CN110453107A - Graphene-tungsten carbide collaboration enhancing Cu-base composites preparation method - Google Patents

Graphene-tungsten carbide collaboration enhancing Cu-base composites preparation method Download PDF

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CN110453107A
CN110453107A CN201910706269.4A CN201910706269A CN110453107A CN 110453107 A CN110453107 A CN 110453107A CN 201910706269 A CN201910706269 A CN 201910706269A CN 110453107 A CN110453107 A CN 110453107A
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powder
graphene
copper
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tungsten carbide
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CN110453107B (en
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何春年
徐志航
赵乃勤
师春生
沙军威
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Tianjin University
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    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/17—Metallic particles coated with metal
    • 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
    • B22F3/001—Starting from powder comprising reducible metal compounds
    • 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
    • B22F3/12—Both compacting and sintering
    • B22F3/14—Both compacting and sintering simultaneously
    • 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
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
    • 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
    • C22C1/058—Mixtures of metal powder with non-metallic powder by reaction sintering (i.e. gasless reaction starting from a mixture of solid metal compounds)
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper

Abstract

The present invention relates to a kind of graphene-tungsten carbide collaboration enhancing Cu-base composites preparation methods, include the following steps: to weigh ammonium metatungstate, Gerhardite, DEXTROSE ANHYDROUS and NaCl, the Enough Dl water that can dissolve NaCl is added, obtains homogeneous and transparent precursor solution；Drying solid powder is obtained, mixed-powder presoma is obtained after grinding；The high-temperature calcination under hydrogen atmosphere protection obtains the self-assembly powder of the graphene-supported tungsten nano particle of three-dimensional sodium chloride-, copper nano particles；Cleaning and drying obtain the graphene powder of load nanometer tungsten particle, copper nano particles；Obtain acetic acid copper-coated graphite alkene composite powder；Calcining obtains graphene-copper Particles dispersed powder；Obtaining graphene-tungsten carbide collaboration enhances copper-based block composite material.

