CN104611648B - Method for reinforcing magnesium matrix composite through carbon nanotubes coated with magnesium oxide - Google Patents
Method for reinforcing magnesium matrix composite through carbon nanotubes coated with magnesium oxide Download PDFInfo
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Abstract
The invention provides a method for reinforcing a magnesium matrix composite through carbon nanotubes coated with magnesium oxide. 1-5 g of carbon nanotubes chemically coated with magnesium oxide and larger than or equal to 250ml of an acetone solution are mixed and then subjected to ultrasonic dispersion for 1-4 h to obtain uniformly dispersed carbon nanotube and acetone mixed liquor; AZ91 magnesium alloy powder with mass larger than or equal to 95 g and grain size smaller than or equal to 325 meshes is added to the mixed liquor, and then the mixed liquor is stirred mechanically under ultrasonic waves for 1-4 h to obtain mixed slurry; the mixed slurry is subjected to filtration and vacuum drying, then transferred into a die, and subjected to cold pressing under the pressure of 100-600 MPa at a room temperature; a composite after cold pressing is sintered for 2-4 h under the protection of argon at the temperature of 500-600 DEG C; the sintered composite is subjected to hot extrusion at the temperature of 350-400 DEG C. The method is low in process cost, safe, reliable and easy to operate; the carbon nanotubes coated with magnesium oxide are uniformly distributed in magnesium alloy and have high bonding strength with interfaces of matrixes, the grain refinement effect is remarkable, the composite has excellent performance and the method is suitable for industrially preparing the high-performance magnesium alloy composite reinforced by the carbon nanotubes.
Description
Technical field
The invention belongs to field of metal preparation, particularly to the preparation method of magnesium base composite material.
Background technology
In recent years, with the fast development of the high-technology fields such as Aero-Space, machinery, automobile and electron trade, to magnesium
The demand of based composites sharply increases.Magnesium base composite material has specific strength, specific stiffness height, high-wearing feature, high vibration damping
The advantages of property, receive unprecedented attention.And CNT (carbon nanotubes, cnts) found from 1991
Since, due to its superior comprehensive mechanical property (elastic modelling quantity is about 100 times of steel in more than 1tpa, intensity), studied
Persons expect this excellent enhancing is mutually introduced in magnesium alloy substrate it is intended to obtain high-performance magnesium base composite material first.So
And, up to the present strengthen the not breakthrough progress of composite material of magnesium alloy research, its key problem master with regard to cnts
Concentrate on following 3 aspects: one is how to take suitable method that CNT is evenly dispersed in matrix, and and base
Body combines well；Two is how to solve that carbon nano tube surface activity is low, a difficult problem poor with magnesium alloy wettability；How three be
CNT is made to keep complete structure in high-temperature sintering process.Nanoscale magnesium (magnesium oxide, mgo) and magnesium
There are good Lattice Orientation Relations, can be used as the heterogeneous equiax crystal of magnesium matrix.If coating one layer in carbon nano tube surface
Uniform magnesium oxide, then can be effectively improved dispersibility in magnesium matrix for the CNT, refinement magnesium matrix tissue, and can improve
CNT and the interface bond strength of magnesium matrix.
Content of the invention
The purpose of the present invention is to overcome the deficiencies in the prior art, provides one kind coated magnesium oxide CNT to strengthen magnesio
The method of composite.
The present invention is achieved by the following technical solutions.
Preparation method of the present invention comprises the following steps.
(1) ultrasonic disperse after the CNT after 1-5g chemistry coated magnesium oxide being mixed with the acetone soln of >=250 ml
1-4h obtains homodisperse CNT acetone mixture.
(2) by quality >=95g, the az91 magnesium alloy powder of granularity≤325 mesh is added in step (1) gained mixed liquor,
Obtain after carrying out ultrasonic+mechanical agitation 1-4h simultaneously and disperse more uniform mixed serum.
(3) step (2) gained mixed serum is carried out filtering, be vacuum dried after be transferred in mould, carry out cold at room temperature
Pressure, pressure is 100-600mpa.
