CN110293229B - Graphene film-iron alloy composite material and preparation method thereof - Google Patents
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Abstract
The invention discloses a graphene film-iron alloy composite material and a preparation method thereof. The composite material comprises a graphene film layer and an iron alloy layer, the volume fraction of the graphene film is 35-68%, the graphene film-iron alloy composite material has the bending strength of 347-504MPa, the Brinell hardness of more than 45HB, the thermal conductivity of 374-530W/(m.K), and the thermal expansion coefficient of (5.9-7.5) multiplied by 10‑6K; the iron alloy layer contains 0.05-0.3% of vanadium, 0.3-0.9% of titanium and 0.2-1% of zinc by mass. The heat management material provided by the invention has high heat conductivity, high strength and low expansion coefficient.
Description
Technical Field
The invention belongs to the field of composite materials with ferroalloy as a matrix, and particularly relates to a graphene film-ferroalloy composite material and a preparation method thereof.
Background
With the continuous development of the electronic industry technology, the design and production of electronic components are continuously developing towards miniaturization, integration, lightweight and high efficiency, so that the heat density of the electronic components in the working process is continuously increased, and higher requirements on the heat conductivity, strength and expansion performance of the used heat management material are provided.
In the existing heat management materials, the W/Si, Mo/Si and SiC/Al composite materials have good heat conduction and thermal expansion properties, but the density is high and the heat conduction property can not meet the requirements of the electronic industry which develops at a high speed. The thermal conductivity of the diamond/Al composite material can reach 500-600W/(m.K), but the volume fraction of diamond generally reaches about 60 percent, and the diamond has high hardness and high price, so that the material is difficult to process and has high cost. The graphite sheet/Al composite material has good processing performance, and when the volume fraction reaches 80-90%, the in-plane thermal conductivity can reach 600-. However, the volume fraction is too high, so that the preparation of the material is difficult and the mechanical properties of the material are low. For the heat dissipation material applied to the IGBT, it is necessary to simultaneously consider the thermal conductivity, mechanical strength, and thermal expansion performance. Therefore, there is an urgent need for more suitable reinforcement materials for metal matrix composites for thermal management. The in-plane thermal conductivity of the artificially synthesized graphene film can reach up to 1200-1900W/(m.K), and the method has been commercialized and successfully applied to heat dissipation of mobile phones and computers.
However, in the existing thermal management material, the graphene film does not react with metals such as aluminum and copper, the interface bonding force is poor, the graphene film is not easy to form a whole and is easy to delaminate, and the thermal conductivity is low. In addition, the bending strength of the material can not reach more than 350MPa required by the IGBT, so that the heat dissipation assembly is subjected to fatigue fracture. It is therefore necessary to develop high strength thermal management materials.
Disclosure of Invention
Aiming at the defects or improvement requirements of the prior art, the invention provides a graphene film-iron alloy composite material and a preparation method thereof, aiming at adopting iron alloy and graphene film for compounding, thereby enhancing the mechanical property and meeting the requirements of IGBT while ensuring the thermal conductivity of the material, and thus solving the technical problems of poor interface bonding force, easy delamination and poor strength and hardness of the existing thermal management material.
In order to achieve the above object, according to one aspect of the present invention, there is provided a graphene film-iron alloy composite material comprising a graphene film layer and an iron alloy layer, wherein the graphene film has a volume fraction of 35 to 68%, the graphene film-iron alloy composite material has a bending strength of 347--6K; the iron alloy layer contains 0.05-0.3% of vanadium, 0.3-0.9% of titanium and 0.2-1% of zinc by mass.
Preferably, the graphene film-iron alloy composite material comprises 28-39% of nickel, 0.02-0.03% of carbon, 0.1-0.7% of chromium and 0.4-1% of silicon in percentage by mass.
Preferably, the graphene film-iron alloy composite material has an iron alloy melting point of 1050-1230 ℃.
Preferably, in the graphene film-iron alloy composite material, titanium in the iron alloy layer is covalently bonded with carbon element on the surface of the graphene film to form titanium carbide.
Preferably, the graphene film layer of the graphene film-iron alloy composite material has a thickness of 30-50 μm and an in-plane thermal conductivity of 1200-1900W/(m.K).
Preferably, the graphene film-iron alloy composite material, the iron alloy layer thereof, has a thickness of 30 to 200 μm.
