CN114369740A - Preparation method of graphene/aluminum complex - Google Patents
Preparation method of graphene/aluminum complex Download PDFInfo
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- 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
- 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
- B22F3/02—Compacting only
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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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C21/00—Alloys based on aluminium
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
Abstract
The invention discloses a preparation method of a graphene/aluminum complex, which comprises the steps of preparing graphene/aluminum electrostatic self-assembly powder by adopting an electrostatic self-assembly method, wherein the graphene is single-layer, double-layer or multi-layer graphene or graphene oxide, hydrogenated graphene and fluorinated graphene, carrying out vacuum ball milling on aluminum powder and the graphene/aluminum electrostatic self-assembly powder to prepare graphene/aluminum mixed powder, carrying out cold press molding on the graphene/aluminum mixed powder, placing a pressed compact in a vacuum hot-pressing sintering furnace for sintering at 400-450 ℃, and raising the furnace temperature to 580-620 ℃ for secondary sintering to obtain the graphene/aluminum complex. According to the invention, the graphene is subjected to surface modification treatment, the adsorption effect between the graphene and aluminum powder is strengthened, the graphene and aluminum are uniformly coated by adopting a multi-stage uniform powder mixing and dispersing method, the graphene/aluminum complex is prepared by combining cold pressing and hot pressing technologies, and the graphene is uniformly distributed in a pure aluminum matrix and has good interface combination.
Description
Technical Field
The invention belongs to the field of metal matrix composite materials, and relates to a preparation method of a graphene/aluminum complex.
Background
At present, the preparation methods of graphene reinforced aluminum-based, magnesium-based, titanium-based, steel-based and other metal-based composite materials mainly comprise a liquid method, a powder metallurgy method and an infiltration method. Usually, a transition metal layer is generated by plating Cu, Ni, Al and the like on the surface of the graphene, so that the structural integrity of the graphene is protected. However, the graphene sheet layer is thin and small in size, and the technology for plating the metal layer on the surface of the graphene sheet layer is complex and difficult to control, and has great pollution, so that the practicability, effectiveness, economy and the like of the technology are limited; graphene does not undergo surface treatment, but graphene is light in weight and small in size, so that the graphene has a problem of uniform dispersion during use.
The problem of how to control the harmful interface reaction between the graphene and the metal matrix without damaging the special structure of the graphene in the preparation process exists by introducing the graphene into the metal. In the prior art, a transition metal layer is generated by plating Cu, Ni, Al and the like on the surface of graphene to protect the structural integrity of the graphene, but the graphene has thin sheet layers and small size, the technology for plating the metal layer on the surface of the graphene is complex and is difficult to control, the pollution is extremely high, and the practicability, effectiveness, economy and the like of the technology are limited; graphene is not treated, but graphene is light and small in size, so that the graphene has the problem of uniform dispersion during use. The method introduces graphene into a metal system, and has the problems that the difference of the metal system and the temperature environment of the metal melt is large, so that the special structure of the graphene is not damaged in the preparation process, and the harmful interface reaction between the graphene and an aluminum substrate is controlled. The patent technology (application publication number: 105112732A) of the Beijing aviation materials institute, Wang Xudong and the like adopts the working procedures of mechanical mixing, low-temperature ball milling (participation of liquid nitrogen), ball milling sheath vacuum degassing, hot isostatic pressing, turning sheath removal, extrusion and the like to prepare the graphene/aluminum alloy base composite material with the graphene content of 0.1-5.0 wt.%. According to the preparation method of the composite material, only V-shaped mixed powder needs 24-48 hours, and long-time ball milling, hot isostatic pressing, sheath processing and removing, and degassing are performed, so that the whole process flow and the production period are long, and the difficulty in reducing the manufacturing cost is high.
Disclosure of Invention
The invention aims to provide a preparation method of a graphene/aluminum composite, which solves the problem that graphene is not easy to disperse uniformly when being introduced into a metal melt in the existing method.
