CN106334790A - Method for preparing graphene sheet loaded nickel reinforced aluminum composite through in-situ catalyzing of solid carbon source on aluminum powder surface - Google Patents

Method for preparing graphene sheet loaded nickel reinforced aluminum composite through in-situ catalyzing of solid carbon source on aluminum powder surface Download PDF

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CN106334790A
CN106334790A CN201610919241.5A CN201610919241A CN106334790A CN 106334790 A CN106334790 A CN 106334790A CN 201610919241 A CN201610919241 A CN 201610919241A CN 106334790 A CN106334790 A CN 106334790A
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powder
composite
epoxy resin
ethanol
carbon source
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CN106334790B (en
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赵乃勤
刘兴海
李家俊
何春年
师春生
刘恩佐
李群英
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Tianjin University
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/05Mixtures of metal powder with non-metallic powder
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12Both compacting and sintering
    • B22F3/14Both compacting and sintering simultaneously
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12Both compacting and sintering
    • B22F3/14Both compacting and sintering simultaneously
    • B22F2003/145Both compacting and sintering simultaneously by warm compacting, below debindering temperature
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00Aspects linked to processes or compositions used in powder metallurgy

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacture Of Alloys Or Alloy Compounds (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention discloses a method for preparing a graphene sheet loaded nickel reinforced aluminum composite through in-situ catalyzing of a solid carbon source on the aluminum powder surface. The method comprises the steps that epoxy resin serving as a network forming agent and absolute ethyl alcohol serving as a dispersing agent are mixed into a solution; pure aluminum powder is used as a substrate raw material, nitrate hexahydrate is used as a catalyzer, anhydrous dextrose is used as the carbon source, the pure aluminum powder, the nitrate hexahydrate and the anhydrous dextrose are added into the solution for water bath dissolving with the mass ratio being 150-250 to 4-6 to 0.8-1.2, and an Ni2+ epoxy resin/Al loaded network-shaped mixture is obtained; ethylenediamine is used as a network curing agent, and an Ni2+ epoxy resin/Al loaded composite with a stable structure is obtained; the composite is roasted to obtain Ni loaded graphene nanosheet GNS/Al composite powder; and finally, the composite powder is placed in a vacuum hot pressing furnace for sinter molding.

Description

Aluminium powder surface in situ catalysis preparing graphene by utilizing solid carbon source piece nickel-loaded strengthens aluminum and is combined The method of material
Technical field
The present invention relates to a kind of load nickel aluminum composite wood using powder metallurgy fabricated in situ graphene nanometer sheet (gns) The method of material, belongs to powder metallurgical technology.
Background technology
Aluminum light weight, is all preferable and cheap material of a kind of electrical and thermal conductivity, ductility, damping capacity, extensively General it is applied to machinery, automobile, Aero-Space, electronic apparatus, defence and military and the industrial circle such as civilian.But, fine aluminium material strong Degree is very low, is easy to fracture in a lot of structural member application aspect or destroys, service life is short, causes serious consequence, brings Greatly lose.Relatively nervous with social development, scientific and technological progress and utilization of energy, people are for the material of high-strength light Propose more demands, the aluminium alloy being prepared into by adding different alloying elements in fine aluminium can significantly improve fine aluminium Intensity, however, these techniques complex and much outer added elements expensive, simultaneously for after these alloyings aluminum close Payment organization performance evaluation aspect is complex specifically to strengthen reason it is difficult to determine.Aluminum matrix composite is as high-strength light material The representative of material, disclosure satisfy that this requirement of people, and it is fairly simple substantially to strengthen the analysis such as reason, structure property process.Tradition Composite preparation process typically add in the base after the second phase with certain technological forming.But, always former to sacrifice Based on some performances of beginning material.Composite method is equally applicable to the preparation of aluminum matrix composite, according to composite Materials Design Rule (ec=(1-f) em+fep), while being added in realization strengthening effect of the second phase, the one of matrix material can also be overcome Not enough a bit, thus obtaining the aluminium of high-strength light, and overcome the shortcomings of traditional method.
