CN109439964A - Carbon nanotube-graphene collaboration reinforced aluminum matrix composites mechanical property preparation method - Google Patents

Carbon nanotube-graphene collaboration reinforced aluminum matrix composites mechanical property preparation method Download PDF

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CN109439964A
CN109439964A CN201811047083.4A CN201811047083A CN109439964A CN 109439964 A CN109439964 A CN 109439964A CN 201811047083 A CN201811047083 A CN 201811047083A CN 109439964 A CN109439964 A CN 109439964A
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carbon nanotube
graphene
powder
carbon
mixed
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何春年
杨立壮
赵乃勤
沙军威
师春生
唐宇
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Tianjin University
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Tianjin University
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • 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
    • B22F3/10—Sintering only
    • B22F3/1003—Use of special medium during sintering, e.g. sintering aid
    • B22F3/1007—Atmosphere
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • 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
    • B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • 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
    • 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
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26—Deposition of carbon only
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • 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
    • B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
    • B22F2003/208—Warm or hot extruding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • 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

Abstract

The present invention relates to a kind of carbon nanotube-graphene collaboration reinforced aluminum matrix composites mechanical property preparation methods, steps are as follows: preparation carbon nanotube-graphene composite strengthening phase: using sucrose as carbon source, using nickel powder as template, using pluronic F127 as dispersing agent, it is dissolved in deionized water jointly with carbon nanotube, it is adequately stirred, obtains mixed solution；It while being stirred solution and heats, so that water sufficiently evaporates, obtains mixed-powder；The mixed-powder of above-mentioned acquisition is placed in Noah's ark, the flat-temperature zone that Noah's ark is put into high temperature process furnances is then subjected to chemical vapour deposition reaction；By reaction product as sufficiently being corroded in iron chloride corrosive liquid；The molding of carbon nanotube-graphene reinforced aluminum matrix composites.