The technical scheme adopted by the invention is that the preparation method of the graphene/aluminum composite comprises the following steps:
step 1, preparing graphene/aluminum electrostatic self-assembly powder by adopting an electrostatic self-assembly method, wherein the mass percent of graphene is 4.0-10.0 wt.%, and the graphene is single-layer, double-layer or multi-layer graphene, or graphene oxide, hydrogenated graphene and fluorinated graphene;
step 2, taking a proper amount of aluminum powder and the graphene/aluminum electrostatic self-assembly powder prepared in the step 1 to perform vacuum ball milling, and preparing graphene/aluminum mixed powder, wherein the mass percent of graphene is less than or equal to 1.0 wt.%;
step 3, carrying out cold press molding on the graphene/aluminum mixed powder to obtain a pressed blank;
and 4, placing the pressed compact in a vacuum hot-pressing sintering furnace for sintering at 400-450 ℃, and raising the furnace temperature to 580-620 ℃ for secondary sintering to obtain the graphene/aluminum composite.
Wherein, the step 1 specifically comprises the following steps:
step 1.1, adding graphene into deionized water, and carrying out ultrasonic oscillation for 20-30 min to obtain a graphene turbid liquid;
step 1.2, adding one or more of surfactants such as sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, hexadecyl ammonium bromide and polyvinylpyrrolidone into the graphene turbid liquid, and then stirring until the surfactants are completely dissolved to complete surface polarization modification treatment on the graphene;
and step 1.3, adding aluminum powder into the turbid liquid obtained in the step 1.2, continuously stirring until the aluminum powder and the graphene are uniformly adsorbed to obtain a colloidal suspension, standing until the colloidal suspension is obviously layered, and filtering and vacuum drying the precipitate to obtain the flocculent graphene/aluminum electrostatic self-assembly powder.
In the step 1.2, the mass ratio of the addition amount of the surfactant to the graphene is 2-10: 1.
in the step 2, firstly placing the graphene/aluminum electrostatic self-assembly powder, the grinding balls and the ball-milling medium stearic acid in a vacuum ball mill for ball milling and dispersion for 20-50 min, then adding aluminum powder into a ball-milling tank for ball milling, wherein the ball-material ratio is 5-10: 1, the rotating speed of the ball mill is 100-300 r/min, the ball-milling time is 2-4 h, adopting an intermittent ball-milling method, controlling the temperature of the ball-milling tank to be less than or equal to 40 ℃, and fully wrapping the aluminum powder with the graphene in the repeated cold welding and cracking processes to obtain the graphene/aluminum mixed powder.
In the step 3, the pressure of the graphene/aluminum mixed powder is 10 MPa-60 MPa.
The step 4 specifically comprises the following steps:
step 4.1, placing the pressed compact in a vacuum hot-pressing sintering furnace, then raising the temperature of the furnace to 25-200 ℃, and carrying out vacuum pumping treatment in the temperature raising process to ensure that the vacuum degree in the furnace is less than or equal to 1.0 multiplied by 10-2Pa；
Step 4.2, raising the furnace temperature of the vacuum hot-pressing sintering furnace to 400-450 ℃ to sinter the pressed blank for 1-3 h;
and 4.3, raising the furnace temperature of the vacuum hot-pressing sintering furnace to 580-620 ℃ to perform secondary sintering on the pressed blank, wherein the sintering time is 2-3 h, and obtaining the graphene/aluminum composite body after sintering.
In step 4.2, the temperature rise speed of the furnace temperature is 5-15 ℃/min, the sintering mode is thermal sintering or hot-pressing sintering, and the pressure applied to the pressed compact during the hot-pressing sintering is 10-100 MPa.
In step 4.3, the secondary sintering is thermal sintering or hot-pressing sintering, and the pressure applied to the green compact during the hot-pressing sintering is 10MPa to 100 MPa.
The invention has the beneficial effects that: the method has the advantages that the graphene is subjected to surface modification treatment, the adsorption effect between the graphene and aluminum powder is strengthened, a multi-stage uniform powder mixing and dispersing method is adopted, the graphene and the aluminum are uniformly coated with each other, a graphene/aluminum composite body is prepared by combining cold pressing and hot pressing technologies, the graphene is uniformly distributed in a pure aluminum matrix and has good interface combination, the composite body is added into aluminum alloy melts such as pure aluminum, Al-Si, Al-Mg, Al-Cu and the like in an intermediate alloy mode, the dispersion problem of the graphene in the matrix and the interface control combination problem of the graphene/metal matrix are effectively solved, the process method is strong in controllability, the graphene/aluminum composite material can be popularized and applied to bulk metals such as magnesium alloy, titanium alloy, steel and the like, and the method is simple, efficient, short in production period and low in preparation cost. In addition, in the process of preparing the graphene/aluminum composite, the graphene and aluminum can be uniformly coated with each other by adopting a simple process; the graphene surface coating material and the matrix of the composite are both aluminum, which is beneficial to better fusion between graphene and a metal matrix when the graphene/aluminum composite is applied to a graphene reinforced metal matrix composite.
