CN105081310A - Method for preparing grapheme reinforced aluminum matrix composite material - Google Patents
Method for preparing grapheme reinforced aluminum matrix composite material Download PDFInfo
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Abstract
The invention relates to a method for preparing a grapheme reinforced aluminum matrix composite material. The method aims at solving the technical problems that in an existing method for preparing the grapheme reinforced aluminum matrix composite material, the grapheme dispersibility is poor, and agglomeration is prone to happening. The method includes the steps that (1) oxidized grapheme is prepared; (2) surface modification on aluminum powder is carried out; (3) oxidized grapheme-aluminum composite powder is prepared; and (4) the grapheme reinforced aluminum matrix composite material is prepared. An electrostatic self-assembly method is adopted in the method, so that graphene is evenly dispersed in an aluminum matrix to enable the graphene to be more evenly dispersed, phenomena of damage to graphene size and work hardening generated on the aluminum matrix during ball-milling treatment are avoided, and graphene agglomeration is prevented; in addition, the mechanical property of the composite material is obviously improved; and compared with a pure aluminum material, the strength of extension is improved by 10%-20%, and the hardness is improved by 10%-30%.
Description
Technical field
The present invention relates to a kind of method preparing Graphene reinforced aluminum matrix composites.
Background technology
It is little that aluminum matrix composite has density, and corrosion resistance is strong, and electrical and thermal conductivity performance is excellent, the advantages such as good processability, thus become the main flow of current metal-base composites research.Along with the development of automobile and aerospace field, especially in space space, to the specific strength of metal-base composites in the adverse circumstances such as ionising radiation, specific modulus, corrosion resistance, the performance requirements such as conductive and heat-conductive are higher, and traditional ceramic fibre and reinforced particulate can not meet the requirement to material.
Carbonaceous material (carbon fiber, graphite and CNT etc.) has high conductive and heat-conductive coefficient, good mechanical property, is ideal aluminum matrix composite reinforcement.Wherein, CNT is a kind of one-dimensional material, and form the coaxial pipe of several layers to tens of layers primarily of the carbon atom in hexagonal array, diameter is generally 2 ~ 20nm.CNT has excellent mechanical property, and intensity is 10 ~ 100 times of hardness of steel, and Young's modulus reaches 1TPa, and in addition, CNT also has excellent electrical and thermal conductivity performance.Due to mechanics and the physical property of excellence, one of CNT aluminum matrix composite reinforcement being considered to most prospect.But recent researches finds, CNT to be joined in aluminum substrate the enhancing effect of aluminum matrix composite and not obvious as reinforcement.This mainly because have very strong Van der Waals force between CNT, easily reunites, and CNT is difficult to realize dispersed in aluminum substrate.
Graphene be a kind of by carbon atom with sp
2the hexangle type of hybridized orbit composition is honeycomb lattice, only has the two-dimensional material of a carbon atom thickness.In recent years because its high Young's modulus (1TPa), high fracture strength (125GPa), super-high heat-conductive coefficient (5000Wm
-1k
-1) and electron mobility (200000cm
2v
-1s
-1) cause very big concern.Compared to CNT, the two-dimensional structure of Graphene makes Graphene relatively more easily control and be dispersed in aluminum substrate, therefore give full play to the enhancing effect of Graphene, prepare the concern that high performance Graphene reinforced aluminum matrix composites has caused more and more researcher.
But it is at the early-stage about the research of Graphene reinforced aluminum matrix composites, up to the present the research of Graphene reinforced aluminum matrix composites does not make a breakthrough, this is mainly because Graphene has very large specific area, and surface energy is high, also has strong reunion tendency.Therefore, in the process preparing Graphene reinforced aluminum matrix composites, crucial step is exactly seek new technique to be dispersed in aluminum substrate by graphene uniform.Current ball-milling method is the main method of graphene dispersion, although ball-milling method can realize large-scale production, ball-milling method often damages the size of Graphene and causes work hardening to aluminum substrate, weakens the strengthening effect of Graphene.
