CN107893169A - A kind of preparation method of CNT and graphene hybrid reinforced metal-matrix composites - Google Patents
A kind of preparation method of CNT and graphene hybrid reinforced metal-matrix composites Download PDFInfo
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- CN107893169A CN107893169A CN201711071194.4A CN201711071194A CN107893169A CN 107893169 A CN107893169 A CN 107893169A CN 201711071194 A CN201711071194 A CN 201711071194A CN 107893169 A CN107893169 A CN 107893169A
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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
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0084—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ carbon or graphite as the main non-metallic constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
- C22C2026/002—Carbon nanotubes
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Abstract
A kind of preparation method of CNT and graphene hybrid reinforced metal-matrix composites, belong to scattered and composite the preparation field of CNT.This method makes CNT effectively scattered in metallic matrix by adding graphene oxide and series of process flow, and improves the content of CNT in composite, reduces the oxidation of metallic matrix.The main implementation steps of this method are：(1) preparation of CNT graphene dispersing solution；(2) preparation of CNT graphene metal-base composites.The advantages that this method has the new impurity of the introducing that dispersion effect is good, easy to operate, technological process is short, less, and environmental pollution is small.
Description
Technical field
The invention belongs to the scattered and field of composite material preparation of CNT, and in particular to a kind of CNT and graphite
The preparation method of alkene hybrid reinforced metal-matrix composites.
Background technology
Since 1991, CNT (Carbon Nanotube, abbreviation CNT) was male by the Iijima spring of Japan Electronics Corporation
(S.Iijima) since doctor has found, because it has excellent mechanics, calorifics, electric property, materialogy etc. has been widely used in it
All trades and professions.CNT is seamless, the hollow tube that the graphene film formed by carbon atom is rolled into, and is one-dimensional carbon material,
Its axial strength is high, and axial Young's modulus is up to 100GPa close to 2Tpa, tensile strength, is 100 times of steel.In addition, it is high
Modulus of elasticity, big specific surface area, good high-temperature stability, good anti-friction wear-resistant, high-termal conductivity etc., make it can be with
As the preferable enhancing phase of the matrix nano composites such as the stable ceramics polymer of high intensity, metal.
Although CNT has many good characteristics and specific function, it has very high draw ratio, greatly
Specific surface area and very high surface energy, in order to reduce free energy, CNT can spontaneous reunion.This spontaneous reunion tendency,
It is not disperseed in the base, have impact on the performance of single-root carbon nano-tube excellent mechanical property, hot property, electrical property, so as to
Influence the performance of carbon nano tube compound material.
Therefore before CNT is added into the matrix of composite, it is necessary to carry out pre-dispersed.Process for dispersing point
For Physical and chemical method.Physical is scattered etc. including stirring, ultrasound, centrifugation, ball milling.But physical method effect difference is unstable
It is fixed, therefore it is often used as aid dispersion.Such as " A new technique for dispersion of carbon
nanotube in a metal melt”(Xiaoshu Zeng.Materials Science and Engineering,
(2010) 5335~5340) in a text, ball-milling treatment has been carried out to CNT, test result indicates that CNT is in ball milling
Under percussion, CNT aggregate is opened to a certain extent, preferably non-oxidation can be disperseed.In " Dispersion
Stability of multi~walled carbon nanotubes in refrigerant with addition of
In surfactant " (Lingnan Lin.Applied Thermal Engineering 91 (2015) 163~171), experiment
As a result it is tentatively scattered to show that 60~90min of ultrasound can also be carried out effectively to CNT.Chemical method includes：Covalent bond is repaiied
Decorations, i.e., be chemically modified by covalent bond effect in CNTs side wall and/or top；Non-covalent bond is modified, that is, utilizes surface
Activating agent or hydrophilic molecule compound are wrapped in CNTs outer walls.(awarded in " a kind of method for improving CNT dispersiveness "
Weigh the A of publication No. CN 104861743) invention in, disclose a kind of covalent bond modification method, process for dispersing be first by cyclodextrin and
Silane coupler KH560 carries out reacting obtained KH560/ β~CD；Then CNT is acidified so that on CNT
Substantial amounts of hydroxyl and carboxyl are introduced, obtains being acidified CNT；Finally KH560/ β~CD and acidifying CNT are reacted
Cyclo-dextrin-modified CNT is made.In addition, the method for having a large amount of non-covalent bond modifications is also suggested, such as " TAB pairs of dispersing agent C
Itd is proposed in the influence of carbon nano tube suspension dispersive property " (the Journal of Inorganic Materials such as Xiao Qi, page 2007,1122~1125)
Using cetyl trimethylammonium bromide as dispersant, the carbon nano tube suspension of favorable dispersibility is prepared for.