According to another aspect of the present invention, there is provided a method for preparing the graphene film-iron alloy composite material, comprising the steps of:
(1) pretreatment of raw materials: cleaning and drying the surface of the graphene film for later use; uniformly mixing the iron alloy powder materials prepared according to the formula table for later use;
(2) stacking the iron alloy powder and the graphene film layer by layer in a mould to a required thickness of 1 × 10-2The graphene film-iron alloy is prepared by vacuum hot pressing processing in a vacuum environment with more than PaA gold composite material.
Preferably, in the preparation method of the graphene film-iron alloy composite material, in the step (1), the surface of the graphene film is cleaned and dried for standby application, and the specific method is that the graphene film is ultrasonically cleaned for several times by acetone so as to remove oil stains or dirt on the surface of the graphene film.
Preferably, in the preparation method of the graphene film-iron alloy composite material, in the step (1), the graphene film is provided with uniform through holes, the aperture is between 1 and 3mm, and the distance between two adjacent circle centers is between 4 and 10 mm.
Preferably, in the preparation method of the graphene film-iron alloy composite material, the vacuum hot-pressing conditions in step (2) are as follows: the hot pressing temperature is 1050 ℃ and 1230 ℃; the hot pressing pressure is 40-80 MPa; the hot pressing pressure maintaining time is 0.5-3 hours.
In general, compared with the prior art, the technical scheme of the invention reduces the melting point of the alloy due to the addition of elements such as zinc, titanium, vanadium and the like, so that the preparation is easier; in addition, various elements can well react with graphite, so that the binding force of the graphene film and iron is improved, and the low-temperature fluidity is enhanced; in addition, the graphene film is drilled, and ferroalloy powder is filled in the graphene film, so that the two materials are better combined, and the hardness and the bending strength of the composite material are improved. The heat management material provided by the invention has high heat conductivity, high strength and low expansion coefficient.
Drawings
Fig. 1 is a flow chart of a method for preparing a graphene film-iron alloy composite material according to the present invention;
fig. 2 is a longitudinal-sectional electron microscope image of the graphene film-iron alloy composite material in example 2 of the present invention;
fig. 3 is a cross-sectional electron microscope image of the graphene film-iron alloy composite material in example 2 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The graphene film-iron alloy composite material provided by the invention has a layered structure and comprises a graphene film layer and an iron alloy layer, wherein the volume fraction of the graphene film is 35-68%;
the graphene film layer has the thickness of 30-50 mu m and the in-plane thermal conductivity of 1200-1900W/(m.K);
the iron alloy layer contains 0.05-0.3% by mass of vanadium (V), 0.3-0.9% by mass of titanium (Ti), and 0.2-1% by mass of zinc (Zn). The iron alloy has better fluidity at the melting point of 1050-. Although the machinability of iron is stronger than the metal base of the thermal management materials commonly used, such as silicon, aluminum. However, although the thermal conductivity of iron is relatively common and can be improved by compounding with a graphene film, this also means that the ratio of the graphene film increases, the difficulty of compounding increases, and the improvement of the overall machinability is not desirable. Therefore, the ferroalloy is adopted to balance various properties of the metal base of the thermal management material, so that the wettability and the interface bonding strength of the graphene film and the metal base are improved, and the mechanical processing property and the thermal property of the thermal management material meet the requirements. The preferred embodiment of the metal-based iron alloy used as the heat management material should also have a lower melting point and better processability, thereby reducing the energy consumption in the production process and the requirements on production equipment.
Titanium in the iron alloy layer and carbon elements on the surface of the graphene film are combined into a form of titanium carbide through covalent bonds.
Preferably, the iron alloy contains 28 to 39 mass% of nickel (Ni), 0.02 to 0.03 mass% of carbon (C), 0.1 to 0.7 mass% of chromium (Cr), and 0.4 to 1 mass% of silicon (Si).
Nickel can improve the strength of iron alloy and maintain good plasticity and toughnessThe composite material has better processing performance due to the covalent bonding mode; the nickel has higher corrosion resistance to acid and alkali, has antirust and heat-resistant capabilities at high temperature, and reduces the oxidation loss of the graphene film layer in the metal compounding process; the chromium reacts with carbon element on the surface of the graphene film at high temperature to generate chromium carbide (Cr)3C2) The existence of the covalent bond enables the two to be combined more tightly, and meanwhile, the strength, the hardness and the wear resistance can be obviously improved, so that the composite material is helped to obtain good processing performance; the silicon can obviously improve the elastic limit, yield point and tensile strength of the iron alloy and can react with carbon elements on the surface of the graphene film at high temperature to form silicon carbide (SiC), and the silicon carbide and the SiC exist in a covalent bond form to improve the interface bonding force.
