CN111101013A - Preparation method of novel graphene-aluminum composite material and graphene-aluminum composite material - Google Patents
Preparation method of novel graphene-aluminum composite material and graphene-aluminum composite material Download PDFInfo
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- CN111101013A CN111101013A CN201911415715.2A CN201911415715A CN111101013A CN 111101013 A CN111101013 A CN 111101013A CN 201911415715 A CN201911415715 A CN 201911415715A CN 111101013 A CN111101013 A CN 111101013A
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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
- C22C1/10—Alloys containing non-metals
- C22C1/1005—Pretreatment of the non-metallic additives
- C22C1/101—Pretreatment of the non-metallic additives by coating
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- 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
- C22C21/00—Alloys based on aluminium
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/223—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating specially adapted for coating particles
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
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Abstract
The invention discloses a preparation method of a novel graphene-aluminum composite material, which comprises the following steps: forming an aluminum film on the graphene powder by adopting a magnetron sputtering method to obtain modified graphene powder; adding the modified graphene powder into molten aluminum, and stirring to uniformly disperse the modified graphene powder in the molten aluminum to obtain a mixed system; and curing and molding the mixed system. The invention discloses a graphene-aluminum composite material.
Description
Technical Field
The invention relates to the technical field of materials, in particular to a preparation method of a novel graphene-aluminum composite material and the graphene-aluminum composite material.
Background
Aluminum and aluminum alloy have high specific strength and are widely applied to various aspects of social life. Graphene is a two-dimensional nanomaterial composed of carbon atoms, and is in a single-layer sheet structure (with a thickness of only a few nanometers). Due to the unique two-dimensional honeycomb crystal structure and extremely high bond strength, the graphene composite material is the hardest nano material with the highest specific strength in the world, the breaking strength of the nano material is as high as 130GPa, and the graphene composite material is used for preparing graphene metal composite materials based on the excellent characteristics of graphene.
Poor wettability between graphene and an aluminum matrix causes difficulty in sufficient function of graphene in the aluminum matrix and may affect dispersibility of graphene in the aluminum matrix, and particularly when a graphene-aluminum composite material is prepared by a melt casting method, graphene added to molten aluminum is hardly likely to be uniformly dispersed in the aluminum matrix.
Disclosure of Invention
In view of the above, it is necessary to provide a method for preparing a novel graphene-aluminum composite material and a graphene-aluminum composite material, aiming at the technical problem that graphene is not easily dispersed in an aluminum matrix.
A preparation method of a novel graphene-aluminum composite material comprises the following steps:
forming an aluminum film on the graphene powder by adopting a magnetron sputtering method to obtain modified graphene powder;
adding the modified graphene powder into molten aluminum, and stirring to uniformly disperse the modified graphene powder in the molten aluminum to obtain a mixed system; and
and heating the mixed system, and curing and forming.
In one embodiment, the temperature of the molten aluminum liquid is 300-400 ℃.
In one embodiment, the sheet diameter of the graphene powder in the modified graphene powder is 100nm to 5 μm, and the thickness is 0.6nm to 10 nm.
In one embodiment, the thickness of the aluminum film in the modified graphene powder is 100 nm-10 μm.
In one embodiment, in the modified graphene powder, the aluminum film forms a continuous phase on the graphene powder.
In one embodiment, the aluminum film covers more than 99% of the graphene powder.
In one embodiment, the step of forming the aluminum film on the graphene powder by using a magnetron sputtering method includes:
arranging the graphene powder on the surface of a sample platform of a working chamber of a magnetron sputtering instrument;
respectively arranging two aluminum sputtering targets on two opposite sides of the sample stage, wherein the opposite directions are parallel to the surface of the sample stage; and
and starting the magnetron sputtering instrument to enable the aluminum particles on the aluminum sputtering target to splash to the graphene powder to form the aluminum film.
In one embodiment, the vacuum degree in the working chamber of the magnetron sputtering instrument in the magnetron sputtering process is below 4 Pa.
In one embodiment, the plasma current of the working chamber of the magnetron sputtering instrument during magnetron sputtering is 4 mA-6 mA.
The graphene-aluminum composite material is prepared by the preparation method of the novel graphene-aluminum composite material.
