CN110293229A - A kind of graphene film-ferroalloy composite material and preparation method - Google Patents
A kind of graphene film-ferroalloy composite material and preparation method Download PDFInfo
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
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- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
- B22F7/04—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
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- C—CHEMISTRY; METALLURGY
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/46—Ferrous alloys, e.g. steel alloys containing chromium with nickel with vanadium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/50—Ferrous alloys, e.g. steel alloys containing chromium with nickel with titanium or zirconium
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Abstract
The invention discloses a kind of graphene film-ferroalloy composite material and preparation methods.The composite material includes graphene film layer and iron alloy layer, the volume fraction of graphene film is 35-68%, the graphene film-ferroalloy composite material, bending strength is 347-504MPa, Brinell hardness is in 45HB or more, for thermal conductivity at 374-530W/ (mK), thermal expansion coefficient is (5.9-7.5) × 10‑6/K；The iron alloy layer contains mass fraction vanadium 0.05-0.3%, titanium 0.3-0.9% and zinc 0.2-1%.Thermal management materials provided by the invention have high heat conductance, high intensity and low-expansion coefficient.
Description
Technical field
The invention belongs to the field of compound material that ferroalloy is matrix, more particularly, to a kind of graphene film-ferroalloy
Composite material and preparation method.
Background technique
With the continuous development of electronic industrial technology, the design of electronic component and production constantly to miniaturization, it is integrated,
Lightweight, efficient direction are developed, and cause its course of work heat density constantly to increase, this is just to used thermal management materials
Thermal conductivity, intensity and expansion character more stringent requirements are proposed.
In existing thermal management materials, although W/Si, Mo/Si and SiC/Al composite material have good thermally conductive and heat swollen
Swollen performance, but its density is high and heating conduction be no longer satisfied high speed development electronics industry requirement.Diamond/Al is compound
The thermal conductivity of material can reach 500-600W/ (mK), but the volume fraction of diamond commonly reaches 60% or so at this time, due to
Diamond hardness is big and high price is expensive, this is difficult to this kind of material and at high cost.Graphite flake/Al composite processing
Can be preferable, and when volume fraction reaches 80-90%, thermal conductivity can reach 600-783W/ (mK) in face.But due to body
Fraction is excessively high, so as to become very difficult and material mechanical property lower for material preparation.For the heat dissipation for being applied to IGBT
For material, need to combine its thermal conductivity, mechanical strength and hot expansibility.Therefore, heat management metal-based compound
Material is badly in need of more suitable reinforcement material.Thermal conductivity may be up to 1200-1900W/ (mK) in artificial synthesized graphite alkene film surface,
And have been carried out the heat dissipation for being commercialized and being successfully applied to mobile phone and computer.
However in existing thermal management materials, graphene film is not reacted with metals such as aluminium, copper, and interface binding power is poor, no
It easily forms an entirety and is easy layering, cause thermal conductivity not high.In addition, the bending strength performance of material is unable to reach IGBT requirement
350MPa or more, lead to radiating subassembly fatigue fracture.It is therefore desirable to develop high-intensitive thermal management materials.
Summary of the invention
Aiming at the above defects or improvement requirements of the prior art, the present invention provides a kind of graphene film-ferroalloy is compound
Material and preparation method thereof, its object is to compound using ferroalloy and graphene film, thus guaranteeing the thermal conductivity of material
Meanwhile reinforcing mechanical performance, meet the requirement of IGBT, thus solves the poor easy layering of existing thermal management materials interface binding power
The technical issues of with intensity, difference of hardness.
To achieve the above object, according to one aspect of the present invention, a kind of graphene film-ferroalloy composite wood is provided
Material comprising graphene film layer and iron alloy layer, the volume fraction of graphene film are 35-68%, the graphene film-ferroalloy
Composite material, bending strength 347-504MPa, Brinell hardness is in 45HB or more, and thermal conductivity is up to 530W/ (mK), thermal expansion
Coefficient is (5.9-7.5) × 10-6/K；The iron alloy layer, containing mass fraction vanadium 0.05-0.3%, titanium 0.3-0.9%, with
And zinc 0.2-1%.