The graphene film-iron alloy composite material has bending strength of 347-504MPa, Brinell hardness of more than 45HB, thermal conductivity of 530W/(m.K), and thermal expansion coefficient of (5.9-7.5) multiplied by 10-6and/K is between.
The preparation method of the graphene film-iron alloy composite material provided by the invention comprises the following steps:
(1) pretreatment of raw materials: cleaning and drying the surface of the graphene film for later use, wherein the specific method is that the graphene film is ultrasonically cleaned for a plurality of times by acetone so as to remove oil stains or dirt on the surface of the graphene film; and uniformly mixing the iron alloy powder materials prepared according to the formula table for later use.
Preferably, the graphene film is provided with uniform through holes, the aperture is between 1 and 3mm, and the distance between two adjacent circle centers is between 4 and 10 mm.
(2) Stacking the iron alloy powder and the graphene film layer by layer in a mould to a required thickness of 1 × 10-2The graphene film-iron alloy composite material is prepared by vacuum hot pressing processing in a vacuum environment with the pressure of Pa above; the hot pressing temperature is 1050 ℃ and 1230 ℃; the hot pressing pressure is 40-80 MPa; the hot pressing pressure maintaining time is 0.5-3 hours.
The following are examples:
example 1
The graphene film-iron alloy composite material provided by the invention has a layered structure and comprises a graphene film layer and an iron alloy layer, wherein the volume fraction of the graphene film is 35%;
the graphene film layer has a thickness of 30 mu m and an in-plane thermal conductivity of 1900W/(m.K);
the thickness of the iron alloy layer is 200 mu m, and the component proportion (mass fraction) is as follows:
0.3% of vanadium (V), 0.5% of titanium (Ti), and 0.2% of zinc (Zn), 34% of nickel (Ni), 0.02% of carbon (C), 0.7% of chromium (Cr), and 0.4% of silicon (Si), with the remainder being iron (Fe).
The graphene film-iron alloy composite material is prepared by the following method:
(1) pretreatment of raw materials: cleaning and drying the surface of the graphene film for later use, wherein the specific method is that the graphene film is ultrasonically cleaned for a plurality of times by acetone so as to remove oil stains or dirt on the surface of the graphene film; and uniformly mixing the iron alloy powder materials prepared according to the formula table for later use.
(2) Drilling 60 holes with the diameter of 2mm on the graphene film at equal intervals, stacking the iron alloy powder and the graphene film layer by layer in a mould to the thickness of 12mm, and performing vacuum hot-pressing processing to prepare the graphene film-iron alloy composite material; the hot pressing temperature is 1160 ℃; the hot pressing pressure is 40 MPa; the hot pressing dwell time was 0.5 hour.
The graphene film-iron alloy composite material has bending strength 468MPa and Brinell hardness 48HB as determined by a universal tester, the thermal conductivity 374W/(m.K) of the graphene film-iron alloy composite material is determined by NEZSCH LFA 467, and the thermal expansion coefficient is 5.9 multiplied by 10-6/K。
Example 2
The graphene film-iron alloy composite material provided by the invention has a layered structure and comprises a graphene film layer and an iron alloy layer, wherein the volume fraction of the graphene film is 50%;
the graphene film layer has the thickness of 40 mu m and the in-plane thermal conductivity of 1500W/(m.K);
the thickness of the iron alloy layer is 50 μm, and the component ratio (mass fraction) is as follows:
0.1% vanadium (V), 0.9% titanium (Ti), and 0.7% zinc (Zn), 28% nickel (Ni), 0.025% carbon (C), 0.4% chromium (Cr), and 1% silicon (Si), with the remainder being iron (Fe). The ingredients are present in powder form.
The graphene film-iron alloy composite material is prepared by the following method:
(1) pretreatment of raw materials: cleaning and drying the surface of the graphene film for later use, wherein the specific method is that the graphene film is ultrasonically cleaned for a plurality of times by acetone so as to remove oil stains or dirt on the surface of the graphene film; and uniformly mixing the iron alloy powder materials prepared according to the formula table for later use.
