CN111088441A - Preparation method of high-electric-conductivity heat-conduction metal-based composite material - Google Patents
Preparation method of high-electric-conductivity heat-conduction metal-based composite material Download PDFInfo
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- CN111088441A CN111088441A CN201911391087.9A CN201911391087A CN111088441A CN 111088441 A CN111088441 A CN 111088441A CN 201911391087 A CN201911391087 A CN 201911391087A CN 111088441 A CN111088441 A CN 111088441A
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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
- C22C1/1005—Pretreatment of the non-metallic additives
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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
Abstract
The invention relates to a preparation method of a high-electric-conductivity heat-conduction metal-based composite material, which comprises the steps of adding graphene and a swelling agent into an organic solvent, mixing and carrying out ultrasonic pre-dispersion to obtain a dispersion, uniformly adhering the dispersion to metal particles, drying, putting the metal particles into molten metal liquid, and rapidly swelling the metal particles under the action of high temperature, so that the graphene is effectively introduced into a metal-based material, the dispersion effect of the graphene is greatly improved, and the efficient contact between the graphene and the metal-based material is obtained. Compared with the prior art, the preparation method of the high-electric-conductivity heat-conduction metal-based composite material has the advantages of capability of realizing excellent dispersion and combination of metal and graphene, better electric and heat conductivity, low cost, simple process, better material quality and contribution to large-scale production.
Description
Technical Field
The invention relates to the technical field of preparation methods of composite materials, in particular to a preparation method of a high-electric-conductivity heat-conduction metal-based composite material.
Background
The graphene is a novel two-dimensional nano material, has a very stable structure, has excellent physical properties such as ultrahigh electron mobility, electric conductivity, thermal conductivity, Young modulus, low thermal expansion coefficient and the like, and has a peculiar quantum effect. Furthermore, the strength was as high as 1.0lTpa, 100 times that of structural steel, while the density was only 1/5 for structural steel. Due to the fact that the graphene is low in density, the density of the material can be reduced while the strength of the metal material is improved. Thus. The graphene composite material prepared by compounding the graphene and the metal has excellent performances of low thermal expansion, high conductivity, high thermal conductivity, light weight, high strength and the like, and meets the requirements of the fields of actual military industry, power cables, automobile industry, electrical appliance industry and semiconductors.
The main scientific and engineering problems of the graphene reinforced metal-based nanocomposite material at present comprise:
(1) how to realize the rapid and efficient dispersion of graphene in a metal matrix;
(2) how to obtain good interface bonding between the graphene nanofiller and the aluminum-based material;
(3) how to increase the melting point of the aluminum alloy and ensure that the structure of the graphene filler is not damaged at the heat treatment process temperature.
Due to the fact that the graphene material has a very large specific surface area, the density difference between the metal matrix and the graphene nano-filler is large, and great difficulty is brought to uniform dispersion of the graphene nano-sheets in the metal matrix. In addition, the graphene nanofillers tend to overlap each other to lower their surface energy, thereby resulting in easy agglomeration during nanocomposite preparation and application and adversely affecting the mechanical, electrical, thermal, etc. properties of the composite.
The effective dispersion of graphene in a metal matrix becomes a primary problem to be solved for preparing the graphene/metal composite material. In the prior art, the graphene and the metal powder cannot be completely and uniformly dispersed by simply and mechanically mixing the graphene and the metal powder. In order to reduce the phenomenon of graphene agglomeration, ultrasonic dispersion, wet mechanical stirring and mixing, ball milling, planetary high-energy ball milling, surface modification, electrostatic adsorption and the like are difficult to solve for the composite powder material.
Disclosure of Invention
The invention aims to provide a preparation method of a high-electric-conductivity heat-conduction metal-based composite material, which is used for solving the problem that the existing graphene is effectively dispersed in a metal matrix and effectively improving the electrical, mechanical and thermal properties of the composite material.
In order to solve the technical purpose, the invention provides a preparation method of a high-electric-conductivity heat-conduction metal-based composite material and the composite material obtained by the preparation method.