Drawings
FIG. 1 is a morphology of a graphene oxide/aluminum composite prepared in example 1 of the present invention;
fig. 2 is a cut-off profile view of a graphene oxide/aluminum composite prepared in example 1 of the present invention;
fig. 3 is a gold phase diagram of a graphene oxide/aluminum composite prepared in example 1 of the present invention;
fig. 4 is a gold phase diagram of the graphene oxide reinforced aluminum matrix composite prepared in example 1 of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
Example 1
A preparation method of a graphene oxide/aluminum composite comprises the following steps:
step 1, preparing graphene oxide/aluminum electrostatic self-assembly powder by adopting an electrostatic self-assembly method, which specifically comprises the following steps:
step 1.1, adding 0.8g of graphene oxide into 1600ml of deionized water, and carrying out ultrasonic oscillation for 20min to obtain a graphene oxide turbid liquid; the sheet size of the graphene oxide is 50 nm-2 mu m, the graphene oxide with amphiphilicity is easier to disperse in various solvents, and is easier to perform polar surface modification treatment and strengthen the adsorption effect between the graphene oxide and aluminum powder.
Step 1.2, adding 4g of surfactant cetyl ammonium bromide into the graphene oxide turbid liquid, stirring for 5min-6min until the surfactant is completely dissolved, skimming off white floating foams on the surface, standing for 20min, and modifying the surface of the graphene oxide by utilizing the polarization effect of the surfactant; the mass ratio of the addition amount of the surfactant to the graphene oxide is (2-10): 1;
step 1.3, adding 19.2g of atomized pure aluminum powder with the purity of 99.99% and the average diameter of 40 μm into the turbid liquid obtained in step 1.2, continuously stirring until the aluminum powder and the graphene oxide are uniformly adsorbed to obtain a colloidal suspension, standing until the colloidal suspension is obviously layered, filtering and vacuum drying the precipitate to obtain the flocculent graphene oxide/aluminum electrostatic self-assembly powder with the graphene oxide content of 4.0 wt.%.
Step 2, placing the graphene oxide/aluminum electrostatic self-assembly powder, the grinding balls and 1.6g of ball-milling medium stearic acid in a vacuum ball mill for ball-milling dispersion, firstly carrying out ball-milling for 20min, and then adding 140g of aluminum powder into a ball-milling tank, wherein the total ball-material ratio is 5: 1, and the vacuum degree is 5.0 multiplied by 10-2Pa, the rotating speed of the ball mill is 300r/min, the ball milling time is 3 hours, an intermittent ball milling method is adopted, the ball milling is carried out for 20 minutes, the ball milling is stopped for 30 minutes, the temperature of a ball milling tank is ensured to be less than or equal to 40 ℃, so that the aluminum powder is fully wrapped with the graphene oxide in the repeated cold welding and cracking processes, and the graphene oxide/aluminum ball milling mixed powder with the graphene oxide content of 0.5 wt.% is prepared;
step 3, carrying out cold press molding on the graphene oxide/aluminum ball mill mixed powder to obtain a cylindrical green compact with the diameter of 40mm and the thickness of about 20mm, wherein the pressure intensity is 30MPa in the cold press molding process;
and 4, placing the pressed compact in a vacuum hot-pressing sintering furnace for step hot sintering, wherein the specific operation steps are as follows:
step 4.1, placing the pressed compact in a vacuum hot-pressing sintering furnace, then raising the temperature of the furnace to 40 ℃, and carrying out vacuum pumping treatment in the temperature raising process to ensure that the vacuum degree in the furnace is 2.0 multiplied by 10-3Pa；
Step 4.2, raising the furnace temperature of the vacuum hot-pressing sintering furnace to 450 ℃ to perform hot sintering on the pressed compact, wherein the hot sintering time is 1h, and the temperature rise speed of the furnace temperature is 10 ℃/min;
and 4.3, raising the furnace temperature of the vacuum hot-pressing sintering furnace to 580 ℃ to perform hot-pressing sintering on the pressed compact, wherein the sintering time is 3 hours, the pressure applied to the pressed compact during sintering is 50MPa, and the graphene oxide/aluminum composite is obtained after sintering.
