CN108842131A - A kind of three-dimensional grapheme/carbon/carbon-copper composite material preparation method of high thermal conductivity - Google Patents
A kind of three-dimensional grapheme/carbon/carbon-copper composite material preparation method of high thermal conductivity Download PDFInfo
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- CN108842131A CN108842131A CN201810707965.2A CN201810707965A CN108842131A CN 108842131 A CN108842131 A CN 108842131A CN 201810707965 A CN201810707965 A CN 201810707965A CN 108842131 A CN108842131 A CN 108842131A
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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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/60—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using solids, e.g. powders, pastes
- C23C8/62—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using solids, e.g. powders, pastes only one element being applied
- C23C8/64—Carburising
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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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
- C22C1/1015—Pretreatment of the non-metallic additives by preparing or treating a non-metallic additive preform
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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
- C22C9/00—Alloys based on copper
Abstract
The present invention relates to a kind of three-dimensional grapheme/carbon/carbon-copper composite material preparation methods of high thermal conductivity.Its key step includes：It is transferred in PTPE mold after configuring certain density graphene dispersing solution, mold is placed in liquid nitrogen surface and is rapidly frozen, then freeze-drying obtains directional three-dimensional grapheme foam, and bulk alloy is finally placed in grapheme foam surface（Perpendicular to orientation direction）It is placed in silica crucible, pressureless infiltration is carried out in tube furnace, obtains graphene/copper composite material.The present invention prepares the three-dimensional net structure graphene aligned in conjunction with freeze-drying by liquid nitrogen rapid cooling, and the graphene/copper composite material of even tissue is prepared by pressureless infiltration.The three-dimensional network connectivity structure of graphene aligned can increase passage of heat in composite material prepared by the present invention, play graphene to the greatest extent in the excellent properties of thermally conductive aspect, improve the heating conduction of composite material.Process simple possible of the invention, step is easily operated, high safety and reliability, low in cost, can be used for being mass produced.
Description
Technical field：
The invention belongs to field of metal matrix composite, specifically include a kind of graphene/copper of three-dimensional structure with high thermal conductivity
The preparation method of composite material.
Technical background：
Metal-base composites（MMCs）The excellent performance for having both metallic matrix and reinforcement, because of good heating conduction and
Mechanical performance is widely used in various industries.Be widely studied application at present has silicon carbide/aluminium and diamond/aluminum（Copper）It is compound
Material, but the two itself all has some disadvantages.For example, silicon carbide/aluminium composite material thermal conductivity generally can reach 170 ~
200 W/mK, but the thermal expansion coefficient of aluminum substrate is big, and fracture toughness is low, it is difficult to promote its application.So far, reinforced phase
Dispersion, the principal element for restricting MMCs development is still with the interface cohesion of matrix and interfacial reaction etc..
The discovery of graphene causes global concern.Graphene be it is a kind of by carbon atom withsp 2The connection of hydridization form
And the crystalline material of the bi-dimensional cellular shape structure formed, intensity and carrier mobility with superelevation, negative thermal expansion coefficient
And high thermal conductivity.Graphene and its derivative also have a high electrical and thermal conductivity performance, the specific surface area of superelevation and good
Wetability.Experiment test, single-layer graphene can reach ~ 5300 W/ (m in the thermal conductivity being parallel on crystal layer direction·
K), 3000 W/ much higher than CNTs (m K), even more 10 times or more of common metal (such as Cu, Ag, Au).Graphene conduct
Reinforced phase can significantly improve the mechanical property of composite material, and can not only improving the intensity of composite material, to be also able to maintain matrix good
Toughness.For the planar structure of graphene but also it is easy to reunite, anticipation is often not achieved in practical reinforcing effect but then
Result.Three-dimensional network graphene-structured has many advantages, such as porous structure, low defect, not only it is possible to prevente effectively from graphene is easily rolled into a ball
The shortcomings that poly-/difficult dispersion, can play the distinctive high thermal conduction characteristic of graphene connected network structure with perfection；With three-dimensional graphite
For alkene as in the metallic matrix of reinforced phase, the connected network structure of graphene can form many new passage of heat, increase
Passage of heat, so that the advantages of giving full play to graphene high thermal conductivity, obtains graphene/metallic composite of high thermal conductivity.
