CN106334790B - The method that aluminium powder surface in situ is catalyzed preparing graphene by utilizing solid carbon source piece nickel-loaded enhancing aluminium composite material - Google Patents
The method that aluminium powder surface in situ is catalyzed preparing graphene by utilizing solid carbon source piece nickel-loaded enhancing aluminium composite material Download PDFInfo
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- CN106334790B CN106334790B CN201610919241.5A CN201610919241A CN106334790B CN 106334790 B CN106334790 B CN 106334790B CN 201610919241 A CN201610919241 A CN 201610919241A CN 106334790 B CN106334790 B CN 106334790B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- 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
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B22F2003/145—Both compacting and sintering simultaneously by warm compacting, below debindering temperature
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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Abstract
A kind of method that the present invention discloses aluminium powder surface in situ catalysis preparing graphene by utilizing solid carbon source piece nickel-loaded enhancing aluminium composite material, comprising: using epoxy resin as network former, using dehydrated alcohol as dispersant wiring solution-forming；Using pure aluminium powder as matrix material, it is (150-250): 4-6:(0 according to pure aluminium powder, Nickelous nitrate hexahydrate, DEXTROSE ANHYDROUS mass ratio using DEXTROSE ANHYDROUS as carbon source using Nickelous nitrate hexahydrate as catalyst, water-bath dissolution in above-mentioned solution 8-1.2) is added, obtains Ni2+The network-like mixture of laden epoxy/Al；Using ethylenediamine as network curing agent, the Ni of stable structure is obtained2+Laden epoxy/Al composite material.Composite material calcining obtains Ni load graphene nanometer sheet GNS/Al composite powder；Finally, the composite powder is placed in sinter molding in vacuum hotpressing stove.
Description
Technical field
Nickel aluminum composite wood is loaded using powder metallurgy fabricated in situ graphene nanometer sheet (GNS) the present invention relates to a kind of
The method of material, belongs to powder metallurgical technology.
Background technique
Aluminium light weight is all preferable and cheap material of a kind of electrical and thermal conductivity, ductility, damping capacity, extensively
It is general to be applied to machinery, automobile, aerospace, electronic apparatus, defence and military and the industrial circles such as civilian.But fine aluminium material is strong
Degree is very low, is easy to fracture in many structural member application aspects or destroys, service life is short, causes serious consequence, brings
Greatly loss.With relatively nervous, material of the people for high-strength light of social development, scientific and technological progress and using energy source
More demands are proposed, fine aluminium can be significantly improved by adding the aluminium alloy that different alloying elements is prepared into fine aluminium
Intensity, however, these the process is more complicated and many outer added elements are expensive, simultaneously for the aluminium conjunction after these alloyings
It is complex in terms of payment organization performance evaluation, it is difficult to determine specific enhancing reason.Aluminum matrix composite is as high-strength light material
The representative of material can satisfy this requirement of people, and it is fairly simple obvious to enhance the analytic processes such as reason, structure property.Tradition
Composite material preparation process usually add in the base after the second phase with certain technological forming.But always to sacrifice original
Based on the certain performances of beginning material.Composite material method is equally applicable to the preparation of aluminum matrix composite, according to composite Materials Design
Rule (Ec=(1-f) Em+fEp), the addition of the second phase can also overcome the one of basis material while realizing strengthening effect
It is a little insufficient, to obtain the aluminium of high-strength light, and overcome the shortcomings of conventional method.
Graphene as a kind of novel material, in addition to electronic apparatus, the energy, in terms of application, it also has
There is excellent mechanical property, is the intensity found so far and the highest material of toughness.It in recent ten years, is to increase with graphene
The research of the graphene reinforced aluminum matrix composites of strong body preparation increases year by year, quickly grows.So far, most of research collection
In prepared in graphene reinforced aluminum matrix composites in outer addition, pass through the works such as mechanical ball mill, molecular level mixing, melting and casting
Skill molding.But the above method inevitably will cause the destruction of graphene-structured, while also be difficult to ensure graphene in basis material
In it is evenly dispersed.So this is also the bottleneck place studied at present.To sum up, graphene in the base uniform how is solved
Dispersion and structural integrity become where the focus for currently preparing graphene reinforced aluminum matrix composites.So far, most researchs
Personnel prepare graphene reinforced aluminum matrix composites using method of the addition degradative reduction graphene oxide into aluminum substrate.
