A kind of method that graphene disperses in metal powder
Technical field
The present invention relates to technical field of graphene, more particularly to a kind of method that graphene disperses in metal powder.
Background technology
Graphene is a kind of cellular monoatomic layer two-dimensional film formed with sp2 hydridization by carbon atom, is to build other
The basic structural unit of dimension carbon material (zero dimension fullerene, one-dimensional carbon nanotube, three-dimensional graphite).Graphene has extremely excellent
Electricity, calorifics, mechanics and optical property, in fields such as microelectronic component, battery, sensor, transparent conductive film, composite materials
It has broad application prospects.
Graphene intensity makes it obtain in the composite up to 130GPa, the excellent mechanical performance that Young's modulus is 1100GPa
To being widely applied.The key of graphene application is how to realize graphene in the composite evenly dispersed.Aoxidize stone
Black alkene has preferable dispersibility, can be relatively easy to be dispersed between metal-powder, pass through follow-up hot pressing, hot isostatic pressing etc.
Mode realizes the consolidation of composite granule, to prepare graphene metal-base composites.Relative to graphene oxide, graphene
Have the performances such as better mechanics, electricity, heat conduction, by reasonably disperseing, consolidation method, the graphene of higher performance can be obtained
Metal-base composites.
Since graphene surface is almost without functional group, it is difficult to be scattered in alone in water or organic solvent, emulsification pretreatment is
In the case of being aided with emulsifier under the action of high speed shear, the quick, evenly dispersed of two or more objectionable intermingling phases is realized
Effect.
High-shearing dispersion emulsifying machine is exactly efficiently, rapidly and uniformly by a phase or multiple phases (liquid, solid, gas)
Enter the process of another immiscible continuous phase (liquids in general).And each phase is immiscible in general.
When external energy inputs, two kinds of material recombinations become homogeneous phase.High tangential velocity and high frequency caused by rotor high speed rotation
The powerful kinetic energy that mechanical effect is brought, make material in the narrow gap of stator and rotor by strong machinery and aquashear, from
Heart extruding, hits tearing and the comprehensive functions such as turbulent flow at liquid layer friction, forms suspension (solid-liquid), lotion (liquid/liquid) and
Foam (gas/liquid).To keep immiscible solid phase, liquid phase, gas phase common corresponding maturation process and appropriate additive
Under effect, the dispersion and emulsion of moment uniform, fine finally obtains stable high-quality product by moving in circles for high frequency.
Invention content
The present invention provides a kind of method that graphene disperses in metal powder, this method by high speed shearing emulsification,
Graphene uniform suspension is obtained, the drying and grinding after divided metallic powder is added and obtains the mixed of uniform graphene metal powder
It closes, to obtain the graphene metal-base composites of higher performance
Realize that above-mentioned purpose technical solution of the present invention is as follows:
A kind of method that graphene disperses in metal powder, which is characterized in that described method includes following steps:
(1) suspension of emulsification pretreatment configuration graphene, emulsifier and solvent;
(2) it heats and stirs configuration metal powder and the mixture of the suspension obtains paste mixture;
(3) dry paste mixture, the graphene metal mixed powder for grinding evenly dispersed.
Preferably, 0.2 μm~50 μm of graphene film diameter described in step (1), preparation method include redox, liquid phase stripping
It is removed from ball milling.
Preferably, the high shear homogeneous emulsifying machine of step (1) the high speed emulsification pretreatment include on vertical direction that
This rabbling mechanism, supporting mechanism and rabbling mechanism height adjustment mechanism disposed in parallel;
The rabbling mechanism from top to bottom successively include homogeneous motor (4), transmission shaft (3), several connecting rods (2) and
Homogeneous stirring-head (1);
The homogeneous blender (4) is supported by lifting arm (5);
Described transmission shaft (3) one end exports axis connection with homogeneous motor (4), and the other end is mutually fitted with homogeneous stirring-head (1)
Match;
The homogeneous stirring-head (1) is fixedly connected by three connecting rods (2) with homogeneous motor (4) lower part;
The supporting mechanism includes lifting arm (5), lifting support (6), splash-back (9), pedestal (10) successively from top to bottom
And the support sucker (12) and universal wheel (13) being arranged under pedestal (10);
The height adjustment mechanism includes driving section (11), lead screw (7) and elevating motor (8) successively from top to bottom;
The right end in the lifting arm (5) is arranged in institute driving section (11), and the through-hole of the driving section (11) is equipped with and lead screw
(7) compatible internal thread;
Lead screw (7) both ends are rotatable parallel set on lifting support (6) side wall upper part;Lead screw (7) bottom with
Elevating motor (8) exports axis connection;
The elevating motor (8) is set to lifting support (6) lower sidewall.