Observing the tissue morphology of the prepared graphene oxide/aluminum composite body, wherein fig. 1 is a morphology chart of the graphene oxide/aluminum composite body prepared in example 1, fig. 2 is a cut-off morphology chart of the graphene oxide/aluminum composite body prepared in example 1, and fig. 3 is a gold phase chart of the graphene oxide/aluminum composite body prepared in example 1, and as can be seen from fig. 1-3, the graphene oxide/aluminum composite body prepared by the method disclosed by the invention has a good bonding interface between graphene oxide and aluminum, and does not contain Al in the graphene oxide/aluminum composite body through XRD detection4C3And (4) phase(s).
After the graphene oxide/aluminum composite prepared in example 1 is crushed, the graphene oxide/aluminum composite is added to a pure aluminum melt according to a mass ratio of 2 wt.% to form a graphene oxide reinforced aluminum-based composite, so that the mass ratio of graphene oxide in the graphene oxide reinforced aluminum-based composite is about 0.01 wt.%, and fig. 4 is a gold phase diagram of the graphene oxide reinforced aluminum-based composite.
Example 2
A preparation method of a graphene/aluminum composite comprises the following steps:
step 1, preparing graphene/aluminum electrostatic self-assembly powder by adopting an electrostatic self-assembly method, which specifically comprises the following steps:
step 1.1, adding single-layer graphene into deionized water, and carrying out ultrasonic oscillation for 22min to obtain a graphene turbid liquid;
step 1.2, adding a surfactant sodium dodecyl benzene sulfonate into the graphene turbid liquid, and then stirring until the surfactant is completely dissolved to complete surface polarization modification treatment on the graphene; the mass ratio of the addition amount of the surfactant to the graphene is 4: 1.
step 1.3, adding aluminum powder into the turbid liquid obtained in the step 1.2, continuously stirring until the aluminum powder and graphene are uniformly adsorbed to obtain a colloidal suspension, standing until the colloidal suspension is obviously layered, filtering and vacuum drying the precipitate to obtain flocculent graphene/aluminum electrostatic self-assembly powder, wherein the mass percent of the graphene is 5 wt.%;
step 2, firstly placing the graphene/aluminum electrostatic self-assembly powder, the grinding balls and a ball-milling medium stearic acid in a vacuum ball mill for ball-milling and dispersing for 30min, then adding aluminum powder into a ball-milling tank for ball-milling, wherein the ball-material ratio is 7: 1, the rotating speed of the ball mill is 150r/min, the ball-milling time is 2.5h, and controlling the temperature of the ball-milling tank to be less than or equal to 40 ℃ by adopting an intermittent ball-milling method, so that the aluminum powder is fully wrapped with graphene in the repeated cold welding and cracking processes, and then the graphene/aluminum mixed powder is prepared, wherein the mass percent of the graphene is 0.8 wt.%;
step 3, carrying out cold press molding on the graphene/aluminum mixed powder to obtain a pressed compact, wherein the pressure born by the pressed compact in the cold press molding process is 30 MPa;
and 4, placing the pressed compact in a vacuum hot-pressing sintering furnace for step hot sintering, wherein the specific operation steps are as follows:
step 4.1, placing the pressed compact in a vacuum hot-pressing sintering furnace, then raising the temperature of the furnace to 100 ℃, and carrying out vacuum pumping treatment in the temperature raising process to ensure that the vacuum degree in the furnace is 3.0 multiplied by 10-3Pa；
Step 4.2, raising the furnace temperature of the vacuum hot-pressing sintering furnace to 400 ℃ to perform hot sintering on the pressed blank, wherein the hot sintering time is 1.5h, and the temperature rise speed of the furnace temperature is 5 ℃/min;
and 4.3, raising the furnace temperature of the vacuum hot-pressing sintering furnace to 600 ℃ to perform hot-pressing sintering on the pressed compact, wherein the sintering time is 2.5h, the pressure applied to the pressed compact during sintering is 10MPa, and the graphene/aluminum composite is obtained after sintering.
