CN108517435A - A kind of magnetic-levitation train nano-sized carbon enhancing Cu-base composites and preparation method thereof - Google Patents
A kind of magnetic-levitation train nano-sized carbon enhancing Cu-base composites and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of magnetic-levitation train nano-sized carbons to enhance Cu-base composites, it is characterised in that：By surface be modified carbon nanotube 0.1 ~ 5%, by surface be modified graphene 0.1 ~ 5%, powdered graphite 2 ~ 10%, chromium powder end 1 ~ 4%, lead powder end 1 ~ 8%, tin powder 2 ~ 10%, zirconium powder 0.1 ~ 1%, lanthanum powder 0.01 ~ 0.5%, surplus be copper powders；The carbon nanotube being wherein modified by surface is that carbon nanotube is used the carbon nanotube that gallic acid aqueous solution is modified, and the graphene being modified by surface is that graphene is used the graphene that rutin aqueous solution is modified.Cu-base composites impurity content of the present invention is low, and keeps addition reinforced phase constituent structure complete, and a variety of adding ingredients can play total humidification, significantly improve the intensity, hardness and current-carrying frictional wear performance of Cu-base composites.In addition, the invention also discloses a kind of above-mentioned Cu-base composites preparation method, this method is simple for process, is readily produced, and has broad application prospects.
Description
Technical field
The present invention relates to a kind of Cu-base composites, more particularly to a kind of nano-sized carbon enhancing Cu-base composites and its preparation
Method belongs to the preparing technical field of composite material.
Background technology
Since carbon nanotube and graphene are found respectively, just studied by numerous scholars, carbon nanotube is due to it
Unique structure and with the performances such as excellent optics, calorifics, electricity and mechanics, there is high mechanical strength and ideal bullet
Property, low coefficient of thermal expansion, the excellent characteristics such as size is small；Graphene has high intensity, big specific surface area and preferable
Elongation percentage.Carbon nanotube and graphene are all the ideal materials as composite material reinforced phase.
Carbon nanotube and graphene are by widely as the reinforced phase of composite material, and in polymer matrix composite side
Face achieves quick development.In metal-base composites, Cu-base composites with performances such as its excellent conduction, heat conduction and
It is widely used as electronic material, sliding block material, contact material, heat exchange material etc..Therefore, nano-sized carbon is enhancing copper-based composite wood
It is concerned in terms of material.
But carbon nanotube and graphene apply in enhancing metal-base composites that there is also many difficulties.On the one hand,
Since carbon nanotube and graphene are all nano materials, there is great specific surface area and specific surface energy, there are prodigious model morals
Hua Li, it is easy to reunite and tangle, be difficult in metallic matrix evenly dispersed.On the other hand, the surface of carbon nanotube and graphene
Expression activitiy is low, poor with the wetability of metallic matrix, therefore the interface cohesion between carbon nanotube and graphene and metallic matrix
Intensity difference.These factors have seriously affected the performances such as mechanics, electricity, the fretting wear of metal-base composites.
To solve the above-mentioned problems, the preparation methods such as chemical plating and molecular level mixing method are suggested and are largely ground
Study carefully, but these method and processes are complicated, energy consumption is big, and has centainly to the structure of carbon nanotube and graphene in pre-processing process
Destruction, it will weaken its enhancing effect.
Carbon nanotube and graphene are all ideal reinforcing materials, but the increasing of one-dimensional carbon nanotube and two-dimensional graphene
Mechanism has different by force, and the two is mixed and is used as reinforced phase, can combine the advantage of the two, improves to Cu-base composites
Enhancing effect.
Chinese patent application 201410354188.x discloses a kind of carbon nanotube reinforced copper-base composite material and its preparation
Method is first modified carbon nanotube using gallic acid aqueous solution, then with copper powders, powdered graphite and Ti3SiC2Powder
End carries out ball milling, and hot pressed sintering obtains the carbon nanotube reinforced copper-base composite material.But pressure-loaded when due to hot pressed sintering
Direction is unidirectional, and Cu-base composites is caused to have certain anisotropy, and performance has differences in different directions.
Chinese patent application 201510537320.5 discloses a kind of method preparing graphene enhancing Cu-base composites,
Graphene oxide is prepared first, and surface is modified, and then prepares graphene oxide-copper composite powder, last hot pressed sintering obtains institute
State Cu-base composites.But pressure-loaded direction is unidirectional when due to hot pressed sintering, and Cu-base composites is caused to have one
Fixed anisotropy, and single graphene is single to the enhancing effect of Cu-base composites as reinforced phase.
Invention content
It is an object of the invention to overcome carbon nanotube in the presence of the prior art and graphene to be applied to composite material
In, it is difficult to fully coordinate with basis material and play the problem of it enhances effect completely, it is copper-based compound to provide a kind of nano-sized carbon enhancing
Material.
The present invention enhances the humidification that Cu-base composites give full play to various material compositions, and it is strong to improve composite material
Degree and current-carrying frictional wear so that Cu-base composites realize better comprehensive performance, and then meet the need of different application condition
It asks.
In order to achieve the above-mentioned object of the invention, the present invention provides following technical schemes：
A kind of nano-sized carbon enhancing Cu-base composites, including the following ingredient of weight percent are made：
The carbon nanotube 0.1~5% being modified by surface, the graphene 0.1~5%, the powdered graphite 2 that are modified by surface
~10%, chromium powder end 1~4%, lead powder end 1~8%, tin powder 2~10%, zirconium powder 0.1~1%, lanthanum powder 0.01~
0.5%, surplus is copper powders.