Summary of the invention
The purpose of the present invention is to provide a kind of convenient powder metallurgy fabricated in situ graphene nanometer sheet load nickel aluminum is multiple
The method of condensation material.This method can effectively overcome the shortcomings that traditional added graphite alkene piece reinforced aluminum matrix composites, this side
Method process is relatively easy, and obtained composite materials property is good.To achieve the above object, the present invention passes through following technical side
Case is implemented:
A kind of method of aluminium powder surface in situ catalysis preparing graphene by utilizing solid carbon source piece nickel-loaded enhancing aluminium composite material, packet
Include the following steps:
(1) using epoxy resin as network former, using dehydrated alcohol as dispersing agent, according to epoxy resin, dehydrated alcohol body
Product is than being 1:(15~20) uniformly mix wiring solution-forming；
(2) using pure aluminium powder as matrix material, using Nickelous nitrate hexahydrate as catalyst, using DEXTROSE ANHYDROUS as carbon source, according to
Pure aluminium powder, Nickelous nitrate hexahydrate, DEXTROSE ANHYDROUS mass ratio are (150-250): 4-6:(0,8-1.2) it is added in above-mentioned (1) and matches
It is dissolved in the solution of system, heating water bath stirring obtains Ni2+The network-like mixture of laden epoxy/Al.
(3) using ethylenediamine as network curing agent, by according to ethyl alcohol 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 ethyl alcohol in this mixed solution volatilizees totally
Washing, drying, obtain the Ni of stable structure2+Laden epoxy/Al composite material.
(4) composite powder obtained in step (3) is placed in quartzy Noah's ark, is put into horizontal pipe furnace and is sintered,
Temperature is 350-450 DEG C, using argon gas as carrier gas, thermally decomposes glucose, obtains graphene nanometer sheet；It is afterwards to carry with hydrogen/argon gas
Gas removes epoxy networks template in the 500-700 DEG C of above-mentioned powder of sintering, obtains Ni load graphene nanometer sheet GNS/Al
Composite powder；Finally, the composite powder is placed in sinter molding in vacuum hotpressing stove.
Preferably, it is mixed after 100 DEG C of step 1) epoxy resin heating with ethanol solution.Step 4) is in epoxy networks mould
When plate, argon flow control grows hydrogen flowing quantity during graphene nanometer sheet in 60ml/min or so, glucose pyrolytic deposition
Control is controlled in 50ml/min or so, argon flow in 200ml/min or so, and in vacuum sintering funace, pressure is set as
45MPa, temperature are 600 DEG C, and dwell time 1-2h cools to room temperature with the furnace after pressure maintaining, obtains block materials.
The method that the present invention uses the additional powder metallurgy of growth in situ graphene nanometer sheet is first uniformly divided on aluminium powder surface
Dissipate three-dimensional structure graphene nanometer sheet, after by vacuum heating-press sintering technique, prepare compactness height, good mechanical performance
Aluminum matrix composite.The invention has the following advantages that the method for directlying adopt growth in situ first, makes solid carbon source glucose
More uniform load is realized on aluminium powder surface.Secondly, using this method simple process and low cost, the graphene prepared
Nanometer sheet reinforced aluminum matrix composites, method of the tensile property better than the outer addition addition degradative reduction graphene oxide of tradition.
The present invention prepares graphene nanometer sheet using growth in situ and powder metallurgic method, and realizes to aluminum matrix material
Reinforcing, for high-strength aluminium on structural member application have preferable prospect.
Detailed description of the invention
Fig. 1 is the scanned photograph that graphene nanometer sheet is generated after restoring in embodiment 1.
Fig. 2 is the transmission photo that graphene nanometer sheet is generated after restoring in embodiment 1.
Fig. 3 is the infrared spectrum photo of powder after restoring in embodiment 4.
Fig. 4 is the raman spectrum photo of powder after restoring in embodiment 5.
Fig. 5 is the XRD spectra photo of powder after restoring 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
It further illustrates that the present invention, these examples are served only for illustrating the present invention below with reference to example, is not intended to limit the present invention.