Preferably, the graphene film-ferroalloy composite material, the ferroalloy contain mass fraction nickel 28-39%,
Carbon 0.02-0.03%, chromium 0.1-0.7% and silicon 0.4-1%.
Preferably, the graphene film-ferroalloy composite material, the ferroalloy fusing point is at 1050-1230 DEG C.
Preferably, the graphene film-ferroalloy composite material, titanium and graphene membrane surface carbon member in the iron alloy layer
Element is in the form of covalently bonded synthesizes titanium carbide.
Preferably, the graphene film-ferroalloy composite material, the graphene film layer, thickness is at 30-50 μm, face
Interior thermal conductivity is 1200-1900W/ (mK).
Preferably, the graphene film-ferroalloy composite material, the iron alloy layer, thickness is at 30-200 μm.
Other side according to the invention provides a kind of preparation side of the graphene film-ferroalloy composite material
Method comprising following steps:
(1) graphene membrane surface pretreatment of raw material: is cleaned up into dried for standby；It will be according to iron made from formula table
Alloy powder material is stand-by after mixing；
(2) ferroalloy powder and graphene film are successively stacked to required thickness in a mold, 1 × 10-2Pa with
On vacuum environment under through vacuum hotpressing be processed into the graphene film-ferroalloy composite material.
Preferably, the graphene film-ferroalloy composite material preparation method, step (1) are described by graphene film
Surface clean is clean and dry stand-by, and specific method is that graphene film acetone is cleaned by ultrasonic for several times, to remove graphene film table
The greasy dirt in face is dirty.
Preferably, the graphene film-ferroalloy composite material preparation method, step (1) the graphene film tool
There is uniform through bore, aperture is 1 between 3mm, and the spacing in adjacent two center of circle is between 4-10mm.
Preferably, the graphene film-ferroalloy composite material preparation method, step (2) the Vacuum Heat press strip
Part is as follows: 1050-1230 DEG C of hot pressing temperature；Hot pressing pressure is 40-80MPa；The hot pressing dwell time is 0.5-3 hours.
In general, through the invention it is contemplated above technical scheme is compared with the prior art, due to zinc, titanium, vanadium etc.
The addition of element reduces the fusing point of alloy, is more easier preparation；In addition, the addition of various elements can be very good and stone
Ink reaction, improves the binding force of graphene film and iron, enhances low temperature flow；Also, graphene film drills, and allows ferroalloy
Powder is filled wherein, combines two kinds of materials more preferable, while also improving the hardness and bending strength of composite material.The present invention mentions
The thermal management materials of confession have high heat conductance, high intensity, low-expansion coefficient.
Detailed description of the invention
Fig. 1 is graphene film provided by the invention-ferroalloy composite material preparation method flow chart；
Fig. 2 is graphene film-ferroalloy composite material longitudal section electron microscope picture in the embodiment of the present invention 2；
Fig. 3 is graphene film-ferroalloy composite material cross section electron microscope picture in the embodiment of the present invention 2.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below each other it
Between do not constitute conflict and can be combined with each other.
Graphene film provided by the invention-ferroalloy composite material has layer structure, including graphene film layer and iron close
Layer gold, the volume fraction of graphene film are 35-68%；
The graphene film layer, thickness thermal conductivity in 30-50 μm, face is 1200-1900W/ (mK)；
Iron alloy layer contains mass fraction vanadium (V) 0.05-0.3%, titanium (Ti) 0.3-0.9% and zinc (Zn) 0.2-
1%.The ferroalloy, at 1050-1230 DEG C, has preferable flowing at 1050-1100 DEG C of lower temperature range in fusing point
Property, graphene film compound tense can form stable and firm binding force under lower processing temperature, to improve whole stone
The machining property of black alkene film-ferroalloy composite material, thickness is at 30-200 μm.Although the machining property of iron is better than
Commonly used thermal management materials Metal Substrate, such as silicon, aluminium.However the thermal conductivity of iron is more common, although can by with graphite
Alkene film is compound so as to improve thermal conductivity, but also implies that graphene film accounting rises in this way, and compound difficulty increases, whole machine
Tool processing performance improves undesirable.Therefore thermal management materials Metal Substrate properties are balanced using ferroalloy, to improve graphite
The wellability of alkene film and Metal Substrate, interface cohesion dynamics, so that the machining property of thermal management materials and hot be able to satisfy are wanted
It asks.The ferroalloy as thermal management materials Metal Substrate of preferred embodiment, should also have lower fusing point and preferable processability
Can, to reduce the energy consumption in production process and the requirement to production equipment.
