CN103014399B - Preparation method of enhanced magnesium-based composite material of carbon nanotubes - Google Patents
Preparation method of enhanced magnesium-based composite material of carbon nanotubes Download PDFInfo
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- CN103014399B CN103014399B CN201210589983.8A CN201210589983A CN103014399B CN 103014399 B CN103014399 B CN 103014399B CN 201210589983 A CN201210589983 A CN 201210589983A CN 103014399 B CN103014399 B CN 103014399B
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Abstract
The invention relates to a preparation method of an enhanced magnesium-based composite material of carbon nanotubes, relates to a preparation method of a nanometer composite material, and mainly solves the technical problems that the carbon nanotubes are difficultly scattered uniformly in a magnesium alloy matrix and the tensile strength of the enhanced magnesium-based composite material is low. The preparation method comprises the following steps of: firstly, carrying out mixing and ball milling on Zn powder and the carbon nanotubes to obtain composite powder; secondly, pressing the composite powder and magnesium powder into precast blocks after uniformly mixing the composite powder and the magnesium powder; and finally, adding the precast blocks into the molten magnesium powder, heating until obtaining metal solution, and transferring the metal solution into a die to be pressed, thus obtaining the enhanced magnesium-based composite material of the carbon nanotubes, wherein the tensile strength of the enhanced magnesium-based composite material is 195-210 MPa, and the elongation rate of the enhanced magnesium-based composite material is 13-15%. According to the preparation method of the enhanced magnesium-based composite material of the carbon nanotubes, the tensile strength is high, the dispersity is good, and the enhanced magnesium-based composite material of the carbon nanotubes can be applied to the fields of aerospace, automobiles and sports equipments.
Description
Technical field
The present invention relates to the preparation method of nano composite material.
Background technology
Carbon nanotube (carbon nanotubes, CNTs) be by the curling seamless nano level tubular material forming of single or multiple lift graphite flake, because its unique structure carbon nano tube has good performance, as heat-resisting, corrosion-resistant, heat shock resistance, self-lubricating etc., its Young's modulus and diamond are suitable, being about 1TPa, is 5 times of left and right of steel.Carbon nanotube also has good electrical property and thermal characteristics, and Single Carbon Nanotubes thermal conductivity vertically can reach 3000Wm
-5k
-a, its coefficient of thermal expansion is very low, still has stability well in the time of 700 DEG C, and therefore, carbon nanotube once finding just to cause that people pay attention to widely, became wild phase desirable in matrix material in 1991.
But because the wettability of carbon nanotube and magnesium alloy is bad, and its nano level size also makes to produce powerful Van der Waals force between carbon nanotube and very easily reunite, this all makes the reinforced effects of carbon nanotube in matrix material not bring into play completely.So how to make carbon nanotube be dispersed into uniformly the key of preparing nano Mg base composite material for success in matrix metal, for carbon nanotube is disperseed uniformly in magnesium alloy, people attempt changing at carbon nano tube surface plating Ni the wettability of carbon nanotube and magnesium alloy, but or can not solve well the problem that carbon nanotube is reunited, thereby affected the reinforced effects of carbon nanotube, the composite material tensile strength after enhancing is lower.
Summary of the invention
The present invention will solve carbon nanotube in magnesium alloy substrate, to be difficult to the low technical problem of magnesium base composite material tensile strength after dispersed and enhancing, and a kind of preparation method of Carbon Nanotubes/Magnesiuum Matrix Composite is provided.