Description

Graphene-tungsten carbide collaboration enhancing Cu-base composites preparation method
Technical field
The present invention relates to a kind of fabricated in situ graphene-tungsten carbide collaboration enhancing Cu-base composites preparation methods, belong to In nano material preparation technology.
Background technique
Cu-base composites have high intensity, and fabulous electrical and thermal conductivity performance is expected to be applied to resistance welding electrode, collection At circuit lead frame and high-speed rail contact line.For meet demand, addition the upgrading for composite property of reinforced phase To vital effect.According to the difference of enhancing phase morphology dimension, can be classified as: zero-dimension nano particle, 1-dimention nano Pipe, nano wire, two-dimensional nano piece.Wherein, zero-dimension nano particle possesses the hardness of superelevation, there is good obstruction dislocation ability, In The strength of materials promotes aspect significant effect, but usually the nano particle interface cohesion poor with matrix also splits the easy germinating of material Line leads to toughness of material severe exacerbation.Compared to zero-dimension nano particle, two-dimensional graphene then because have biggish specific surface area, In material deformation process, bridge joint and deflection can be played the role of to crackle, to keep even improving toughness of material.Cause This, if nano particle and graphene are introduced into composite material, collaboration enhancing will preferably improve material property.
Currently, nano particle and graphene collaboration to be introduced into Cu-base composites and be primarily present following difficult point: additional Method is easy to cause the reunion of graphene and nano particle, deteriorates material property, because nano particle reduces with size, specific surface It can be continuously improved, tendency of reuniting is serious, in addition, the interface cohesion of particle and graphene and matrix is poor, is unfavorable for promoting material Performance；And in-situ method is difficult to accomplish the collaboration distribution of graphene and nano particle at present, because of fabricated in situ or the nanometer of precipitation Particle is typically easy to occur in the interface of graphene and matrix, and the nano particle for being published on interface limits its enhancing effect Fruit, therefore how graphene and nano particle collaboration to be introduced into Cu-base composites, it is still the weight to require study Want problem in science.
The present invention is reacted using graphene and carbide tungsten, introduces hard ceramic phase tungsten carbide nanometer Particle reaches graphene and carbide nanoparticles two-phase reinforcing effect, and the intensity of material is significantly improved, toughness Preferable holding is obtained.
Summary of the invention
The preparation method for enhancing Cu-base composites is cooperateed with the invention proposes a kind of graphene and tungsten carbide nano particle, This method process is simple, low in cost, and the composite material prepared in this approach, nano particle and graphene are evenly distributed, and has The tough mechanical property having both.Technical solution is as follows:
A kind of preparation method of graphene-tungsten carbide collaboration enhancing Cu-base composites, including the following steps:
(1) ammonium metatungstate ((NH is weighed with molar ratio W:Cu:C:NaCl=1:1:10:1504)6H2W12O40·XH20), three Nitric hydrate copper (Cu (NO3)2·H2O), DEXTROSE ANHYDROUS (C6H12O6) and NaCl, be added can dissolve NaCl it is enough go from Sub- water obtains homogeneous and transparent precursor solution.
(2) precursor solution by previous step preparation is freeze-dried, and is obtained drying solid powder, is obtained mixed powder after grinding Last presoma；
(3) by powder precursor obtained in the previous step high-temperature calcination under atmosphere protection, atmosphere is hydrogen, is warming up to 720- 780 DEG C, heat preservation a period of time, cooling down, 50~100 DEG C/min of cooling rate average out to obtain three-dimensional sodium chloride-stone later The self-assembly powder of black alkene load tungsten nano particle, copper nano particles；
(4) self-assembly powder prepared by previous step is filtered using deionized water, removes NaCl, after it is dry in vacuum The graphene powder of load nanometer tungsten particle, copper nano particles is dried to obtain in dry case；
(5) the mass fraction 1%-1.5% according to graphene in Cu-base composites weighs copper acetate monohydrate (Cu (AC)2H2O) and graphene powder obtained in the previous step, Enough Dl water and ammonia solvent copper acetate, ultrasonic treatment is added Afterwards, it is placed in stirring in 70-80 DEG C of water-bath to be evaporated and dry, grinding obtains acetic acid copper-coated graphite alkene composite powder；
(6) by composite powder obtained in the previous step high-temperature calcination under atmosphere protection, atmosphere is hydrogen, is warming up to 600 DEG C, Heat preservation a period of time, cooling down, 50~100 DEG C/min of cooling rate average out to, obtain graphene-copper Particles dispersed powder later End；
(7) composite powder obtained in the previous step is subjected to hot pressed sintering, sintering temperature is 700-900 DEG C, vacuum degree < 10- 4Pa, for a period of time, obtain graphene-tungsten carbide collaboration enhances copper-based block composite material to sintered heat insulating.
Compared with prior art, advantage of the process is that the second phase nanometer particle tungsten carbide is in hot-forming process What middle tungsten and graphene reaction in-situ generated, this makes nano particle and Copper substrate with good Lattice Matching relationship, and Particle size is small, and furthermore graphene and tungsten carbide nano particle are evenly distributed in Copper substrate, plays collaboration reinforcing effect.
Detailed description of the invention
Fig. 1 is the load nanometer tungsten particle being prepared, the graphene powder SEM picture of copper particle
Fig. 2 is the load nanometer tungsten particle being prepared, the graphene powder XRD spectrum of copper particle
Fig. 3 is the graphene-copper Particles dispersed powder SEM picture being prepared
Fig. 4 is the graphene-tungsten carbide collaboration enhancing Cu-base composites block SEM picture being prepared
Fig. 5 is the tensile property curve of the composite material being prepared and fine copper
All attached drawings are 1 product characterization result of example.
The present invention does not address place and is suitable for the prior art.
Specific embodiment
The specific implementation example of preparation method of the present invention is given below.Example is only used for further illustrating preparation side of the invention Method is not intended to limit the protection scope of the claim of this application.
Example 1