Embodiment 1
By Al powder: Nickelous nitrate hexahydrate: it is molten that DEXTROSE ANHYDROUS by quality (g) is added to epoxy resin/ethyl alcohol than 200:5:1
It in liquid (4.5ml epoxy resin, 75ml ethyl alcohol), is slowly added dropwise 2.5ml ethylenediamine (EDA), heating water bath stirring.Temperature is set as
90 DEG C, mixing time 5h, drying after above-mentioned dried powder is washed with deionized is taken out when ethyl alcohol volatilizees totally, 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 hydrogen (gas flow setting
In 50~100ml/min), protective atmosphere is argon gas (gas flow is set in 200ml/min).Recovery time is 1h.Exist afterwards
600 DEG C of heating and thermal insulation 1h, atmosphere are argon gas, remove epoxy resin template.The scanned photograph of material is as shown in Figure 1, thoroughly after reduction
It is as shown in Figure 2 to penetrate photo.
Embodiment 2
By Al powder: Nickelous nitrate hexahydrate: DEXTROSE ANHYDROUS is added to epoxy resin/ethyl alcohol than 200:5:0.2 by quality (g)
It in solution (5g epoxy resin, 75ml ethyl alcohol), is slowly added dropwise 2.5ml ethylenediamine (EDA), heating water bath stirring.Temperature is set as
90 DEG C, mixing time 5h, drying after above-mentioned dried powder is washed with deionized is taken out when ethyl alcohol volatilizees totally, 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 hydrogen (gas flow setting
In 50~100ml/min), protective atmosphere is argon gas (gas flow is set in 200ml/min).Recovery time is 1h.Exist afterwards
600 DEG C of heating and thermal insulation 1h, atmosphere are argon gas, remove epoxy resin template.
Embodiment 3
By Al powder: Nickelous nitrate hexahydrate: DEXTROSE ANHYDROUS is added to epoxy resin/ethyl alcohol than 200:5:1.8 by quality (g)
It in solution (5g epoxy resin, 75ml ethyl alcohol), is slowly added dropwise 2.5ml ethylenediamine (EDA), heating water bath stirring.Temperature is set as
90 DEG C, mixing time 5h, drying after above-mentioned dried powder is washed with deionized is taken out when ethyl alcohol volatilizees totally, 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 hydrogen (gas flow setting
In 50~100ml/min), protective atmosphere is argon gas (gas flow is set in 200ml/min).Recovery time is 1h.Exist afterwards
600 DEG C of heating and thermal insulation 1h, atmosphere are argon gas, remove epoxy resin template.
Embodiment 4
By Al powder: Nickelous nitrate hexahydrate: it is molten that DEXTROSE ANHYDROUS by quality (g) is added to epoxy resin/ethyl alcohol than 200:5:1
It in liquid (5g epoxy resin, 75ml ethyl alcohol), is slowly added dropwise 2.5ml ethylenediamine (EDA), heating water bath stirring.Temperature is set as 90
DEG C, mixing time 5h takes out drying after above-mentioned dried powder is washed with deionized, by above-mentioned powder when ethyl alcohol volatilizees totally
Reduction treatment is carried out 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 (gas flow is set in 200ml/min).Recovery time is 1h.Afterwards 600
DEG C heating and thermal insulation 1h, atmosphere is argon gas, removes epoxy resin template.Above-mentioned CVD complete powder is subjected to infrared test, test knot
Fruit is as shown in Figure 3.
Embodiment 5
By Al powder: Nickelous nitrate hexahydrate: it is molten that DEXTROSE ANHYDROUS by quality (g) is added to epoxy resin/ethyl alcohol than 200:5:1
It in liquid (5g epoxy resin, 75ml ethyl alcohol), is slowly added dropwise 2.5ml ethylenediamine (EDA), heating water bath stirring.Temperature is set as 90
DEG C, mixing time 5h takes out drying after above-mentioned dried powder is washed with deionized, by above-mentioned powder when ethyl alcohol volatilizees totally
Reduction treatment is carried out 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 (gas flow is set in 200ml/min).Recovery time is 1h.Afterwards 600
DEG C heating and thermal insulation 1h, atmosphere is argon gas, removes epoxy resin template.Above-mentioned CVD complete powder is carried out to the test of Raman map,
Test results are shown in figure 4.