Summary of the invention
The object of the invention is to solve that existing to prepare the graphene dispersion existed in Graphene reinforced aluminum matrix composites poor, the technical problem of easily reuniting, and a kind of method preparing Graphene reinforced aluminum matrix composites is provided.
A kind of method preparing Graphene reinforced aluminum matrix composites of the present invention is carried out according to the following steps:
One, prepare graphene oxide: under the condition of ice-water bath to be equipped with 46mL the concentrated sulfuric acid conical flask in add 1g graphite powder and 1g sodium nitrate, mix and blend 20min under the condition of ice-water bath, 6g potassium permanganate is added under the condition of ice-water bath, stir 40min, obtain the mixed liquor of green purple, be be incubated 1h under the condition of 30 DEG C ~ 40 DEG C in temperature by the mixed liquor of green purple, then be the distilled water adding 40mL under the condition of 30 DEG C ~ 40 DEG C in temperature, be be incubated 30min under the condition of 85 DEG C ~ 95 DEG C in temperature, obtain brown mixture, the distilled water of 100mL and the hydrogen peroxide of 6mL is added at ambient temperature in brown mixture, obtain jonquilleous mixed liquor, then with mass concentration be 3% hydrochloric acid solution and the jonquilleous mixed liquor of distilled water cyclic washing be 6 ~ 7 to pH, filter, freeze drying 12h, obtain electronegative graphene oxide,
Two, the surface modification of aluminium powder: aluminium powder being joined mass fraction is in the CTAB solution of 1%, ultrasonic disperse 20min ~ 60min, then magnetic agitation 1h ~ 2h, with distilled water washing, filters, obtains the positively charged aluminium powder that CTAB modifies; The weight of described aluminium powder and mass fraction are the volume ratio of the CTAB solution of 1% is 1g:(1mL ~ 2mL);
Three, graphene oxide-aluminium composite powder is prepared: the positively charged aluminium powder that CTAB 100g step 2 obtained modifies joins in the distilled water of 100mL, at room temperature stirs 30min, obtains aluminium powder suspension; Take electronegative graphene oxide 0.1g ~ 0.5g ultrasonic disperse 1h in the distilled water of 50mL that step one obtains, obtain graphene oxide water-borne dispersions; Graphene oxide water-borne dispersions is joined in aluminium powder suspension, obtain mixed liquor, being uniformly mixed liquid to mixed liquor color is that water white transparency makes electronegative graphene oxide be adsorbed onto positively charged aluminium powder surface by electrostatic attraction, filter, freeze drying 8h, obtains graphene oxide-aluminium composite powder;
Four, the preparation of Graphene reinforced aluminum matrix composites: it is in the mould of graphite that graphene oxide step 3 prepared-aluminium composite powder joins material, 1h ~ 2h is sintered under be 25MPa and temperature being the condition of 600 DEG C at argon shield, pressure, naturally cool to room temperature, obtain Graphene reinforced aluminum matrix composites; The die surface of described graphite scribbles boron nitride impervious barrier.
The method of the present invention's electrostatic self-assembled effectively by graphene uniform be dispersed in aluminum substrate make graphene dispersion evenly, to the destruction of Graphene size and the work hardening phenomenon that produces aluminum substrate simultaneously when avoiding ball-milling treatment, prevent the generation of Graphene agglomeration, and improve the mechanical property of material significantly, improve 10% ~ 20% compared to the tensile strength of pure aluminum material, hardness improves 10% ~ 30%.
