CN106399873B - A kind of preparation method of coating alumina whisker nanotube enhancing magnesium-based composite material - Google Patents
A kind of preparation method of coating alumina whisker nanotube enhancing magnesium-based composite material Download PDFInfo
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Abstract
A kind of preparation method of coating alumina whisker nanotube enhancing magnesium-based composite material; first prepare coating alumina whisker nanotube; then magnesium alloy powder is imported in coating alumina whisker nano-tube material suspension and obtains batch mixing; 60~80 DEG C of vacuum dryings; ball milling crucible, the lower ball milling of argon gas protection are imported again；50~100MPa is pressed into prefabricated section；It is put into mould, with 7~10 DEG C/min heating rates mould to 10~20 DEG C of subsolidus, then continues to heat with 3~5 DEG C/min again and control its solid rate to obtain coating alumina whisker nanotube enhancing magnesium-based composite material in 70~90% scopes.The present invention has the advantages that simple, safety, low cost are easily operated and controllable.
Description
Technical field
The invention belongs to material to prepare shaping technical field.
Background technology
Magnesium-based composite material has light as a kind of metallic based structures material, and specific strength and specific stiffness are high, good lead
Conductance hot property and damping capacity, the features such as casting character is excellent, it is set to have bigger in metal-base composites
Potential application foreground.But magnesium alloy, equally there is also elasticity modulus is small, intensity is not high, thermal coefficient of expansion is high, size under high temperature
The shortcomings of stability is poor and wears no resistance so that magnesium alloy has larger limitation as structural material.It is difficult to meet high
Strength structure materials demand.
In recent years, using fiber or particle to magnesium alloy enhancing for composite, the magnesium-based composite material 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 as a kind of tube with a large amount of special excellent properties, such as high intensity, high resiliency, high-ratio surface
Long-pending, heat-resisting, corrosion-resistant, heat conduction and electric conductivity etc., imply carbon nanotubes has huge application in metal material enhancing research
Prospect.The modulus of carbon nanotubes is identical with diamond, and theoretical strength has reached 106Megapascal, is 100 times of steel, and density is only
For the 1/6 of steel, while it has both extremely excellent toughness and structural stability again, is the preferable choosing as composite material enhancing phase
Select.Right carbon pipe is due to its stable SP2Structure, shows very poor wetability at the same time, carbon nanotubes is easily rolled into a ball in fusion-casting process
Poly- and wrapping phenomena causes not strong with metallic matrix interfacial bonding property, is unfavorable for the enhancing of composite property.Therefore, how to subtract
Few agglomeration of the carbon nanotubes in Metal Forming Process, and improve the wetability of itself and matrix to become processability excellent
The key of carbon nano-tube reinforced metal-matrix composite material.
For crystal whisker-shaped carbon nanotube as a kind of new structure carbon nanotubes, 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, outer diameter 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 carbon nanotubes to a certain extent, be carbon nanotubes
Industrialization with providing greatly possibility.
Aluminium oxide because its with good refractory performance while, point can be formed in nano alumina particles surface at high temperature
Spar or magnesia, will substantially improve its wetability, can be as the intermediate material for improving wetability.
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 CNT surface, hydrothermal decomposition its
Colloid, obtains oxidation applicator.To achieve the purpose that to optimize wetability by being modified CNT surface, right this method step is answered
It is miscellaneous, time length, and simple substance cannot be coated in CNT surface, there is 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 carbon nano-tube reinforced metal-matrix composite material.But this is several
The defects of kind method is also it is clear that for CNT as the flowing of melt is reunited seriously, enhancing distributed mutually is uneven under casting condition
It is even.Powder metallurgy fails effectively to be solved as popular research direction, interface cohesion and fine and close sex chromosome mosaicism.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 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 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 CNT easily reunites under rheological condition, and the performance raising to composite material is unfavorable.
In publication number CN101376170, entitled " manufacturing equipment of magnesium base-carbon nano tube compound material and its manufacturer
In method ", first carry out magnesium and strengthen the powder mixing of phase particle, heating, recycles a kind of injection device to import the mixture
Extrusion die.Though this method is using thixotroping shaping as innovation, but under this method, to reach mobility effect, magnesium alloy powder melts
Change degree is higher, can still produce and cast similar enhancing phase agglomeration traits so that the carbon produced in powder mixed process is received
Mitron dispersion effect weakens.The present invention mainly has following difference with this method：（1）In this method, magnesium alloy powder is hanged by methanol
Floating carbon nanotubes and ball-milling treatment uniformly mix carbon nanotubes；（2）In this method, the high solid fraction of mixed-powder is controlled, no
Rheological characteristic can be produced, avoids the carbon nanotubes under molten condition from reuniting.