According to the preparation method, an aluminum film is formed on graphene powder to obtain modified graphene powder, and then the modified graphene powder is mixed with molten aluminum liquid to prepare the graphene-aluminum composite material. The aluminum film is formed on the surface of the graphene powder, so that the dispersion of the graphene powder in molten state aluminum liquid is facilitated, a mixed system with uniform materials can be obtained, and the graphene aluminum composite material with uniformly dispersed graphene in aluminum is further obtained. Traditional low temperature ball-milling powder metallurgy preparation graphite alkene aluminium combined material needs low temperature ball-milling with graphite alkene and aluminite powder misce bene, low temperature ball-milling process cycle is longer, and only there is simple mechanical meshing effect between graphite alkene and the aluminite powder, a good interface bonding is not formed, be difficult to realize real homodisperse in the smelting process, and hot isostatic pressing and hot extrusion in its forming technology all have the problem of industrial production that can't serialization, if will enlarge corresponding equipment, required transformation cost is high. The graphene modified by the method can be directly used for preparing the composite material with uniformly dispersed graphene by a stirring casting method, so that the cost is low, and the expanded production can be carried out.
Further, the inventor finds that, compared with other traditional methods, a more uniform and stable aluminum film can be prepared on the graphene powder by adopting the magnetron sputtering method, and the structural characteristics of the graphene are not damaged in the process of preparing the aluminum film.
Drawings
Fig. 1 is a schematic structural diagram of a preparation method of a novel graphene aluminum composite material according to an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of a conventional magnetron sputtering apparatus;
fig. 3 is a schematic structural diagram of a magnetron sputtering apparatus according to an embodiment of the present invention.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Referring to fig. 1, an embodiment of the present application provides a method for preparing a novel graphene aluminum composite material, including:
s100, forming an aluminum film 140 on the graphene powder 120 by adopting a magnetron sputtering method to obtain modified graphene powder 100;
s200, adding the modified graphene powder 100 into molten aluminum 200, and stirring to uniformly disperse the modified graphene powder 100 in the molten aluminum 200 to obtain a mixed system; and
s300, heating the mixed system, and curing and molding.
According to the embodiment of the invention, the modified graphene powder 100 is obtained by forming the aluminum film 140 on the graphene powder 120, and then the modified graphene powder 100 is mixed with the molten aluminum liquid 200 to prepare the graphene aluminum composite material. The aluminum film 140 is formed on the surface of the graphene powder 120, so that the dispersion of the graphene powder 120 in the molten state aluminum liquid 200 is facilitated, a mixed system with uniform materials can be obtained, and the graphene aluminum composite material with uniformly dispersed graphene in aluminum is further obtained. Traditional low temperature ball-milling powder metallurgy preparation graphite alkene aluminium combined material needs low temperature ball-milling with graphite alkene and aluminite powder misce bene, low temperature ball-milling process cycle is longer, and only there is simple mechanical meshing effect between graphite alkene and the aluminite powder, a good interface bonding is not formed, be difficult to realize real homodisperse in the smelting process, and hot isostatic pressing and hot extrusion in its forming technology all have the problem of industrial production that can't serialization, if will enlarge corresponding equipment, required transformation cost is high. According to the method disclosed by the invention, the composite material with uniformly dispersed graphene can be prepared directly by a stirring casting method after the graphene is modified, the cost is low, and the expanded production can be carried out.
In step S100, an aluminum film 140 is formed on the graphene powder 120 by a magnetron sputtering method. The inventors have found that, compared with other conventional methods, the magnetron sputtering method can be used to prepare a more uniform and stable aluminum film 140 on the graphene powder 120, and the structural characteristics of graphene are not damaged in the process of preparing the aluminum film 140.
In an embodiment, in the modified graphene powder 100, the sheet diameter of the graphene powder 120 may be 100nm to 5 μm. In an embodiment, in the modified graphene powder 100, the thickness of the graphene powder 120 may be 0.6nm to 10 nm. The graphene powder 120 can better exert the structural characteristics in the aluminum matrix within the size range, so that the graphene-aluminum composite material has better mechanical properties and electrical properties.