CTAB is softex kw, softex kw is a kind of quaternary ammonium salt cationic surfactant, polar end containing hydrophobic Long carbon chain and positively charged, in the present invention when joining in the aqueous solution of softex kw by aluminium powder, lammonium bromide can be adsorbed on aluminium powder surface makes its surface with positive charge.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the graphene oxide of preparation in test one step one;
Fig. 2 is the XRD figure of graphene oxide and graphite, and curve 1 is the graphene oxide of preparation in test one step one, and curve 2 is the graphite powder in test one step one;
Fig. 3 be in test one step one preparation graphene oxide FT-IR figure;
Fig. 4 is the SEM figure of graphene oxide-aluminium composite powder prepared by test four step 3;
Fig. 5 is the XRD figure of Graphene reinforced aluminum matrix composites and fine aluminium, and curve 1 is Graphene reinforced aluminum matrix composites prepared by test four, and curve 2 is fine aluminium prepared by test one;
Fig. 6 is the TEM figure of Graphene reinforced aluminum matrix composites prepared by test four, and 1 is Graphene, and region A is aluminium;
Fig. 7 is tensile strength and the percentage elongation figure of the Graphene reinforced aluminum matrix composites of different quality mark, and curve 1 is percentage elongation, and curve 2 is tensile strength;
Fig. 8 is the Vickers hardness figure of the Graphene reinforced aluminum matrix composites of different quality mark;
Fig. 9 is the SEM figure of the rear fracture of pure aluminum material stretching prepared by test one;
Figure 10 is the SEM figure of the rear fracture of Graphene reinforced aluminum matrix composites stretching prepared by test two;
Figure 11 is the SEM figure of the rear fracture of Graphene reinforced aluminum matrix composites stretching prepared by test three;
Figure 12 is the SEM figure of the rear fracture of Graphene reinforced aluminum matrix composites stretching prepared by test four.
Detailed description of the invention
Detailed description of the invention one: present embodiment is a kind of method preparing Graphene reinforced aluminum matrix composites, specifically carries out according to the following steps:
One, prepare graphene oxide: under the condition of ice-water bath to be equipped with 46mL the concentrated sulfuric acid conical flask in add 1g graphite powder and 1g sodium nitrate, mix and blend 20min under the condition of ice-water bath, 6g potassium permanganate is added under the condition of ice-water bath, stir 40min, obtain the mixed liquor of green purple, be be incubated 1h under the condition of 30 DEG C ~ 40 DEG C in temperature by the mixed liquor of green purple, then be the distilled water adding 40mL under the condition of 30 DEG C ~ 40 DEG C in temperature, be be incubated 30min under the condition of 85 DEG C ~ 95 DEG C in temperature, obtain brown mixture, the distilled water of 100mL and the hydrogen peroxide of 6mL is added at ambient temperature in brown mixture, obtain jonquilleous mixed liquor, then with mass concentration be 3% hydrochloric acid solution and the jonquilleous mixed liquor of distilled water cyclic washing be 6 ~ 7 to pH, filter, freeze drying 12h, obtain electronegative graphene oxide,
Two, the surface modification of aluminium powder: aluminium powder being joined mass fraction is in the CTAB solution of 1%, ultrasonic disperse 20min ~ 60min, then magnetic agitation 1h ~ 2h, with distilled water washing, filters, obtains the positively charged aluminium powder that CTAB modifies; The weight of described aluminium powder and mass fraction are the volume ratio of the CTAB solution of 1% is 1g:(1mL ~ 2mL);
Three, graphene oxide-aluminium composite powder is prepared: the positively charged aluminium powder that CTAB 100g step 2 obtained modifies joins in the distilled water of 100mL, at room temperature stirs 30min, obtains aluminium powder suspension; Take electronegative graphene oxide 0.1g ~ 0.5g ultrasonic disperse 1h in the distilled water of 50mL that step one obtains, obtain graphene oxide water-borne dispersions; Graphene oxide water-borne dispersions is joined in aluminium powder suspension, obtain mixed liquor, being uniformly mixed liquid to mixed liquor color is that water white transparency makes electronegative graphene oxide be adsorbed onto positively charged aluminium powder surface by electrostatic attraction, filter, freeze drying 8h, obtains graphene oxide-aluminium composite powder;
Four, the preparation of Graphene reinforced aluminum matrix composites: it is in the mould of graphite that graphene oxide step 3 prepared-aluminium composite powder joins material, 1h ~ 2h is sintered under be 25MPa and temperature being the condition of 600 DEG C at argon shield, pressure, naturally cool to room temperature, obtain Graphene reinforced aluminum matrix composites; The die surface of described graphite scribbles boron nitride impervious barrier.