Example 3
A preparation method of a graphene/aluminum composite comprises the following steps:
step 1, preparing graphene/aluminum electrostatic self-assembly powder by adopting an electrostatic self-assembly method, which specifically comprises the following steps:
step 1.1, adding double-layer graphene into deionized water, and carrying out ultrasonic oscillation for 25min to obtain a graphene turbid liquid;
step 1.2, adding a surfactant sodium dodecyl benzene sulfonate into the graphene turbid liquid, and then stirring until the surfactant is completely dissolved to complete surface polarization modification treatment on the graphene; the mass ratio of the addition amount of the surfactant to the graphene is 5: 1.
step 1.3, adding aluminum powder into the turbid liquid obtained in the step 1.2, continuously stirring until the aluminum powder and graphene are uniformly adsorbed to obtain a colloidal suspension, standing until the colloidal suspension is obviously layered, filtering and vacuum drying the precipitate to obtain flocculent graphene/aluminum electrostatic self-assembly powder, wherein the mass percent of the graphene is 7 wt.%;
step 2, firstly placing the graphene/aluminum electrostatic self-assembly powder, the grinding balls and a ball-milling medium stearic acid in a vacuum ball mill for ball-milling and dispersing for 25min, then adding aluminum powder into a ball-milling tank for ball-milling, wherein the ball-material ratio is 8: 1, the rotating speed of the ball mill is 200r/min, the ball-milling time is 3h, and controlling the temperature of the ball-milling tank to be less than or equal to 40 ℃ by adopting an intermittent ball-milling method, so that the aluminum powder is fully wrapped with graphene in the repeated cold welding and cracking processes, and then the graphene/aluminum mixed powder is prepared, wherein the mass percentage of the graphene is 0.6 wt%;
step 3, carrying out cold press molding on the graphene/aluminum mixed powder to obtain a pressed compact, wherein the pressure born by the pressed compact in the cold press molding process is 50 MPa;
and 4, placing the pressed compact in a vacuum hot-pressing sintering furnace for step hot sintering, wherein the specific operation steps are as follows:
step 4.1, pressing the green compactPlacing in a vacuum hot-pressing sintering furnace, heating to 150 deg.C, and vacuumizing to make the vacuum degree in the furnace 2.0 × 10-3Pa；
Step 4.2, raising the furnace temperature of the vacuum hot-pressing sintering furnace to 420 ℃ to perform hot sintering on the pressed blank, wherein the hot sintering time is 2.5h, and the temperature rise speed of the furnace temperature is 12 ℃/min;
and 4.3, raising the furnace temperature of the vacuum hot-pressing sintering furnace to 590 ℃, carrying out hot-pressing sintering on the pressed compact for 2h, applying pressure on the pressed compact during sintering to 60MPa, and obtaining the graphene/aluminum composite body after sintering.
Example 4
A preparation method of a hydrogenated graphene/aluminum composite comprises the following steps:
step 1, preparing hydrogenated graphene/aluminum electrostatic self-assembly powder by adopting an electrostatic self-assembly method, which specifically comprises the following steps:
step 1.1, adding hydrogenated graphene into deionized water, and performing ultrasonic oscillation for 30min to obtain a hydrogenated graphene turbid liquid;
step 1.2, adding a surfactant sodium dodecyl benzene sulfonate into the hydrogenated graphene turbid liquid, and then stirring until the surfactant is completely dissolved, thereby completing surface polarization modification treatment on the hydrogenated graphene; the mass ratio of the addition amount of the surfactant to the hydrogenated graphene is 7: 1.