Preferably, emulsifier described in step (1) include from ethyl cellulose, lauryl sodium sulfate, Qula it is logical, poly- third
The one or more of emulsifiers selected in olefin(e) acid sodium, polyethylene glycol, polyvinyl alcohol and polyvinylpyrrolidone.
Preferably, solvent described in step (1) includes from deionized water, methanol, ethyl alcohol, isopropanol, acetone, NMP, trichlorine
The one or more selected in methane, toluene and carbon tetrachloride.
Preferably, graphene, emulsifier and solvent ratios described in step (1) are 10g:(2~20) g:(500~1000)
ml。
Preferably, step (1) the shearing step is 5~60min of speed down cut in 5000~12000r/min.
Preferably, it is carried out in beaker in step (2);The metal powder includes from aluminium powder, magnesium powder, titanium valve, nickel powder, zirconium
A kind of metal powder selected in powder, iron powder, copper powder and high temperature alloy powder.
Preferably, metal powder described in step (2) and suspension liquid proportional are (500~1500) g:(300~1000) ml.
Preferably, 30~90 DEG C of heating water bath is heated to be described in step (2);The stirring is 50~1000r/ of rate
The mechanical agitation of min.
Preferably, described in step (3) it is dry for dry 8 in 30~90 DEG C of baking oven~for 24 hours.
Preferably, grinding described in step (3) includes hand-ground and mechanical lapping;Process of lapping can in air or protect
It protects in atmosphere.
Compared with the immediate prior art, technical solution provided by the invention has following excellent effect:
(1) dispersion effect of the graphene in metal powder is good;
(2) graphene non-recurring structure in dispersion process destroys, and maintains the good characteristic of graphene;
(3) environmental-friendly, dispersion process is without using soda acid;
(4) dispersion of the invention is carried out by high shear homogeneous emulsifying machine, and dispersion effect is good, and equipment has sucker suction solid
It is fixed, it is therefore prevented that displacement is dangerous.
Description of the drawings
Fig. 1 is the structural schematic diagram of high shear homogeneous emulsifying machine of the present invention;
Fig. 2 is that 2 liquid phase of embodiment removes graphene dispersion in Al alloy powder surface electron-microscope scanning figure
Wherein:1:Homogeneous stirring-head;2:Connecting rod;3:Transmission shaft;4:Homogeneous motor;5:Lifting arm;6:Lifting support;
7:Lead screw;8:Elevating motor;9:Splash-back;10:Pedestal;11:Driving section;12:Support sucker;13:Universal wheel.
Specific implementation mode
The present invention provides a kind of dispersing method of graphene in metal powder, this method by high speed shearing emulsification,
Graphene uniform suspension is obtained, the drying and grinding after divided metallic powder is added and obtains the mixed of uniform graphene metal powder
It closes, to obtain the graphene metal-base composites of higher performance.
The high shear homogeneous emulsifying machine that 1 present invention of embodiment uses
Including 1, three connecting rod 2 of homogeneous stirring-head, transmission shaft 3, homogeneous motor 4, it is used to support homogeneous motor 4
Lifting arm 5, the lifting support 6 being slidably connected with lifting arm, lead screw 7, elevating motor 8, splash-back 9 and pedestal 10, homogeneous stirs
It mixes first 1 to be fixedly connected with 4 lower part of homogeneous motor by several connecting rods 2, particularly, connecting rod 2 is evenly distributed on transmission shaft 3
Periphery, while meeting homogenizer rigidity, additionally it is possible to reduce cost, connecting rod 2 is no more than 8,3 one end of transmission shaft with
Homogeneous motor 4 exports axis connection, and the other end is adapted with homogeneous stirring-head 1, and rotatable parallel be set in 7 both ends of lead screw lifts
6 side wall upper part of holder, elevating motor 8 are set to 6 lower sidewall of lifting support, and 7 bottom of lead screw connects with 8 output shaft of elevating motor
It connects, lifting support 6 and splash-back 9 are set to 10 upper surface of pedestal, and 9 height of splash-back is higher than 7 bottom of lead screw, prevents material splash
It influences electric part to stablize, lifting arm 5 is additionally provided with the driving section 11 coordinated with lead screw 7, and the through-hole of driving section 11 is equipped with and lead screw 7
Compatible internal thread, lifting support 6 are equipped with limiting device, enhance fixed effect, mitigate the pressure that lead screw 7 is subject to driving section 11
Power improves service life, and 10 lower surface of pedestal is equipped with support sucker 12, by supporting the absorption principle of sucker 12 to play fixed work
With 10 lower surface of pedestal is equipped with universal wheel 13, is moved easily equipment, in use, elevating motor 8 drives lead screw 7 to rotate, with silk
The driving section 11 that bar 7 coordinates is moved up and down along 7 axial direction of lead screw, and homogeneous motor 4 and lifting arm 5 are just with about 11 driving section
Movement realizes homogeneous stirring-head 1 and is adapted to different vessels size and makes raise and reduce action.