The shaping of traditional semisolid die forging experienced half admittedly the preparation of blank, reheat and three procedures of die-forging forming.
Shaped relative to traditional semisolid die forging, short route semisolid contour forming has following features：（1）Obtaining semi solid slurry
Afterwards, can the once-forming and complex-shaped workpiece of acquisition.（2）Semi-solid-state shaping belongs to near-net forming, easily reaches shape and sets
Meter requires.（3）Semi solid slurry blank has preferable thixotropy, and at low shear rates, slurry behaves like solid-state, without bright
Aobvious mobility, enhancing are mutually not easy to reunite.（4）The viscosity of semi solid slurry blank is high compared to liquid metal and is relatively easy to control,
In whole cavity filling process, it is more steady that semisolid fills type.
Short route semisolid contour forming is the combination of Semi-Solid Thixoforming and contour forging technique.Its microstructure of semisolid, which includes, uniformly divides
In the spheric grain of remaining liquid phase, and there is high solid fraction.The shaping of traditional semisolid die forging experienced half preparation of blank, again admittedly
New heating and three procedures of die-forging forming.Shaped relative to traditional semisolid die forging, this short route high solid fraction half is solid
State die-forging forming, it is not necessary to prepare blank and reheat step, can once-forming and acquisition after semi solid slurry is obtained
Complex-shaped workpiece.Forming period is significantly shortened while the advantages of semisolid die forging shapes is ensured.
The content of the invention
The purpose of the present invention is to propose to a kind of preparation method of coating alumina whisker nanotube enhancing magnesium-based composite material.
The present invention is achieved by the following scheme.
A kind of preparation method of coating alumina whisker Carbon Nanotubes/Magnesiuum Matrix Composite of the present invention, including
Following steps：
（1）Whisker carbon nanotubes is put into the pre-dispersed 6 ~ 8h of ultrasound in pure salpeter solution, temperature is 60 ~ 80 DEG C, is cooled to
After room temperature, cleaned with deionized water, centrifuge to neutrality, then dried in vacuum drying chamber, it is spare.
（2）By aluminum nitrate and through step（1）The whisker carbon nanotubes of pretreatment is added in methanol solution, and ultrasound 40~
60min, obtains whisker carbon nanotube suspension, wherein whisker carbon nanotubes and nitric acid al mole ratio 1:0.4~1:1；
（3）Through step（2）Whisker carbon nanotube suspension import hydrothermal reaction kettle in, wherein suspension volume accounts for instead
Answer the molten product 25%~40% of kettle.Place into reacting furnace and heat, 100~120 DEG C are warming up to 1~5 DEG C/min, keep the temperature 1~2h, then
After being warming up to 150 DEG C with 1~3 DEG C/min, 8~12h is kept the temperature；Low temperature drying is filtered after being cooled to room temperature with 5 ~ 10 DEG C/min.
（4）Through step（3）Gained mixing material be put into corundum crucible with 400 ~ 700 DEG C of high-temperature roastings 1 ~ 5 it is small when, obtain
To the whisker carbon nano-tube material of coating alumina, the process whole process vacuum protection.
（5）The whisker carbon nano-tube material of coating alumina is put into low power ultrasonic vibration≤30min in methanol, is applied
Cover the whisker carbon nanotube suspension of aluminium oxide.
（6）Magnesium alloy powder is added to step（5）Stirred in gained suspension, obtain mixing batch mixing, and it is true at 60 ~ 80 DEG C
Sky drying, the whisker carbon nanotubes of wherein coating alumina account for the 2% ~ 8% of magnesium alloy silty amount.
（7）Step（6）Obtained batch mixing adds ball milling crucible and carries out ball milling, and whole process is passed through argon gas in the mechanical milling process
Protected.
（8）Step（7）Gained mixed-powder is put into 50 ~ 100MPa in mould and is pressed into prefabricated section.
（9）Step（8）Gained prefabricated section is put into corresponding mold groove, with 7 ~ 10 DEG C/min heating rate's moulds
Tool is to 10 ~ 30 DEG C of subsolidus.Continue to heat with 3 ~ 5 DEG C/min and control its solid rate in 70 ~ 90% scopes.