step 1.3, adding aluminum powder into the turbid liquid obtained in the step 1.2, continuously stirring until the aluminum powder and the hydrogenated graphene are uniformly adsorbed to obtain a colloidal suspension, standing until the colloidal suspension is obviously layered, filtering and vacuum drying the precipitate to obtain flocculent hydrogenated graphene/aluminum electrostatic self-assembly powder, wherein the mass percent of the hydrogenated graphene is 8 wt.%;
step 2, firstly placing the hydrogenated graphene/aluminum electrostatic self-assembly powder, grinding balls and a ball-milling medium stearic acid in a vacuum ball mill for ball-milling and dispersing for 35min, then adding aluminum powder into a ball-milling tank for ball-milling, wherein the ball-material ratio is 10: 1, the rotating speed of the ball mill is 250r/min, the ball-milling time is 3.5h, and adopting an intermittent ball-milling method to control the temperature of the ball-milling tank to be less than or equal to 40 ℃ so that the aluminum powder is fully wrapped with the hydrogenated graphene in the repeated cold welding and cracking processes to obtain hydrogenated graphene/aluminum mixed powder, wherein the mass percentage of the hydrogenated graphene is 0.8 wt%;
step 3, carrying out cold press molding on the hydrogenated graphene/aluminum mixed powder to obtain a pressed compact, wherein the pressure born by the pressed compact in the cold press molding process is 60 MPa;
and 4, placing the pressed compact in a vacuum hot-pressing sintering furnace for step hot sintering, wherein the specific operation steps are as follows:
step 4.1, placing the pressed compact in a vacuum hot-pressing sintering furnace, then raising the temperature of the furnace to 180 ℃, and carrying out vacuum pumping treatment in the temperature raising process to ensure that the vacuum degree in the furnace is 1.0 multiplied by 10-3Pa；
Step 4.2, raising the furnace temperature of the vacuum hot-pressing sintering furnace to 440 ℃ to perform hot sintering on the pressed blank, wherein the hot sintering time is 1.5h, and the temperature rise speed of the furnace temperature is 15 ℃/min;
and 4.3, raising the furnace temperature of the vacuum hot-pressing sintering furnace to 600 ℃ to perform hot-pressing sintering on the pressed compact, wherein the sintering time is 3h, the pressure applied to the pressed compact during sintering is 80MPa, and the hydrogenated graphene/aluminum composite is obtained after sintering.
Example 5
A preparation method of a fluorinated graphene/aluminum composite comprises the following steps:
step 1, preparing fluorinated graphene/aluminum electrostatic self-assembly powder by adopting an electrostatic self-assembly method, which specifically comprises the following steps:
step 1.1, adding fluorinated graphene into deionized water, and carrying out ultrasonic oscillation for 22min to obtain a fluorinated graphene turbid liquid;
step 1.2, adding a surfactant sodium dodecyl benzene sulfonate into the fluorinated graphene turbid liquid, and then stirring until the surfactant is completely dissolved, thereby completing surface polarization modification treatment on the fluorinated graphene; the mass ratio of the addition amount of the surfactant to the fluorinated graphene is 10: 1.
step 1.3, adding aluminum powder into the turbid liquid obtained in the step 1.2, continuously stirring until the aluminum powder and the fluorinated graphene are uniformly adsorbed to obtain a colloidal suspension, standing until the colloidal suspension is obviously layered, filtering and vacuum drying the precipitate to obtain flocculent fluorinated graphene/aluminum electrostatic self-assembly powder, wherein the mass percent of the fluorinated graphene is 10 wt.%;
step 2, firstly placing the fluorinated graphene/aluminum electrostatic self-assembly powder, grinding balls and a ball-milling medium stearic acid in a vacuum ball mill for ball milling and dispersion for 50min, then adding aluminum powder into a ball-milling tank for ball milling, wherein the ball-material ratio is 10: 1, the rotating speed of the ball mill is 300r/min, the ball-milling time is 4h, and adopting an intermittent ball-milling method to control the temperature of the ball-milling tank to be less than or equal to 40 ℃ so that the aluminum powder is fully wrapped with the fluorinated graphene in the repeated cold welding and cracking processes, thus obtaining the fluorinated graphene/aluminum mixed powder, wherein the mass percentage of the fluorinated graphene is 1.0 wt.%;
step 3, carrying out cold press molding on the fluorinated graphene/aluminum mixed powder to obtain a pressed compact, wherein the pressure born by the pressed compact in the cold press molding process is 45 MPa;
and 4, placing the pressed compact in a vacuum hot-pressing sintering furnace for step hot sintering, wherein the specific operation steps are as follows:
step 4.1, placing the pressed compact in a vacuum hot-pressing sintering furnace, then raising the temperature of the furnace to 200 ℃, and carrying out vacuum pumping treatment in the temperature raising process to ensure that the vacuum degree in the furnace is 1.0 multiplied by 10-3Pa；
Step 4.2, raising the furnace temperature of the vacuum hot-pressing sintering furnace to 450 ℃ to perform hot sintering on the pressed compact, wherein the hot sintering time is 1.2h, and the temperature rise speed of the furnace temperature is 10 ℃/min;
and 4.3, raising the furnace temperature of the vacuum hot-pressing sintering furnace to 620 ℃ to perform hot-pressing sintering on the pressed compact, wherein the sintering time is 2 hours, the pressure applied to the pressed compact during sintering is 50MPa, and the fluorinated graphene/aluminum composite is obtained after sintering.