Sodium chloride 21.9g, glucose 0.601g, ammonium metatungstate 0.615g are weighed, copper nitrate 0.604g is placed in a beaker, It weighs 70mL deionized water and pours into beaker and dissolve, magnetic agitation 6h pours into uniformly mixed liquid in culture dish, then will Culture dish freezes for 24 hours under the conditions of being placed in -20 DEG C of freezer compartment of refrigerator；Sample after freezing is put in freeze drier and is lyophilized, is frozen Dry condition are as follows: -20 DEG C, freeze-drying time is for 24 hours.Sample after freeze-drying is ground to obtain presoma composite powder (powder diameter~100 Mesh)；Precursor powder is placed in tube furnace, and in a hydrogen atmosphere (10 DEG C/min of heating rate, 750 DEG C of holding temperature, heat preservation Time 2h, gas flow 200mL/min) high-temperature calcination, it is rapidly cooled to room temperature after heat preservation and (drops to 100 DEG C in 5min), Calcined powder is placed in 500ml beaker, 400ml deionized water is added, magnetic agitation 30min keeps sodium chloride all molten It in Xie Yushui, then filters, the powder that will be obtained after suction filtration is placed in 500ml beaker, and 400ml deionized water, ultrasound is added 10min is filtered again, and filtered sample is put into 70 DEG C of vacuum drying ovens dry 3h to get load nanometer tungsten particle, copper is arrived The graphene powder of particle.
Graphene 0.12g is weighed, copper acetate monohydrate 37.06g is placed in a beaker (graphene content is 1wt.%), is added 40ml deionized water and 75ml dehydrated alcohol after ultrasonic 30min, are put into magnetic agitation in 75 DEG C of water-baths, are evaporated, be subsequently placed into 12h is dried in 200 DEG C of convection ovens, is pulverized.By powder be put into tube furnace in a hydrogen atmosphere (10 DEG C of heating rate/ Min, 600 DEG C of holding temperature, soaking time 1h, gas flow 100mL/min) high-temperature calcination, it is quickly cooled to after heat preservation Room temperature (drops to 100 DEG C) in 5min, pulverize.Obtained powder is placed inIt is hot-forming in graphite jig, sintering parameter For 10 DEG C/min of heating rate, 800 DEG C of heat preservation 1h, vacuum degree < 10-4MPa obtains graphene-tungsten carbide collaboration enhancing Cu-based bulk Composite material.
Example 2
Sodium chloride 21.9g, glucose 0.601g, ammonium metatungstate 0.615g are weighed, copper nitrate 0.604g is placed in a beaker, and is claimed Amount 70mL deionized water, which is poured into beaker, to be dissolved, and magnetic agitation 6h pours into uniformly mixed liquid in culture dish, then will training Feeding ware freezes for 24 hours under the conditions of being placed in -20 DEG C of freezer compartment of refrigerator；Sample after freezing is put in freeze drier and is lyophilized, is lyophilized Condition are as follows: -20 DEG C, freeze-drying time is for 24 hours.Sample after freeze-drying is ground to obtain presoma composite powder (powder diameter~100 Mesh)；Precursor powder is placed in tube furnace, and in a hydrogen atmosphere (10 DEG C/min of heating rate, 750 DEG C of holding temperature, heat preservation Time 2h, gas flow 200mL/min) high-temperature calcination, it is rapidly cooled to room temperature after heat preservation and (drops to 100 DEG C in 5min), Calcined powder is placed in 500ml beaker, 400ml deionized water is added, magnetic agitation 30min keeps sodium chloride all molten It in Xie Yushui, then filters, the powder that will be obtained after suction filtration is placed in 500ml beaker, and 400ml deionized water, ultrasound is added 10min is filtered again, and filtered sample is put into 70 DEG C of vacuum drying ovens dry 3h to get load nanometer tungsten particle, copper is arrived The graphene powder of particle.
Graphene 0.06g is weighed, copper acetate monohydrate 37.25g is placed in a beaker (graphene content is 0.5wt.%), adds Enter 40ml deionized water and 75ml dehydrated alcohol, after ultrasonic 30min, is put into magnetic agitation in 75 DEG C of water-baths, is evaporated, then put Enter in 200 DEG C of convection ovens and dry 12h, pulverizes.Powder is put into tube furnace (heating rate 10 in a hydrogen atmosphere DEG C/min, and 600 DEG C of holding temperature, soaking time 1h, gas flow 100mL/min) high-temperature calcination, it is quickly cooled down after heat preservation To room temperature (dropping to 100 DEG C in 5min), pulverize.Obtained powder is placed inIt is hot-forming in graphite jig, sintering ginseng Number is 10 DEG C/min of heating rate, 800 DEG C of heat preservation 1h, vacuum degree < 10-4It is copper-based to obtain graphene-tungsten carbide collaboration enhancing by MPa Block composite material.
Example 3
Sodium chloride 21.9g, glucose 0.601g, ammonium metatungstate 0.615g are weighed, copper nitrate 0.604g is placed in a beaker, and is claimed Amount 70mL deionized water, which is poured into beaker, to be dissolved, and magnetic agitation 6h pours into uniformly mixed liquid in culture dish, then will training Feeding ware freezes for 24 hours under the conditions of being placed in -20 DEG C of freezer compartment of refrigerator；Sample after freezing is put in freeze drier and is lyophilized, is lyophilized Condition are as follows: -20 DEG C, freeze-drying time is for 24 hours.Sample after freeze-drying is ground to obtain presoma composite powder (powder diameter~100 Mesh)；Precursor powder is placed in tube furnace, and in a hydrogen atmosphere (10 DEG C/min of heating rate, 750 DEG C of holding temperature, heat preservation Time 2h, gas flow 200mL/min) high-temperature calcination, it is rapidly cooled to room temperature after heat preservation and (drops to 100 DEG C in 5min), Calcined powder is placed in 500ml beaker, 400ml deionized water is added, magnetic agitation 30min keeps sodium chloride all molten It in Xie Yushui, then filters, the powder that will be obtained after suction filtration is placed in 500ml beaker, and 400ml deionized water, ultrasound is added 10min is filtered again, and filtered sample is put into 70 DEG C of vacuum drying ovens dry 3h to get load nanometer tungsten particle, copper is arrived The graphene powder of particle.
Graphene 0.18g is weighed, copper acetate monohydrate 36.87g is placed in a beaker (graphene content is 1.5wt.%), adds Enter 40ml deionized water and 75ml dehydrated alcohol, after ultrasonic 30min, is put into magnetic agitation in 75 DEG C of water-baths, is evaporated, then put Enter in 200 DEG C of convection ovens and dry 12h, pulverizes.Powder is put into tube furnace (heating rate 10 in a hydrogen atmosphere DEG C/min, and 600 DEG C of holding temperature, soaking time 1h, gas flow 100mL/min) high-temperature calcination, it is quickly cooled down after heat preservation To room temperature (dropping to 100 DEG C in 5min), pulverize.Obtained powder is placed inIt is hot-forming in graphite jig, sintering ginseng Number is 10 DEG C/min of heating rate, 800 DEG C of heat preservation 1h, vacuum degree < 10-4It is copper-based to obtain graphene-tungsten carbide collaboration enhancing by MPa Block composite material.