Detailed description of the invention two: the difference of present embodiment and detailed description of the invention one is: the mass concentration of the concentrated sulfuric acid described in step one is 98%.Other are identical with detailed description of the invention one.
Detailed description of the invention three: the difference of present embodiment and detailed description of the invention one or two is: the weight of the aluminium powder described in step 2 and mass fraction are the volume ratio of the CTAB solution of 1% is 1g:1mL.Other are identical with detailed description of the invention one or two.
Detailed description of the invention four: the difference of present embodiment and detailed description of the invention one to three is: take graphene oxide 0.3g ultrasonic disperse 1h in the distilled water of 50mL that step one obtains in step 3, obtain graphene oxide water-borne dispersions.Other are identical with detailed description of the invention one to three.
Detailed description of the invention five: the difference of present embodiment and detailed description of the invention one to four is: it is in the mould of graphite that graphene oxide step 3 prepared in step 4-aluminium composite powder joins material; 2h is sintered under be 25MPa and temperature being the condition of 600 DEG C at argon shield, pressure; naturally cool to room temperature, obtain Graphene reinforced aluminum matrix composites.Other are identical with detailed description of the invention one to four.
By following verification experimental verification beneficial effect of the present invention:
Test one: this test is contrast test, prepares fine aluminium, and concrete grammar is:
Aluminium powder being joined material is in the mould of graphite, sinters 1h ~ 2h, naturally cool to room temperature, obtain fine aluminium at argon shield, pressure under be 25MPa and temperature being the condition of 600 DEG C; The die surface of described graphite scribbles boron nitride impervious barrier.
Test two: a kind of method preparing Graphene reinforced aluminum matrix composites, specifically carry out according to the following steps:
One, prepare graphene oxide: under the condition of ice-water bath to be equipped with 46mL the concentrated sulfuric acid conical flask in add 1g graphite powder and 1g sodium nitrate, mix and blend 20min under the condition of ice-water bath, 6g potassium permanganate is added under the condition of ice-water bath, stir 40min, obtain the mixed liquor of green purple, be be incubated 1h under the condition of 35 DEG C in temperature by the mixed liquor of green purple, then be the distilled water adding 40mL under the condition of 35 DEG C in temperature, be be incubated 30min under the condition of 90 DEG C in temperature, obtain brown mixture, the distilled water of 100mL and the hydrogen peroxide of 6mL is added at ambient temperature in brown mixture, obtain jonquilleous mixed liquor, then with mass concentration be 3% hydrochloric acid solution and the jonquilleous mixed liquor of distilled water cyclic washing be 6 ~ 7 to pH, filter, freeze drying 12h, obtain electronegative graphene oxide,
Two, the surface modification of aluminium powder: 100g aluminium powder being joined 100mL mass fraction is in the CTAB solution of 1%, ultrasonic disperse 40min, then magnetic agitation 2h, with distilled water washing, filters, obtains the positively charged aluminium powder that CTAB modifies;
Three, graphene oxide-aluminium composite powder is prepared: the positively charged aluminium powder that CTAB 100g step 2 obtained modifies joins in the distilled water of 100mL, at room temperature stirs 30min, obtains aluminium powder suspension; Take electronegative graphene oxide 0.1g ultrasonic disperse 1h in the distilled water of 50mL that step one obtains, obtain graphene oxide water-borne dispersions; Graphene oxide water-borne dispersions is joined in aluminium powder suspension, obtain mixed liquor, being uniformly mixed liquid to mixed liquor color is that water white transparency makes electronegative graphene oxide be adsorbed onto positively charged aluminium powder surface by electrostatic attraction, filter, freeze drying 8h, obtains graphene oxide-aluminium composite powder;
Four, the preparation of Graphene reinforced aluminum matrix composites: it is in the mould of graphite that graphene oxide step 3 prepared-aluminium composite powder joins material, 2h is sintered under be 25MPa and temperature being the condition of 600 DEG C at argon shield, pressure, naturally cool to room temperature, obtain Graphene reinforced aluminum matrix composites; The die surface of described graphite scribbles boron nitride impervious barrier.