The preparation method of Carbon Nanotubes/Magnesiuum Matrix Composite of the present invention carries out according to the following steps:
The volume ratio of one, pressing carbon nanotube and Zn powder is (0.25 ~ 1): 1, and be that 100 ~ 300rpm, ratio of grinding media to material are (5 ~ 10) by carbon nanotube and Zn powder at rotating speed: under 1 condition, ball milling 8 ~ 12h, obtains carbon nanotube/Zn powder composite powder;
Two, be (2.5 ~ 3.5) by the composite powder of step 1 and the volume ratio of magnesium powder: 1, after being mixed, the composite powder of step 1 and magnesium powder be placed in mould, be that under 180 ~ 200 DEG C, the pressure condition that is 140 ~ 160MPa, compacting 4 ~ 6min, obtains prefabricated section in temperature;
Three, in the prefabricated section obtaining by step 2, the mass ratio of Zn powder and magnesium powder is 6:(90 ~ 98), prefabricated section is joined in the magnesium powder of melting, be to be incubated 4 ~ 5min under the condition of 580 DEG C ~ 600 DEG C in temperature, low whipping speed is under the condition of 300 ~ 400rpm, mechanical stirring 10 ~ 15min, obtain metallic solution, in metallic solution, pass into ultrasonic wave again, ultrasonic power is 500 ~ 550w, the supersound process time is 15 ~ 25min, leave standstill after 3 ~ 5min, pour in advance in temperature is the mould of preheating under the condition of 350 ~ 450 DEG C and carry out die casting, die casting pressure is 60 ~ 70MPa, pressurize 4 ~ 6min, obtain carbon nanotube/magnesium base composite material.
Preparation method of the present invention passes through first by Zn powder and carbon nanotube mixing and ball milling, effectively break up the carbon nanotube of reunion and make the surface that is dispersed in Zn powder of even carbon nanotube, then by stirring and being aided with ultrasonic concussion, make being dispersed in magnesium alloy substrate of even carbon nanotube, effectively solve carbon nanotube homodisperse problem in matrix metal, fully play the reinforced effects of carbon nanotube, as cast condition carbon nanotube/the magnesium base composite material obtaining by preparation method of the present invention, its tensile strength is 195 ~ 210MPa, unit elongation is 13 ~ 15%, can be applicable to aerospace, automobile, sports equipment field.
Brief description of the drawings
Fig. 1 is the stereoscan photograph of carbon nanotube/Zn powder composite powder that in embodiment 1, step 1 obtains;
Fig. 2 is the stereoscan photograph of the carbon nanotube described in step 1 in embodiment 1;
Fig. 3 is the tensile strength graphic representation of test two; Wherein curve A is the tensile strength curve of carbon nanotube/magnesium base composite material of preparing of embodiment 1, the tensile strength curve that curve B is Mg-6Zn.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the preparation method of the Carbon Nanotubes/Magnesiuum Matrix Composite of present embodiment carries out according to the following steps:
The volume ratio of one, pressing carbon nanotube and Zn powder is (0.25 ~ 1): 1, and be that 100 ~ 300rpm, ratio of grinding media to material are (5 ~ 10) by carbon nanotube and Zn powder at rotating speed: under 1 condition, ball milling 8 ~ 12h, obtains carbon nanotube/Zn powder composite powder;
Two, be (2.5 ~ 3.5) by the composite powder of step 1 and the volume ratio of magnesium powder: 1, after being mixed, the composite powder of step 1 and magnesium powder be placed in mould, be that under 180 ~ 200 DEG C, the pressure condition that is 140 ~ 160MPa, compacting 4 ~ 6min, obtains prefabricated section in temperature;
Three, in the prefabricated section obtaining by step 2, the mass ratio of Zn powder and magnesium powder is 6:(90 ~ 98), prefabricated section is joined in the magnesium powder of melting, be to be incubated 4 ~ 5min under the condition of 580 DEG C ~ 600 DEG C in temperature, low whipping speed is under the condition of 300 ~ 400rpm, mechanical stirring 10 ~ 15min, obtain metallic solution, in metallic solution, pass into ultrasonic wave again, ultrasonic power is 500 ~ 550w, the supersound process time is 15 ~ 25min, leave standstill after 3 ~ 5min, pour in advance in temperature is the mould of preheating under the condition of 350 ~ 450 DEG C and carry out die casting, die casting pressure is 60 ~ 70MPa, pressurize 4 ~ 6min, obtain carbon nanotube/magnesium base composite material.
Embodiment two: present embodiment is different from embodiment one: in step 1, ratio of grinding media to material is (6 ~ 7): 1, other step and parameter are identical with embodiment one.