Claims (1)

1. a kind of graphene-tungsten carbide collaboration enhancing Cu-base composites preparation method, including the following steps:
(1) ammonium metatungstate ((NH is weighed with molar ratio W:Cu:C:NaCl=1:1:10:1504)6H2W12O40·XH20), three hydration Copper nitrate (Cu (NO3)2·H2O), DEXTROSE ANHYDROUS (C6H12O6) and NaCl, the Enough Dl water that can dissolve NaCl is added, Obtain homogeneous and transparent precursor solution.
(2) precursor solution by previous step preparation is freeze-dried, and drying solid powder is obtained, before obtaining mixed-powder after grinding Drive body；
(3) by powder precursor obtained in the previous step high-temperature calcination under atmosphere protection, atmosphere is hydrogen, is warming up to 720-780 DEG C, heat preservation a period of time, cooling down, 50~100 DEG C/min of cooling rate average out to obtain three-dimensional sodium chloride-graphite later Alkene loads the self-assembly powder of tungsten nano particle, copper nano particles；
(4) self-assembly powder prepared by previous step is filtered using deionized water, remove NaCl, after in vacuum oven In be dried to obtain load nanometer tungsten particle, copper nano particles graphene powder；
(5) the mass fraction 1%-1.5% according to graphene in Cu-base composites weighs copper acetate monohydrate (Cu (AC)2· H2O) and graphene powder obtained in the previous step, it is added Enough Dl water and ammonia solvent copper acetate, after ultrasonic treatment, is placed in Stirring is evaporated and dries in 70-80 DEG C of water-bath, and grinding obtains acetic acid copper-coated graphite alkene composite powder；
(6) by composite powder obtained in the previous step high-temperature calcination under atmosphere protection, atmosphere is hydrogen, is warming up to 600 DEG C, heat preservation For a period of time, cooling down, 50~100 DEG C/min of cooling rate average out to later, obtain graphene-copper Particles dispersed powder；
(7) composite powder obtained in the previous step is subjected to hot pressed sintering, sintering temperature is 700-900 DEG C, vacuum degree < 10-4Pa is burnt Knot heat preservation a period of time, obtaining graphene-tungsten carbide collaboration enhances copper-based block composite material.
CN201910706269.4A 2019-08-01 2019-08-01 Preparation method of graphene-tungsten carbide synergistically enhanced copper-based composite material Expired - Fee Related CN110453107B (en)

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CN117463999A (en) * 2023-12-28 2024-01-30 天津大学 Copper-based conductive composite material and preparation method and application thereof

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