solid phase
Ultrasonic device is opened after 40% scope for rate and simultaneously mixing time is controlled in 1min to ultrasonic disperse under electromagnetic equipment collaboration, ultrasound
Power 2.0Kw, is subsequently poured into corresponding mould and is cooled to room temperature, and obtains the aluminium base of many walls nanotube material of simple substance copper clad/2024
Semi-solid blank.
Claims (2)
- A kind of 1. preparation method of simple substance copper clad multi-walled carbon nanotube/aluminum matrix composite semi-solid blank, it is characterized in that bag Include following steps：（1）By multi-walled carbon nanotube 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, spare；（2）By copper nitrate and through step（1）The multi-walled carbon nanotube of pretreatment is added in ethanol solution, and ultrasound 40~ 60min, obtains multi-walled carbon nanotube suspension, wherein multi-walled carbon nanotube and copper nitrate molar ratio 1:0.4~1:1；（3）Through step（2）Multi-walled carbon nanotube suspension import hydrothermal reaction kettle in, wherein suspension volume accounts for reaction Kettle volume 25%~50%；Place into reacting furnace and heat, be warming up to 180~200 DEG C with 1~5 DEG C/s, keep the temperature 1~2h, then with 1 After~5 DEG C/s is warming up to 300 DEG C, 8~12h is kept the temperature；Take out, reaction kettle sealing is air-cooled, filters low temperature drying, obtains pre- saw lumber Material；（4）Through step（3）Gained preformed material is put into vacuum tube furnace, 300 ~ 500 DEG C of high temperature roastings after being put into corundum crucible Burn 3 it is small when, obtain many walls nanotube material of simple substance copper clad；（5）Step（4）The many walls nanotube material of obtained simple substance copper clad is mixed with Al alloy powder, be put into ball milling crucible into Row ball milling, time control in 30 ~ 60min, many walls nanotube quality of materials of wherein simple substance copper clad account for Al alloy powder 2% ~ 4%, which is passed through argon gas and is 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 and continues to heat with 1 ~ 3 DEG C/min in ultrasonic magnetic agitation stove and control its solid rate in 20 ~ 40% Scope, ultrasound is ultrasound indirectly, and Power Control is simultaneously passed through argon gas protection, surpasses in 1.0 ~ 2.0kW, frequency 20KHz, stirring at low speed Sound magnetic agitation time control is in 1 ~ 3min；（7）Step（6）Gained semi solid slurry pours into corresponding mould cooling, obtains simple substance copper clad multi-walled carbon nanotube/aluminium Base composite material semi-solid state blank.
- 2. preparation method according to claim 1, it is characterized in that step（3）The hydrothermal reaction kettle liner is polytetrafluoro Ethene.
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| CN109207781A (en) * | 2018-09-17 | 2019-01-15 | 南昌大学 | A kind of pressing method improving 7075 aluminium alloys |
| 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 |
| US10941464B1 (en) | 2020-06-30 | 2021-03-09 | The Florida International University Board Of Trustees | Metal nanoparticle composites and manufacturing methods thereof by ultrasonic casting |
| CN113444906B (en) * | 2021-06-10 | 2023-06-16 | 湘潭大学 | Method for preparing carbon nano tube reinforced light aluminum-based alloy |
| CN113373341A (en) * | 2021-06-18 | 2021-09-10 | 苏州第一元素纳米技术有限公司 | Manufacturing process of carbon nano tube reinforced aluminum electric power fitting |
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