（10）Step（9）Gained moulding mixture carries out die-forging forming, pressure head control in 40 ~ 100mm/s speed, pressurize 15 ~
5min postcoolings to room temperature obtains the whisker Carbon Nanotubes/Magnesiuum Matrix Composite drip molding of coating alumina.
The present invention has following uniqueness：（1）Solution uses methanol, itself has larger volatility, and pressure bigger is right
The surface tension for reducing solution is beneficial.（2）This method is easy and effective to be suitable for batch production.（3）This method is not required to expensive instrument,
Reaction temperature is relatively low, and danger coefficient is low.（4）Carbon nanotubes is combined under the conditions of magnesium alloy semi solid state with matrix, is had more preferable
Interface at the same time, avoids the reunion of carbon nanotubes under the conditions of founding.
Brief description of the drawings
Composite material microscopic structure of the attached drawing 1 prepared by embodiment 1.
Embodiment
The present invention will be described further by following embodiments.
Embodiment 1.
By whisker carbon nanotubes, the pre-dispersed 8h of ultrasound, temperature are 60 DEG C in pure salpeter solution, after being cooled to room temperature, are spent
Ionized water cleaning, centrifuge to neutrality, is then dried for standby in vacuum drying chamber.With aluminum nitrate and the whisker carbon nanometer of above-mentioned drying
Pipe adds ultrasound 40min in methanol solution as raw material；Wherein whisker carbon nanotubes, 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 instead
Answer the molten product 25% of kettle.Place into reacting furnace and heat, be warming up to 100 DEG C with 5 DEG C/min, keep the temperature 1h, then be warming up to 3 DEG C/min
After 150 DEG C, 8h is kept the temperature；Low temperature drying is filtered after being cooled to room temperature with 5 DEG C/min to be put into corundum crucible with 500 DEG C of high-temperature roastings
3 it is small when, whole vacuum protection, obtains the whisker carbon nano-tube material of coating alumina.
Mass percent is put into low power in methanol for the whisker carbon nanotubes of 2% coating alumina of magnesium alloy powder to surpass
Acoustic shock swings to obtain the whisker carbon nanotube suspension of coating alumina, time control 20min.The AZ61 powder of corresponding mass is put
Enter suspension and obtain mixing batch mixing and in 100 DEG C of vacuum dryings.Gained mixed-powder is put into 50MPa in mould and is pressed into
Block, gained prefabricated section are put into corresponding mold groove, heated with the 10 DEG C/min heating rates mould to 500 DEG C
Argon gas protection is passed through in journey.Continue to heat with 3 DEG C/min and control its solid rate in 90% or so it is rear carry out die-forging forming processing,
With 40mm/s pressure head speed, the dwell time is 5min postcoolings to room temperature, obtains whisker carbon nanotubes/AZ61 of coating alumina
Magnesium-based composite material drip molding.
Embodiment 2.
By whisker carbon nanotubes 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.With aluminum nitrate and the whisker carbon nanotubes of above-mentioned drying
As raw material, ultrasound 30min in methanol solution is added；Wherein whisker carbon nanotubes, 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 reaction kettle
Molten product 30%.Place into reacting furnace and heat, be warming up to 120 DEG C with 3 DEG C/min, keep the temperature 1h, then 150 DEG C are warming up to 1 DEG C/min
Afterwards, 10h is kept the temperature；It is put into after filtering low temperature drying after being cooled to room temperature with 7 DEG C/min in corundum crucible with 600 DEG C of high-temperature roastings 2
Hour, whole process imports argon gas protection, obtains the whisker carbon nano-tube material of coating alumina.
Mass percent is put into low power in methanol for the whisker carbon nanotubes of 3% coating alumina of Al alloy powder to surpass
Acoustic shock swings to obtain the whisker carbon nanotube suspension of coating alumina, time control 20min.By the AZ91D magnesium of corresponding mass
Alloyed powder imports suspension and obtains mixing batch mixing and in 100 DEG C of vacuum dryings.It is cold that gained mixed-powder is put into 100MPa in mould
Briquet is pressed, gained prefabricated section is put into corresponding mold groove, with 10 DEG C/min heating rates mould to 450
DEG C, argon gas or vacuum protection in heating process.Continue to heat with 5 DEG C/min and control its solid rate in 80% or so rear carry out mould
Forging molding processing, with 70mm/s pressure head speed, the dwell time is 5min postcoolings to room temperature, obtains the whisker carbon of coating alumina
Nanotube/AZ61D magnesium-based composite material drip moldings.
Embodiment 3.