Embodiment three: present embodiment is different from embodiment one or two: in step 2, compacting is to carry out under the condition that is 150MPa at 190 DEG C, pressure, press time is 5min, and other step and parameter are identical with embodiment one or two.
Embodiment four: present embodiment is different from one of embodiment one to three: in step 3, in prefabricated section, the mass ratio of Zn powder and magnesium powder is 6:94, and other step and parameter are identical with one of embodiment one to three.
Embodiment five: present embodiment is different from one of embodiment one to four: after prefabricated section being joined in step 3 in the magnesium powder of melting, be to be incubated 2 ~ 3min under the condition of 580 DEG C in temperature, other step and parameter are identical with one of embodiment one to four.
Embodiment six: present embodiment is different from one of embodiment one to five: in step 3, when supersound process, ultrasonic bar stretches into about 40cm under metallic solution liquid level, and other step and parameter are identical with one of embodiment one to five.
Embodiment seven: present embodiment is different from one of embodiment one to six: in step 3, the supersound process time is 20min, and time of repose is 4min, and other step and parameter are identical with one of embodiment one to six.
Embodiment eight: present embodiment is different from one of embodiment one to seven: in step 3, cast temperature is 400 DEG C, die casting pressure is 65MPa, pressurize 5min, other step and parameter are identical with one of embodiment one to seven.
With following verification experimental verification beneficial effect of the present invention:
The preparation method of the Carbon Nanotubes/Magnesiuum Matrix Composite of embodiment 1, the present embodiment carries out according to the following steps:
One, being 0.25:1 by the volume ratio of carbon nanotube and Zn powder, is that under 200rpm, the ratio of grinding media to material condition that is 6.5:1, ball milling 12h, obtains carbon nanotube/Zn powder composite powder by carbon nanotube and Zn powder at rotating speed;
Two, be 3:1 by the volume ratio of the composite powder of step 1 and magnesium powder, after the composite powder of step 1 and magnesium powder are mixed, being placed in mould, is under 190 DEG C, the pressure condition that is 150MPa in temperature, compacting 5min, obtaining diameter is 60mm, the prefabricated section that thickness is 10mm;
Three, in the prefabricated section obtaining by step 2, the mass ratio of Zn powder and magnesium powder is 6:94, prefabricated section is joined in the magnesium powder of melting, be to be incubated 4min under the condition of 580 DEG C in temperature, then mechanical stirring 10min under the condition that low whipping speed is 300rpm, in metallic solution, pass into ultrasonic wave again, ultrasonic power is 500w, treatment time is 20min, leave standstill after 3min, pour in advance in temperature is the mould of preheating under the condition of 300 DEG C and carry out die casting, die casting pressure is 65MPa, and pressurize 5min, obtains carbon nanotube/magnesium base composite material.
The preparation method of the Carbon Nanotubes/Magnesiuum Matrix Composite of embodiment 2, the present embodiment carries out according to the following steps:
One, being 0.5:1 by the volume ratio of carbon nanotube and Zn powder, is that under 300rpm, the ratio of grinding media to material condition that is 6.5:1, ball milling 12h, obtains carbon nanotube/Zn powder composite powder by carbon nanotube and Zn powder at rotating speed;
Two, be 3:1 by the volume ratio of the composite powder of step 1 and magnesium powder, after the composite powder of step 1 and magnesium powder are mixed, being placed in mould, is under 190 DEG C, the pressure condition that is 150MPa in temperature, compacting 5min, obtaining diameter is 60mm, the prefabricated section that thickness is 10mm;
Three, in the prefabricated section obtaining by step 2, the mass ratio of Zn powder and magnesium powder is 6:94, prefabricated section is joined in the magnesium powder of melting, be to be incubated 4min under the condition of 580 DEG C in temperature, then mechanical stirring 10min under the condition that low whipping speed is 350rpm, in metallic solution, pass into ultrasonic wave again, ultrasonic power is 500w, treatment time is 20min, leave standstill after 5min, pour in advance in temperature is the mould of preheating under the condition of 300 DEG C and carry out die casting, die casting pressure is 70MPa, and pressurize 5min, obtains carbon nanotube/magnesium base composite material.