Boden etc.（Nano Letters, 2014, 14: 3640-3644.）It is prepared by high-energy ball milling and discharge plasma sintering
Graphene/metallic composite and the heating conduction for studying composite material, the results showed that graphene is in prepared composite material
Now uniform layered distribution and self orientation dry-out phenomenon, thus the thermal conductivity of composite material is rendered as apparent anisotropy.
Therefore by three-dimensional grapheme structure infiltration into metal material can utmostly play the excellent heating conduction of graphene,
Prepare three-dimensional grapheme/metallic composite of excellent thermal conductivity.
The present invention is directed to make full use of the network-in-dialing structure of three-dimensional grapheme, passage of heat is increased, matrix is improved and closes
The thermal conductivity of gold；In combination with the thinking of alloying, alloying element is added in parent metal（Ti or Cr）, pass through matrix alloy
In active element and reinforcement generate interfacial reaction, provide required boundary moisture condition for pressureless infiltration, solution stone
The problem of black alkene wetting difference easy to reunite and with Copper substrate obtains the stone of the three-dimensional net structure of the good high thermal conductivity of interface cohesion
Black alkene/carbon/carbon-copper composite material.
Summary of the invention
Based on the special structure of three-dimensional grapheme and excellent heat-conductive characteristic, it is fixed that the present invention is prepared by freeze-drying
To the grapheme foam skeleton of three-dimensional net structure, later by preparing without pressing molten infiltration that copper alloy is filled among skeleton
The graphene/copper composite material of the three-dimensional net structure of high thermal conductivity out.The specific steps are that：
（1）Certain density graphene oxide dispersion is configured, is subsequently transferred in PTPE mold, mold is placed in liquid nitrogen
Surface is rapidly frozen, and the grapheme foam of the three-dimensional net structure aligned is then freeze-dried；
（2）Enough bulk alloys are disposed vertically in step（1）Grapheme foam surface obtained（Perpendicular to orientation direction）
It is placed in silica crucible, carries out pressureless infiltration in tube furnace, obtain graphene/copper composite material.
Preferably, it is characterized in that step（1）Middle graphene oxide is laminated structure, and diameter is 10 ~ 50 μm, with a thickness of 2
~ 10 nm, single layer rate be about 99%, purity 99.8%.
Preferably, it is characterized in that step（1）In, dispersion solvent is selected as ethyl alcohol, methanol, one of acetone in solution.
Preferably, it is characterized in that the step（1）In, the concentration of graphene oxide solution is 5 ~ 10 mg/mL.
Preferably, it is characterized in that the step（1）In, ultrasonic disperse device frequency is controlled 10000 ~ 20000
Hz, 0.5 ~ 1.0 h of ultrasonic time, ultrasonic temperature are controlled at 20 ~ 45 DEG C.
Preferably, it is characterized in that the step（1）In, the time of freeze-drying is 24 ~ 72 h, relative degree of vacuum 10
Pa。
Preferably, it is characterized in that the step（2）In, bulk alloy is one kind of copper-titanium alloy or chromiumcopper.
Preferably, it is characterized in that the step（2）In, the parameter of pressureless infiltration is：Temperature is 1000 ~ 1200 DEG C,
Soaking time is 1 ~ 2 h, and heating rate is 5 ~ 10 DEG C/min, rate of temperature fall：5 ~ 20 DEG C/min, argon flow 40
~ 100 sccm。
The method of the present invention has the advantage that compared to the preparation method of existing thermal conductivity graphene/carbon/carbon-copper composite material：（1）Graphite
The three-dimensional net structure that vertical arrangement is formed between alkene and Copper substrate, increases passage of heat, reduces interface resistance, is conducive to
The promotion of composite material heating conduction, during high temperature pressure-free infiltration, three-dimensional graphene framework is conducive to the infiltration of copper；（2）
Interfacial reaction occurs under the high temperature conditions for graphene and the matrix of alloying, appropriate interfacial product is generated in interface, to change
It has been apt to the combination at interface, has further reduced interface resistance.