By whisker carbon nanotubes 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.With aluminum nitrate and the whisker carbon nanotubes of above-mentioned drying
As raw material, ultrasound 60min in methanol solution is added；Wherein whisker carbon nanotubes, aluminum nitrate and methanol molar ratio are 1:1:
182, obtain the whisker carbon nanotube suspension of coating alumina；The suspension is imported in hydrothermal reaction kettle, wherein suspension
Volume accounts for the molten product 40% of reaction kettle.Place into reacting furnace and heat, 120 DEG C are warming up to 3 DEG C/min, keep the temperature 1h, then with 1 DEG C/
After min is warming up to 150 DEG C, 12h is kept the temperature；After being cooled to room temperature with 10 DEG C/min filter low temperature drying after be put into corundum crucible with
When 700 DEG C of high-temperature roastings 1 are small, whole process imports argon gas protection, obtains the whisker carbon nano-tube material of coating alumina.
Mass percent is put into low power in methanol for the whisker carbon nanotubes of 2% coating alumina of magnesium alloy powder to surpass
Acoustic shock swings to obtain the whisker carbon nanotube suspension of coating alumina, time control 20min.The AZ31 magnesium of corresponding mass is closed
Bronze imports suspension and obtains mixing batch mixing and in 100 DEG C of vacuum dryings.Gained mixed-powder is put into 150MPa in mould and is cold-pressed
Briquet, gained prefabricated section are put into corresponding mold groove, with the 10 DEG C/min heating rates mould to 530 DEG C,
Argon gas or vacuum protection in heating process.Continue to heat with 5 DEG C/min and control its solid rate in 70% or so it is rear carry out die forging into
Type processing, with 100mm/s pressure head speed, the dwell time is 10min postcoolings to room temperature, and the whisker carbon for obtaining coating alumina is received
Mitron/AZ31 magnesium-based composite material drip moldings.
Claims (1)
- A kind of 1. preparation method of coating alumina whisker Carbon Nanotubes/Magnesiuum Matrix Composite, it is characterized in that including following several A step：（1）Whisker carbon nanotubes is put into the pre-dispersed 6 ~ 8h of ultrasound in pure salpeter solution, 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 aluminum nitrate and through step（1）The whisker carbon nanotubes of pretreatment is added in methanol solution, 40~60min of ultrasound, Obtain whisker carbon nanotube suspension, wherein whisker carbon nanotubes and nitric acid al mole ratio 1:0.4~1:1；（3）Through step（2）Whisker carbon nanotube suspension import hydrothermal reaction kettle in, wherein suspension volume accounts for reaction kettle Volume 25%~40%；Place into reacting furnace and heat, be warming up to 100~120 DEG C with 1~5 DEG C/min, keep the temperature 1~2h, then with 1 After~3 DEG C/min is warming up to 150 DEG C, 8~12h is kept the temperature；Low temperature drying is filtered after being cooled to room temperature with 5 ~ 10 DEG C/min；（4）Through step（3）Gained mixing material be put into corundum crucible with 400 ~ 700 DEG C of high-temperature roastings 1 ~ 5 it is small when, applied The whisker carbon nano-tube material of aluminium oxide is covered, the process whole process vacuum protection；（5）The whisker carbon nano-tube material of coating alumina is put into low power ultrasonic vibration≤30min in methanol, obtains coating oxygen Change the whisker carbon nanotube suspension of aluminium；（6）Magnesium alloy powder is added to step（5）Stirred in gained suspension, obtain mixing batch mixing, and dry in 60 ~ 80 DEG C of vacuum Dry, the whisker carbon nanotubes of wherein coating alumina accounts for the 2% ~ 8% of magnesium alloy silty amount；（7）Step（6）Obtained batch mixing adds ball milling crucible and carries out ball milling, and whole process is passed through argon gas progress in the mechanical milling process Protection；（8）Step（7）Gained mixed-powder is put into 50 ~ 100MPa in mould and is pressed into prefabricated section；（9）Step（8）Gained prefabricated section is put into corresponding mold groove, with 7 ~ 10 DEG C/min heating rates mould extremely 10 ~ 30 DEG C of subsolidus；Continue to heat with 3 ~ 5 DEG C/min and control its solid rate in 70 ~ 90% scopes；（10）Step（9）Gained moulding mixture carries out die-forging forming, and pressure head is controlled after 40 ~ 100mm/s speed, 15 ~ 5min of pressurize It is cooled to room temperature to obtain the whisker Carbon Nanotubes/Magnesiuum Matrix Composite drip molding of coating alumina.
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