A preparation method of a high-electric-conductivity heat-conduction metal-based composite material comprises the following steps:
(1) adding graphene and a swelling agent into an organic solvent, mixing and carrying out ultrasonic treatment to obtain a dispersion;
(2) adding the obtained dispersion to metal particles, and stirring until the dispersion is uniformly adhered to the metal particles;
(3) drying the metal particles adhered with the dispersion;
(4) melting at least one metal, stirring, adding the dried metal particles adhered with the dispersoid, and continuing stirring;
(5) and (5) cooling and forming.
According to the preparation method of the high-electric-conductivity and heat-conductivity metal matrix composite material, 0.001-0.8 part of graphene is added into each part of the dispersion.
According to the preparation method of the high-electric-conductivity heat-conduction metal-based composite material, the swelling agent is at least one of sodium tetraborate, rosin, potassium chloride, sodium carbonate, silicon dioxide and calcium fluoride, and 0.002-0.6 part of the swelling agent is added into each part of the dispersion.
In the preparation method of the metal matrix composite with high electrical and thermal conductivity, the organic solvent is at least one of methanol, ethanol, acetone and isopropyl alcohol solution.
According to the preparation method of the high-electric-conductivity and heat-conductivity metal matrix composite material, the particle size of the metal particles is 0.1um to 300 mm.
In the preparation method of the metal matrix composite with high electrical and thermal conductivity, the metal is at least one of aluminum, copper, gold, silver, tin, zinc, vanadium, titanium, iron, nickel, cobalt, manganese, molybdenum, neodymium, chromium, tantalum, indium, lead, tungsten, magnesium, ruthenium, palladium, osmium, niobium, rhenium, lanthanum, cerium, europium, gadolinium, terbium, holmium, erbium, yttrium and rhenium.
The preparation method of the high electric and heat conductive metal matrix composite material comprises the step (1) of carrying out ultrasonic treatment for 0.1-24 hours.
In the preparation method of the metal matrix composite with high electrical and thermal conductivity, the stirring time in the step (2) is 0.1-48 hours.
In the preparation method of the metal matrix composite with high electrical and thermal conductivity, the drying temperature in the step (3) is 40-200 ℃.
The control method for the preparation method of the metal matrix composite with high electrical and thermal conductivity is characterized in that in the step (4), the metal is melted in a furnace with the temperature of 230-.
The invention has the beneficial effects that: according to the preparation method of the high-electric-conductivity and heat-conduction metal-based composite material, the graphene and the swelling agent are added into the organic solvent to be mixed and subjected to ultrasonic pre-dispersion to obtain the dispersion, the dispersion is uniformly adhered to the metal particles and dried, then the metal particles are put into the molten metal liquid, and the metal particles are rapidly swelled under the action of high temperature, so that the graphene is effectively introduced into the metal-based material, the dispersion effect of the graphene is greatly improved, and the efficient contact between the graphene and the metal-based material is obtained. Compared with the prior art, the preparation method of the high-electric-conductivity heat-conduction metal-based composite material has the advantages of capability of realizing excellent dispersion and combination of metal and graphene, better electric and heat conductivity, low cost, simple process, better material quality and contribution to large-scale production.
The high-electric-conductivity heat-conduction metal-based composite material and the composite material prepared by the preparation method can be applied to the fields of military industry, power cables, automobile industry, electric appliance industry and semiconductors.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is an illustration of aluminum particles with dispersion adhered thereto in accordance with an embodiment of the present invention.
Fig. 2 and 3 are photographs of graphene-aluminum alloy composite material in the embodiment of the invention.
Fig. 4 is a photograph of a shear cross section of a graphene aluminum alloy composite according to an embodiment of the present invention.
Fig. 5 is a raman spectrum of the graphene-aluminum alloy composite material according to the embodiment of the present invention.