(2) Drilling 50 holes with the diameter of 2mm in a graphene film at equal intervals, stacking the ferroalloy powder and the graphene film layer by layer in a mould until the thickness is 12mm, and performing vacuum hot-pressing processing to obtain the graphene film-ferroalloy composite material; the hot pressing temperature is 1050 ℃; the hot pressing pressure is 80 MPa; the hot pressing dwell time was 3 hours.
The graphene film-iron alloy composite material has bending strength of 347MPa and Brinell hardness of 46HB as determined by a universal tester, the thermal conductivity of 434W/(m.K) of the graphene film-iron alloy composite material is determined by NEZSCH LFA 467, and the thermal expansion coefficient is 6.3 multiplied by 10-6/K。
Example 3
The graphene film-iron alloy composite material provided by the invention has a layered structure and comprises a graphene film layer and an iron alloy layer, wherein the volume fraction of the graphene film is 68%;
the graphene film layer has the thickness of 50 mu m and the in-plane thermal conductivity of 1200W/(m.K);
the thickness of the iron alloy layer is 120 mu m, and the component proportion (mass fraction) is as follows:
0.05% of vanadium (V), 0.5% of titanium (Ti), and 1% of zinc (Zn), 39% of nickel (Ni), 0.03% of carbon (C), 0.1% of chromium (Cr), and 0.6% of silicon (Si), with the remainder being iron (Fe). The ingredients are present in powder form.
The graphene film-iron alloy composite material is prepared by the following method:
(1) pretreatment of raw materials: cleaning and drying the surface of the graphene film for later use, wherein the specific method is that the graphene film is ultrasonically cleaned for a plurality of times by acetone so as to remove oil stains or dirt on the surface of the graphene film; and uniformly mixing the iron alloy powder materials prepared according to the formula table for later use.
(2) Drilling 40 holes with the diameter of 2mm on the graphene film at equal intervals, then stacking the iron alloy powder and the graphene film layer by layer in a mould to the thickness of 12mm, and carrying out vacuum hot-pressing processing to prepare the graphene film-iron alloy composite material; the hot pressing temperature is 1230 ℃; the hot pressing pressure is 50 MPa; the hot pressing dwell time was 1 hour.
The graphene film-iron alloy composite material has the bending strength of 388MPa and the Brinell hardness of 47HB determined by a universal tester, the thermal conductivity 466W/(m.K) of the graphene film-iron alloy composite material is determined by NEZSCH LFA 467, and the thermal expansion coefficient is 7.5 multiplied by 10-6/K。
Example 4
The graphene film-iron alloy composite material provided by the invention has a layered structure and comprises a graphene film layer and an iron alloy layer, wherein the volume fraction of the graphene film is 68%;
the graphene film layer has the thickness of 40 mu m and the in-plane thermal conductivity of 1500W/(m.K);
the thickness of the iron alloy layer is 80 μm, and the component ratio (mass fraction) is as follows:
0.3% of vanadium (V), 0.9% of titanium (Ti), and 0.7% of zinc (Zn), 34% of nickel (Ni), 0.02% of carbon (C), 0.4% of chromium (Cr), and 0.6% of silicon (Si), with the remainder being iron (Fe). The ingredients are present in powder form.
The graphene film-iron alloy composite material is prepared by the following method:
(1) pretreatment of raw materials: cleaning and drying the surface of the graphene film for later use, wherein the specific method is that the graphene film is ultrasonically cleaned for a plurality of times by acetone so as to remove oil stains or dirt on the surface of the graphene film; and uniformly mixing the iron alloy powder materials prepared according to the formula table for later use.
(2) Drilling 40 holes with the diameter of 2mm on the graphene film at equal intervals, then stacking the iron alloy powder and the graphene film layer by layer in a mould to the thickness of 12mm, and carrying out vacuum hot-pressing processing to prepare the graphene film-iron alloy composite material; the hot pressing temperature is 1160 ℃; the hot pressing pressure is 80 MPa; the hot pressing dwell time was 3 hours.