Specific embodiment:
Embodiment 1
By graphene oxide（Piece diameter is 10 μm, with a thickness of 2 nm）It is dispersed in ethanol solution, 0.5 h of ultrasonic disperse is configured to
The graphene oxide solution of 5 mg/mL of concentration.It is subsequently transferred in PTPE mold（15 × 15 × 3 cm of die size）, by mold
It is placed in 10 min of liquid nitrogen surface, freezing is oriented from the top to the bottom, is later freeze-dried sample, drying time
For 48 h, the grapheme foam of three-dimensional net structure is obtained；By enough blocky copper-titanium alloy（5 wt.% Ti）It is placed in orientation three
Tie up the grapheme foam surface of network structure（Perpendicular to graphene orientation direction）It is placed in silica crucible, is carried out in tube furnace
Pressureless infiltration is vacuumized first and is heated, and is heated to 1100 DEG C with the heating rate of 10 DEG C/min, is kept the temperature 30 min, guarantees
Alloy is heated evenly, sufficiently fusing and degasification.Then in 1200 DEG C of 120 min of heat preservation, room is then cooled to 20 DEG C/min
Temperature obtains graphene/copper composite material.Most afterwards through measuring, heat conductivity obtained is 520 W/ (m·K)。
Embodiment 2
By graphene oxide（Piece diameter is 20 μm, with a thickness of 2 nm）It is dispersed in ethanol solution, 0.5 h of ultrasonic disperse is configured to
The graphene oxide solution of 5 mg/mL of concentration.It is subsequently transferred in PTPE mold（15 × 15 × 3 cm of die size）, by mold
It is placed in 10 min of liquid nitrogen surface, freezing is oriented from the top to the bottom, is later freeze-dried sample, drying time
For 48 h, the grapheme foam of three-dimensional net structure is obtained；By enough blocky copper-titanium alloy（5 wt.% Ti）It is placed in orientation three
Tie up the grapheme foam surface of network structure（Perpendicular to graphene orientation direction）It is placed in silica crucible, is carried out in tube furnace
Pressureless infiltration is vacuumized first and is heated, and is heated to 1100 DEG C with the heating rate of 10 DEG C/min, is kept the temperature 30 min, guarantees
Alloy is heated evenly, sufficiently fusing and degasification.Then in 1200 DEG C of 120 min of heat preservation, room is then cooled to 20 DEG C/min
Temperature obtains graphene/copper composite material.Most afterwards through measuring, heat conductivity obtained is 585 W/ (m·K)。
Embodiment 3
By graphene oxide（Piece diameter is 20 μm, with a thickness of 2 nm）It is dispersed in ethanol solution, 0.5 h of ultrasonic disperse is configured to
The graphene oxide solution of 10 mg/mL of concentration.It is subsequently transferred in PTPE mold（15 × 15 × 3 cm of die size）, by mould
Tool is placed in 10 min of liquid nitrogen surface, is oriented freezing from the top to the bottom, is later freeze-dried sample, when dry
Between be 48 h, obtain the grapheme foam of three-dimensional net structure；By enough blocky copper-titanium alloy（5 wt.% Ti）It is placed in orientation
The grapheme foam surface of three-dimensional net structure（Perpendicular to graphene orientation direction）Be placed in silica crucible, tube furnace into
Row pressureless infiltration, vacuumizes first and heats, and is heated to 1100 DEG C with the heating rate of 10 DEG C/min, keeps the temperature 30 min, protects
Card alloy is heated evenly, sufficiently fusing and degasification.Then in 1200 DEG C of 120 min of heat preservation, then cooled to 20 DEG C/min
Room temperature obtains graphene/copper composite material.Most afterwards through measuring, heat conductivity obtained is 612 W/ (m·
K)。
Embodiment 4
By graphene oxide（Piece diameter is 20 μm, with a thickness of 2 nm）It is dispersed in ethanol solution, 0.5 h of ultrasonic disperse is configured to
The graphene oxide solution of 5 mg/mL of concentration.It is subsequently transferred in PTPE mold（15 × 15 × 3 cm of die size）, by mold
It is placed in 10 min of liquid nitrogen surface, freezing is oriented from the top to the bottom, is later freeze-dried sample, drying time
For 48 h, the grapheme foam of three-dimensional net structure is obtained；By enough blocky chromiumcoppers（5 wt.% Cr）It is placed in orientation three
Tie up the grapheme foam surface of network structure（Perpendicular to graphene orientation direction）It is placed in silica crucible, is carried out in tube furnace
Pressureless infiltration is vacuumized first and is heated, and is heated to 1100 DEG C with the heating rate of 10 DEG C/min, is kept the temperature 30 min, guarantees
Alloy is heated evenly, sufficiently fusing and degasification.Then in 1200 DEG C of 120 min of heat preservation, room is then cooled to 20 DEG C/min
Temperature obtains graphene/copper composite material.Most afterwards through measuring, heat conductivity obtained is 597 W/ (m·K)。
Above example will be helpful to those skilled in the art and further understand the present invention, but not limit this in any form
Invention.It should be pointed out that those skilled in the art, without departing from the inventive concept of the premise, may be used also
To make several modifications and improvements.These are all within the scope of protection of the present invention.