Fig. 6 is SEM and EDS images of a cross section of a graphene aluminum alloy composite material according to an embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
The embodiment provides a preparation method of a high-electric-conductivity heat-conduction metal-matrix composite material, which comprises the following steps:
adding graphene and a swelling agent into an organic solvent, mixing and carrying out ultrasonic treatment for 1 hour to obtain a dispersion.
Wherein, the graphene accounts for 0.05 part, the swelling agent accounts for 0.02 part, and the organic solvent accounts for 0.93 part.
The swelling agent is sodium tetraborate.
Of course, the swelling agent may be at least one of sodium tetraborate, rosin, potassium chloride, sodium carbonate, silica, and calcium fluoride
The organic solvent is methanol and acetone, and the volume ratio of the methanol to the acetone is 1: 1.
of course, the organic solvent may be at least one of methanol, ethanol, acetone, and an isopropyl alcohol solution.
The resulting dispersion was added to metallic aluminum particles, and stirred for 2 hours, whereby the dispersion was uniformly adhered to the metallic aluminum particles.
Wherein the particle size of the metal aluminum particles is 5 mm. The metallic aluminum particles may be regularly shaped spheres, tetrahedrons, trihedrons, etc., or irregularly shaped stereostructures. When the metallic aluminum particles have a regular three-dimensional structure, the particle diameter refers to the diameter or the diameter of a circumscribed circle. When the metallic aluminum particles are in a three-dimensional structure with irregular shape, the particle size refers to the maximum length thereof.
The metallic aluminum particles to which the dispersion was adhered were dried at a temperature of 50 degrees to obtain metallic aluminum particles as shown in fig. 1.
Melting and stirring the metal aluminum in a melting furnace with the temperature of 600-1500 ℃, filling the melting furnace with anti-oxidation gas, adding the dried metal aluminum particles adhered with the dispersoid, and continuing stirring.
And cooling and forming to obtain the composite material.
Fig. 2 and 3 show photographs of the composite material as an actual photograph, and fig. 4 shows a photograph of a cut section of the composite material.
Fig. 5 shows a raman spectrum of the surface of the composite material of this example. The metal does not generate a Raman signal, the graphene has an obvious Raman signal, the graphene of the embodiment has an obvious Raman signal, and the G peak is obviously enhanced compared with the D peak, which indicates that the graphene exists in the composite material.
Fig. 6 is SEM and EDS images of the cross section. It can be seen that the carbon content of the composite material of this example is significantly increased, indicating that graphene was successfully mixed with aluminum.
According to different requirements, the metal in the above embodiment can be replaced by at least one of gold, silver, copper, tin, zinc, vanadium, titanium, iron, nickel, cobalt, manganese, molybdenum, neodymium, chromium, tantalum, tungsten, magnesium, ruthenium, palladium, osmium, niobium, indium, lead, rhenium, lanthanum, cerium, europium, gadolinium, terbium, holmium, erbium, yttrium and rhenium. According to different requirements, the metal particles in the above embodiments can be replaced by one of gold, silver, copper, tin, zinc, vanadium, titanium, iron, nickel, cobalt, manganese, molybdenum, neodymium, chromium, tantalum, tungsten, magnesium, ruthenium, palladium, osmium, niobium, indium, lead, rhenium, lanthanum, cerium, europium, gadolinium, terbium, holmium, erbium, yttrium and rhenium. Accordingly, the temperature of the furnace is the temperature of the metal with the highest melting point.
Example two
The embodiment provides a preparation method of a high-electric-conductivity heat-conduction metal-matrix composite material, which comprises the following steps:
adding graphene and a swelling agent into an organic solvent, mixing and carrying out ultrasonic treatment for 10 hours to obtain a dispersion.
Wherein, the graphene accounts for 0.2 part, the swelling agent accounts for 0.3 part, and the organic solvent accounts for 0.5 part.
The swelling agent is sodium tetraborate and potassium chloride.
The organic solvent is isopropyl ketone.
The resulting dispersion was added to metallic aluminum particles, and stirred for 5 hours, whereby the dispersion was uniformly adhered to the metallic aluminum particles.