The mass concentration of the concentrated sulfuric acid described in step one is 98%.
Test three: a kind of method preparing Graphene reinforced aluminum matrix composites, specifically carry out according to the following steps:
One, prepare graphene oxide: under the condition of ice-water bath to be equipped with 46mL the concentrated sulfuric acid conical flask in add 1g graphite powder and 1g sodium nitrate, mix and blend 20min under the condition of ice-water bath, 6g potassium permanganate is added under the condition of ice-water bath, stir 40min, obtain the mixed liquor of green purple, be be incubated 1h under the condition of 35 DEG C in temperature by the mixed liquor of green purple, then be the distilled water adding 40mL under the condition of 35 DEG C in temperature, be be incubated 30min under the condition of 90 DEG C in temperature, obtain brown mixture, the distilled water of 100mL and the hydrogen peroxide of 6mL is added at ambient temperature in brown mixture, obtain jonquilleous mixed liquor, then with mass concentration be 3% hydrochloric acid solution and the jonquilleous mixed liquor of distilled water cyclic washing be 6 ~ 7 to pH, filter, freeze drying 12h, obtain electronegative graphene oxide,
Two, the surface modification of aluminium powder: 100g aluminium powder being joined 100mL mass fraction is in the CTAB solution of 1%, ultrasonic disperse 40min, then magnetic agitation 2h, with distilled water washing, filters, obtains the positively charged aluminium powder that CTAB modifies;
Three, graphene oxide-aluminium composite powder is prepared: the positively charged aluminium powder that CTAB 100g step 2 obtained modifies joins in the distilled water of 100mL, at room temperature stirs 30min, obtains aluminium powder suspension; Take electronegative graphene oxide 0.3g ultrasonic disperse 1h in the distilled water of 50mL that step one obtains, obtain graphene oxide water-borne dispersions; Graphene oxide water-borne dispersions is joined in aluminium powder suspension, obtain mixed liquor, being uniformly mixed liquid to mixed liquor color is that water white transparency makes electronegative graphene oxide be adsorbed onto positively charged aluminium powder surface by electrostatic attraction, filter, freeze drying 8h, obtains graphene oxide-aluminium composite powder;
Four, the preparation of Graphene reinforced aluminum matrix composites: it is in the mould of graphite that graphene oxide step 3 prepared-aluminium composite powder joins material, 2h is sintered under be 25MPa and temperature being the condition of 600 DEG C at argon shield, pressure, naturally cool to room temperature, obtain Graphene reinforced aluminum matrix composites; The die surface of described graphite scribbles boron nitride impervious barrier.
The mass concentration of the concentrated sulfuric acid described in step one is 98%.