But not only dispersion effect is poor for Physical, and mechanical external force can the unique structure of destroying carbon nanometer tube；Covalent bond
Though modification method to a certain extent can disperse CNT, by carbon pipe side wall or top be introduced directly into functional group come
Realize that CNT disperses, the structure of carbon pipe can be changed, influence the performance of its special performance.Non-covalent bond modification method is disperseed carbon and received
During mitron, mainly with physical absorption, do not produce covalent bond, thus will not destroying carbon nanometer tube structure.Non-covalent bond dispersant
Mainly based on ionic, it has a hydrophilic group and a lipophilic group, passes through the association and ion between hydrophobic chain
Centrifugation caused by charge repulsion and hydration is scattered to realize between head base, and this allows for surfactant can be in water
Admirably dispersing Nano carbon tubes, and dispersion effect is slightly worse in the organic solvents such as alcohol.In the system of the active metal such as magnesium composite
During standby, the organic solvents such as absolute ethyl alcohol are often used as solvent in order to reduce oxidation, but this have impact on CNT
It is scattered in metallic matrix, limit CNT content in metallic matrix；If with water equal solvent to carbon in preparation process
Nanotube and metal dust are mixed, then metal dust can produce severe oxidation.Therefore find it is new, can be in metallic matrix
The method of middle dispersing Nano carbon tubes is necessary.
The content of the invention
Effect is not in metallic matrix primarily directed to current conventional method dispersing Nano carbon tubes for the technical purpose of the present invention
The problem of good, a kind of neither destroying carbon nanometer tube structure of exploitation, and other a large amount of materials are not introduced, can also be in metallic matrix
Fine dispersion CNT, and the oxidation of metallic matrix is reduced, improve content of the CNT in metallic composite
Method.The method is realized when adding CNT, reduces the oxidation of metallic matrix, and CNT improves same in content
Shi Youxiao disperses, so as to improve carbon nanotube metal based composite materials performance.
A kind of preparation method of CNT and graphene hybrid reinforced metal-matrix composites, is by following technical side
What case was realized.Its step is：
(1) preparation of CNT graphene dispersing solution；(2) preparation of CNT graphene metal-base composites.
It is specific as follows：
(1) preparation of CNT graphene dispersing solution
The graphene oxide and CNT for weighing certain mass are added in inorganic solvent, are well mixed, are preferably aoxidized
The mass ratio of graphene and CNT is (0.1~10):1, solvent is preferably deionized water.
By above-mentioned mixed liquor room temperature ultrasound, while with mechanical agitation.It is preferred that the ultrasonic agitation time is 20~120min.
Above-mentioned CNT used can be single-walled carbon nanotube, multi-walled carbon nanotube or two kinds of CNT different contents
Combination, and the purity of CNT is preferably not less than 95.0wt.%.Graphene oxide used preferably uses the μ of piece interlamellar spacing 5~10
M, 1~2nm of thickness.