Titanium is with graphene membrane surface carbon in the form of covalently bonded synthesizes titanium carbide in the iron alloy layer.
Preferred embodiment, the ferroalloy contain mass fraction nickel (Ni) 28-39%, carbon (C) 0.02-0.03%, chromium (Cr)
0.1-0.7% and silicon (Si) 0.4-1%.
Nickel can improve the intensity of ferroalloy, and keep good plasticity and toughness, be made by way of covalent bonding
Composite material has preferable processing performance；Nickel has higher corrosion resistance to soda acid, there is antirust and resistance to thermal energy at high temperature
Power reduces oxidation loss of the graphene film layer in metal composite process；Chromium is anti-with graphene membrane surface carbon at high temperature
Chromium carbide (Cr should be generated3C2), the presence of covalent bond both makes to combine closer, while can also significantly improve intensity, hardness and resistance to
Mill property helps composite material to obtain good processing performance；Silicon can significantly improve the elastic limit of ferroalloy, yield point and tension
Intensity simultaneously can react to form silicon carbide (SiC) with graphene membrane surface carbon at high temperature, and the two exists in the form of covalent bond
Improve interface binding power.
The graphene film-ferroalloy composite material, bending strength 347-504MPa, Brinell hardness 45HB or more, thermal conductivity
Rate reaches 530W/ (mK), and thermal expansion coefficient is at (5.9-7.5) × 10-6Between/K.
Graphene film provided by the invention-ferroalloy composite material preparation method, comprising the following steps:
(1) pretreatment of raw material: the graphene membrane surface is cleaned up into dried for standby, specific method is by graphene film
For several times with acetone ultrasonic cleaning, to remove the greasy dirt of graphene membrane surface or dirty；It will be according to iron alloy powder made from formula table
Powder material mixing is stand-by after having.
Preferably, the graphene film has uniform through bore, and aperture is 1 between 3mm, and the spacing in adjacent two center of circle is in 4-
Between 10mm.
(2) ferroalloy powder and graphene film are successively stacked to required thickness in a mold, 1 × 10-2Pa with
On vacuum environment under through vacuum hotpressing be processed into the graphene film-ferroalloy composite material；Hot pressing temperature 1050-1230
℃；Hot pressing pressure is 40-80MPa；The hot pressing dwell time is 0.5-3 hours.
The following are embodiments:
Embodiment 1
Graphene film provided by the invention-ferroalloy composite material has layer structure, including graphene film layer and iron close
Layer gold, the volume fraction of graphene film are 35%；
The graphene film layer, thickness is at 30 μm, and thermal conductivity is 1900W/ (mK) in face；
For its thickness of the iron alloy layer at 200 μm, composition proportion (mass fraction) is as follows:
Vanadium (V) 0.3%, titanium (Ti) 0.5% and zinc (Zn) 0.2%, nickel (Ni) 34%, carbon (C) 0.02%, chromium (Cr)
0.7% and silicon (Si) 0.4%, remaining as iron (Fe).
The graphene film-ferroalloy composite material is prepared as follows:
(1) pretreatment of raw material: the graphene membrane surface is cleaned up into dried for standby, specific method is by graphene film
For several times with acetone ultrasonic cleaning, to remove the greasy dirt of graphene membrane surface or dirty；It will be according to iron alloy powder made from formula table
Powder material is stand-by after mixing.
(2) graphene film is bored to the hole that 60 diameters are 2mm at equal intervals, then by the ferroalloy powder and graphene
Film is successively stacked to thickness 12mm in a mold, is processed into the graphene film-ferroalloy composite material through vacuum hotpressing；Heat