Embodiment 6
By Al powder: Nickelous nitrate hexahydrate: it is molten that DEXTROSE ANHYDROUS by quality (g) is added to epoxy resin/ethyl alcohol than 200:5:1
It in liquid (5g epoxy resin, 75ml ethyl alcohol), is slowly added dropwise 2.5ml ethylenediamine (EDA), heating water bath stirring.Temperature is set as 90
DEG C, mixing time 5h takes out drying after above-mentioned dried powder is washed with deionized, by above-mentioned powder when ethyl alcohol volatilizees totally
Reduction treatment is carried out 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 (gas flow is set in 200ml/min).Recovery time is 1h.Afterwards 600
DEG C heating and thermal insulation 1h, atmosphere is argon gas, removes epoxy resin template.Above-mentioned CVD complete powder is carried out to the test of XRD, test
As a result as shown in Figure 5.
Embodiment 7
By Al powder: Nickelous nitrate hexahydrate: it is molten that DEXTROSE ANHYDROUS by quality (g) is added to epoxy resin/ethyl alcohol than 200:5:1
It in liquid (5g epoxy resin, 75ml ethyl alcohol), is slowly added dropwise 2.5ml ethylenediamine (EDA), heating water bath stirring.Temperature is set as 90
DEG C, mixing time 5h takes out drying after above-mentioned dried powder is washed with deionized, by above-mentioned powder when ethyl alcohol volatilizees totally
Reduction treatment is carried out 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 (gas flow is set in 200ml/min).Recovery time is 1h.Afterwards 600
DEG C heating and thermal insulation 1h, atmosphere is argon gas, removes epoxy resin template.By the graphene nanometer sheet of above-mentioned preparation/aluminium composite powder
Carried out in vacuum sintering furnace hot-forming, pressure is set as 45MPa or so, and temperature is 600 DEG C, and the dwell time is 1~2h, protects
Cool to room temperature after pressure with the furnace.Its tensile property is tested under universal testing machine, tensile strength reaches 224MPa.It stretches
For curve as shown in Fig. 6 blue curve, fracture apperance is as shown in Figure 7.
Embodiment 8
By Al powder: Nickelous nitrate hexahydrate: DEXTROSE ANHYDROUS is added to epoxy resin/ethyl alcohol than 200:5:0.2 by quality (g)
It in solution (5g epoxy resin, 75ml ethyl alcohol), is slowly added dropwise 2.5ml ethylenediamine (EDA), heating water bath stirring.Temperature is set as
90 DEG C, mixing time 5h, drying after above-mentioned dried powder is washed with deionized is taken out when ethyl alcohol volatilizees totally, 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 hydrogen (gas flow setting
In 50~100ml/min), protective atmosphere is argon gas (gas flow is set in 200ml/min).Recovery time is 1h.Exist afterwards
600 DEG C of heating and thermal insulation 1h, atmosphere are argon gas, remove epoxy resin template.By the graphene nanometer sheet of above-mentioned preparation/aluminium composite powder
End carries out hot-forming in vacuum sintering furnace, and pressure is set as 45MPa or so, and temperature is 600 DEG C, and the dwell time is 1~2h,
Cool to room temperature after pressure maintaining with the furnace.Its tensile property is tested under universal testing machine, tensile strength reaches 192MPa.It draws
Curve is stretched as shown in Fig. 6 green curve.
Embodiment 9
By Al powder: Nickelous nitrate hexahydrate: DEXTROSE ANHYDROUS is added to epoxy resin/ethyl alcohol than 200:5:1.8 by quality (g)
It in solution (5g epoxy resin, 75ml ethyl alcohol), is slowly added dropwise 2.5ml ethylenediamine (EDA), heating water bath stirring.Temperature is set as
90 DEG C, mixing time 5h, drying after above-mentioned dried powder is washed with deionized is taken out when ethyl alcohol volatilizees totally, 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 hydrogen (gas flow setting
In 50~100ml/min), protective atmosphere is argon gas (gas flow is set in 200ml/min).Recovery time is 1h.Exist afterwards
600 DEG C of heating and thermal insulation 1h, atmosphere are argon gas, remove epoxy resin template.By the graphene nanometer sheet of above-mentioned preparation/aluminium composite powder
End carries out hot-forming in vacuum sintering furnace, and pressure is set as 45MPa or so, and temperature is 600 DEG C, and the dwell time is 1~2h,
Cool to room temperature after pressure maintaining with the furnace.Its tensile property is tested under universal testing machine, tensile strength reaches 197MPa.It draws
Curve is stretched 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 or so, and temperature is 600 DEG C, protects
The pressure time is 1~2h, cools to room temperature with the furnace after pressure maintaining.Its tensile property is tested under universal testing machine, is stretched strong
Degree reaches 92MPa.Stress strain curve is as shown in Fig. 6 black curve.