Above-mentioned CNT graphene oxide dispersion is dried, drying temperature preferable temperature is 80 DEG C~200 DEG C,
It is preferred that drying time is 7~24h.Dried powder is reduced under inert gas shielding, reduction temperature be 300 DEG C~
700 DEG C, the recovery time is 2~8h, obtains CNT graphene mixed-powder.
Above-mentioned CNT graphene mixed-powder is added in organic solvent, room temperature ultrasound, while stirred with machinery
Mix；It is preferred that the ultrasonic agitation time is 20~120min, you can obtains CNT graphene dispersing solution.
Organic solvent preferably is selected from acetone, ethanol, methanol etc..
(2) preparation of CNT graphene metal-base composites
The metallic matrix powder of quality needed for weighing, preferred particle size is 50~1000 mesh, and it is made to be added to step (1)
It is stirred in the CNT graphene dispersing solution obtained, mixing time is 15~120min, and the mixture after stirring is placed in
Vacuum drying chamber is dried in vacuo, and preferably drying temperature is 60 DEG C~120 DEG C, and drying time is 60~180min；
Dried mixed powder is subjected to extrusion forming, extrusion ratio is 10~25.It is preferred that extrusion temperature is 300~450 DEG C.
Inert gas, which only shields, to be not involved in reacting, preferably argon gas etc..
Scattered content of the CNT in metallic matrix can be adjusted as needed using the method for the present invention, i.e.,
Scattered content of the CNT in metallic matrix can be improved, can at least reach 7wt% content, even more high.
Process for dispersing of the present invention has the following advantages that：Whole preparation process is simple, and flow is short, can solve carbon nanometer
Bad dispersibility, content of the pipe in metallic matrix are low and metallic matrix is oxidizable during being mixed with CNT asks
Topic.Graphene oxide promotes the scattered of CNT, is not limited to realize in the inorganic solvents such as water, also can in organic solvent
Play a role so that metal dust and CNT can mix in organic solvent, so as to reduce because being contacted with water and air
Caused by oxidation, for improve CNT metallic matrix dispersiveness, reduce metallic matrix oxidation, improve CNT exist
Content in composite provides a brand-new, convenient effective process, further improves the items of composite
Performance, there are bright prospects.
Brief description of the drawings
Fig. 1 is the dispersed CNT graphene solution photo obtained in example 1；
Fig. 2 is by scattered CNT graphene TEM photos in example 1, and the upper right corner is the diffraction spot of CNT；
Fig. 3 is that the composite powder of example 1~5 is squeezed into rod photo；
Fig. 4 is the composite metallograph of example 4；
Embodiment
The present invention is further illustrated with reference to specific embodiment, it should be pointed out that following examples are served only for
Bright specific implementation method of the invention, can not limit rights protection scope of the present invention.
Embodiment 1
(1) graphene oxide and 500mg CNTs for weighing 100mg are added in 60ml deionized waters, will be above-mentioned mixed
Liquid room temperature ultrasound 20min is closed, with mechanical agitation while ultrasonic.Above-mentioned mixed dispersion liquid is placed in drying box, temperature is
200 DEG C, drying time is 7 hours.Dried solid is taken out, is placed in tubular type furnace reduction, temperature is 300 DEG C, during insulation
Between be 8 hours.Powder after reduction is added in 160ml acetone, room temperature ultrasound 20min, stirred while ultrasonic with machinery
Mix.
(2) the pure magnesium powders of 49.4g are weighed to be added in dispersion liquid obtained by (1), stir 40min.Then vacuum is placed on to do
Dry case Inner, drying temperature are 70 DEG C, time 180min.Dried powder is subjected to extrusion forming, extrusion temperature 350
DEG C, extrusion ratio 10.
Embodiment 2
(1) graphene oxide and 100mg CNTs for weighing 700mg are added in 80ml distilled water, by above-mentioned mixing
Liquid room temperature ultrasound 60min, with mechanical agitation while ultrasonic.Above-mentioned mixed dispersion liquid is placed in drying box, temperature 80
DEG C, drying time is 24 hours.Dried solid is taken out, is placed in tubular type furnace reduction, temperature is 400 DEG C, soaking time
For 6 hours.Powder after reduction is added in 180ml absolute ethyl alcohols, room temperature ultrasound 60min, with machinery while ultrasonic
Stirring.