As a kind of new material, except the application at aspects such as electronic apparatus, the energy, catalysis, it also has Graphene There is excellent mechanical property, be intensity and the toughness highest material of discovery so far.In recent ten years, with Graphene for increasing The research of the Graphene reinforced aluminum matrix composites of strong body preparation increases year by year, quickly grows.So far, great majority research collection In prepare in Graphene reinforced aluminum matrix composites in outer addition, by works such as mechanical ball milling, molecular level mixing, melting and castings Skill molding.But, said method can cause the destruction of graphene-structured unavoidably, be also difficult to ensure that Graphene in matrix material simultaneously In dispersed.So, this is also the bottleneck place of current research.To sum up, how to solve Graphene in the base uniform Disperse and structural integrity becomes the focus place currently preparing Graphene reinforced aluminum matrix composites.So far, most researchs Personnel prepare Graphene reinforced aluminum matrix composites using adding the method in aluminum substrate for the degradative reduction graphene oxide.
Content of the invention
It is an object of the invention to provide a kind of convenient powder metallurgy fabricated in situ graphene nanometer sheet load nickel aluminum is multiple The method of condensation material.The method can effectively overcome the shortcoming of traditional added graphite alkene piece reinforced aluminum matrix composites, this side Method process is relatively easy, and obtained composite materials property is good.For achieving the above object, the present invention passes through following technical side Case is carried out:
A kind of aluminium powder surface in situ is catalyzed the method that preparing graphene by utilizing solid carbon source piece nickel-loaded strengthens aluminium composite material, bag Include the following step:
(1) with epoxy resin as network former, with dehydrated alcohol as dispersant, according to epoxy resin, dehydrated alcohol body Long-pending ratio is 1:(15~20) uniformly mix wiring solution-forming;
(2) with pure aluminium powder as matrix material, with Nickelous nitrate hexahydrate as catalyst, with anhydrous glucose as carbon source, according to Pure aluminium powder, Nickelous nitrate hexahydrate, anhydrous glucose mass ratio are (150-250): 4-6:(0,8-1.2) add in above-mentioned (1) and join Dissolve in the solution of system, heating in water bath stirs, and obtains ni2+The network-like mixture of laden epoxy/al.
(3) with ethylenediamine for network firming agent, by according to ethanol volume ratio be 2.5:75 ratio, ethylenediamine is slow It is added drop-wise in the solution of above-mentioned steps (2), is made into mixed solution, by composite powder when ethanol volatilizees totally in this mixed solution Wash, be dried, obtain constitutionally stable ni2+Laden epoxy/al composite.
(4) composite powder obtaining in step (3) is placed in quartzy Noah's ark, puts into sintering in horizontal pipe furnace, Temperature is 350-450 DEG C, with argon as carrier gas, thermally decomposes glucose, obtains graphene nanometer sheet;Afterwards with hydrogen/argon for carrying Gas, sinters above-mentioned powder in 500-700 DEG C, removes epoxy networks template, obtains ni load graphene nanometer sheet gns/al Composite powder;Finally, this composite powder is placed in sinter molding in vacuum hotpressing stove.
Preferably, step 1) mix with ethanol solution after the heating of 100 DEG C of epoxy resin.Step 4) in epoxy networks mould During plate, argon flow amount controls in 60ml/min, hydrogen flowing quantity during glucose pyrolytic deposition growth graphene nanometer sheet Control in 50ml/min, argon flow amount controls in 200ml/min, and in vacuum sintering funace, pressure is set as 45mpa, temperature is 600 DEG C, and the dwell time is 1-2h, and pressurize cools to room temperature with the furnace after terminating, obtains block materials.
The method that the present invention adopts the additional powder metallurgy of growth in situ graphene nanometer sheet, first uniformly divides on aluminium powder surface The graphene nanometer sheet of scattered three dimensional structure, after through vacuum heating-press sintering technique, it is high to prepare compactness, good mechanical performance Aluminum matrix composite.The invention has the advantages that the method directly adopting growth in situ first, make solid carbon source glucose Realize more uniformly loading on aluminium powder surface.Secondly, Graphene using the method process is simple, with low cost, preparing Nanometer sheet reinforced aluminum matrix composites, its tensile property is better than the method that the outer addition of tradition adds degradative reduction graphene oxide.
The present invention prepares graphene nanometer sheet using growth in situ and powder metallurgic method, and achieves to aluminum matrix material Strengthening, have preferable prospect for application on structural member for the high-strength aluminium.
Brief description
Fig. 1 is the scanned photograph of generation graphene nanometer sheet after reduction in embodiment 1.