(4) composite after step (3) gained being colded pressing argon protection under, sinter 2-4h, sintering temperature be 500～
600℃.
(5) finally the composite after step (4) sintering is carried out hot extrusion at a temperature of 350～400 DEG C.
Present invention process low cost, safe and reliable, simple to operate, coated magnesium oxide CNT is distributed all in the magnesium alloy
Even and high with basal body interface bond strength, substantially, composite property is excellent for its grain refining effect, is suitable to preparation of industrialization high
Performance CNT strengthens composite material of magnesium alloy.
Brief description
The chemical coated magnesium oxide CNT (mgo-cnts) that Fig. 1 is prepared for the present invention is in az91 magnesium alloy powder
Distribution situation.
The az91 alloy that Fig. 2 is prepared for the present invention and az91/3.0wt.%mgo-cnts composite microscopic structure.Wherein,
A is az91 alloy microscopic structure, and b is az91/3.0wt.%mgo-cnts composite microscopic structure.
The az91/3.0wt.%mgo-cnts composite fracture apperance situation that Fig. 3 is prepared for the present invention.
Fig. 4 is the EDAX results of the corresponding a regional location of fracture apperance shown in Fig. 3.
Specific embodiment
The present invention will be described further by following examples.
Embodiment 1.
First stirring 30min after the CNT after 1g chemistry coated magnesium oxide and the mixing of 300ml acetone soln is surpassed again
Sound dispersion 2h obtains homodisperse CNT acetone mixture；Again the az91 magnesium alloy powder that 99g granularity is 325 mesh is added
Obtain after entering ultrasonic mechanical agitation 2h simultaneously in mixed liquor and disperse more uniform mixed serum, shift after filtering and being vacuum dried
To mould, colded pressing at room temperature, pressure is 100mpa；By the composite after colding pressing under argon protection, sinter 2h,
Sintering temperature is 600 DEG C；Finally the composite after sintering is carried out hot extrusion at a temperature of 380 DEG C and az91/1.0wt.% is obtained
Mgo-cnts composite.Mechanics Performance Testing is carried out to az91/1.0wt.%mgo-cnts composite, its tensile strength
Reach 220-240mpa, elongation percentage reaches 11.2-12.5%, hardness is 75.9-80.6hv, is a kind of composite wood of excellent in mechanical performance
Material.
Embodiment 2.
First stirring 30min after the CNT after 3g chemistry coated magnesium oxide and the mixing of 500ml acetone soln is surpassed again
Sound dispersion 2h obtains homodisperse CNT acetone mixture；Again the az91 magnesium alloy powder that 97g granularity is 325 mesh is added
Obtain after entering ultrasonic mechanical agitation 2h simultaneously in mixed liquor and disperse more uniform mixed serum, shift after filtering and being vacuum dried
To mould, colded pressing at room temperature, pressure is 100mpa；By the composite after colding pressing under argon protection, sinter 2h,
Sintering temperature is 600 DEG C；Finally the composite after sintering is carried out hot extrusion at a temperature of 380 DEG C and az91/3.0wt.% is obtained
Mgo-cnts composite.Mechanics Performance Testing is carried out to az91/3.0wt.%mgo-cnts composite, its tensile strength
Reach 300-345mpa, elongation percentage reaches 11-12.7%, hardness is 81-96hv, is a kind of composite of good mechanical properties.
Embodiment 3.
First stirring 30min after the CNT after 5g chemistry coated magnesium oxide and the mixing of 600ml acetone soln is surpassed again
Sound dispersion 2h obtains homodisperse CNT acetone mixture；Again the az91 magnesium alloy powder that 95g granularity is 325 mesh is added
Obtain after entering ultrasonic mechanical agitation 2h simultaneously in mixed liquor and disperse more uniform mixed serum, shift after filtering and being vacuum dried
To mould, colded pressing at room temperature, pressure is 100mpa；By the composite after colding pressing under argon protection, sinter 2h,
Sintering temperature is 600 DEG C；Finally the composite after sintering is carried out hot extrusion at a temperature of 380 DEG C and az91/5.0wt.% is obtained
Mgo-cnts composite.Mechanics Performance Testing is carried out to az91/5.0wt.%mgo-cnts composite, its tensile strength
Reach 251-272mpa, elongation percentage reaches 11.2-12.3%, hardness is 79-85hv, is a kind of composite of good mechanical performance.