Embodiment 11
By Al powder: Nickelous nitrate hexahydrate: DEXTROSE ANHYDROUS is added in ethanol solution 75ml by quality (g) than 200:5:1,
Heating water bath stirring.Temperature is set as 90 DEG C, mixing time 5h, when ethyl alcohol volatilization totally when take out above-mentioned dried powder spend from
It is dry after sub- water washing, above-mentioned powder is subjected to reduction treatment in horizontal pipe furnace.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 gas
min).Recovery time is 1h.Afterwards in 600 DEG C of heating and thermal insulation 1h, atmosphere is argon gas, removes epoxy resin template.Sintered powder
End scanning pattern is as shown in Figure 8 a.
Embodiment 12
Al powder: Nickelous nitrate hexahydrate is added to epoxy resin/ethanol solution (5g asphalt mixtures modified by epoxy resin than 200:5 by quality (g)
Rouge, 75ml ethyl alcohol) in, it is slowly added dropwise 2.5ml ethylenediamine (EDA), heating water bath stirring.Temperature is set as 90 DEG C, mixing time
5h takes out drying after above-mentioned dried powder is washed with deionized, by above-mentioned powder in horizontal tube when ethyl alcohol volatilizees totally
Reduction treatment is carried out in furnace.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 (gas flow is set in 200ml/min).Recovery time is 1h.Afterwards in 600 DEG C of heating and thermal insulations
1h, atmosphere are argon gas, remove epoxy resin template.Sintered powder scanning pattern is as shown in Figure 8 b.
Embodiment 13
By Al powder: DEXTROSE ANHYDROUS by quality (g) than 200:1 be added to epoxy resin/ethanol solution (5g epoxy resin,
75ml ethyl alcohol) in, it is slowly added dropwise 2.5ml ethylenediamine (EDA), heating water bath stirring.Temperature is set as 90 DEG C, mixing time 5h,
Drying after above-mentioned dried powder is washed with deionized is taken out when ethyl alcohol volatilizees totally, 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 (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 gas, removes epoxy resin template.Sintered powder scanning pattern is as shown in Figure 8 c.It is bent by four stretchings in Fig. 6
Line can be seen that in Al powder: Nickelous nitrate hexahydrate: when DEXTROSE ANHYDROUS=200:5:1 (blue curve), the tension of composite material
Intensity reaches peak value (224MPa), and the tensile strength (92MPa) compared to fine aluminium is higher by 143%, and elongation percentage also maintains nearly 10%,
Unlikely decline is too many.The content of DEXTROSE ANHYDROUS is higher or the relatively low effect that can all reduce enhancing.
Claims (2)
1. a kind of method of aluminium powder surface in situ catalysis preparing graphene by utilizing solid carbon source nanometer sheet nickel-loaded enhancing aluminium composite material,
Include the following steps:
(1) using epoxy resin as network former, using dehydrated alcohol as dispersing agent, according to epoxy resin, dehydrated alcohol volume ratio
For 1:(15-20), uniformly mixing is made into epoxy resin/ethanol solution；
(2) using pure aluminium powder as matrix material, using Nickelous nitrate hexahydrate as catalyst, using DEXTROSE ANHYDROUS as carbon source, according to fine aluminium
Powder, Nickelous nitrate hexahydrate, DEXTROSE ANHYDROUS mass ratio are (150~250): (4~6): (0.8~1.2) is added in above-mentioned (1)
Dissolution and heating water bath stirring in epoxy resin/ethanol solution of preparation, obtain DEXTROSE ANHYDROUS package Ni2+Load epoxy
Resin/A1 mixed solution；
(3) using ethylenediamine as network curing agent, ethylenediamine is slowly added dropwise for 2.5:75 according to ethylenediamine, dehydrated alcohol volume ratio
Into mixed solution obtained in above-mentioned steps (2), heating water bath stirring, totally to the dehydrated alcohol volatilization in this mixed solution
When, the DEXTROSE ANHYDROUS of acquisition is wrapped up into Ni2+Laden epoxy/A1 composite powder is washed and is dried, and is obtained compound
Powder；
(4) composite powder obtained in step (3) is placed in quartzy Noah's ark, is put into horizontal pipe furnace and is sintered, temperature 350
DEG C~450 DEG C, using argon gas as carrier gas, DEXTROSE ANHYDROUS is thermally decomposed, obtains graphene nanometer sheet；It is afterwards to carry with hydrogen/argon gas
Gas removes epoxy networks template in the 500-700 DEG C of above-mentioned powder of sintering, obtains graphene nanometer sheet load Ni enhancing aluminium
Composite powder；Finally, the composite powder is placed in sinter molding in vacuum hotpressing stove.