Fig. 2 is the transmission photo of generation graphene nanometer sheet after reduction in embodiment 1.
Fig. 3 is the infrared spectrum photo of powder after reduction in embodiment 4.
Fig. 4 is the Raman spectrogram photo of powder after reduction in embodiment 5.
Fig. 5 is the xrd spectrogram photo of powder after reduction in embodiment 6.
Fig. 6 is stress strain curve in embodiment 7,8,9,10.
Fig. 7 is the scanned photograph of stretching fracture in embodiment 7.
Fig. 8 a is the scanned photograph of powder in embodiment 11.
Fig. 8 b is the scanned photograph of powder in embodiment 12.
Fig. 8 c is the scanned photograph of powder in embodiment 13.
Specific embodiment
Further illustrate the present invention with reference to example, these examples are served only for the present invention is described, are not intended to limit the present invention.
Embodiment 1
By al powder: Nickelous nitrate hexahydrate: it is molten that anhydrous glucose is added to epoxy resin/ethanol by quality (g) than 200:5:1 In liquid (4.5ml epoxy resin, 75ml ethanol), it is slowly added dropwise 2.5ml ethylenediamine (eda), heating in water bath stirs.Temperature is set as 90 DEG C, mixing time 5h, take out when ethanol volatilizees totally and be dried after above-mentioned dried powder is washed with deionized, by above-mentioned powder End carries out reduction treatment in horizontal pipe furnace.Reduction temperature is set in 400 DEG C, and reducing atmosphere is that (gas flow sets hydrogen In 50~100ml/min), protective atmosphere is argon (gas flow is set in 200ml/min).Recovery time is 1h.Exist afterwards 600 DEG C of heating and thermal insulation 1h, atmosphere is argon, removes epoxy resin template.After reduction, the scanned photograph of material is as shown in figure 1, thoroughly Penetrate photo as shown in Figure 2.
Embodiment 2
By al powder: Nickelous nitrate hexahydrate: anhydrous glucose is added to epoxy resin/ethanol by quality (g) than 200:5:0.2 In solution (5g epoxy resin, 75ml ethanol), it is slowly added dropwise 2.5ml ethylenediamine (eda), heating in water bath stirs.Temperature is set as 90 DEG C, mixing time 5h, take out when ethanol volatilizees totally and be dried after above-mentioned dried powder is washed with deionized, by above-mentioned powder End carries out reduction treatment in horizontal pipe furnace.Reduction temperature is set in 400 DEG C, and reducing atmosphere is that (gas flow sets hydrogen In 50~100ml/min), protective atmosphere is argon (gas flow is set in 200ml/min).Recovery time is 1h.Exist afterwards 600 DEG C of heating and thermal insulation 1h, atmosphere is argon, removes epoxy resin template.
Embodiment 3
By al powder: Nickelous nitrate hexahydrate: anhydrous glucose is added to epoxy resin/ethanol by quality (g) than 200:5:1.8 In solution (5g epoxy resin, 75ml ethanol), it is slowly added dropwise 2.5ml ethylenediamine (eda), heating in water bath stirs.Temperature is set as 90 DEG C, mixing time 5h, take out when ethanol volatilizees totally and be dried after above-mentioned dried powder is washed with deionized, by above-mentioned powder End carries out reduction treatment in horizontal pipe furnace.Reduction temperature is set in 400 DEG C, and reducing atmosphere is that (gas flow sets hydrogen In 50~100ml/min), protective atmosphere is argon (gas flow is set in 200ml/min).Recovery time is 1h.Exist afterwards 600 DEG C of heating and thermal insulation 1h, atmosphere is argon, removes epoxy resin template.
Embodiment 4
By al powder: Nickelous nitrate hexahydrate: it is molten that anhydrous glucose is added to epoxy resin/ethanol by quality (g) than 200:5:1 In liquid (5g epoxy resin, 75ml ethanol), it is slowly added dropwise 2.5ml ethylenediamine (eda), heating in water bath stirs.Temperature is set as 90 DEG C, mixing time 5h, take out when ethanol volatilizees totally and be dried after above-mentioned dried powder is washed with deionized, by above-mentioned powder Carry out reduction treatment in horizontal pipe furnace.Reduction temperature is set in 400 DEG C, and reducing atmosphere is that (gas flow is set in hydrogen 50~100ml/min), protective atmosphere is argon (gas flow is set in 200ml/min).Recovery time is 1h.Afterwards 600 DEG C heating and thermal insulation 1h, atmosphere is argon, removes epoxy resin template.Powder complete for above-mentioned cvd is carried out infrared test, test knot Fruit is as shown in Figure 3.