Wherein, the carbon nanotube being modified by surface is the carbon nanotube using gallic acid solution modification.
The graphene being modified by surface is the graphene using rutin solution modification.
Cu-base composites of the present invention combine two kinds of carbon nanomaterials as nanometer reinforcing phase, and coordinate powdered graphite and
Various metals powder raw material designs to obtain the composite reinforcing material of completely new acid bronze alloy and nano-carbon material.It is excellent by modification
Change, carbon nanotube and graphene dispersion are good, and addition is applied to can be good at playing its humidification in composite material, so
Afterwards, the whole material composition mixing ratio relational design of composite reinforcing material finally makes material by largely optimizing and revising
Comprehensive performance is optimal, and can realize the extremely low effect of wear with current, can preferably be applied to special current-carrying friction workpiece
In manufacture.
Show that the weight percent when each component in Cu-base composites is above-mentioned by a large amount of experimental study of inventor
When ratio, the performance of each component can generate the effect of total enhancing.On the one hand, it is formed between carbon nanotube and graphene and Copper substrate
Preferable interface cohesion, enhancing effect significantly improve；On the other hand, graphite self-lubricating effect is given full play to, the current-carrying of copper is changed
Wear Mechanism is changed into the abrasive wear of composite material by the adhesive wear of fine copper；Also, adjustment control carbon nanotube,
The usage ratio of graphene and powdered graphite, additionally it is possible to carbon film is formed between friction is secondary, to play the role of anti-attrition.And other
Ingredient, the additional proportion process optimization at chromium powder end, lead powder end, tin powder, zirconium powder and lanthanum powder, on the one hand can be with Copper substrate
Solid solution is formed, realizes on the other hand solution strengthening effect can adjust/reduce Copper substrate crystallite dimension, play refined crystalline strengthening
Effect, attrition mechanism of the optimization Cu-base composites between friction is secondary, significantly reduces the rate of wear.
Further, the carbon nanotube being modified by surface is the carbon nanotube using gallic acid solution modification, carbon
The mass ratio of nanotube and gallic acid is 1:0.5-8, gallic acid is to be dissolved in the gallic acid matter in gallic acid solution
Gauge.Preferably, the mass ratio of carbon nanotube and gallic acid is 1:2-6, suitable gallic acid mass ratio, it is ensured that be modified
The gallic acid total amount being adsorbed in journey in carbon nanotube is suitable so that dispersion effect and reduction performance influence mutually equilibrium.
Gallic acid, also known as gallic acid, chemical formula C6H2(OH)3COOH belongs to polyphenols.Gallic acid
In be connected to hydroxyl on phenyl ring there is extremely strong activity, combined with carbon nano tube surface, to carbon nanotube progress surface
Modification；Gallic acid can also be adsorbed in carbon nano tube surface by non-chemical effect.Two-way interaction both helped to improve
The dispersibility of carbon nanotube, and shear action will not be generated to carbon nanotube, cause chemical damage.
Preferably, the gallic acid solution is the gallic acid solution of 1%-100% saturations.
Preferably, gallic acid solution is gallic acid aqueous solution.
Gallic acid is first dissolved in solution in advance, is then allowed to attract each other with carbon nanotube, uniformly be inhaled
Attached modification, carbon nano-tube modification is more abundant, and dispersion effect is more preferable.The 1%-100% is with the saturation of gallic acid solution
Solution is calculated as 100% concentration, 1% concentration relative to the saturated solution of gallic acid solution dilute 100 times with
Solution afterwards.
Preferably, the gallic acid solution is the gallic acid solution of 20%-100% concentration.Select concentration suitable
Gallic acid solution, higher solution concentration are conducive to gallic acid in solution and preferably interact with carbon nanotube, realize
It is modified.
Preferably, the quality of the carbon nanotube and the volume ratio of gallic acid aqueous solution are 0.05~0.4g:20~
80mL, preferably 0.05~0.2g:30~50mL；It is further preferred that the body of the quality of the carbon nanotube and gallic acid aqueous solution
Product is than being 0.1g:40mL.The concentration of the gallic acid aqueous solution is 0.3-1.15g/100mL.
Further, the graphene being modified by surface is the graphene using rutin solution modification, graphene and reed
The mass ratio of fourth is 1:0.5-8.Rutin is to dissolve in terms of rutin quality in the solution.Appropriate rutin forms graphene appropriate
Modified intensity.
Rutin, also known as rutin, citrin are the Typical Representatives of flavonols.Rutin can be with due to the presence of aromatic structure
The pi-conjugated interactions of π-occur with graphene surface, absorption on the surface of graphene, is grafted active group, changed on the surface of graphene
Kind dispersion performance；On the other hand, the phenolic hydroxyl group of rutin itself can interact with the defect sites of graphene surface, Jin Erxiu
Graphene surface is adornd, simultaneously because the presence of hydroxyl isoreactivity group can also be in the more active groups of surface graft and biological work(
It can macromolecular.Both sides collective effect is more advantageous to the dispersion performance for improving graphene, and not bad destruction graphene is complete
Structure.
Preferably, the rutin solution is rutin aqueous solution.
Preferably, the rutin solution is the rutin solution of 1%-100% saturations.The concentration of rutin solution be relative to
The relative scale of 100% saturation rutin solution.Preferably, rutin solution is the rutin solution of 20%-100% saturations.
