CN110643846B - Preparation method of carbon nano tube reinforced magnesium alloy - Google Patents
Preparation method of carbon nano tube reinforced magnesium alloy Download PDFInfo
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- CN110643846B CN110643846B CN201911079241.9A CN201911079241A CN110643846B CN 110643846 B CN110643846 B CN 110643846B CN 201911079241 A CN201911079241 A CN 201911079241A CN 110643846 B CN110643846 B CN 110643846B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
- C22C1/1047—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- 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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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/06—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
- C22C2026/002—Carbon nanotubes
Abstract
A preparation method of carbon nano tube reinforced magnesium alloy belongs to the technical field of nano materials. The preparation method of the carbon nano tube reinforced magnesium alloy comprises the following steps: s1, preparing the carbon nano tube into carbon nano tube paper with large aperture and porosity, and evaporating elemental magnesium at high temperature to generate a uniform nano magnesium crystal layer on the surface of the carbon nano tube paper; s2, directly adding the carbon nanotube paper coated with the nano magnesium crystal layer into the magnesium or magnesium alloy semi-molten mass in an inert gas atmosphere, pressurizing, stirring and mixing uniformly, and obtaining the carbon nanotube reinforced magnesium alloy composite material by a semi-solid casting method. The method adopted by the invention is simple and easy to operate, and is suitable for industrial casting production.
Description
Technical Field
The invention relates to a technology in the field of nano materials, in particular to a preparation method of a carbon nano tube reinforced magnesium alloy.
Background
Carbon Nanotubes (CNTs) are a class of novel carbon materials, hollow seamless tubular nanostructures made of single or multiple layers of graphite sheets that are crimped. The average Young modulus of the multi-wall carbon nano-tube is about 1.8 multiplied by 1012Pa, which is 100 times of that of steel, the bending strength can reach 14.2GPa, the existing strain energy can reach 100KeV, the super-strong mechanical property is shown, and the density is only 1/6 of the steel. The calculation finds that the carbon nano tube can release stress through the pentagon and heptagon pairs when stressed, shows good self-lubricating performance, and shows good prospect for the application of the self-lubricating performance of the carbon nano tube. In addition, the carbon nano tube also has the characteristics of excellent optics, field emission, strong acid and strong alkali resistance, high temperature oxidation resistance and the like. Thus, carbon nanotubes are one of the ideal candidates for reinforcing composite materials.
The magnesium-based composite material has good wear-resistant thermal property and good heat-conducting property. Low density, easy processing and easy recovery, and has very good application prospect in the fields of aerospace, electronic industry and the like. Although the research and development work of carbon nanotube reinforced magnesium-based composite materials at home and abroad has achieved some results, the reinforcing effect of the carbon nanotubes on the composite materials is not as expected due to the problems of dispersion and wettability of the carbon nanotubes in matrix tissues and the like.
The present invention has been made to solve the above-mentioned problems occurring in the prior art.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a preparation method of a carbon nano tube reinforced magnesium alloy, which adopts a semi-solid casting process and is suitable for industrial production.
The invention comprises the following steps:
s1, preparing the carbon nanotube into carbon nanotube paper with large aperture and large porosity, and evaporating the elemental magnesium at high temperature or sputtering the elemental magnesium in a cold state to generate a uniform nano magnesium crystal layer on the surface of the carbon nanotube paper;
s2, directly adding the carbon nanotube paper coated with the nano magnesium crystal layer into the magnesium or magnesium alloy semi-molten mass in an inert gas atmosphere, pressurizing, stirring and mixing uniformly, and obtaining the carbon nanotube reinforced magnesium alloy composite material by a semi-solid casting method.
Preferably, the carbon nanotube is at least one of a single-walled carbon nanotube and a multi-walled carbon nanotube, the diameter is 20-180 nm, and the length is 10-20 μm.
Preferably, the thickness of the carbon nanotube paper is 350-450 μm.
Preferably, the preparation method of the carbon nanotube paper comprises the following steps:
s11, mixing the carbon nano tube, the surfactant and the mixed solution of deionized water and alcohol, and performing ultrasonic treatment to uniformly disperse the mixture to obtain carbon nano tube slurry;
s12, uniformly coating the carbon nanotube slurry prepared in the step S11 on the surface of the rough copper foil, and drying at 70-80 ℃;
and S13, tearing off the carbon nanotube film dried in the step S12 and rolling the carbon nanotube film into a carbon nanotube paper roll to obtain the carbon nanotube paper with large aperture and large porosity.
Preferably, the surfactant is a nonionic surfactant, including but not limited to PEG, PVP, PVA.
Preferably, the ratio of the deionized water to the alcohol is 1: 1-2, and during operation, the CNT is soaked by the alcohol and then the deionized water is added.
Preferably, the semi-molten mass is obtained by heating magnesium or magnesium alloy to 420-660 ℃.
Preferably, the preparation method of the carbon nanotube paper comprises the following steps:
s11, mixing the carbon nano tube, the surfactant and the mixed solution of deionized water and alcohol, and uniformly dispersing by means of ultrasound, sanding, stirring and the like to obtain carbon nano tube slurry;
s12, uniformly coating the obtained carbon nanotube slurry on the surface of the raw copper foil, and drying at 70-80 ℃;
and S13, tearing off the dried carbon nanotube film and rolling into a carbon nanotube paper roll to obtain the carbon nanotube paper.