Embodiment 5
By al powder: Nickelous nitrate hexahydrate: it is molten that anhydrous glucose is added to epoxy resin/ethanol by quality (g) than 200:5:1 In liquid (5g epoxy resin, 75ml ethanol), it is slowly added dropwise 2.5ml ethylenediamine (eda), heating in water bath stirs..Temperature is set as 90 DEG C, mixing time 5h, take out when ethanol volatilizees totally and be dried after above-mentioned dried powder is washed with deionized, by above-mentioned powder Carry out reduction treatment in horizontal pipe furnace.Reduction temperature is set in 400 DEG C, and reducing atmosphere is that (gas flow is set in hydrogen 50~100ml/min), protective atmosphere is argon (gas flow is set in 200ml/min).Recovery time is 1h.Afterwards 600 DEG C heating and thermal insulation 1h, atmosphere is argon, removes epoxy resin template.Powder complete for above-mentioned cvd is carried out the test of Raman collection of illustrative plates, Test result is as shown in Figure 4.
Embodiment 6
By al powder: Nickelous nitrate hexahydrate: it is molten that anhydrous glucose is added to epoxy resin/ethanol by quality (g) than 200:5:1 In liquid (5g epoxy resin, 75ml ethanol), it is slowly added dropwise 2.5ml ethylenediamine (eda), heating in water bath stirs..Temperature is set as 90 DEG C, mixing time 5h, take out when ethanol volatilizees totally and be dried after above-mentioned dried powder is washed with deionized, by above-mentioned powder Carry out reduction treatment in horizontal pipe furnace.Reduction temperature is set in 400 DEG C, and reducing atmosphere is that (gas flow is set in hydrogen 50~100ml/min), protective atmosphere is argon (gas flow is set in 200ml/min).Recovery time is 1h.Afterwards 600 DEG C heating and thermal insulation 1h, atmosphere is argon, removes epoxy resin template.Powder complete for above-mentioned cvd is carried out the test of xrd, test Result is as shown in Figure 5.
Embodiment 7
By al powder: Nickelous nitrate hexahydrate: it is molten that anhydrous glucose is added to epoxy resin/ethanol by quality (g) than 200:5:1 In liquid (5g epoxy resin, 75ml ethanol), it is slowly added dropwise 2.5ml ethylenediamine (eda), heating in water bath stirs..Temperature is set as 90 DEG C, mixing time 5h, take out when ethanol volatilizees totally and be dried after above-mentioned dried powder is washed with deionized, by above-mentioned powder Carry out reduction treatment in horizontal pipe furnace.Reduction temperature is set in 400 DEG C, and reducing atmosphere is that (gas flow is set in hydrogen 50~100ml/min), protective atmosphere is argon (gas flow is set in 200ml/min).Recovery time is 1h.Afterwards 600 DEG C heating and thermal insulation 1h, atmosphere is argon, removes epoxy resin template.By the graphene nanometer sheet of above-mentioned preparation/aluminum composite powder Vacuum sintering furnace is carried out hot-forming, pressure is set as 45mpa, temperature is 600 DEG C, the dwell time is 1~2h, protects Pressure cools to room temperature with the furnace after terminating.Test its tensile property under universal testing machine, its tensile strength reaches 224mpa.Stretching , as shown in Fig. 6 blue curve, fracture apperance is as shown in Figure 7 for curve.
Embodiment 8
By al powder: Nickelous nitrate hexahydrate: anhydrous glucose is added to epoxy resin/ethanol by quality (g) than 200:5:0.2 In solution (5g epoxy resin, 75ml ethanol), it is slowly added dropwise 2.5ml ethylenediamine (eda), heating in water bath stirs..Temperature is set as 90 DEG C, mixing time 5h, take out when ethanol volatilizees totally and be dried after above-mentioned dried powder is washed with deionized, by above-mentioned powder End carries out reduction treatment in horizontal pipe furnace.Reduction temperature is set in 400 DEG C, and reducing atmosphere is that (gas flow sets hydrogen In 50~100ml/min), protective atmosphere is argon (gas flow is set in 200ml/min).Recovery time is 1h.Exist afterwards 600 DEG C of heating and thermal insulation 1h, atmosphere is argon, removes epoxy resin template.By the graphene nanometer sheet of above-mentioned preparation/aluminum composite powder End carries out hot-forming in vacuum sintering furnace, and pressure is set as 45mpa, and temperature is 600 DEG C, and the dwell time is 1~2h, Pressurize cools to room temperature with the furnace after terminating.Test its tensile property under universal testing machine, its tensile strength reaches 192mpa.Draw Stretch curve as shown in Fig. 6 green curve.