Further, the quality of the graphene and the volume ratio of rutin aqueous solution are 0.05~0.4g：20~80mL.It is preferred that
For 0.05~0.2g：30~50mL.The concentration of the rutin aqueous solution is 0.3-1.2g/100mL.It is further preferred that the graphene
The volume ratio of quality and rutin aqueous solution be 0.1g:40mL.
The carbon nanotube being modified by surface be the graphene that is modified by carbon nanotube and by surface with good dispersion,
The low feature of impurity content, and maintain complete structure.
Further, the carbon nanotube being modified by surface is the carbon nanotube using gallic acid solution modification, institute
It is the graphene using rutin solution modification to state the graphene being modified by surface.
Modifying process is as follows：Carbon nanotube is put into gallic acid solution, ultrasonic disperse, stood, filtered, it is dry, it obtains
To modified carbon nanotube.
Graphene is put into rutin solution, ultrasonic disperse, stood, filtered, it is dry, obtain modified graphene.
Preferably, the ultrasonic disperse time is 20~40min, and the quiescent time is 12~36h, the vacuum drying
Temperature is 60 DEG C~80 DEG C, and the vacuum drying time is 1~8h.
Preferably, the ultrasonic disperse time is 20~30min, and the quiescent time is 18~30h, the vacuum drying
Temperature is 60 DEG C~70 DEG C, and the vacuum drying time is 1~4h.
Preferably, the ultrasonic disperse time is 30min, and the quiescent time is that for 24 hours, the vacuum drying temperature is 60
DEG C, the vacuum drying time is 2h.
In above-mentioned carbon nanotube and graphene method of modifying, changed using what completely new physical absorption, chemisorption integrated
Property method, high efficient and reliable does not generate the pollutants such as waste water, spent acid, simple for process, is readily produced, and modified effect is reliable and stable.
Further, the nano-sized carbon enhances Cu-base composites, including the following ingredient of weight percent is made：By table
The carbon nanotube 0.1~2% of face modification, graphene 0.1~2%, powdered graphite 5~8%, chromium powder end 1 by surface modification
~3%, lead powder end 2~5%, tin powder 5~8%, zirconium powder 0.2~0.6%, lanthanum powder 0.01~0.2%, surplus are copper powder
End.
Further, the nano-sized carbon enhances Cu-base composites, including the following ingredient of weight percent is made：By table
The carbon nanotube 0.4-1.0% that face is modified, the end graphene 0.2-0.4%, powdered graphite 6-7%, chromium powder by surface modification
1.5-2.5%, lead powder end 3.5-4.5%, tin powder 6-7%, zirconium powder 0.3-0.5%, lanthanum powder 0.05-0.13%, surplus
For copper powders.
Further, the nano-sized carbon enhances Cu-base composites, including the following ingredient of weight percent is made：By table
The carbon nanotube 0.8% of face modification, graphene 0.2%, powdered graphite 6.5%, chromium powder end 2%, the lead powder being modified by surface
End 4%, tin powder 6%, zirconium powder 0.4%, lanthanum powder 0.1%, surplus are copper powders.
It is a further object of the present invention to provide a kind of methods preparing above-mentioned enhancing Cu-base composites, pass through optimization design
The preparation method of Cu-base composites, it is ensured that prepare various material compositions coordinate to obtain Cu-base composites performance it is more preferable
Reach expected design level, meet design application demand.
A kind of preparation method of Cu-base composites, includes the following steps：
(1) carbon nanotube is added in gallic acid aqueous solution, ultrasonic disperse is static, and filtering takes filter residue to carry out vacuum
It is dry, obtain the carbon nanotube being modified by surface；
Graphene is added in rutin aqueous solution, ultrasonic disperse is static, and filtering takes filter residue to be dried in vacuo, and obtains
The graphene being modified by surface；
(3) by the carbon nanotube being modified by surface, the graphene, copper powders, powdered graphite, the chromium powder that are modified by surface
End, lead powder end, tin powder, zirconium powder and the mixing of lanthanum powder, carry out ball milling, obtain composite powder；
(4) composite powder is subjected to cold moudling, obtains composite material green compact；
(5) composite material green compact is subjected to HIP sintering, it is cooling, obtain nano-sized carbon enhancing Cu-base composites.
Prepared by the present invention first carries out corresponding modification by carbon nanotube and graphene in Cu-base composites method and makes
Be converted into the carbon nanomaterial with good dispersion, then with other raw material mixing and ball millings so that various material compositions fill
It is allocated as with mixed material is formed, finally by composite powder cold moudling, HIP sintering, it is copper-based compound to obtain nano-sized carbon enhancing
Material.Entire preparation method is simple, with strong points, high for the pretreatment transformation efficiency of nano-carbon material, mixed in ball milling
When closing material, the full and uniform dispersion of carbon nanomaterial, humidification is maximumlly embodied and is played, final multiple
The bulk property performance of condensation material reaches expected design, and mechanical strength higher, comprehensive wearability are more outstanding.
Further, in the step (3) ball milling use agate ball and agate spherical tank, rotational speed of ball-mill be 200~450 turns/
Min, Ball-milling Time are 40~120min.
Preferably, in the step (3) ball milling use agate ball and agate spherical tank, rotational speed of ball-mill be 300~400 turns/
Min, Ball-milling Time are 40~90min.Rotational speed of ball-mill and Ball-milling Time are optimized and revised, ball mill mixing effect is preferably realized, makes
Various raw material mixture homogeneities are obtained, the stability of material composition more preferably, is more advantageous to final sinter molding composite material quality and carries
It rises.It is highly preferred that ball milling uses agate ball and agate spherical tank in the step (3), rotational speed of ball-mill is 350 turns/min, when ball milling
Between be 60min.