Wherein the particle size of the metal aluminum particles is 10 mm. The metallic aluminum particles may be regularly shaped spheres, tetrahedrons, trihedrons, etc., or irregularly shaped stereostructures. When the metallic aluminum particles have a regular three-dimensional structure, the particle diameter refers to the diameter or the diameter of a circumscribed circle. When the metallic aluminum particles are in a three-dimensional structure with irregular shape, the particle size refers to the maximum length thereof.
And drying the metal aluminum particles adhered with the dispersion at the temperature of 100 ℃ to obtain the metal aluminum particles.
Melting and stirring metal aluminum and zinc in a furnace with the temperature of 800-1000 ℃, filling anti-oxidation gas, adding the dried metal aluminum particles adhered with the dispersoid, and continuing stirring.
And cooling and forming to obtain the composite material.
According to different requirements, the metal in the above embodiment can be replaced by at least one of gold, silver, copper, tin, zinc, vanadium, titanium, iron, nickel, cobalt, manganese, molybdenum, neodymium, chromium, tantalum, tungsten, magnesium, ruthenium, palladium, osmium, niobium, indium, lead, rhenium, lanthanum, cerium, europium, gadolinium, terbium, holmium, erbium, yttrium and rhenium. According to different requirements, the metal particles in the above embodiments can be replaced by one of gold, silver, copper, tin, zinc, vanadium, titanium, iron, nickel, cobalt, manganese, molybdenum, neodymium, chromium, tantalum, tungsten, magnesium, ruthenium, palladium, osmium, niobium, indium, lead, rhenium, lanthanum, cerium, europium, gadolinium, terbium, holmium, erbium, yttrium and rhenium. Accordingly, the temperature of the furnace is the temperature of the metal with the highest melting point.
EXAMPLE III
The embodiment provides a preparation method of a high-electric-conductivity heat-conduction metal-matrix composite material, which comprises the following steps:
adding graphene and a swelling agent into an organic solvent, mixing and carrying out ultrasonic treatment for 20 hours to obtain a dispersion.
Wherein, the graphene accounts for 0.5 part, the swelling agent accounts for 0.1 part, and the organic solvent accounts for 0.4 part.
The swelling agent is rosin, silicon dioxide and calcium fluoride.
The organic solvent is ethanol and isopropyl acetone, and the volume ratio of the ethanol to the isopropyl acetone is 1: 1.
The resulting dispersion was added to metallic zinc particles and stirred for 20 hours, whereby the dispersion was uniformly adhered to the metallic zinc particles.
Wherein the particle size of the metal zinc particles is 15 mm. The metallic zinc particles can be regularly shaped spheres, tetrahedrons, trihedrons, etc., or irregularly shaped stereostructures. When the metallic aluminum particles have a regular three-dimensional structure, the particle diameter refers to the diameter or the diameter of a circumscribed circle. When the metallic aluminum particles are in a three-dimensional structure with irregular shape, the particle size refers to the maximum length thereof.
And drying the metal zinc particles adhered with the dispersoid at the temperature of 150 ℃ to obtain the metal zinc particles.
Melting and stirring metal copper and zinc in a melting furnace at 1100-2000 ℃, filling anti-oxidation gas, adding the dried metal zinc particles adhered with the dispersoid, and continuing stirring.
And cooling and forming to obtain the composite material.