In an embodiment, in the modified graphene powder 100, the thickness of the aluminum film 140 may be 100nm to 10 μm. The thickness of the aluminum film 140 and the size of the graphene powder 120 are matched with each other, so that the modified graphene powder 100 can be more easily dispersed by using the size effect, and the aluminum film 140 can be more easily mixed with the molten aluminum liquid 200 into a single phase in the further heating process, thereby avoiding the formation of the aluminum film 140 and the solidification of the molten aluminum into a layered structure, and further improving the mechanical properties of the aluminum matrix.
In an embodiment, the temperature of the molten aluminum 200 may be 300 ℃ to 400 ℃. Compared with other temperatures, in this temperature range, the aluminum film 140 on the modified graphene powder 100 can be more easily and uniformly dispersed in the molten aluminum 200. In one embodiment, the temperature of the molten aluminum 200 may be 320-340 deg.C, 340-360 deg.C, 360-380 deg.C or 380-400 deg.C.
In an embodiment, in the modified graphene powder 100, the aluminum film 140 forms a continuous phase on the graphene powder 120. That is, the aluminum is not dispersed on the surface of the graphene powder 120 in a dot shape, but wraps the graphene powder 120 in the aluminum film 140 in a wrapping state. In an embodiment, the aluminum film 140 covers more than 99% of the graphene powder 120, and substantially reaches a completely wrapped state, so as to prevent the exposed graphene powder 120 from contacting the molten aluminum 200 when the modified graphene is initially mixed in the molten aluminum 200, thereby preventing the modified graphene powder 100 from being dispersed in the molten aluminum 200.
In an embodiment, the step of forming the aluminum film 140 on the graphene powder 120 by using a magnetron sputtering method may include:
s120, arranging the graphene powder 120 on the surface of a sample platform 340 of a working chamber of a magnetron sputtering instrument;
s140, respectively disposing two aluminum sputtering targets 320 on two opposite sides of the sample stage, wherein the opposite directions are parallel to the surface of the sample stage; and
and S160, starting the magnetron sputtering instrument to enable the aluminum particles on the aluminum sputtering target 320 to be splashed onto the graphene powder 120 to form the aluminum film 140.
Referring to fig. 2 and 3, the conventional magnetron sputtering coating apparatus is to arrange a cathode sputtering target 320 'above a sample platform 340', however, this arrangement can only coat one surface of the sample, and is suitable for coating a flat sample, and thus is not suitable for coating the graphene powder 120 of the present application. The adoption of the traditional instrument can cause that the graphene cannot be uniformly coated after the spraying of the graphene is finished. In the embodiment of the invention, the arrangement of the magnetron sputtering coating instrument is improved, the two aluminum sputtering targets 320 are arranged in the horizontal direction and are respectively arranged on the two sides of the sample platform 340, so that the graphene powder 120 on the sample platform 340 can be ensured to be coated more uniformly.
In an embodiment, the vacuum degree in the working chamber of the magnetron sputtering apparatus during magnetron sputtering may be less than 4Pa, so as to avoid oxidation of graphene or aluminum during magnetron sputtering.
In one embodiment, the plasma current of the working chamber of the magnetron sputtering apparatus during magnetron sputtering can be 4 mA-6 mA.
In one embodiment, the magnetron sputtering power may be 3kw to 4 kw.
In the step S200, the stirring speed of adding the modified graphene powder 100 into the molten aluminum 200 and stirring may be 150rpm to 200 rpm. In an embodiment, the stirring time may be 20min to 90min, and the specific time may be determined according to the actual mixing system amount and the addition ratio of the modified graphene.
In step S300, the aluminum film 140 on the modified graphene powder 100 is melted by heating and is integrated with the molten aluminum liquid 200 around the aluminum film, and the heating temperature is higher than the melting point of aluminum.
The embodiment of the invention also provides a graphene-aluminum composite material prepared by the preparation method of the novel graphene-aluminum composite material in any one of the embodiments.
Example 1
1g of graphene powder 120 is placed on the surface of a sample platform 340 of a magnetron sputtering instrument working chamber shown in FIG. 3, and the air pressure in the working chamber is pumped to be below 4Pa by vacuumizing. The plasma current was adjusted to 5mA, the time was adjusted to 2min, and the aluminum sputtering targets 320 were horizontally disposed on both sides of the sample stage 340. The graphene powder 120 has a sheet diameter of 1 μm and a thickness of 1 nm.
The modified graphene powder 100 of the aluminum-plated film 140 is collected, and the thickness of the obtained modified graphene separated aluminum film 140 is about 2 μm.