Further, the pressure that cold moudling is suppressed in the step (4) is 400~700MPa.
In conjunction with inventor's test of many times research, cold moudling pressure reaches in above range, it can be ensured that composite powder is former
Material compacting compacts, it is integral sintered after material compactness it is good, high mechanical strength.Preferably, cold moudling pressure in the step (4)
The pressure of system is 500~600MPa.
It is highly preferred that the pressure that cold moudling is suppressed in the step (4) is 600MPa.
Further, the temperature of HIP sintering is 800~1000 DEG C in the step (5), the pressure of HIP sintering
Power is 80~100MPa, and the time of HIP sintering is 1~3h.By inventor's test of many times research, burnt in hot isostatic pressing
During knot, it is sintered using above-mentioned sintering temperature, pressure, time parameter most beneficial for composite material final molding effect is realized
Gained composite material consistency, cohesive force are best.
Preferably, the temperature of HIP sintering is 850~950 DEG C in the step (5), the pressure of HIP sintering
Time for 90~100MPa, HIP sintering is 1~2h.In conjunction with invention test situation, preferably above-mentioned HIP sintering
Temperature, pressure, time parameter, reinforced phase and matrix are interspersed uniformly in sinter molding composite material, element phase counterdiffusion, increase
The effect of the effect of strong phase gets a promotion.It is highly preferred that the temperature of HIP sintering is 900 DEG C in the step (5), heat etc. is quiet
The pressure of pressure sintering is 100MPa, and the time of HIP sintering is 2h.
New solution provided by the invention can mainly realize following technique effect：
1. nano-sized carbon of the present invention enhancing Cu-base composites material composition studies for a long period of time iteration by inventor, propose completely newly
Optimization ingredient application and mixing ratio relationship so that mechanical strength, wearability, wear with current of Cu-base composites etc.
Universality can comprehensively be optimized, and magnetic suspension train conductive member application requirement is met.
2. Cu-base composites of the present invention prepare material composition by completely new preferred design, each component content ratio
Example is mutually related adjustment so that Cu-base composites material composition can generate coordinated and be total to humidification, change copper
The metallographic of metal material matrix in based composites forms completely new alloy basis phase, coordinates nano-sized carbon humidification, significantly
The performances such as intensity and the current-carrying frictional wear of Cu-base composites are improved, its density is reduced.
3. in nano-sized carbon enhancing Cu-base composites of the present invention, carbon nanotube and graphene are specifically subjected to surface respectively
It is modified, compared with non-modified carbon nanomaterial, there is preferably dispersibility, lower impurity content, and maintain carbon nanometer
Pipe and graphene-structured integrality, the enhancing effect being applied in composite material is good, gives full play to the performance advantage of nano material
Feature.
4. the present invention provides Cu-base composites preparation method, coordinate the formula composition and match ratio of completely new optimization design
Example is given full play to material composition formula and the enhancing of Cu-base composites performance is made using heat and other static pressuring processes sinter molding
With, and control in sintering process that all directions pressure is equal, the Cu-base composites of structure even compact are obtained, are effectively played
The comprehensive performance advantage of new material.
Description of the drawings：
Fig. 1 is the SEM figures (× 3000 times) of composite powder after ball milling.
Fig. 2 is the BSE figures (× 1000 times) of nano-sized carbon enhancing Cu-base composites.
Fig. 3 is the EDS results of nano-sized carbon enhancing Cu-base composites matrix.
Fig. 4 is the SEM figures (× 80000 times) of the compression fracture of nano-sized carbon enhancing Cu-base composites.
Fig. 5 is the SEM figures (× 20000 times) of the shear fracture of nano-sized carbon enhancing Cu-base composites.
Specific implementation mode
With reference to test example and specific implementation mode, the present invention is described in further detail.But this should not be understood
It is only limitted to embodiment below for the range of the above-mentioned theme of the present invention, it is all that this is belonged to based on the technology that the content of present invention is realized
The range of invention.Carbon nanotube and graphene involved in present example are purchased from the Chinese Academy of Sciences and transmit the limited public affairs of organic chemistry
Department.
<Embodiment 1>
Modified carbon nano-tube
By carbon nanotube by being added in the gallic acid aqueous solution of 10 μ g/mL, ultrasonic disperse 30min, wherein carbon nanometer
The ratio between the weight of pipe and the volume of gallic acid aqueous solution are 0.1g:40mL；Standing filters afterwards for 24 hours, goes filter residue true at 60 DEG C
The dry 2h of sky, obtains the carbon nanotube being modified by surface.
By comparing the shape characteristic of the carbon nanotube being modified by surface and the carbon nanotube being modified without surface, hair
The carbon nanotube being now modified without surface is in the cotton-shaped or pencil of group, bad dispersibility；The carbon nano tube surface being modified by surface
It is bright and clean, it is observed that many single carbon nanotubes, and draw ratio variation is little.
The surface treated carbon nanotube 0.1g prepared in the present embodiment 1 is dispersed in 100mL deionized waters,
After standing 5 days, precipitation gradually increases under the effect of gravity, but dispersity is still maintained between carbon nanotube；Simultaneously with without
The carbon nanotube for crossing surface modification compares, and starts to precipitate after standing 1 day, and reunite.Show prepared by embodiment 1
By surface be modified carbon nanotube have excellent dispersibility.