1160 DEG C of temperature of pressure；Hot pressing pressure is 40MPa；The hot pressing dwell time is 0.5 hour.
It is measured by universal testing machine, the graphene film-ferroalloy composite material bending strength 468MPa, Brinell hardness is
48HB measures the graphene film-ferroalloy heat conductivity 374W/ (mK) through NEZSCH LFA 467, thermal expansion
Coefficient is 5.9 × 10-6/K。
Embodiment 2
Graphene film provided by the invention-ferroalloy composite material has layer structure, including graphene film layer and iron close
Layer gold, the volume fraction of graphene film are 50%；
The graphene film layer, thickness is at 40 μm, and thermal conductivity is 1500W/ (mK) in face；
For its thickness of the iron alloy layer at 50 μm, composition proportion (mass fraction) is as follows:
Vanadium (V) 0.1%, titanium (Ti) 0.9% and zinc (Zn) 0.7%, nickel (Ni) 28%, carbon (C) 0.025%, chromium (Cr)
0.4% and silicon (Si) 1%, remaining as iron (Fe).Various composition exists in the form of a powder.
The graphene film-ferroalloy composite material is prepared as follows:
(1) pretreatment of raw material: the graphene membrane surface is cleaned up into dried for standby, specific method is by graphene film
For several times with acetone ultrasonic cleaning, to remove the greasy dirt of graphene membrane surface or dirty；It will be according to iron alloy powder made from formula table
Powder material is stand-by after mixing.
(2) graphene film is bored to the hole that 50 diameters are 2mm at equal intervals, the ferroalloy is then added into powder and graphite
Alkene film is successively stacked to thickness 12mm in a mold, is processed into the graphene film-ferroalloy composite material through vacuum hotpressing；
1050 DEG C of hot pressing temperature；Hot pressing pressure is 80MPa；The hot pressing dwell time is 3 hours.
It is measured by universal testing machine, the graphene film-ferroalloy composite material bending strength 347MPa, Brinell hardness is
46HB measures the graphene film-ferroalloy heat conductivity 434W/ (mK) through NEZSCH LFA 467, thermal expansion
Coefficient is 6.3 × 10-6/K。
Embodiment 3
Graphene film provided by the invention-ferroalloy composite material has layer structure, including graphene film layer and iron close
Layer gold, the volume fraction of graphene film are 68%；
The graphene film layer, thickness is at 50 μm, and thermal conductivity is 1200W/ (mK) in face；
For its thickness of the iron alloy layer at 120 μm, composition proportion (mass fraction) is as follows:
Vanadium (V) 0.05%, titanium (Ti) 0.5% and zinc (Zn) 1%, nickel (Ni) 39%, carbon (C) 0.03%, chromium (Cr)
0.1% and silicon (Si) 0.6%, remaining as iron (Fe).Various composition exists in the form of a powder.
The graphene film-ferroalloy composite material is prepared as follows:
(1) pretreatment of raw material: the graphene membrane surface is cleaned up into dried for standby, specific method is by graphene film
For several times with acetone ultrasonic cleaning, to remove the greasy dirt of graphene membrane surface or dirty；It will be according to iron alloy powder made from formula table
Powder material is stand-by after mixing.
(2) graphene film is bored to the hole that 40 diameters are 2mm at equal intervals, then by the ferroalloy powder and graphene
Film is successively stacked to thickness 12mm in a mold, is processed into the graphene film-ferroalloy composite material through vacuum hotpressing；Heat
1230 DEG C of temperature of pressure；Hot pressing pressure is 50MPa；The hot pressing dwell time is 1 hour.
It is measured by universal testing machine, the graphene film-ferroalloy composite material bending strength 388MPa, Brinell hardness is
47HB measures the graphene film-ferroalloy heat conductivity 466W/ (mK) through NEZSCH LFA 467, thermal expansion
Coefficient is 7.5 × 10-6/K。
Embodiment 4
Graphene film provided by the invention-ferroalloy composite material has layer structure, including graphene film layer and iron close
Layer gold, the volume fraction of graphene film are 68%；
The graphene film layer, thickness is at 40 μm, and thermal conductivity is 1500W/ (mK) in face；
For its thickness of the iron alloy layer at 80 μm, composition proportion (mass fraction) is as follows:
Vanadium (V) 0.3%, titanium (Ti) 0.9% and zinc (Zn) 0.7%, nickel (Ni) 34%, carbon (C) 0.02%, chromium (Cr)
0.4% and silicon (Si) 0.6%, remaining as iron (Fe).Various composition exists in the form of a powder.