Accompanying drawing 1 deployment conditions in magnesium alloy powder for the cnts after coated magnesium oxide under the conditions of embodiment 2, in figure can
See, cnts is evenly distributed in alloy powder surface, do not find significantly to reunite, mechanical agitation+ultrasonic disperse technique energy is described
Preferably the cnts of coated magnesium oxide is mixed homogeneously with magnesium alloy powder.
Accompanying drawing 2 is az91 alloy and az91/3.0wt.%mgo-cnts composite microscopic structure under the conditions of embodiment 2.Figure
Middle display, after adding the cnts after coated magnesium oxide, its crystallite dimension substantially attenuates, and serves preferable refined crystalline strengthening effect.
Fig. 3,4 be embodiment 2 under the conditions of az91/3.0wt.%mgo-cnts composite fracture apperance and energy spectrum analysiss, figure
Visible in 3, it is evenly embedded in magnesium alloy substrate in network structure thing, send out in conjunction with corresponding diagram 3a region spectroscopy detection in Fig. 4
Now this net contains c, mg and o element, therefore can determine that this net distribution works is the cnts after coated magnesium oxide.Thus
It can be seen that, the cnts after coated magnesium oxide is evenly distributed in magnesium alloy substrate in netted, plays more preferable overlap joint crystal grain and crystalline substance
The effect on boundary, interface bond strength higher so as to well serve improve composite machinery performance effect.
Claims (1)
1. a kind of method of use coated magnesium oxide Carbon Nanotubes/Magnesiuum Matrix Composite, is characterized in that comprising the following steps:
(1) after mixing the CNT after 3g chemistry coated magnesium oxide with the acetone soln of 500 ml, stirring 30min is ultrasonic again
Dispersion 2h obtains homodisperse CNT acetone mixture；
(2) by quality 97g, granularity is that the az91 magnesium alloy powder of 325 mesh is added in step (1) gained mixed liquor, enters simultaneously
Obtain after ultrasonic+mechanical agitation 2h of row and disperse more uniform mixed serum；
(3) step (2) gained mixed serum is carried out filtering, be vacuum dried after be transferred in mould, colded pressing at room temperature, pressure
Power is 100mpa；
(4) composite after step (3) gained being colded pressing, under argon protection, sinters 2h, and sintering temperature is 600 DEG C；
(5) finally the composite after step (4) sintering is carried out hot extrusion at a temperature of 380 DEG C.
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| CN106399873B (en) * | 2016-09-09 | 2018-05-11 | 南昌大学 | A kind of preparation method of coating alumina whisker nanotube enhancing magnesium-based composite material |
| CN109022861B (en) * | 2018-09-30 | 2020-09-22 | 华南理工大学 | Grain refinement method of Mg-Al series alloy |
| CN113355549B (en) * | 2021-06-09 | 2022-05-13 | 南昌大学 | Method for reinforcing magnesium matrix composite material by coating carbon nano tube with rare earth oxide |
| CN115747594B (en) * | 2022-12-27 | 2023-05-16 | 宜春学院 | Method for reinforcing magnesium-based composite material by using spike rod structure modified carbon nano tube |
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| CN103014567A (en) * | 2012-11-29 | 2013-04-03 | 南昌大学 | Method for preparing carbon nanotube enhanced magnesium-based composite material |
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Non-Patent Citations (1)
| Title |
|---|
| 氧化镁包覆CNTs增强的AZ91D基复合材料的力学性能;袁秋红等;《特种铸造及有色冶金》;20141231;第34卷(第12期);第1307-1310页 * |
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