<Embodiment 2>
Modified carbon nano-tube
According to the method for embodiment 1, change a concentration of 5 μ g/mL, the 15 μ g/mL of gallic acid aqueous solution, remaining with reality
It applies that example 1 is identical, respectively obtains the carbon nanotube of surface modification.
The gallic acid aqueous solution surface treatment through a concentration of 5 μ g/mL, 15 μ g/mL respectively that will be prepared in the present embodiment 2
Carbon nanotube 0.1g be dispersed in 100mL deionized waters, stand 2~3 days after, under the effect of gravity precipitation gradually increase
It is more, but dispersity is still maintained between carbon nanotube.
In conjunction with the embodiments 1 and embodiment 2 as a result, through gallic acid aqueous solution surface it is modified carbon nanotube dispersibility
Good, impurity content reduces；And the effect that surface is modified as a concentration of 10 μ g/mL of gallic acid aqueous solution is best.
<Embodiment 3>
Modified graphene
By graphene by being added in the rutin aqueous solution of 0.02 μ g/mL, ultrasonic disperse 30min, the wherein weight of graphene
The ratio between amount and the volume of rutin aqueous solution are 0.1g:40mL；Standing filters afterwards for 24 hours, goes filter residue to be dried in vacuo 2h at 60 DEG C, obtains
To the graphene being modified by surface.
By comparing the SEM figures of the graphene that is modified by surface and the graphene being modified without surface, discovery without
The graphene of surface modification is crossed in the cotton-shaped or pencil of group, bad dispersibility；The graphene surface being modified by surface is bright and clean, Ke Yiguan
Many single graphenes are observed, and change in size is little.
The surface treated graphene 0.1g prepared in the present embodiment 3 is dispersed in 100mL deionized waters, it is quiet
After setting 5 days, precipitation gradually increases under the effect of gravity, but dispersity is still maintained between graphene；Simultaneously with without table
The graphene that face is modified compares, and starts to precipitate after standing 1 day, and reunite.Show process prepared by embodiment 3
The graphene that surface is modified has excellent dispersibility.
<Embodiment 4>
Modified graphene
According to the method for embodiment 3, change a concentration of 0.01 μ g/mL, the 0.04 μ g/mL of gallic acid aqueous solution, remaining
It is same as Example 3, respectively obtain the carbon nanotube of surface modification.
The gallic acid aqueous solution table through a concentration of 0.01 μ g/mL, 0.04 μ g/mL respectively that will be prepared in the present embodiment 4
The carbon nanotube 0.1g of surface treatment is dispersed in 100mL deionized waters, stand 2~3 days after, precipitate under the effect of gravity by
It is cumulative more, but dispersity is still maintained between carbon nanotube.
In conjunction with the embodiments 3 and embodiment 4 as a result, through gallic acid aqueous solution surface it is modified carbon nanotube dispersibility
Good, impurity content reduces；And the effect that surface is modified as a concentration of 0.02 μ g/mL of gallic acid aqueous solution is best.
<Embodiment 5>
Cu-base composites
(1) carbon nanotube being modified by surface in Example 1；(2) by weight, using agate ball and agate
Spherical tank by 1 part by surface be modified carbon nanotube, 6.5 parts of powdered graphites, 2 parts of chromium powder ends, 4 parts of lead powder ends, 6 parts of tin powders,
0.4 part of zirconium powder, 0.1 part of lanthanum powder and 80 parts of copper powders carry out ball milling and mix powder, and rotating speed is 350 turns/min, and Ball-milling Time is
50min；(3) composite powder is subjected to cold moudling, pressure 600MPa；(4) obtained block materials are subjected to hot isostatic pressing
2h, HIP sintering temperature are 900 DEG C, pressure 100MPa, rapid cooling, obtain nano-sized carbon enhancing Cu-base composites.
<Embodiment 6>
Cu-base composites
The graphene being modified by surface in Example 3；(2) by weight, using agate ball and agate spherical tank
Graphene, 6.5 parts of powdered graphites, 2 parts of chromium powder ends, 4 parts of lead powder ends, 6 parts of tin powders, the 0.4 part of zirconium that 1 part is modified by surface
Powder, 0.1 part of lanthanum powder and 80 parts of copper powders carry out ball milling and mix powder, and rotating speed is 300 turns/min, Ball-milling Time 60min；(3)
Composite powder is subjected to cold moudling, pressure 600MPa；(4) obtained block materials are subjected to hot isostatic pressing 2h, heat etc. is quiet
It is 900 DEG C, pressure 90MPa to press sintering temperature, rapid cooling, obtains nano-sized carbon enhancing Cu-base composites.
<Embodiment 7>
Cu-base composites
The carbon nanotube being modified by surface in Example 1, the graphite being modified by surface in Example 3
Alkene；(2) by weight, carbon nanotube, the 0.5 part of process being modified 0.5 part by surface using agate ball and agate spherical tank
The graphene of surface modification, 6.5 parts of powdered graphites, 2 parts of chromium powder ends, 4 parts of lead powder ends, 6 parts of tin powders, 0.4 part of zirconium powder, 0.1
Part lanthanum powder and 80 parts of copper powders carry out ball millings and mix powder, and rotating speed is 350 turns/min, Ball-milling Time 60min；(3) by composite powder
End carries out cold moudling, pressure 600MPa；(4) obtained block materials are subjected to hot isostatic pressing 2h, HIP sintering temperature
Degree is 900 DEG C, pressure 100MPa, rapid cooling, obtains nano-sized carbon enhancing Cu-base composites.