Dispersion steps of 2 graphene of the present invention of embodiment in metal powder:
(1) by the 10g graphenes of 20 μm of piece diameter made from oxidation-reduction method and 5g ethyl celluloses be added to 500ml go from
In sub- water, using the high shear homogeneous emulsifying machine of embodiment 1 in the speed down cut 30min of 5000r/min, even suspension is obtained
Liquid;
(2) the 500ml suspension after disperseing emulsification pretreatment is placed in beaker, and 1000g aluminium powders to be disperseed are added and start to use
The speed of 500r/min carries out mechanical agitation, and 60 DEG C of heating of circulator bath while stirring obtain half-dried muddy mixture;
(3) by half-dried muddy mixture, dry 16h, drying temperature are 60 DEG C in vacuum drying oven, make graphene metal
Mixture of powders is completely dried;
(4) graphene metal powder mixture after hand-ground is dried in air obtains evenly dispersed graphene gold
Belong to mixed-powder.
Dispersion steps of 3 graphene of the present invention of embodiment in metal powder:
(1) the 10g graphenes of 10 μm of piece diameter made from liquid phase stripping method and 10g lauryl sodium sulfate are added to
In 500ml methanol, using the high shear homogeneous emulsifying machine of embodiment 1 in the speed down cut 40min of 6000r/min, obtain equal
Even suspension;
(2) the 500ml suspension after disperseing emulsification pretreatment is placed in beaker, and 800g aluminium powders to be disperseed are added and start to use
The speed of 700r/min carries out mechanical agitation, and 45 DEG C of heating of circulator bath while stirring obtain half-dried muddy mixture;
(3) by half-dried muddy mixture, dry 20h, drying temperature are 45 DEG C in vacuum drying oven, make graphene metal
Mixture of powders is completely dried;
(4) graphene metal powder mixture after mechanical lapping is dried in air obtains evenly dispersed graphene gold
Belong to mixed-powder.
Dispersion steps of 4 graphene of the present invention of embodiment in metal powder:
(1) by the 10g graphenes of 30 μm of piece diameter made from ball milling stripping method and 10g Sodium Polyacrylates and 5g polyethylene glycol
It is added in the mixed solution of 500ml methanol and 200ml acetone, using the high shear homogeneous emulsifying machine of embodiment 1 in 10000r/
The speed down cut 50min of min obtains unit for uniform suspension;
(2) the 600ml suspension after disperseing emulsification pretreatment is placed in beaker, and 1200g aluminium powders to be disperseed are added and start to use
The speed of 850r/min carries out mechanical agitation, and 80 DEG C of heating of circulator bath while stirring obtain half-dried muddy mixture;
(3) by half-dried muddy mixture, for 24 hours, drying temperature is 80 DEG C, makes graphene metal for drying in vacuum drying oven
Mixture of powders is completely dried;
(4) graphene metal powder mixture after mechanical lapping is dried in Ar, obtains evenly dispersed graphene metal
Mixed-powder.
2~embodiment of embodiment, 4 obtained graphene metal mixed powder is handled as follows respectively:It is cold-pressed into
Then base carries out hot extrusion, extrusion ratio 20 at 440 DEG C after vacuum degassing 2h:1, obtain closely knit graphene/aluminum composite wood
Obtained material, is carried out the performance test of mechanical property, heat conductivility and damping capacity by material, and test result is shown in Table 1.
The performance of composite material obtained by the powder of 1 2~embodiment of embodiment 4 of table
The above embodiments are merely illustrative of the technical solutions of the present invention rather than is limited, the common skill of fields
Art personnel, which should be appreciated that, can be modified or replaced equivalently the specific implementation mode of the present invention with reference to above-described embodiment,
These are applying for pending claim protection model without departing from any modification of spirit and scope of the invention or equivalent replacement
Within enclosing.