After the aluminum material is melted into molten aluminum liquid 200, the obtained modified graphene powder 100 is put into the aluminum liquid 200 in a manner of medium alloy, and stirred for 30min at 180rpm, so as to assist the dispersibility of the modified graphene powder 100, and obtain a uniformly dispersed mixed system.
And after stirring, heating and pouring the uniform phase mixed system, and cooling to obtain the graphene-aluminum composite material, wherein the mass fraction of graphene in the graphene composite material is 0.5%.
Comparative example 1
Mixing the aluminum powder with the granularity of 20 mu m and the graphene powder 120 in a powder mixer, and mixing for 48 hours to obtain mixed powder. And putting the mixed powder into a ball mill for low-temperature ball milling. After ball milling for 5 hours at low temperature, the mixed powder is put into a steel sheath, and hot isostatic pressing, heat preservation and pressure maintaining are carried out for 2 hours at 400 ℃ and 100 MPa. And then removing the sheath to obtain the graphene-aluminum composite material.
Comparative example 2
The comparative example 2 is substantially the same as the example 1 except that the graphene powder 120 is directly put into the aluminum liquid 200 without coating the aluminum film 140 with the graphene powder 120.
The graphene aluminum composite materials obtained in example 1 and comparative examples 1 to 2 were subjected to mechanical property and conductivity measurement, and the results are shown in table 1.
TABLE 1
| Group of | Stretch resistance (MPa) | Elongation at Break (%) | Conductivity ((IACS)) |
| Example 1 | 109.57 | 27.53 | 61.89 |
| Comparative example 1 | 115.53 | 23.57 | 59.87 |
| Comparative example 2 | 76.75 | 32.51 | 61.75 |
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A preparation method of a novel graphene-aluminum composite material comprises the following steps:
forming an aluminum film on the graphene powder by adopting a magnetron sputtering method to obtain modified graphene powder;
adding the modified graphene powder into molten aluminum, and stirring to uniformly disperse the modified graphene powder in the molten aluminum to obtain a mixed system; and
and heating the mixed system, and curing and forming.
2. The preparation method of the novel graphene aluminum composite material as claimed in claim 1, wherein the temperature of the molten aluminum is 300 ℃ to 400 ℃.
3. The preparation method of the novel graphene-aluminum composite material according to claim 1, wherein the sheet diameter of the graphene powder in the modified graphene powder is 100nm to 5 μm, and the thickness is 0.6nm to 10 nm.
4. The preparation method of the novel graphene-aluminum composite material according to claim 1, wherein the thickness of the aluminum film in the modified graphene powder is 100nm to 10 μm.
5. The method for preparing the novel graphene-aluminum composite material according to claim 1, wherein the aluminum film forms a continuous phase on the graphene powder in the modified graphene powder.
6. The method for producing the novel graphene-aluminum composite material according to claim 5, wherein the aluminum film covers 99% or more of the graphene powder.
7. The preparation method of the novel graphene-aluminum composite material according to claim 1, wherein the step of forming the aluminum film on the graphene powder by using a magnetron sputtering method comprises:
arranging the graphene powder on the surface of a sample platform of a working chamber of a magnetron sputtering instrument;
respectively arranging two aluminum sputtering targets on two opposite sides of the sample stage, wherein the opposite directions are parallel to the surface of the sample stage; and
and starting the magnetron sputtering instrument to enable the aluminum particles on the aluminum sputtering target to splash to the graphene powder to form the aluminum film.
8. The method for preparing the novel graphene-aluminum composite material according to claim 1, wherein a degree of vacuum in a working chamber of the magnetron sputtering apparatus during magnetron sputtering is 4Pa or less.
9. The preparation method of the novel graphene-aluminum composite material according to claim 1, wherein a plasma current of a working chamber of the magnetron sputtering apparatus during magnetron sputtering is 4 mA-6 mA.
10. A graphene-aluminum composite material prepared by the method for preparing a novel graphene-aluminum composite material according to any one of claims 1 to 9.
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Cited By (2)
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| CN113718125A (en) * | 2021-08-11 | 2021-11-30 | 武汉材料保护研究所有限公司 | Graphene reinforced aluminum-based composite material with high conductivity and preparation method thereof |
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Application publication date: 20200505 |