<Embodiment 8>
Cu-base composites
The carbon nanotube being modified by surface in Example 1, the graphite being modified by surface in Example 3
Alkene；(2) by weight, carbon nanotube, the 0.1 part of process being modified 0.8 part by surface using agate ball and agate spherical tank
The graphene of surface modification, 6.5 parts of powdered graphites, 2 parts of chromium powder ends, 4 parts of lead powder ends, 6 parts of tin powders, 0.4 part of zirconium powder, 0.1
Part lanthanum powder and 80 parts of copper powders carry out ball millings and mix powder, and rotating speed is 350 turns/min, Ball-milling Time 60min；(3) by composite powder
End carries out cold moudling, pressure 600MPa；(4) obtained block materials are subjected to hot isostatic pressing 2h, HIP sintering temperature
Degree is 900 DEG C, pressure 100MPa, rapid cooling, obtains nano-sized carbon enhancing Cu-base composites.
<Comparative example 1>
Cu-base composites
(1) by weight, using agate ball and agate spherical tank by 7.5 parts of powdered graphites, 2 parts of chromium powder ends, 4 parts of lead powder
End, 6 parts of tin powders, 0.4 part of zirconium powder, 0.1 part of lanthanum powder and 80 parts of copper powders carry out ball milling and mix powder, and rotating speed is 350 turns/min,
Ball-milling Time is 60min；(2) composite powder is subjected to cold moudling, pressure 600MPa；(3) by obtained block materials into
Row hot isostatic pressing 2h, HIP sintering temperature are 900 DEG C, and pressure 100MPa, rapid cooling obtains Cu-base composites.
<Comparative example 2>
Cu-base composites
(1) by weight, the modification stone prepared by modified carbon nano-tube prepared by 2 parts of embodiments 1,0.5 part of embodiment 3
Black alkene, 5 parts of powdered graphites, 3 parts of chromium powder ends, 3.5 parts of lead powder ends, 4 parts of tin powders, 0.2 part of lanthanum powder and 81.8 parts of copper powders are mixed
It closes, carrying out ball milling using agate ball and agate spherical tank mixes powder, and rotating speed is 350 turns/min, Ball-milling Time 60min；It (2) will be compound
Powder carries out cold moudling, pressure 600MPa；(3) obtained block materials are subjected to hot isostatic pressing 2h, HIP sintering
Temperature is 900 DEG C, and pressure 100MPa, rapid cooling obtains Cu-base composites.
<Comparative example 3>
Cu-base composites
(1) by weight, the modified carbon nano-tube that is prepared 2 parts of embodiments 1 using agate ball and agate spherical tank, 0.5
Modified graphene, 5 parts of powdered graphites, 4 parts of lead powder ends, 6 parts of tin powders, 0.4 part of zirconium powder, 0.1 part of lanthanum prepared by part embodiment 3
Powder and 82 parts of copper powders carry out ball milling and mix powder, and rotating speed is 350 turns/min, Ball-milling Time 60min；(2) by composite powder into
Row cold moudling, pressure 600MPa；(3) obtained block materials are subjected to hot isostatic pressing 2h, HIP sintering temperature is
900 DEG C, pressure 100MPa, rapid cooling obtains Cu-base composites.
<Comparative example 4>
Cu-base composites
(1) by weight, the modified carbon nano-tube that is prepared 2 parts of embodiments 1 using agate ball and agate spherical tank, 0.5
Modified graphene prepared by part embodiment 3,5 parts of powdered graphites, 2 parts of chromium powder ends, 10 parts of tin powders, 0.4 part of zirconium powder, 0.1 part
Lanthanum powder and 80 parts of copper powders carry out ball milling and mix powder, and rotating speed is 350 turns/min, Ball-milling Time 60min；(2) by composite powder
Carry out cold moudling, pressure 600MPa；(3) obtained block materials are subjected to hot isostatic pressing 2h, HIP sintering temperature
It it is 900 DEG C, pressure 100MPa, rapid cooling obtains Cu-base composites.
<Comparative example 5>
Cu-base composites
(1) by weight, the modified carbon nano-tube that is prepared 2 parts of embodiments 1 using agate ball and agate spherical tank, 0.5
Modified graphene, 5 parts of powdered graphites, 3 parts of chromium powder ends, 5 parts of lead powder ends, 0.4 part of zirconium powder, 0.1 part of lanthanum prepared by part embodiment 3
Powder and 84 parts of copper powders carry out ball milling and mix powder, and rotating speed is 350 turns/min, Ball-milling Time 60min；(2) by composite powder into
Row cold moudling, pressure 600MPa；(3) obtained block materials are subjected to hot isostatic pressing 2h, HIP sintering temperature is
900 DEG C, pressure 100MPa, rapid cooling obtains Cu-base composites.
<Test 1>
The Cu-base composites being prepared using the test above-described embodiment such as electron microscope, the test of section Example
As a result as follows：
Fig. 1 is the SEM pictures of the composite powder after ball milling in embodiment 5, and the carbon nanotube being modified by surface in figure is equal
Even to be dispersed between copper particle, the graphite dispersion of sheet is embedded between copper particle；Due to the mechanism in mechanical milling process,
A series of variations such as particle deformation, rupture and cold welding occur, form copper particle cluster.