2. the preparation method of composite material according to claim 1, which is characterized in that step 4) is in removal epoxy resin net
When network template, argon flow is controlled in 60ml/min；Hydrogen flowing quantity is controlled in 50ml/min in DEXTROSE ANHYDROUS thermal decomposition process,
Argon flow is controlled in 200ml/min, and during vacuum heating-press sintering, pressure is set as 45MPa, and temperature is 600 DEG C, pressure maintaining
Time is 1-2h, cools to room temperature with the furnace after pressure maintaining, obtains block materials.
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| CN107538016A (en) * | 2017-07-28 | 2018-01-05 | 天津大学 | A kind of method for the interface wellability for improving graphene and fine aluminium |
| 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 |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101859858A (en) * | 2010-05-07 | 2010-10-13 | 中国科学院苏州纳米技术与纳米仿生研究所 | Transparent conducting electrode based on graphene and manufacture method and applications thereof |
| CN103192072A (en) * | 2013-03-19 | 2013-07-10 | 苏州格瑞丰纳米科技有限公司 | Material adopting thin graphene and metal powder composite structure, preparation method and application thereof |
| CN104797524A (en) * | 2012-11-14 | 2015-07-22 | Lg电子株式会社 | Method for preparing graphene and said graphene, electronic device using said graphene |
| CN104843691A (en) * | 2015-04-30 | 2015-08-19 | 深圳市德方纳米科技股份有限公司 | Graphene and preparation method thereof |
| WO2016006943A1 (en) * | 2014-07-09 | 2016-01-14 | 재단법인대구경북과학기술원 | Metal nanowire having core-shell structure coated with graphene, and manufacturing method therefor |
| CN105525124A (en) * | 2016-02-02 | 2016-04-27 | 天津大学 | Preparation method for in-situ synthesis of three-dimensional graphene-reinforced copper-based composite material |
| KR20160053303A (en) * | 2014-11-03 | 2016-05-13 | 충남대학교산학협력단 | Manufacturing method of hyghly dispersible reduced graphene oxide based metal nanoparticle dispersion and metal nanoparticle film using thereof |
-
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Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101859858A (en) * | 2010-05-07 | 2010-10-13 | 中国科学院苏州纳米技术与纳米仿生研究所 | Transparent conducting electrode based on graphene and manufacture method and applications thereof |
| CN104797524A (en) * | 2012-11-14 | 2015-07-22 | Lg电子株式会社 | Method for preparing graphene and said graphene, electronic device using said graphene |
| CN103192072A (en) * | 2013-03-19 | 2013-07-10 | 苏州格瑞丰纳米科技有限公司 | Material adopting thin graphene and metal powder composite structure, preparation method and application thereof |
| WO2016006943A1 (en) * | 2014-07-09 | 2016-01-14 | 재단법인대구경북과학기술원 | Metal nanowire having core-shell structure coated with graphene, and manufacturing method therefor |
| KR20160053303A (en) * | 2014-11-03 | 2016-05-13 | 충남대학교산학협력단 | Manufacturing method of hyghly dispersible reduced graphene oxide based metal nanoparticle dispersion and metal nanoparticle film using thereof |
| CN104843691A (en) * | 2015-04-30 | 2015-08-19 | 深圳市德方纳米科技股份有限公司 | Graphene and preparation method thereof |
| CN105525124A (en) * | 2016-02-02 | 2016-04-27 | 天津大学 | Preparation method for in-situ synthesis of three-dimensional graphene-reinforced copper-based composite material |
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