Test four: a kind of method preparing Graphene reinforced aluminum matrix composites, specifically carry out according to the following steps:
One, prepare graphene oxide: under the condition of ice-water bath to be equipped with 46mL the concentrated sulfuric acid conical flask in add 1g graphite powder and 1g sodium nitrate, mix and blend 20min under the condition of ice-water bath, 6g potassium permanganate is added under the condition of ice-water bath, stir 40min, obtain the mixed liquor of green purple, be be incubated 1h under the condition of 35 DEG C in temperature by the mixed liquor of green purple, then be the distilled water adding 40mL under the condition of 35 DEG C in temperature, be be incubated 30min under the condition of 90 DEG C in temperature, obtain brown mixture, the distilled water of 100mL and the hydrogen peroxide of 6mL is added at ambient temperature in brown mixture, obtain jonquilleous mixed liquor, then with mass concentration be 3% hydrochloric acid solution and the jonquilleous mixed liquor of distilled water cyclic washing be 6 ~ 7 to pH, filter, freeze drying 12h, obtain electronegative graphene oxide,
Two, the surface modification of aluminium powder: 100g aluminium powder being joined 100mL mass fraction is in the CTAB solution of 1%, ultrasonic disperse 40min, then magnetic agitation 2h, with distilled water washing, filters, obtains the positively charged aluminium powder that CTAB modifies;
Three, graphene oxide-aluminium composite powder is prepared: the positively charged aluminium powder that CTAB 100g step 2 obtained modifies joins in the distilled water of 100mL, at room temperature stirs 30min, obtains aluminium powder suspension; Take electronegative graphene oxide 0.5g ultrasonic disperse 1h in the distilled water of 50mL that step one obtains, obtain graphene oxide water-borne dispersions; Being uniformly mixed liquid to mixed liquor color is that water white transparency makes electronegative graphene oxide be adsorbed onto positively charged aluminium powder surface by electrostatic attraction, and filter, freeze drying 8h, obtains graphene oxide-aluminium composite powder;
Four, the preparation of Graphene reinforced aluminum matrix composites: it is in the mould of graphite that graphene oxide step 3 prepared-aluminium composite powder joins material, 2h is sintered under be 25MPa and temperature being the condition of 600 DEG C at argon shield, pressure, naturally cool to room temperature, obtain Graphene reinforced aluminum matrix composites; The die surface of described graphite scribbles boron nitride impervious barrier.
The mass concentration of the concentrated sulfuric acid described in step one is 98%.
Fig. 1 is the SEM figure of the graphene oxide of preparation in test one step one, and as can be seen from the figure the graphene oxide size prepared of this test use Hummers method is large and transparent, shows that this method can obtain the less and large-sized graphene oxide of the number of plies.
Fig. 2 is the XRD figure of graphene oxide and graphite, curve 1 is the graphene oxide of preparation in test one step one, curve 2 is the graphite powder in test one step one, can find out that graphite powder is after the process of Hummers method, because the embedding of group makes sheet interlayer spacing open, simultaneously because the existence of group makes the graphene oxide degree of crystallinity prepared decline, defect increases.
Fig. 3 be in test one step one preparation graphene oxide FT-IR collection of illustrative plates, as can be seen from the figure graphene oxide is 3410cm in wave number
-1near have an obvious absworption peak, the OH stretching vibration of hydroxyl in graphene oxide structure should be belonged to; In figure, wave number is 2920cm
-1and 2850cm
-1peak, place belongs to CH respectively
2antisymmetry, symmetrical stretching vibration peak; 1737cm
-1the absworption peak of position should belong to the stretching vibration peak of carbonyl or carboxyl (C=O); Wave number is 1638cm
-1neighbouring absworption peak belongs to the stretching vibration of C=C; Wave number is 1397cm
-1neighbouring peak belongs to the OH deformation vibration of hydroxyl in structure; Wave number is 1060cm
-1neighbouring peak belongs to the stretching vibration of epoxide group (C-O-C).Just because of the existence of above-mentioned polar group, test the graphene oxide of preparation in a step one in aqueous after ultrasonic process, graphene oxide is with very strong negative electrical charge.
Fig. 4 is the SEM figure of graphene oxide-aluminium composite powder prepared by test four step 3, and as can be seen from the figure graphene oxide is mainly coated on aluminum particle surface, and not obvious agglomeration occurs.
Fig. 5 is the XRD collection of illustrative plates of Graphene reinforced aluminum matrix composites and fine aluminium, curve 1 is Graphene reinforced aluminum matrix composites prepared by test four, curve 2 is fine aluminium prepared by test one, as can be seen from the figure test graphene oxide-aluminium composite powder prepared by four step 3 and do not occur obvious Carbide Phases after oversintering, illustrate that obvious interfacial reaction does not occur Graphene reinforced aluminum matrix composites prepared by test four.