Technical effects
Compared with the prior art, the invention has the following technical effects:
1) a nano magnesium crystal layer is formed on the surface of the carbon nano tube, so that the effective combination of the carbon nano tube and magnesium or magnesium alloy is ensured, the structural integrity of the carbon nano tube is ensured, and the reinforcing effect is obvious;
2) the mechanical fusion method of mixing by pressure stirring is adopted, the uniform distribution of the carbon nano tubes in the magnesium or magnesium alloy is realized, the product has the advantages of the magnesium or magnesium alloy and the carbon nano tube material, the preparation method is simple and easy to operate, high-efficiency and environment-friendly, and the method is suitable for industrial casting production.
Drawings
FIG. 1 is an SEM photograph of carbon nanotube paper coated with nano-magnesium crystal layer prepared in example 1;
fig. 2 is an EDS composition analysis chart of the carbon nanotube paper coated with a nano magnesium crystal layer prepared in example 1.
Detailed Description
The invention is described in detail below with reference to the drawings and the detailed description.
Example 1
The embodiment relates to a preparation method of a carbon nanotube reinforced magnesium alloy, which comprises the following steps:
s1, preparing a powder by weight ratio of CNT: PVP: deionized water: uniformly mixing the raw materials with alcohol of 25:2:300:200, and performing ultrasonic dispersion to obtain carbon nanotube slurry; uniformly coating the obtained carbon nanotube slurry on the surface of a crude copper foil, drying at 70-80 ℃, tearing off a carbon nanotube film, and rolling into a carbon nanotube paper roll for later use;
s2, fixing the obtained carbon nanotube paper roll on a sample rack in a vacuum evaporation chamber, vacuumizing and simultaneously putting magnesium metal powder into a melting tank for melting, filtering molten magnesium and pumping into a crucible in the evaporation chamber, heating the crucible to evaporate the magnesium metal at high temperature, unreeling and reeling the sample rack at a constant rate of 1r/S, and obtaining carbon nanotube paper uniformly coated with nano-magnesium after evaporation is finished;
and S3, adding the carbon nano tube coated with nano magnesium and magnesium alloy powder into a bin of mechanical fusion equipment according to the weight ratio of 0.5-1.5: 99.5-98.5, replacing air in the bin with argon, heating to 700 ℃, simultaneously applying pressure to the raw materials, stirring and mixing for about 2 hours until the raw materials are uniformly mixed, and pouring or extruding into a blank to obtain the carbon nano tube reinforced magnesium alloy composite material blank.
Hot-extruding the carbon nano tube reinforced magnesium alloy composite material blank into a bar material on a 1000t horizontal extruder, wherein the extrusion temperature is 460 ℃, the extrusion speed is 2mm/s, the extrusion ratio is 18:1, and the diameter of the extruded bar material is 15 mm; and (3) carrying out solution treatment on the extruded bar for 4h at 500 ℃, then quenching the extruded bar into water at room temperature, and finally naturally cooling to obtain a finished product.
And (3) observing the shape of the carbon nanotube reinforced magnesium alloy composite material blank prepared in the step S2 by using a Zeiss ultra-high resolution field emission scanning electron microscope (MERLIN Compact (SEM)) and performing energy spectrum analysis (EDS) to obtain an SEM photo shown in figure 1 and an EDS component analysis diagram shown in figure 2, wherein a magnesium crystal layer is uniformly covered on the surface of the carbon nanotube paper as shown in figure 1, and the magnesium crystal layer is uniformly coated on the surface of the carbon nanotube in the pore as shown in the magnification shooting magnification.
The tensile properties of the finished product were tested using a CSS-55100 model electronic universal material tester, and the microhardness of the finished product was tested using a HXS-1000AK microhardness tester (load 100g, load time 10s), and it was found that when the amount of carbon nanotubes added was 1.0%, the tensile strength and the limit strength of the finished product reached peak values of 189MPa and 91HV, respectively.
It is to be emphasized that: the above embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and all simple modifications, equivalent changes and modifications made to the above embodiments according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.
Claims (2)
1. The preparation method of the carbon nanotube reinforced magnesium alloy is characterized by comprising the following steps of:
s1, preparing the carbon nanotube into carbon nanotube paper with large aperture and large porosity, and evaporating the elemental magnesium at high temperature or sputtering the elemental magnesium in a cold state to generate a uniform nano magnesium crystal layer on the surface of the carbon nanotube paper;
s2, directly adding the carbon nanotube paper coated with the nano magnesium crystal layer into the magnesium or magnesium alloy semi-molten mass in an inert gas atmosphere, pressurizing, stirring and mixing uniformly, and obtaining the carbon nanotube reinforced magnesium alloy composite material by a semi-solid casting method;
the preparation method of the carbon nanotube paper comprises the following steps:
s11, mixing the carbon nano tube, the surfactant and the mixed solution of deionized water and alcohol, and performing ultrasonic treatment to uniformly disperse the mixture to obtain carbon nano tube slurry;
s12, uniformly coating the carbon nanotube slurry prepared in the step S11 on the surface of the rough copper foil, and drying at 70-80 ℃;
and S13, tearing off the carbon nanotube film dried in the step S12 and rolling the carbon nanotube film into a carbon nanotube paper roll to obtain the carbon nanotube paper with large aperture and large porosity.
2. The method for preparing a carbon nanotube-reinforced magnesium alloy according to claim 1, wherein the semi-molten mass is obtained by heating magnesium or a magnesium alloy to 420 to 660 ℃.
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| CN101376932B (en) * | 2007-08-31 | 2010-11-10 | 清华大学 | Preparation and preparing apparatus for magnesium-based composite material |
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