In embodiment 5~8, under higher amplification factor, it is crushed it is observed that reinforced phase generation is certain, one
The size for determining reinforced phase in degree reduces, this is because caused by the mechanism of ball milling；With rotational speed of ball-mill and Ball-milling Time
Increase, the evenly dispersed degree of reinforced phase increases, but also increases the destruction of reinforced phase, considers, best rotational speed of ball-mill
For 350 turns/min, ball milling 60min.
Fig. 2 is the BSE pictures of gained nano-sized carbon enhancing Cu-base composites in embodiment 7, and Fig. 3 is Copper substrate in Fig. 2
EDS results.Fig. 2 shows that nano-sized carbon and graphite are interspersed with Copper substrate, and overall distribution is uniform.EDS results table shown in Fig. 3
Bright chromium, lead, tin, zirconium, lanthanum are dissolved into Copper substrate, and the counterdiffusion of element phase, is uniformly distributed in the base in sintering process.
Fig. 4 is the SEM pictures of the compression fracture of Cu-base composites prepared by embodiment 5, it is observed that being deposited on fracture
Carbon nanotube in the base is inlayed with one end in some fractures, in the fracture of Cu-base composites prepared by other embodiment
Above it is similarly observed that broken carbon nanotube and broken graphene, and these broken carbon nanotubes exist with the graphene being crushed
Play a part of bridging and load transmission in Cu-base composites.
Fig. 5 is the SEM figures (× 20000 of the shear fracture of the nano-sized carbon enhancing Cu-base composites prepared in embodiment 7
Times).SEM figures are disconnected from shearing and can be seen that carbon nanotube and graphene dispersion are embedded in Copper substrate, play humidification；Piece
The graphite of stratiform is also embedded in Copper substrate, due to the self-lubricating function of graphite, can significantly improve its friction and wear behavior.
<Test 2>
Density, the consistency of Cu-base composites obtained by above-described embodiment and comparative example are measured using Archimedes method,
And its micro-vickers hardness, compression strength and shear strength are measured, the results are shown in Table 1.
The experimental result of table 1 embodiment 5~8 and comparative example
| Group | Density | Consistency | Vickers hardness | Compression strength | Shear strength |
| Embodiment 5 | 6.71 | 93.58 | 56.86 | 178.62 | 77.45 |
| Embodiment 6 | 6.92 | 96.51 | 58.94 | 194.36 | 78.64 |
| Embodiment 7 | 6.62 | 92.33 | 56.72 | 188.15 | 75.16 |
| Embodiment 8 | 6.78 | 94.56 | 60.12 | 215.89 | 82.23 |
| Comparative example 1 | 6.83 | 95.13 | 36.89 | 126.35 | 48.12 |
| Comparative example 2 | 6.68 | 93.25 | 42.61 | 147.63 | 52.08 |
| Comparative example 3 | 6.75 | 94.06 | 44.32 | 153.06 | 56.86 |
| Comparative example 4 | 6.78 | 94.82 | 44.42 | 149.16 | 51.40 |
| Comparative example 5 | 6.61 | 92.19 | 40.89 | 143.25 | 50.75 |
In table, the unit of every test result is as follows：Density (g/cm3), consistency (%), Vickers hardness (HV), resistance to compression
Intensity (MPa), shear strength (MPa).
As seen from the results in Table 1, the Cu-base composites that the Cu-base composites that prepared by embodiment 8 are prepared with embodiment 5~7
Compare, micro-vickers hardness has been respectively increased 3.26HV, 1.18HV, 13.4HV, compression strength be respectively increased 37.27MPa,
12.78MPa, 3.69MPa, 10.07MPa is respectively increased in 21.53MPa, 107.74MPa, shear strength.Therefore prepared by embodiment 8
The Cu-base composites that are prepared relative to embodiment 5~7 of Cu-base composites, there are more excellent hardness and strength, it is real
Apply the optimum implementation that example 8 is Cu-base composites of the present invention.
Comparative example 1-5 lacks part adding ingredient respectively, and the mechanical property of Cu-base composites is caused to significantly reduce.And reality
It applies a full formula prepared by 5-8 Cu-base composites is made and compare, since preparation process is identical, consistency is not much different.Vickers
Hardness maximum reduces 23.23HV.Compression strength maximum in mechanical property reduces 89.54MPa, shear strength reduces
34.11MPa.Wherein, the reduced performance for lacking the Cu-base composites of two kinds of nano-sized carbons is the most apparent, shows the enhancing of nano-sized carbon
Function and effect are better than other compositions.
By to the analysis of the performance test results of embodiment and comparative example, only when the composition of Cu-base composites by weight
Percentage is the carbon nanotube 0.1~5% being modified by surface, the graphene 0.1~5%, the powdered graphite 2 that are modified by surface
~10%, chromium powder end 1~4%, lead powder end 1~8%, tin powder 2~10%, zirconium powder 0.1~1%, lanthanum powder 0.01~
0.5%, when surplus is copper powders, it can be only achieved effect of the present invention.
<Test 3>
Cu-base composites obtained by above-described embodiment and comparative example are processed into standard component, test different embodiments, right
Cu-base composites wear with current coefficient obtained by ratio, test method are in 5ms-1Friction velocity under, current strength is
20A, pressure size are respectively 5N, 10N, 20N, 30N and 50N, test acquired results such as the following table 2.