Description

The preparation of carbon nanotube-graphene collaboration reinforced aluminum matrix composites mechanical property Method
Technical field
The present invention relates to a kind of preparations that aluminum matrix composite mechanical property is promoted using cold pressing-sintering molding mode Method belongs to field of powder metallurgy.
Background technique
After metal-base composites is suggested for the first time many years ago, metal-base composites is due to its excellent physics It is had received widespread attention with mechanical property.Currently, metal-base composites is widely used in, aerospace etc. is civilian and national defence In industry.Wherein, aluminum matrix composite is applied since ductility is good, machinability is strong, high conductivity, high thermal conductivity and good Corrosion resistance is widely used.But the comprehensive performance of required aluminium and its alloy was wanted due to industrial boom in recent years It is also higher and higher for asking, so traditional preparation and enhancements is no longer satisfied current demand.Therefore, it prepares novel Aluminum matrix composite is the hot spot studied at present.
Compared to traditional reinforced phase, such as ceramic particle, whisker and fiber etc., in recent years, carbon nanomaterial is due to having Extensive concern of the excellent performance by researchers, especially carbon nanotube and graphene.This is because carbon nanotube and stone Black alkene all has the intensity and modulus of superelevation and has high stability, promises to be the ideal of metal-base composites Reinforced phase.Simultaneously as carbon nanotube and graphene all have good conductive and heating conduction, it can be used as reinforcement and be expected to Increase substantially the comprehensive performance of aluminum matrix composite.But due to problems such as dispersibilities, so that the carbon nanotube of preparation Ideal effect is never obtained with graphene reinforced aluminum matrix composites.Therefore, how carbon nanotube and graphene to be improved Enhancing efficiency will become metal-base composites future studies the most important thing.In the research of many functional materials, by carbon Nanotube-graphene alkene mutually prepares composite material as composite strengthening and has been achieved for many excellent achievements, for example, photocatalysis, In electro-catalysis, supercapacitor and lithium ion battery, carbon nanotube-graphene has just played good synergistic effect.This is It is combined because very strong pi-pi bond can be formed between graphene and carbon nanotube, so that carbon nanotube shape on the surface of graphene Structure is reticulated, while graphene intensity can be improved, the load transmission efficiency of graphene also can be enhanced.Therefore, it studies Carbon nanotube-graphene collaboration reinforced aluminum matrix composites have very important significance.
Summary of the invention
It is an object of the invention to propose a kind of graphene of novel carbon nanotube enhancing as composite strengthening Xiang Laizeng The preparation method of strong aluminum matrix composite, mainly by loading netted carbon nanotube on the surface of graphene and passing through chemical bond In conjunction with final to realize being obviously improved for aluminum matrix composite mechanical property.To achieve the above object, the present invention passes through following technology Scheme is realized.
A kind of preparation method of carbon nanotube-graphene collaboration reinforced aluminum matrix composites mechanical property, steps are as follows:
(1) carbon nanotube-graphene composite strengthening phase is prepared: using sucrose as carbon source, using nickel powder as template, with pluronic F127 is dispersing agent, is dissolved in deionized water jointly with carbon nanotube, is adequately stirred, obtain mixed solution, wherein carbon The molar ratio of carbon in nanotube and sucrose is 1:10~30.
(2) it while being stirred solution and heats, so that water sufficiently evaporates, and makes carbon nanotube and sucrose in nickel Powder surface uniform load obtains mixed-powder, then is dried；
(3) mixed-powder by above-mentioned acquisition is placed in Noah's ark, then Noah's ark is put into the constant temperature of high temperature process furnances Area carries out chemical vapour deposition reaction, carries out in the mixed gas that synthesis condition is argon gas and hydrogen ratio is 2:1~3:1 anti- It answers, synthesis temperature is 900~1000 DEG C, and heating rate is 5 DEG C/min~10 DEG C/min, is after reaction carried out sample quick Cooling, obtains reaction product；
(4) by reaction product as sufficiently being corroded in iron chloride corrosive liquid, so that nickel particle is corroded, after dry It obtains；
(5) carbon nanotube-graphene reinforced aluminum matrix composites molding: the carbon nanotube that will first be obtained in step (1) The graphene of enhancing is first adequately ground, and is made to reunite and be reduced.Secondly, the graphene that carbon nanotube enhances is placed in aluminium powder In stainless steel jar mill, wherein wherein ratio of grinding media to material is 1:10, using argon gas as protective gas, mixed-powder is subjected to speed change ball milling The graphene for enhancing carbon nanotube is evenly dispersed in aluminium powder.Finally, the powder after ball milling first to be carried out to 500-600Mpa's Cold moudling carries out the sintering of 1h under conditions of temperature is 600-630 DEG C later, selects argon gas for protective atmosphere, after sintering Block materials carry out hot extrusion under the conditions of 500~600 DEG C, obtain the rodlike compound of carbon nanotube-graphene enhancing later Material.