(2) weigh 49.2g aluminium alloys (1060) powder to be added in dispersion liquid obtained by (1), stir 120min.Then put
In vacuum drying chamber Inner, drying temperature is 85 DEG C, time 120min.Dried powder is subjected to extrusion forming, extruding temperature
Spend for 400 DEG C, extrusion ratio 10.
Embodiment 3
(1) graphene oxide and 900mg CNTs for weighing 100mg are added in 100ml distilled water, by above-mentioned mixing
Liquid room temperature ultrasound 120min, with mechanical agitation while ultrasonic.Above-mentioned mixed dispersion liquid is placed in drying box, temperature is
150 DEG C, drying time is 12 hours.Dried solid is taken out, is placed in tubular type furnace reduction, temperature is 500 DEG C, soaking time
For 5 hours.Powder after reduction is added in 200ml absolute ethyl alcohols, room temperature ultrasound 120min, with machinery while ultrasonic
Stirring.
(2) weigh 49.0g titanium alloys (TA22) powder to be added in dispersion liquid obtained by (1), stir 90min.Then put
In vacuum drying chamber Inner, drying temperature is 100 DEG C, time 80min.Dried powder is subjected to extrusion forming, extruding temperature
Spend for 500 DEG C, extrusion ratio 16.
Embodiment 4
(1) graphene oxide and 100mg CNTs for weighing 10mg are added in 40ml deionized waters, by above-mentioned mixing
Liquid room temperature ultrasound 20min, with mechanical agitation while ultrasonic.Above-mentioned mixed dispersion liquid is placed in drying box, temperature is
110 DEG C, drying time is 13 hours.Dried solid is taken out, is placed in tubular type furnace reduction, temperature is 600 DEG C, during insulation
Between be 4 hours.Powder after reduction is added in 140ml methanol, room temperature ultrasound 20min, stirred while ultrasonic with machinery
Mix.
(2) weigh 49.9g magnesium alloys (ZK61) powder to be added in dispersion liquid obtained by (1), stir 15min.Then put
In vacuum drying chamber Inner, drying temperature is 60 DEG C, time 180min.Dried powder is subjected to extrusion forming, extruding temperature
Spend for 300 DEG C, extrusion ratio 10.
Embodiment 5
(1) graphene oxide and 10mg CNTs for weighing 100mg are added in 50ml pure water, by above-mentioned mixed liquor room
The ultrasonic 90min of temperature, with mechanical agitation while ultrasonic.Above-mentioned mixed dispersion liquid being placed in drying box, temperature is 170 DEG C,
Drying time is 10 hours.Dried solid is taken out, is placed in tubular type furnace reduction, temperature is 700 DEG C, soaking time 2
Hour.Powder after reduction is added in 150ml absolute ethyl alcohols, room temperature ultrasound 20min, stirred while ultrasonic with machinery
Mix.
(2) weigh 49.9g magnesium alloys (AZ91) powder to be added in dispersion liquid obtained by (1), stir 60min.Then put
In vacuum drying chamber Inner, drying temperature is 120 DEG C, time 90min.Dried powder is subjected to extrusion forming, extruding temperature
Spend for 325 DEG C, extrusion ratio 25.
Although listing in detail here and illustrating to be preferable to carry out case, skilled person will appreciate that, it can not take off
Carried out in the case of from marrow of the present invention it is various improve, addition, the mode such as replace, these contents are all identified as belonging to right will
Ask within limited the scope of the present invention.