Embodiment 9
By al powder: Nickelous nitrate hexahydrate: anhydrous glucose is added to epoxy resin/ethanol by quality (g) than 200:5:1.8 In solution (5g epoxy resin, 75ml ethanol), it is slowly added dropwise 2.5ml ethylenediamine (eda), heating in water bath stirs..Temperature is set as 90 DEG C, mixing time 5h, take out when ethanol volatilizees totally and be dried after above-mentioned dried powder is washed with deionized, by above-mentioned powder End carries out reduction treatment in horizontal pipe furnace.Reduction temperature is set in 400 DEG C, and reducing atmosphere is that (gas flow sets hydrogen In 50~100ml/min), protective atmosphere is argon (gas flow is set in 200ml/min).Recovery time is 1h.Exist afterwards 600 DEG C of heating and thermal insulation 1h, atmosphere is argon, removes epoxy resin template.By the graphene nanometer sheet of above-mentioned preparation/aluminum composite powder End carries out hot-forming in vacuum sintering furnace, and pressure is set as 45mpa, and temperature is 600 DEG C, and the dwell time is 1~2h, Pressurize cools to room temperature with the furnace after terminating.Test its tensile property under universal testing machine, its tensile strength reaches 197mpa.Draw Stretch curve as shown in Fig. 6 red curve.
Embodiment 10 (blank control test)
Pure aluminium powder is carried out in vacuum sintering furnace hot-forming, pressure is set as 45mpa, temperature is 600 DEG C, protect The pressure time is 1~2h, and pressurize cools to room temperature with the furnace after terminating.Test its tensile property under universal testing machine, its stretching is strong Degree reaches 92mpa.Stress strain curve is as shown in Fig. 6 black curve.
Embodiment 11
By al powder: Nickelous nitrate hexahydrate: anhydrous glucose is added in ethanol solution 75ml than 200:5:1 by quality (g), Heating in water bath stirs.Temperature is set as 90 DEG C, mixing time 5h, whne ethanol volatilization totally when take out above-mentioned dried powder spend from It is dried after sub- water washing, above-mentioned powder is carried out in horizontal pipe furnace reduction treatment.Reduction temperature is set in 400 DEG C, reduction Atmosphere is hydrogen (gas flow is set in 50~100ml/min), and protective atmosphere is that (gas flow is set in 200ml/ to argon min).Recovery time is 1h.Afterwards in 600 DEG C of heating and thermal insulation 1h, atmosphere is argon, removes epoxy resin template.Powder after sintering End scanning pattern is as shown in Figure 8 a.
Embodiment 12
By al powder: Nickelous nitrate hexahydrate is added to epoxy resin/ethanol solution (5g asphalt mixtures modified by epoxy resin by quality (g) than 200:5 Fat, 75ml ethanol) in, it is slowly added dropwise 2.5ml ethylenediamine (eda), heating in water bath stirs.Temperature is set as 90 DEG C, mixing time 5h, takes out when ethanol volatilizees totally and is dried after above-mentioned dried powder is washed with deionized, by above-mentioned powder in horizontal tube Carry out reduction treatment in stove.Reduction temperature is set in 400 DEG C, and reducing atmosphere is that (gas flow is set in 50~100ml/ to hydrogen Min), protective atmosphere is argon (gas flow is set in 200ml/min).Recovery time is 1h.Afterwards in 600 DEG C of heating and thermal insulations 1h, atmosphere is argon, removes epoxy resin template.Powder scanning pattern after sintering is as shown in Figure 8 b.