The method that the present invention uses chemical vapor deposition first prepares the graphene of carbon nanotube enhancing, can make carbon nanometer Pipe and graphene form strong chemical bond in surface formation reticular structure between carbon nanotube and graphene, prepare Composite strengthening phase out.Secondly, the method by speed change ball milling is adequately mixed composite strengthening phase and aluminium powder, graphite is kept Alkene is sufficiently mixed in aluminium powder while guaranteeing that the quality of graphene is not seriously damaged again.Finally, passing through cold-rolled sintered-hot extrusion Mode prepare rodlike composite material.By the graphene of preparation carbon nanotube enhancing, the intensity of graphene not only can be improved, but also The load transmission efficiency of graphene can be effectively improved, so that the mechanical property of aluminum matrix composite is significantly improved.
Detailed description of the invention
Fig. 1 is the SEM figure that embodiment 1 prepares carbon nanotube used in carbon nanotube enhancing graphene.Carbon is shown in figure The diameter of nanotube is about 50nm or so.
Fig. 2 is the SEM figure that carbon nanotube made from embodiment 1 enhances graphene.It can significantly be observed from the figure It is carbon nanotube loaded to combine closely on the surface of graphene and with graphene, and form reticular structure.
Fig. 3 (a) is the Raman spectrogram that carbon nanotube made from embodiment 1 enhances graphene.It can be into one from the figure Step proves the structural intergrity of graphene, has less defect.
Fig. 3 (b) is the XRD that carbon nanotube made from embodiment 1 enhances graphene.It can see in sample XRD from the figure Only exist graphene peak, it was demonstrated that graphite olefinic impurity obtained is considerably less.
Fig. 4 is the TEM figure that carbon nanotube made from embodiment 1 enhances graphene.As can be seen from the figure in carbon nanometer Pipe is distributed on graphene and combines closely with graphene.
Fig. 5 is the load-deformation curve of fine aluminium made from composite material made from the embodiment of the present invention 1 and comparative example 1.
Specific embodiment
Illustrate the present invention below with reference to specific example, but is not intended to limit the present invention.
Embodiment 1
(1) firstly, nickel powder, sucrose and dispersing agent are placed in 150ml deionized water, then load weighted carbon nanotube is set It in 25ml water, is put into cell disruptor and carries out ultrasonic disperse, carbon nano-tube solution is then put into nickel powder, sucrose and dispersion It in the mixed solution of agent, is placed in blender and stirs and heat, heating temperature is 120 DEG C, after water evaporation, obtains mixed powder End.Mixed-powder is placed in the vacuum oven that temperature is 70 DEG C again and is dried.
(2) mixed-powder obtained in step 1 is placed in tube furnace and carries out chemical synthesis, synthesis atmosphere be argon gas with Hydrogen ratio is the mixed gas of 2:1~3:1, and synthesis temperature is 950 DEG C, and heating rate is 5 DEG C/min~10 DEG C/min, reaction After sample is subjected to fast cooling, obtain mixed-powder.By the powder obtained after reaction as in iron chloride corrosive liquid into Row sufficiently corrosion, it is known that nickel particle is eroded completely.Powder will finally be obtained to be dried, obtain the stone of carbon nanotube enhancing Black alkene.
(3) graphene that carbon nanotube made from step (1)-(2) enhances is pressed by mass fraction 0.4% and 15g aluminium powder Ratio of grinding media to material is that 1:10 is placed in the stainless steel jar mill of 250ml, and aluminum shot diameter is 20-30 μm, and argon gas is poured in ball grinder.It will Mixed-powder carries out the speed change ball milling of 200 turns of 2h and 300 turn of 2h respectively.Mixed composite powder is first carried out 600MPa, Then the cold pressing of 3min carries out the sintering of 630 DEG C, 1h in an argon atmosphere, then by obtained block materials under the conditions of 550 DEG C Hot extrusion is carried out, obtains the rodlike composite material of carbon nanotube-graphene enhancing later.
(4) tensile sample is prepared with rodlike composite material obtained, carries out tensile property test.
Carbon nanotube prepared by this example-graphene reinforced aluminum matrix composites are under cold-rolled sintered-hot extrusion pressure condition Tensile strength be 174.5MPa, elongation percentage 28.23%, as a result as shown in 1 curve of embodiment in Fig. 5.
Comparative example 1
It (1) is that 1:10 is placed in the stainless steel jar mill of 250ml by ratio of grinding media to material by 15g aluminium powder, aluminum shot diameter is 20-30 μm, And argon gas is poured in ball grinder.Mixed-powder is carried out to the speed change ball milling of 200 turns of 2h and 300 turn of 2h respectively.It will be mixed Composite powder first carries out the cold pressing of 600MPa, 3min, then carry out 630 DEG C, the sintering of 1h in an argon atmosphere, then will obtain Block materials carry out hot extrusion under the conditions of 550 DEG C, obtain the rodlike composite material of carbon nanotube-graphene enhancing later.
(2) tensile sample is prepared with rodlike composite material obtained, carries out tensile property test.
Tensile strength of the fine aluminium prepared by this example under cold-rolled sintered-hot extrusion pressure condition is 125MPa, and elongation percentage is 25.3%, as a result as shown in 1 curve of comparative example in Fig. 5.