Claims (9)
- A kind of 1. preparation method of CNT and graphene hybrid reinforced metal-matrix composites, it is characterised in that including with Lower step：(1) preparation of CNT graphene dispersing solution；(2) preparation of CNT graphene metal-base composites；It is specific as follows：(1) preparation of CNT graphene dispersing solutionThe graphene oxide and CNT for weighing certain mass are added in inorganic solvent, are well mixed；By above-mentioned gained carbon Nanotube graphene oxide dispersion is dried, and dried powder is reduced under inert gas shielding, reduction temperature For 300 DEG C~700 DEG C, the recovery time is 2~8h, obtains CNT graphene mixed-powder；By above-mentioned CNT graphite Alkene mixed-powder is added in organic solvent, room temperature ultrasound, while with mechanical agitation；(2) preparation of CNT graphene metal-base compositesThe metallic matrix powder of quality, is added in the CNT graphene dispersing solution obtained by step (1) needed for weighing Row stirring, is placed in vacuum drying chamber by the mixture after stirring and is dried in vacuo；Dried mixed powder is squeezed into Type.
- 2. according to a kind of preparation side of CNT and graphene hybrid reinforced metal-matrix composites described in claim 1 Method, it is characterised in that the mass ratio of graphene oxide and CNT is (0.1~10):1, inorganic solvent is deionized water.
- 3. according to a kind of preparation side of CNT and graphene hybrid reinforced metal-matrix composites described in claim 1 Method, it is characterised in that step (1) is well mixed for mixed liquor room temperature ultrasound, while with mechanical agitation, and the ultrasonic agitation time is 20~120min；CNT graphene oxide dispersion is dried, drying temperature is 80 DEG C~200 DEG C, drying time For 7~24h.
- 4. according to a kind of preparation side of CNT and graphene hybrid reinforced metal-matrix composites described in claim 1 Method, it is characterised in that CNT used is single-walled carbon nanotube, multi-walled carbon nanotube or two kinds of CNT different contents Combination, and the purity of CNT is preferably not less than 95.0wt.%；Graphene oxide used preferably uses the μ of piece interlamellar spacing 5~10 M, 1~2nm of thickness.
- 5. according to a kind of preparation side of CNT and graphene hybrid reinforced metal-matrix composites described in claim 1 Method, it is characterised in that dried powder is reduced under inert gas shielding, and reduction temperature is 300 DEG C~700 DEG C, also The former time is 2~8h.
- 6. according to a kind of preparation side of CNT and graphene hybrid reinforced metal-matrix composites described in claim 1 Method, it is characterised in that CNT graphene mixed-powder is added in organic solvent, room temperature ultrasound, while with machinery Stirring, ultrasonic agitation time are 20~120min, and organic solvent is selected from acetone, ethanol, methanol.
- 7. according to a kind of preparation side of CNT and graphene hybrid reinforced metal-matrix composites described in claim 1 Method, it is characterised in that step (2) vacuum drying temperature is 60 DEG C~120 DEG C, and drying time is 60~180min.
- 8. according to a kind of preparation side of CNT and graphene hybrid reinforced metal-matrix composites described in claim 1 Method, dried mixed powder is subjected to extrusion forming, extrusion ratio is 10~25, and extrusion temperature is 300~450 DEG C.
- 9. the CNT and graphene hybrid buildup Metal Substrate that are prepared according to the method described in claim any one of 1-8 Composite.
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Cited By (4)
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| CN108517435A (en) * | 2018-05-21 | 2018-09-11 | 西南交通大学 | A kind of magnetic-levitation train nano-sized carbon enhancing Cu-base composites and preparation method thereof |
| CN114540651A (en) * | 2022-01-25 | 2022-05-27 | 北京工业大学 | Graphene reinforced magnesium matrix composite material with in-situ double-interface structure and preparation method thereof |
| CN114836645A (en) * | 2022-04-06 | 2022-08-02 | 西北工业大学 | Preparation method of carbon nanotube-graphene hybrid porous preform with designable configuration |
| US20220371954A1 (en) * | 2018-10-29 | 2022-11-24 | C2Cnt, Llc | Use of carbon nanomaterials produced with low carbon footprint to produce composites with low co2 emission |
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