The preparation method of the Carbon Nanotubes/Magnesiuum Matrix Composite of embodiment 3, the present embodiment carries out according to the following steps:
One, being 1:1 by the volume ratio of carbon nanotube and Zn powder, is that under 400rpm, the ratio of grinding media to material condition that is 6.5:1, ball milling 8h, obtains carbon nanotube/Zn powder composite powder by carbon nanotube and Zn powder at rotating speed;
Two, be 3:1 by the volume ratio of the composite powder of step 1 and magnesium powder, after the composite powder of step 1 and magnesium powder are mixed, being placed in mould, is under 190 DEG C, the pressure condition that is 150MPa in temperature, compacting 5min, obtaining diameter is 60mm, the prefabricated section that thickness is 10mm;
Three, in the prefabricated section obtaining by step 2, the mass ratio of Zn powder and magnesium powder is 6:94, prefabricated section is joined in the magnesium powder of melting, be to be incubated 5min under the condition of 580 DEG C in temperature, then mechanical stirring 15min under the condition that low whipping speed is 400rpm, in metallic solution, pass into ultrasonic wave again, ultrasonic power is 500w, treatment time is 20min, leave standstill after 5min, pour in advance in temperature is the mould of preheating under the condition of 300 DEG C and carry out die casting, die casting pressure is 70MPa, pressurize 5min, obtains carbon nanotube/magnesium base composite material.
Test one, carbon nanotube/Zn powder composite powder that step 1 in embodiment 1 is obtained carry out dispersiveness and detect:
Using Quanta200FEG field emission scanning electron microscope is under the condition of 20000 times in magnification, carbon nanotube described in carbon nanotube/Zn powder composite powder and step 1 that observation embodiment 1 step 1 obtains, obtain stereoscan photograph as depicted in figs. 1 and 2, Fig. 1 is the stereoscan photograph of carbon nanotube/Zn powder composite powder of obtaining of embodiment 1 step 1, Fig. 2 is the stereoscan photograph of the carbon nanotube described in embodiment 1 step 1, can be seen by Fig. 1 and Fig. 2 contrast, the carbon nanotube of reuniting is broken up, be dispersed in uniformly Zn powder surface, dispersion effect is good.
Test two, carbon nanotube/magnesium base composite material and Mg-6Zn prepared by embodiment 1 carry out tensile strength test, and test process is as follows:
According to GB/T228-2002 testing standard, adopt metallic substance tensile testing at ambient temperature, with American I nstron-5569 electronic universal material testing machine, carbon nanotube/magnesium base composite material prepared by embodiment 1 and Mg-6Zn carry out tensile strength test, obtain tensile strength graphic representation as shown in Figure 3, wherein curve A is the tensile strength curve of carbon nanotube/magnesium base composite material of preparing of embodiment 1, curve B is the tensile strength curve of Mg-6Zn, the tensile strength that can draw carbon nanotube/magnesium base composite material prepared by embodiment 1 from figure is 200MPa, unit elongation is 13.7%, the tensile strength of Mg-6Zn is 150MPa, unit elongation is 7.7%, carbon nanotube/magnesium base composite material tensile strength prepared by embodiment 1 is higher.
Claims (7)
1. the preparation method of Carbon Nanotubes/Magnesiuum Matrix Composite, is characterized in that this preparation method carries out according to the following steps:
The volume ratio of one, pressing carbon nanotube and Zn powder is (0.25～1): 1, and be that 100～300rpm, ratio of grinding media to material are (5～10) by carbon nanotube and Zn powder at rotating speed: under 1 condition, ball milling 8～12h, obtains carbon nanotube/Zn powder composite powder;
Two, be (2.5～3.5) by the composite powder of step 1 and the volume ratio of magnesium powder: 1, after being mixed, the composite powder of step 1 and magnesium powder be placed in mould, be that under 180～200 DEG C, the pressure condition that is 140～160MPa, compacting 4～6min, obtains prefabricated section in temperature;
Three, in the prefabricated section obtaining by step 2, the mass ratio of Zn powder and magnesium powder is 6:(90～98), prefabricated section is joined in the magnesium powder of melting, be to be incubated 4～5min under the condition of 580 DEG C～600 DEG C in temperature, low whipping speed is under the condition of 300～400rpm, mechanical stirring 10～15min, obtain metallic solution, in metallic solution, pass into ultrasonic wave again, ultrasonic power is 500～550w, the supersound process time is 15～25min, leave standstill after 3～5min, pour in advance in temperature is the mould of preheating under the condition of 350～450 DEG C and carry out die casting, die casting pressure is 60～70MPa, pressurize 4～6min, obtain carbon nanotube/magnesium base composite material.