The Cu-base composites wear with current coefficient of 2 embodiment 5~8 of table and comparative example
| Wear rate | Pressure 5N | Pressure 10N | Pressure 20N | Pressure 30N | Pressure 50N |
| Embodiment 5 | 0.24 | 0.36 | 0.55 | 0.80 | 1.11 |
| Embodiment 6 | 0.25 | 0.36 | 0.58 | 0.81 | 1.13 |
| Embodiment 7 | 0.23 | 0.35 | 0.56 | 0.79 | 1.16 |
| Embodiment 8 | 0.19 | 0.33 | 0.50 | 0.73 | 1.05 |
| Comparative example 1 | 0.67 | 0.88 | 1.03 | 1.15 | 1.54 |
| Comparative example 2 | 0.51 | 0.69 | 0.81 | 0.98 | 1.32 |
| Comparative example 3 | 0.52 | 0.68 | 0.80 | 0.95 | 1.36 |
| Comparative example 4 | 0.57 | 0.78 | 0.93 | 1.10 | 1.37 |
| Comparative example 5 | 0.56 | 0.62 | 0.86 | 1.05 | 1.34 |
* wear rate unit, mgm-1。
Cu-base composites prepared by the embodiment of the present invention known to upper table test result, the formula by optimization design are real
Having showed the mutual matching relationship optimization of different materials improves, and the performance of each component generates the effect of collaboration enhancing, significantly carries
The performances such as the intensity of high Cu-base composites and current-carrying frictional wear, reduce the density of Cu-base composites.When copper-based multiple
Condensation material different from pressure condition under tested when, the coefficient of waste of material is generally held in reduced levels, no
Easily occur largely wearing because of the variation of pressure increasing, shows the wear with current and tradition of the Cu-base composites of the present invention
The abrasion mechanism of Copper substrate conductive material essential change has occurred, comprehensive performance is improved significantly.
And Cu-base composites prepared by comparative example scheme, it is reduced according to different ingredients, it can be seen that different degrees of
Performance degradation, abrasion mechanism are still similar to traditional copper matrix conductive material, can be with the variation of current-carrying intensity, the intensity of pressure
There is wear extent quickly increased variation, so cannot meet extraordinary using working condition requirement.
Claims (9)
1. a kind of nano-sized carbon enhances Cu-base composites, it is characterised in that：Carbon nanotube 0.1 ~ 5%, the process being modified by surface
The graphene 0.1 ~ 5% of surface modification, powdered graphite 2 ~ 10%, chromium powder end 1 ~ 4%, lead powder end 1 ~ 8%, tin powder 2 ~ 10%, zirconium powder
0.1 ~ 1%, lanthanum powder 0.01 ~ 0.5%, surplus are copper powders；
The carbon nanotube being wherein modified by surface is that carbon nanotube is used the carbon nanometer that gallic acid aqueous solution is modified
Pipe, the graphene being modified by surface are that graphene is used the graphene that rutin aqueous solution is modified.
2. Cu-base composites according to claim 1, it is characterised in that：
The carbon nanotube being modified by surface is made through following methods：Carbon nanotube is added to gallic acid aqueous solution
In, ultrasonic disperse is static, and filtering takes filter residue to be dried in vacuo, and obtains the carbon nanotube being modified by surface；
The graphene being modified by surface is made through following methods：Graphene is added in rutin aqueous solution, ultrasound point
It dissipates, static, filtering takes filter residue to be dried in vacuo, and obtains the graphene being modified by surface.
3. Cu-base composites according to claim 2, it is characterised in that：A concentration of the 5 of the gallic acid aqueous solution ~
15μg/mL；A concentration of 0.01 ~ 0.1 μ g/mL of the rutin aqueous solution.
4. Cu-base composites according to claim 2, it is characterised in that：The quality and gallic acid of the carbon nanotube
The volume ratio of aqueous solution is 0.05 ~ 0.4g：20~80mL；
The quality of the graphene is 0.05 ~ 0.4g with the volume ratio of rutin aqueous solution：20~80mL.
5. Cu-base composites according to claim 2, it is characterised in that：The time of the ultrasonic disperse be 20 ~
40min；The static time is 12 ~ 36h；The vacuum drying temperature is 60 DEG C ~ 80 DEG C, the vacuum drying time
For 1 ~ 8h.
6. a kind of preparation method of Cu-base composites as described in claim 1 ~ 5, which is characterized in that include the following steps：
(1) carbon nanotube is added in gallic acid aqueous solution, ultrasonic disperse is static, filtering, takes filter residue to carry out vacuum dry
It is dry, obtain the carbon nanotube being modified by surface；
(2) graphene is added in rutin aqueous solution, ultrasonic disperse is static, and filtering takes filter residue to be dried in vacuo, and obtains
The graphene being modified by surface；
(3) graphene for being modified the carbon nanotube being modified by surface and surface and copper powders, powdered graphite, chromium powder end, lead
Powder, tin powder, zirconium powder, lanthanum powder carry out ball milling, obtain composite powder；
(4) composite powder is subjected to cold moudling, obtains composite material green compact；
(5) composite material green compact is subjected to HIP sintering, it is cooling, obtain nano-sized carbon enhancing Cu-base composites.
7. preparation method according to claim 6, it is characterised in that：Ball milling uses agate ball and agate in the step (3)
Nao spherical tanks, rotational speed of ball-mill are 200 ~ 450 turns/min, and Ball-milling Time is 40 ~ 120min.
8. preparation method according to claim 6, it is characterised in that：The pressure that cold moudling is suppressed in the step (4)
For 400 ~ 700MPa.
9. preparation method according to claim 6, it is characterised in that：The temperature of HIP sintering in the step (5)
It it is 800 ~ 1000 DEG C, the pressure of HIP sintering is 80 ~ 100MPa, and the time of HIP sintering is 1 ~ 3h.
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