Embodiment 13
By al powder: anhydrous glucose by quality (g) than 200:1 be added to epoxy resin/ethanol solution (5g epoxy resin, 75ml ethanol) in, it is slowly added dropwise 2.5ml ethylenediamine (eda), heating in water bath stirs.Temperature is set as 90 DEG C, mixing time 5h, Take out when ethanol volatilizees totally and be dried after above-mentioned dried powder is washed with deionized, by above-mentioned powder in horizontal pipe furnace Carry out reduction treatment.Reduction temperature is set in 400 DEG C, and reducing atmosphere is hydrogen (gas flow is set in 50~100ml/min), Protective atmosphere is argon (gas flow is set in 200ml/min).Recovery time is 1h.Afterwards in 600 DEG C of heating and thermal insulation 1h, gas Atmosphere is argon, removes epoxy resin template.Powder scanning pattern after sintering is as shown in Figure 8 c.Bent by four stretchings in Fig. 6 Line can be seen that in al powder: Nickelous nitrate hexahydrate: during anhydrous glucose=200:5:1 (blue curve), the tension of composite Intensity reaches peak value (224mpa), and the tensile strength (92mpa) comparing fine aluminium exceeds 143%, and elongation percentage also maintains nearly 10%, Unlikely decline is too many.The content of anhydrous glucose is higher or low all to reduce enhanced effect.

Claims (3)

1. a kind of aluminium powder surface in situ is catalyzed the method that preparing graphene by utilizing solid carbon source piece nickel-loaded strengthens aluminium composite material, including The following step:
(1) with epoxy resin as network former, with dehydrated alcohol as dispersant, according to epoxy resin, dehydrated alcohol volume ratio For 1:(15~20) uniformly mix wiring solution-forming;
(2) with pure aluminium powder as matrix material, with Nickelous nitrate hexahydrate as catalyst, with anhydrous glucose as carbon source, according to fine aluminium Powder, Nickelous nitrate hexahydrate, anhydrous glucose mass ratio are (150-250): 4-6:(0,8-1.2) add in above-mentioned (1) and prepare Dissolve in solution, heating in water bath stirs, and obtains ni2+The network-like mixture of laden epoxy/al.
(3) with ethylenediamine for network firming agent, by according to being the ratio of 2.5:75 with ethanol volume ratio, ethylenediamine is slowly added dropwise To in the solution of above-mentioned steps (2), it is made into mixed solution, by composite powder water when ethanol volatilizees totally in this mixed solution Wash, be dried, obtain constitutionally stable ni2+Laden epoxy/al composite.
(4) composite powder obtaining in step (3) is placed in quartzy Noah's ark, puts into sintering, temperature in horizontal pipe furnace For 350-450 DEG C, with argon as carrier gas, thermally decompose glucose, obtain graphene nanometer sheet;Afterwards with hydrogen/argon as carrier gas, in The 500-700 DEG C of above-mentioned powder of sintering, removes epoxy networks template, obtains ni load graphene nanometer sheet gns/al composite powder End;Finally, this composite powder is placed in sinter molding in vacuum hotpressing stove.
2. the preparation method of composite according to claim 1 is it is characterised in that step 1) 100 DEG C of epoxy resin plus Mix with ethanol solution after heat.
3. the preparation method of composite according to claim 1 is it is characterised in that step 4) in epoxy networks mould During plate, argon flow amount controls in 60ml/min, hydrogen flowing quantity during glucose pyrolytic deposition growth graphene nanometer sheet Control in 50ml/min, argon flow amount controls in 200ml/min, and in vacuum sintering funace, pressure is set as 45mpa, temperature is 600 DEG C, and the dwell time is 1-2h, and pressurize cools to room temperature with the furnace after terminating, obtains block materials.
CN201610919241.5A 2016-10-21 2016-10-21 The method that aluminium powder surface in situ is catalyzed preparing graphene by utilizing solid carbon source piece nickel-loaded enhancing aluminium composite material Expired - Fee Related CN106334790B (en)

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CN107574326A (en) * 2017-08-25 2018-01-12 天津大学 The method that original position prepares graphene nanometer sheet/copper/aluminium composite material with mud/brick laminated construction
CN109317690A (en) * 2018-09-28 2019-02-12 天津大学 A kind of preparation method of graphene enhancing aluminum-base composite foamed material
CN110480004A (en) * 2019-08-29 2019-11-22 南京理工大学 The method that hydro-thermal method prepares carbon-coated aluminum nanoparticles

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