2. the preparation method of Carbon Nanotubes/Magnesiuum Matrix Composite according to claim 1, is characterized in that in step 1, ratio of grinding media to material is (6～7): 1.
3. the preparation method of Carbon Nanotubes/Magnesiuum Matrix Composite according to claim 1 and 2, is characterized in that in step 2 that compacting is is to carry out under 190 DEG C, the pressure condition that is 150MPa in temperature, and the press time is 5min.
4. the preparation method of Carbon Nanotubes/Magnesiuum Matrix Composite according to claim 3, is characterized in that in step 3 that in prefabricated section, the mass ratio of Zn powder and magnesium powder is 6:94.
5. the preparation method of Carbon Nanotubes/Magnesiuum Matrix Composite according to claim 3, while it is characterized in that in step 3 supersound process, ultrasonic bar stretches into about 40cm under metallic solution liquid level.
6. the preparation method of Carbon Nanotubes/Magnesiuum Matrix Composite according to claim 3, is characterized in that in step 3 that the supersound process time is 20min, and time of repose is 4min.
7. the preparation method of Carbon Nanotubes/Magnesiuum Matrix Composite according to claim 3, is characterized in that in step 3, cast temperature is 400 DEG C, and die casting pressure is 65MPa, pressurize 5min.
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| CN103451456A (en) * | 2013-06-26 | 2013-12-18 | 浙江天乐新材料科技有限公司 | Method for forcibly dispersing nano particle-reinforced aluminum alloy by using ultrasonic remelting dilution precast block |
| CN103773980A (en) * | 2014-03-04 | 2014-05-07 | 哈尔滨工业大学 | Preparation method of high-performance graphene nanosheet reinforced magnesium matrix composite |
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| CN103773988B (en) * | 2014-03-04 | 2015-09-16 | 哈尔滨工业大学 | A kind of Graphene strengthens the preparation method of magnesium base composite material |
| CN103789590B (en) * | 2014-03-04 | 2016-01-20 | 哈尔滨工业大学 | The preparation method of particle reinforced magnesium base compound material |
| CN104195398B (en) * | 2014-09-12 | 2016-03-23 | 济南大学 | A kind of preparation method of magnesium-yittrium alloy |
| CN104711496B (en) * | 2015-04-01 | 2017-06-06 | 北京工业大学 | Carbon Nanotubes/Magnesiuum Matrix Composite and preparation method thereof |
| CN106119645A (en) * | 2016-07-31 | 2016-11-16 | 余姚市婉珍五金厂 | Alloy material that a kind of axle wheel is special and preparation method thereof |
| CN106244948B (en) * | 2016-09-09 | 2018-02-23 | 南昌大学 | A kind of preparation method for the multi-walled carbon nanotube enhancing magnesium-based composite material for coating elemental copper |
| CN110106411B (en) * | 2019-05-30 | 2020-09-25 | 北京工业大学 | Method for preparing high-content carbon nanotube reinforced magnesium-based composite material by adopting precursor |
| CN110527884B (en) * | 2019-08-30 | 2020-11-20 | 北京工业大学 | Preparation method of high-strength high-thermal-conductivity carbon nanotube reinforced magnesium-based composite material |
| CN111020270B (en) * | 2019-12-19 | 2021-04-23 | 陕西科技大学 | CNTs reinforced magnesium-based composite material and preparation method thereof |
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