Claims (8)
1. a kind of three-dimensional grapheme/carbon/carbon-copper composite material preparation method of high thermal conductivity, which is characterized in that include the following steps：
(1) it is transferred in PTPE mold after configuring certain density graphene oxide dispersion, mold is placed in liquid nitrogen surface
It is rapidly frozen, is then freeze-dried the grapheme foam of the three-dimensional net structure aligned；
(2) enough bulk alloys are disposed vertically in step（1）Grapheme foam surface obtained（Perpendicular to orientation drying side
To）It is placed in silica crucible, carries out pressureless infiltration in tube furnace, obtain graphene/copper composite material.
2. the method as described in claim 1, it is characterized in that step（1）Middle graphene oxide be laminated structure, diameter be 10 ~
50 μm, with a thickness of 2 ~ 10 nm, single layer rate be about 99%, purity 99.8%.
3. the method as described in claim 1, it is characterized in that step（1）In, dispersion solvent is selected as ethyl alcohol in solution, methanol,
One of acetone.
4. the method as described in claim 1, it is characterized in that the step（1）In, the concentration of graphene oxide solution is 5 ~
10 mg/mL。
5. the method as described in claim 1, it is characterized in that the step（1）In, the control of ultrasonic disperse device frequency exists
10000 ~ 20000 Hz, 0.5 ~ 1.0 h of ultrasonic time, ultrasonic temperature are controlled at 20 ~ 45 DEG C.
6. the method as described in claim 1, it is characterized in that the step（1）In, the time of freeze-drying is 24 ~ 72
H, 10 Pa of relative degree of vacuum.
7. the method as described in claim 1, it is characterized in that the step（2）In, bulk alloy is copper-titanium alloy or copper chromium
One kind of alloy.
8. the method as described in claim 1, it is characterized in that the step（2）In, the parameter of pressureless infiltration is：Temperature is
1000 ~ 1200 DEG C, soaking time is 1 ~ 2 h, and heating rate is 5 ~ 10 DEG C/min, rate of temperature fall：5 ~ 20 ℃/
Min, argon flow are 40 ~ 100 sccm.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110586938A (en) * | 2019-10-21 | 2019-12-20 | 西安稀有金属材料研究院有限公司 | Nano carbon-titanium-based composite powder with network structure and application thereof |
| CN110650618A (en) * | 2019-10-29 | 2020-01-03 | Oppo广东移动通信有限公司 | Heat radiating fin, preparation method thereof and electronic equipment |
| CN113659193A (en) * | 2021-08-27 | 2021-11-16 | 西北工业大学 | All-solid-state sodium ion battery cell structure, preparation method and battery |
| CN113804097A (en) * | 2021-11-19 | 2021-12-17 | 北京石墨烯技术研究院有限公司 | Stretchable strain sensor material and preparation method and application thereof |
| CN114540661A (en) * | 2022-01-07 | 2022-05-27 | 西安理工大学 | Graphene reinforced copper-molybdenum composite material with three-dimensional network structure and preparation method thereof |
| WO2023060933A1 (en) * | 2021-10-14 | 2023-04-20 | 广东墨睿科技有限公司 | Directionally-arranged graphene heat-conducting foam, graphene heat-conducting film, preparation method therefor and electronic product |
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| CN113804097A (en) * | 2021-11-19 | 2021-12-17 | 北京石墨烯技术研究院有限公司 | Stretchable strain sensor material and preparation method and application thereof |
| CN114540661A (en) * | 2022-01-07 | 2022-05-27 | 西安理工大学 | Graphene reinforced copper-molybdenum composite material with three-dimensional network structure and preparation method thereof |
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Application publication date: 20181120 |