Claims (8)
1. The preparation method of the graphene/aluminum composite is characterized by comprising the following steps:
step 1, preparing graphene/aluminum electrostatic self-assembly powder by adopting an electrostatic self-assembly method, wherein the mass percent of graphene is 4.0-10.0 wt.%, and the graphene is single-layer, double-layer or multi-layer graphene, or graphene oxide, hydrogenated graphene and fluorinated graphene;
step 2, taking a proper amount of aluminum powder and the graphene/aluminum electrostatic self-assembly powder prepared in the step 1 to perform vacuum ball milling, and preparing graphene/aluminum mixed powder, wherein the mass percent of graphene is less than or equal to 1.0 wt.%;
step 3, carrying out cold press molding on the graphene/aluminum mixed powder to obtain a pressed blank;
and 4, placing the pressed compact in a vacuum hot-pressing sintering furnace for sintering at 400-450 ℃, and raising the furnace temperature to 580-620 ℃ for secondary sintering to obtain the graphene/aluminum composite.
2. The method for preparing a graphene/aluminum composite according to claim 1, wherein the step 1 specifically comprises the following steps:
step 1.1, adding graphene into deionized water, and carrying out ultrasonic oscillation for 20-30 min to obtain a graphene turbid liquid;
step 1.2, adding one or more of surfactants such as sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, hexadecyl ammonium bromide and polyvinylpyrrolidone into the graphene turbid liquid, and then stirring until the surfactants are completely dissolved to complete surface polarization modification treatment on the graphene;
and step 1.3, adding aluminum powder into the turbid liquid obtained in the step 1.2, continuously stirring until the aluminum powder and the graphene are uniformly adsorbed to obtain a colloidal suspension, standing until the colloidal suspension is obviously layered, and filtering and vacuum drying the precipitate to obtain the flocculent graphene/aluminum electrostatic self-assembly powder.
3. The method for preparing the graphene/aluminum composite body according to claim 2, wherein in the step 1.2, the mass ratio of the addition amount of the surfactant to the graphene is 2-10: 1.
4. the preparation method of the graphene/aluminum complex according to claim 1, wherein in the step 2, the graphene/aluminum electrostatic self-assembly powder, the grinding balls and the stearic acid as the ball-milling medium are placed in a vacuum ball mill for ball-milling and dispersion for 20min to 50min, then the aluminum powder is added into a ball-milling tank for ball-milling, the ball-material ratio is 5-10: 1, the rotation speed of the ball mill is 100-300 r/min, the ball-milling time is 2h to 4h, and the temperature of the ball-milling tank is controlled to be less than or equal to 40 ℃ by adopting an intermittent ball-milling method, so that the aluminum powder and the graphene are fully wrapped in the repeated cold-welding and cracking processes, and the graphene/aluminum mixed powder is prepared.
5. The method for preparing the graphene/aluminum composite body according to claim 1, wherein in the step 3, the pressure for cold press molding the graphene/aluminum mixed powder is 10MPa to 60 MPa.
6. The method for preparing the graphene/aluminum composite body according to claim 1, wherein the specific steps of the step 4 are as follows:
step 4.1, placing the pressed compact in a vacuum hot-pressing sintering furnace, then raising the temperature of the furnace to 25-200 ℃, and carrying out vacuum pumping treatment in the temperature raising process to ensure that the vacuum degree in the furnace is less than or equal to 1.0 multiplied by 10-2Pa；
Step 4.2, raising the furnace temperature of the vacuum hot-pressing sintering furnace to 400-450 ℃ to sinter the pressed blank for 1-3 h;
and 4.3, raising the furnace temperature of the vacuum hot-pressing sintering furnace to 580-620 ℃ to perform secondary sintering on the pressed blank, wherein the sintering time is 2-3 h, and obtaining the graphene/aluminum composite body after sintering.
7. The method of claim 6, wherein in the step 4.2, the temperature of the furnace is increased at a rate of 5-15 ℃/min, the sintering mode is thermal sintering or hot-pressing sintering, and the pressure applied to the green compact during the hot-pressing sintering is 10 MPa-100 MPa.
8. The method of claim 7, wherein in the step 4.3, the secondary sintering is thermal sintering or hot-pressing sintering, and the pressure applied to the green compact during the hot-pressing sintering is 10MPa to 100 MPa.
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