Claims (1)

1. a kind of carbon nanotube-graphene collaboration reinforced aluminum matrix composites mechanical property preparation method, steps are as follows:
(1) carbon nanotube-graphene composite strengthening phase is prepared: using sucrose as carbon source, using nickel powder as template, with pluronic F127 For dispersing agent, it is dissolved in deionized water jointly with carbon nanotube, is adequately stirred, obtain mixed solution, wherein carbon nanometer The molar ratio of pipe and the carbon in sucrose is 1:10~30.
(2) it while being stirred solution and heats, so that water sufficiently evaporates, and makes carbon nanotube and sucrose in nickel powder table Face uniform load obtains mixed-powder, then is dried；
(3) mixed-powder by above-mentioned acquisition is placed in Noah's ark, then Noah's ark is put into the flat-temperature zones of high temperature process furnances into Row chemical vapour deposition reaction, it with hydrogen ratio is to be reacted in the mixed gas of 2:1~3:1 that synthesis condition, which is argon gas, is closed It is 900~1000 DEG C at temperature, heating rate is 5 DEG C/min~10 DEG C/min, sample is subjected to fast cooling after reaction, Obtain reaction product；
(4) reaction product, so that nickel particle is corroded, is obtained as sufficiently being corroded in iron chloride corrosive liquid after dry It arrives；
(5) carbon nanotube-graphene reinforced aluminum matrix composites molding: first the carbon nanotube obtained in step (1) is enhanced Graphene first adequately ground, make reunite reduce.Secondly, the graphene of carbon nanotube enhancing is placed in aluminium powder stainless In steel ball grinding jar, wherein wherein ratio of grinding media to material is 1:10, using argon gas as protective gas, mixed-powder progress speed change ball milling is made into carbon The graphene of nanotube enhancing is evenly dispersed in aluminium powder.Finally, the powder after ball milling first to be carried out to the cold pressing of 500-600Mpa Molding carries out the sintering of 1h under conditions of temperature is 600-630 DEG C later, selects argon gas for protective atmosphere, and sintered piece Body material carries out hot extrusion under the conditions of 500~600 DEG C, obtains the rodlike composite material of carbon nanotube-graphene enhancing later.
CN201811047083.4A 2018-09-08 2018-09-08 Carbon nanotube-graphene collaboration reinforced aluminum matrix composites mechanical property preparation method Pending CN109439964A (en)

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Cited By (5)

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CN110331307A (en) * 2019-08-14 2019-10-15 黑龙江科技大学 A kind of graphene carbon nanotube hybrid buildup aluminium bearing material and preparation method thereof
CN110539002A (en) * 2019-09-27 2019-12-06 天津大学 Method for enhancing mechanical property of aluminum matrix composite material by cooperation of multi-element multi-dimensional enhanced phase
CN110576187A (en) * 2019-09-19 2019-12-17 天津大学 preparation method for in-situ synthesis of three-dimensional graphene/one-dimensional carbon nanotube loaded copper nanoparticle material
CN110918978A (en) * 2019-12-16 2020-03-27 哈尔滨工程大学 Reinforcing phase reinforced composite powder with functional layer for use in fusing technology, and preparation method and application thereof
CN111996418A (en) * 2020-08-28 2020-11-27 福州大学 Three-dimensional carbon nano-phase composite reinforced aluminum-based material and preparation method thereof

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CN110918978A (en) * 2019-12-16 2020-03-27 哈尔滨工程大学 Reinforcing phase reinforced composite powder with functional layer for use in fusing technology, and preparation method and application thereof
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CN111996418A (en) * 2020-08-28 2020-11-27 福州大学 Three-dimensional carbon nano-phase composite reinforced aluminum-based material and preparation method thereof
CN111996418B (en) * 2020-08-28 2021-11-02 福州大学 Three-dimensional carbon nano-phase composite reinforced aluminum-based material and preparation method thereof

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