Fig. 6 is the TEM collection of illustrative plates of Graphene reinforced aluminum matrix composites prepared by test four, and 1 is Graphene, and region A is aluminium, and as can be seen from the figure Graphene is mainly distributed in the interface cohesion place of aluminum particle, and the not obvious agglomeration that is uniformly dispersed occurs.
Fig. 7 is tensile strength and the percentage elongation figure of the Graphene reinforced aluminum matrix composites of different quality mark, the mass fraction of Graphene is 0 is fine aluminium prepared by test one, the mass fraction of Graphene is 0.1% is Graphene reinforced aluminum matrix composites prepared by test two, the mass fraction of Graphene is 0.3% is Graphene reinforced aluminum matrix composites prepared by test three, the mass fraction of Graphene is 0.5% is Graphene reinforced aluminum matrix composites prepared by test four, curve 1 is percentage elongation, curve 2 is tensile strength, as can be seen from the figure when the mass fraction of Graphene is 0.3wt%, the tensile strength of Graphene reinforced aluminum matrix composites reaches maximum, percentage elongation reduces gradually along with the increase of Graphene mass fraction.
Fig. 8 is the Vickers hardness figure of the Graphene reinforced aluminum matrix composites of different quality mark, the mass fraction of Graphene is 0 is fine aluminium prepared by test one, the mass fraction of Graphene is 0.1% is Graphene reinforced aluminum matrix composites prepared by test two, the mass fraction of Graphene is 0.3% is Graphene reinforced aluminum matrix composites prepared by test three, the mass fraction of Graphene is 0.5% is Graphene reinforced aluminum matrix composites prepared by test four, as can be seen from the figure, along with the increase of Graphene content, the Vickers hardness of Graphene reinforced aluminum matrix composites presents the trend first increasing and reduce afterwards.The fine aluminium hardness adopting identical hot-pressing sintering technique to prepare is 27HV, and the Vickers hardness testing the Graphene reinforced aluminum matrix composites of the 0.3wt% of three preparations is 35HV, improves 30% compared to fine aluminium; When the addition of Graphene reaches 0.5wt% (test four preparation), the Vickers hardness of Graphene reinforced aluminum matrix composites starts to decline, this may mainly because Graphene too high levels, cause associativity between aluminum particle to decline, composite mesopore is increased the hardness number appearance making composite and is declined.
Fig. 9 is the SEM figure of the rear fracture of pure aluminum material stretching prepared by test one, clearly can find out that from figure the fracture of fine aluminium is obvious dimple shape, belong to typical ductile rupture, this mainly because of sample under a stretching force, aluminum substrate generation plastic deformation, there is serious stress at the boundary of alumina particles to concentrate, and then produce micropore at granule boundary place, these micropores constantly connect and are polymerized, final material disconnects along the boundary of particle, cause the unsticking of particle and particle, and around particle, leave the plastic deformation dimple pattern torn.
Figure 10 is the SEM figure of the rear fracture of Graphene reinforced aluminum matrix composites stretching prepared by test two.Figure 11 is the SEM figure of the rear fracture of Graphene reinforced aluminum matrix composites stretching prepared by test three.Figure 12 is the SEM figure of the rear fracture of Graphene reinforced aluminum matrix composites stretching prepared by test four.As can be seen from the figure, along with the fracture surface of the increase Graphene reinforced aluminum matrix composites of Graphene mass fraction becomes more coarse, the fracture of composite flexible turns to brittle fracture trend gradually.When Graphene mass fraction is 0.5wt%, fracture mainly appears at the interface of blapharoplast.This is because Graphene is mainly present in interface, the combination of blapharoplast in hot pressed sintering process has been isolated in the increase of Graphene mass fraction, when Graphene content is moderate, tensile strength reaches maximum, the decline gradually that the percentage elongation of composite increases with Graphene amount.