The graphene film-ferroalloy composite material is prepared as follows:
(1) pretreatment of raw material: the graphene membrane surface is cleaned up into dried for standby, specific method is by graphene film
For several times with acetone ultrasonic cleaning, to remove the greasy dirt of graphene membrane surface or dirty；It will be according to iron alloy powder made from formula table
Powder material is stand-by after mixing.
(2) graphene film is bored to the hole that 40 diameters are 2mm at equal intervals, then by the ferroalloy powder and graphene
Film is successively stacked to thickness 12mm in a mold, is processed into the graphene film-ferroalloy composite material through vacuum hotpressing；Heat
1160 DEG C of temperature of pressure；Hot pressing pressure is 80MPa；The hot pressing dwell time is 3 hours.
It is measured by universal testing machine, the graphene film-ferroalloy composite material bending strength 504MPa, Brinell hardness is
50HB measures the graphene film-ferroalloy heat conductivity 530W/ (mK) through NEZSCH LFA 467, thermal expansion
Coefficient is 6.3 × 10-6/K。
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all include
Within protection scope of the present invention.
Claims (10)
1. a kind of graphene film-ferroalloy composite material, which is characterized in that including graphene film layer and iron alloy layer, graphene
The volume fraction of film is 35-68%, and the graphene film-ferroalloy composite material, bending strength 347-504MPa, Bu Shi be hard
Degree is in 45HB or more, and for thermal conductivity at 374-530W/ (mK), thermal expansion coefficient is (5.9-7.5) × 10-6/K；The ferroalloy
Layer, contains mass fraction vanadium 0.05-0.3%, titanium 0.3-0.9% and zinc 0.2-1%.
2. graphene film as described in claim 1-ferroalloy composite material, which is characterized in that the ferroalloy contains quality
Score nickel 28-39%, carbon 0.02-0.03%, chromium 0.1-0.7% and silicon 0.4-1%.
3. graphene film as described in claim 1-ferroalloy composite material, which is characterized in that the ferroalloy fusing point exists
1050-1230℃。
4. graphene film as described in claim 1-ferroalloy composite material, which is characterized in that in the iron alloy layer titanium with
Graphene membrane surface carbon is in the form of covalently bonded synthesizes titanium carbide.
5. graphene film as described in claim 1-ferroalloy composite material, which is characterized in that the graphene film layer, thickness
Thermal conductivity is 1200-1900W/ (mK) in 30-50 μm, face.
6. graphene film as described in claim 1-ferroalloy composite material, which is characterized in that the iron alloy layer, thickness
At 30-200 μm.
7. graphene film-ferroalloy composite material preparation method as described in claim 1 to 6 any one, feature exist
In the following steps are included:
(1) graphene membrane surface pretreatment of raw material: is cleaned up into dried for standby；It will be according to ferroalloy made from formula table
Dusty material is stand-by after mixing；
(2) ferroalloy powder and graphene film are successively stacked to required thickness in a mold, 1 × 10-2Pa's or more
The graphene film-ferroalloy composite material is processed into through vacuum hotpressing under vacuum environment.
8. graphene film as claimed in claim 7-ferroalloy composite material preparation method, which is characterized in that step (1) institute
It states and the graphene membrane surface is cleaned up into dried for standby, specific method is to be cleaned by ultrasonic graphene film acetone for several times,
To remove the greasy dirt of graphene membrane surface or dirty.
9. graphene film as claimed in claim 7-ferroalloy composite material preparation method, which is characterized in that step (1) institute
Graphene film is stated with uniform through bore, aperture is 1 between 3mm, and the spacing in adjacent two center of circle is between 4-10mm.
10. graphene film as claimed in claim 7-ferroalloy composite material preparation method, which is characterized in that step (2)
The vacuum hotpressing condition is as follows: 1050-1230 DEG C of hot pressing temperature；Hot pressing pressure is 40-80MPa；The hot pressing dwell time is
0.5-3 hours.
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| CN114029494A (en) * | 2021-11-11 | 2022-02-11 | 西北有色金属研究院 | Preparation method of spiral graphene film/copper laminated composite material |
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| CN114029494B (en) * | 2021-11-11 | 2022-08-02 | 西北有色金属研究院 | Preparation method of spiral graphene film/copper laminated composite material |
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