The graphene film-iron alloy composite material has the bending strength of 504MPa and the Brinell hardness of 50HB measured by a universal tester, the thermal conductivity of 530W/(m.K) of the graphene film-iron alloy composite material is measured by NEZSCH LFA 467, and the thermal expansion coefficient is 6.3 multiplied by 10-6/K。
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (8)
1. The graphene film-iron alloy composite material is characterized by comprising a graphene film layer and an iron alloy layer, wherein the volume fraction of a graphene film is 35-68%, the graphene film-iron alloy composite material has the bending strength of 347-504MPa, the Brinell hardness of more than 45HB, the thermal conductivity of 374-530W/(m.K), and the thermal expansion coefficient of (5.9-7.5) multiplied by 10-6K; the iron alloy layer contains 0.05-0.3% of vanadium, 0.3-0.9% of titanium and 0.2-1% of zinc by mass; the iron alloy contains 28-39% of nickel, 0.02-0.03% of carbon, 0.1-0.7% of chromium and 0.4-1% of silicon by mass; the graphene film is provided with uniform through holes, the aperture is between 1 mm and 3mm, and the distance between two adjacent circle centers is between 4 mm and 10 mm.
2. The graphene film-iron alloy composite material of claim 1, wherein the iron alloy melting point is 1050-1230 ℃.
3. The graphene film-iron alloy composite material of claim 1, wherein the titanium in the iron alloy layer is covalently bonded to the carbon element on the surface of the graphene film in the form of titanium carbide.
4. The graphene film-iron alloy composite material of claim 1, wherein the graphene film layer has a thickness of 30-50 μm and an in-plane thermal conductivity of 1200-1900W/(m-K).
5. The graphene film-iron alloy composite of claim 1, wherein the iron alloy layer has a thickness of 30-200 μ ι η.
6. The method for preparing the graphene film-iron alloy composite material according to any one of claims 1 to 5, comprising the steps of:
(1) pretreatment of raw materials: cleaning and drying the surface of the graphene film for later use; uniformly mixing the iron alloy powder materials prepared according to the formula table for later use;
(2) stacking the iron alloy powder and the graphene film layer by layer in a mould to a required thickness of 1 × 10-2And (3) preparing the graphene film-iron alloy composite material by vacuum hot pressing in a vacuum environment with the pressure of Pa above.
7. The preparation method of the graphene film-iron alloy composite material of claim 6, wherein the graphene film surface is cleaned and dried for later use in step (1), and the method comprises ultrasonically cleaning the graphene film with acetone for several times to remove oil stains or dirt on the graphene film surface.
8. The method for preparing the graphene film-iron alloy composite material according to claim 5, wherein the vacuum hot-pressing conditions in the step (2) are as follows: the hot pressing temperature is 1050 ℃ and 1230 ℃; the hot pressing pressure is 40-80 MPa; the hot pressing pressure maintaining time is 0.5-3 hours.
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| JP2008162036A (en) * | 2006-12-27 | 2008-07-17 | Toyota Motor Corp | Iron based composite material and method for producing iron based composite material |
| CN101445385A (en) * | 2007-11-26 | 2009-06-03 | 仕钦科技企业股份有限公司 | Method for combing graphite plate with metal |
| CN104647830A (en) * | 2015-01-30 | 2015-05-27 | 上海交通大学 | High-heat-conductivity graphite film metal block composite material and preparation method of composite material |
| CN105251993A (en) * | 2015-09-21 | 2016-01-20 | 清华大学 | Method for preparing Fe-graphene particles with assistance of graphene oxide |
| CN106916985A (en) * | 2015-12-28 | 2017-07-04 | 北京有色金属研究总院 | The preparation method of high heat conduction graphite/aluminium composite material |
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| CN106079693A (en) * | 2016-06-21 | 2016-11-09 | 上海多希石墨烯材料科技有限公司 | A kind of Graphene metal composite sheet material and preparation method thereof |
| CN107215058A (en) * | 2017-05-04 | 2017-09-29 | 林俊宝 | A kind of conductive graphite aluminium base and preparation method thereof |
| CN109112504A (en) * | 2017-06-26 | 2019-01-01 | 中国科学院宁波材料技术与工程研究所 | A kind of graphene/copper composite material and its preparation and application |
| CN108149051A (en) * | 2017-12-04 | 2018-06-12 | 中国科学院电工研究所 | A kind of graphene/metallic composite and preparation method thereof |
| CN108531769A (en) * | 2018-04-16 | 2018-09-14 | 厦门奈福电子有限公司 | A kind of graphene-metallic composite and its prepare raw material, method and application |
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