Claims (5)
1. prepare a method for Graphene reinforced aluminum matrix composites, it is characterized in that the method preparing Graphene reinforced aluminum matrix composites is carried out according to the following steps:
One, prepare graphene oxide: under the condition of ice-water bath to be equipped with 46mL the concentrated sulfuric acid conical flask in add 1g graphite powder and 1g sodium nitrate, mix and blend 20min under the condition of ice-water bath, 6g potassium permanganate is added under the condition of ice-water bath, stir 40min, obtain the mixed liquor of green purple, be be incubated 1h under the condition of 30 DEG C ~ 40 DEG C in temperature by the mixed liquor of green purple, then be the distilled water adding 40mL under the condition of 30 DEG C ~ 40 DEG C in temperature, be be incubated 30min under the condition of 85 DEG C ~ 95 DEG C in temperature, obtain brown mixture, the distilled water of 100mL and the hydrogen peroxide of 6mL is added at ambient temperature in brown mixture, obtain jonquilleous mixed liquor, then with mass concentration be 3% hydrochloric acid solution and the jonquilleous mixed liquor of distilled water cyclic washing be 6 ~ 7 to pH, filter, freeze drying 12h, obtain electronegative graphene oxide,
Two, the surface modification of aluminium powder: aluminium powder being joined mass fraction is in the CTAB solution of 1%, ultrasonic disperse 20min ~ 60min, then magnetic agitation 1h ~ 2h, with distilled water washing, filters, obtains the positively charged aluminium powder that CTAB modifies; The weight of described aluminium powder and mass fraction are the volume ratio of the CTAB solution of 1% is 1g:(1mL ~ 2mL);
Three, graphene oxide-aluminium composite powder is prepared: the positively charged aluminium powder that CTAB 100g step 2 obtained modifies joins in the distilled water of 100mL, at room temperature stirs 30min, obtains aluminium powder suspension; Take electronegative graphene oxide 0.1g ~ 0.5g ultrasonic disperse 1h in the distilled water of 50mL that step one obtains, obtain graphene oxide water-borne dispersions; Graphene oxide water-borne dispersions is joined in aluminium powder suspension, obtain mixed liquor, being uniformly mixed liquid to mixed liquor color is that water white transparency makes electronegative graphene oxide be adsorbed onto positively charged aluminium powder surface by electrostatic attraction, filter, freeze drying 8h, obtains graphene oxide-aluminium composite powder;
Four, the preparation of Graphene reinforced aluminum matrix composites: it is in the mould of graphite that graphene oxide step 3 prepared-aluminium composite powder joins material, 1h ~ 2h is sintered under be 25MPa and temperature being the condition of 600 DEG C at argon shield, pressure, naturally cool to room temperature, obtain Graphene reinforced aluminum matrix composites; The die surface of described graphite scribbles boron nitride impervious barrier.
2. a kind of method preparing Graphene reinforced aluminum matrix composites according to claim 1, is characterized in that the mass concentration of the concentrated sulfuric acid described in step one is 98%.
3. a kind of method preparing Graphene reinforced aluminum matrix composites according to claim 1, is characterized in that the weight of the aluminium powder described in step 2 and mass fraction be the volume ratio of the CTAB solution of 1% are 1g:1mL.
4. a kind of method preparing Graphene reinforced aluminum matrix composites according to claim 1, is characterized in that taking in step 3 graphene oxide 0.3g ultrasonic disperse 1h in the distilled water of 50mL that step one obtains, obtains graphene oxide water-borne dispersions.
5. a kind of method preparing Graphene reinforced aluminum matrix composites according to claim 1; it is characterized in that graphene oxide-aluminium composite powder step 3 prepared in step 4 joins material is in the mould of graphite; 2h is sintered under be 25MPa and temperature being the condition of 600 DEG C at argon shield, pressure; naturally cool to room temperature, obtain Graphene reinforced aluminum matrix composites.
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