According to different requirements, the metal in the above embodiment can be replaced by at least one of gold, silver, copper, tin, zinc, vanadium, titanium, iron, nickel, cobalt, manganese, molybdenum, neodymium, chromium, tantalum, tungsten, magnesium, ruthenium, palladium, osmium, niobium, indium, lead, rhenium, lanthanum, cerium, europium, gadolinium, terbium, holmium, erbium, yttrium and rhenium. According to different requirements, the metal particles in the above embodiments can be replaced by one of gold, silver, copper, tin, zinc, vanadium, titanium, iron, nickel, cobalt, manganese, molybdenum, neodymium, chromium, tantalum, tungsten, magnesium, ruthenium, palladium, osmium, niobium, indium, lead, rhenium, lanthanum, cerium, europium, gadolinium, terbium, holmium, erbium, yttrium and rhenium. Accordingly, the temperature of the furnace is the temperature of the metal with the highest melting point.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. The preparation method of the metal matrix composite material with high electric and heat conductivity is characterized by comprising the following steps:
(1) adding graphene and a swelling agent into an organic solvent, mixing and carrying out ultrasonic treatment to obtain a dispersion;
(2) adding the obtained dispersion to metal particles, and stirring until the dispersion is uniformly adhered to the metal particles;
(3) drying the metal particles adhered with the dispersion;
(4) melting at least one metal, stirring, adding the dried metal particles adhered with the dispersoid, and continuing stirring;
(5) and (5) cooling and forming.
2. The method for preparing a metal matrix composite with high electrical and thermal conductivity according to claim 1, wherein 0.001-0.8 parts of graphene is added to each part of the dispersion.
3. The preparation method of the metal matrix composite with high electric and heat conductivity as claimed in claim 1, wherein the swelling agent is at least one of sodium tetraborate, rosin, potassium chloride, sodium carbonate, silicon dioxide and calcium fluoride, and 0.002-0.6 part of the swelling agent is added in each part of the dispersion.
4. The method for preparing the metal matrix composite with high electrical and thermal conductivity according to claim 1, wherein the organic solvent is at least one of methanol, ethanol, acetone and isopropyl alcohol solution.
5. The method for preparing a metal matrix composite with high electrical and thermal conductivity according to claim 1, wherein the particle size of the metal particles is 0.1um to 300 mm.
6. The method for preparing a metal matrix composite with high electrical and thermal conductivity according to claim 1, wherein the metal is at least one of aluminum, copper, gold, silver, tin, zinc, vanadium, titanium, iron, nickel, cobalt, manganese, molybdenum, neodymium, chromium, tantalum, indium, lead, tungsten, magnesium, ruthenium, palladium, osmium, niobium, rhenium, lanthanum, cerium, europium, gadolinium, terbium, holmium, erbium, yttrium and rhenium.
7. The method for preparing a metal matrix composite with high electrical and thermal conductivity according to any one of claims 1 to 6, wherein the time for the ultrasonic treatment in (1) is 0.1 to 24 hours.
8. The method for preparing a metal matrix composite with high electrical and thermal conductivity according to any one of claims 1 to 6, wherein the stirring time in the step (2) is 0.1 to 48 hours.
9. The method for preparing a metal matrix composite with high electrical and thermal conductivity according to any one of claims 1 to 6, wherein the temperature for drying in (3) is 40 to 200 ℃.
10. The method for controlling the preparation method of the metal matrix composite with high electrical and thermal conductivity as claimed in any one of claims 1 to 6, wherein the metal is melted in a furnace (4) at 3500 ℃ and 230 ℃ and then filled with an anti-oxidation gas.
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| CN111804893A (en) * | 2020-08-05 | 2020-10-23 | 东北大学 | Simple harmonic vibration stress frame type device and using method thereof |
| CN112030029A (en) * | 2020-09-11 | 2020-12-04 | 上海超诚科技发展有限公司 | High-conductivity metal composite material, and preparation method and equipment thereof |
| CN114717431A (en) * | 2020-06-09 | 2022-07-08 | 姜春辉 | Graphene metal-based composite material and rapid preparation method thereof |
| CN114719605A (en) * | 2020-06-09 | 2022-07-08 | 姜春辉 | Intelligent injection device for adding materials in metal/alloy smelting process |
| CN114717442A (en) * | 2020-06-09 | 2022-07-08 | 姜春辉 | Graphene metal-based composite material and efficient preparation method thereof |
| CN114719604A (en) * | 2020-06-09 | 2022-07-08 | 姜春辉 | Device and method for adding materials in metal/alloy smelting process |
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