CN105132742B - A kind of Graphene enhancing titanium matrix composite and preparation method thereof - Google Patents
A kind of Graphene enhancing titanium matrix composite and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of Graphene enhancing titanium matrix composite and preparation method thereof, belong to field of compound material.Methods described step is as follows：Graphene powder mix with absolute ethyl alcohol after ultrasonic disperse, and add titanium valve under agitation, obtain mixed slurry；The mixed slurry that will be obtained is transferred in ball grinder, carries out ball milling；The absolute ethyl alcohol in ball milling disposed slurry is removed, powder is obtained；The powder that will be obtained is dried in vacuum drying chamber, obtains dried powder；Dried powder is loaded in graphite jig, lead to argon gas in hot pressing furnace, and apply the pressure of 2~2.12t to graphite jig, 900~1300 DEG C are heated to the heating rate of 10~12 DEG C/min, room temperature is naturally cooled to after 1~1.5h of insulation, the product in graphite jig is that the Graphene strengthens titanium matrix composite.Graphene is evenly distributed in methods described process is simple, and the composite for preparing, and impurity content is few.
Description
Technical field
The present invention relates to a kind of Graphene enhancing titanium matrix composite and preparation method thereof, belong to field of compound material.
Background technology
Titanium or titanium alloy has density low, intensity is high, high-low temperature resistant, it is corrosion-resistant the features such as；Its performance for protruding promotes titanium
And titanium alloy turns into the ideal material of the industries such as war industry, Aero-Space, navigation, automobile, petrochemical industry, biological medicine, from
And turn into the preferable matrix of composite.
Graphene is a kind of carbon atom with sp2The two-dimentional carbon material that the form of hydridization is present, with very excellent conduction
Property, thermal conductivity, and mechanical property.Its elastic modelling quantity and tensile strength can reach 1.05Tpa and 130Gpa respectively.People are
Through to graphene reinforced metal-matrix composite (Gr-MMCs), such as aluminium base, Ni-based, magnesium-based, copper-based has carried out preliminary exploration.
Research finds the enhanced metal-base composites of Graphene with specific strength higher, than elastic modelling quantity and good wearability
Deng.
But graphene reinforced metal-matrix composite can run into a series of problem in sintering, and such as graphene powder is non-
Chang Rongyi reunites, if adding amphoteric surfactant, can cause the introducing of impurity, again easy in the ball milling stage of powder metallurgy
Suffer structural damage.In addition, the research of relevant Graphene enhancing titanium matrix composite has not been reported.
The content of the invention
For defect present in prior art, it is an object of the invention to provide a kind of Graphene enhancing titanium-based composite wood
Material and preparation method thereof, is evenly distributed using Graphene in composite prepared by methods described, and impurity content is few, with higher
Specific strength and compare elastic modelling quantity；The method process is simple.
The purpose of the present invention is achieved through the following technical solutions.
A kind of Graphene strengthens titanium matrix composite, and the volume with Graphene enhancing titanium matrix composite is 100%
Meter, the composition and volume fraction of its each composition：Graphene powder 1.80~1.90%, titanium valve 98.10~98.20%.
A kind of Graphene of the present invention strengthens the preparation method of titanium matrix composite, and methods described step is as follows：
(1) weighing of raw material：First, the number of plies of Graphene is gone out using transmission electron microscope or atomic force microscope observation
L, then the thickness T of L layer graphenes is measured, so that graphene film interlamellar spacing d=T/ (L-1) can be obtained, due to each piece of Graphene
The thickness of layer is an atomic scale, negligible, and the density of Graphene can be calculated according to following formula：
Wherein, PGNPsIt is the density of Graphene, unit is g/cm3；D is graphene film interlamellar spacing, and unit is nm；ρgraphite
It is the density of graphite, is 2.25g/cm3；0.34nm is the piece interlamellar spacing of graphite；
Then, the quality of Graphene is weighed, and calculates its corresponding volume；Further according to the volume of Graphene, phase is weighed
The titanium valve answered；
(2) mixing of powder：Graphene powder mix with absolute ethyl alcohol after 20~30min of ultrasonic disperse, then stirring
Lower addition titanium valve, obtains mixed slurry；The mixed slurry that will be obtained is transferred in ball grinder, adds ball milling pearl, 300~
0.4~2.5h of ball milling under 350r/min；Then, the absolute ethyl alcohol in ball milling disposed slurry is removed, powder is obtained；The powder that will be obtained
10~12h is dried in 90~120 DEG C of vacuum drying chamber, dried powder is obtained；
Wherein, ball milling pearl and the mass ratio of graphene powder and titanium valve are 5~6:1；
(3) hot pressed sintering：Powder dried in step (2) is loaded in graphite jig, mould inside pad graphite paper, with
Anti- titanium valve reacts with mould；Lead to argon gas protection in hot pressing furnace, and apply the pressure of 2~2.12t to graphite jig, with 10~
The heating rate of 12 DEG C/min is heated to 900~1300 DEG C, room temperature is naturally cooled to after 1~1.5h of insulation, in graphite jig
Product is that the Graphene strengthens titanium matrix composite.
Preferably, the inner mast of the graphite jig coats the graphite paper of boron nitride (BN).
Beneficial effect：
Graphene is evenly distributed in Graphene enhancing titanium matrix composite prepared by the present invention, and impurity content is few, has
Specific strength higher and than elastic modelling quantity, 21.3~51.5%, and extension of having no progeny are improve relative to the tensile strength of pure titanium
Rate is higher relative to conventional particles enhancing titanium matrix composite, is a kind of lower cost and mechanical property is excellent up to 14~22%
Different discontinuous reinforcement titanium matrix composite.
In the method for the invention, Ball-milling Time and rotational speed of ball-mill during the strict mixed powder of control ball milling, overlong time,
Rotating speed is too high, easily causes the destruction of material structure；Time is too short, and rotating speed is too low, does not reach well mixed purpose.In ball milling mistake
Cheng Zhong, by the time and the rotating speed that regulate and control ball milling so that Graphene can be uniformly distributed on matrix, and mixed material knot
Structure is complete.Hot pressing and sintering technique under being protected using argon gas, makes the consistency of composite higher, and titanium valve particle is combined preferably,
Enhancing effect is obvious.
Brief description of the drawings
Fig. 1 strengthens the high resolution transmission electron microscopy of titanium matrix composite for Graphene obtained in embodiment 1.
Fig. 2 is the SEM of the stretching fracture of Graphene enhancing titanium matrix composite obtained in embodiment 1
(SEM) figure.
Fig. 3 strengthens SEM (SEM) figure of titanium matrix composite for Graphene obtained in embodiment 2.
Fig. 4 strengthens X-ray diffraction (XRD) spectrogram of titanium matrix composite for Graphene obtained in embodiment 3.
Fig. 5 strengthens the EDS energy spectrum diagrams of titanium matrix composite for Graphene obtained in embodiment 3.
Fig. 6 under Graphene enhancing titanium matrix composite and same process obtained in embodiment 4 the pure titanium of preparation it is accurate quiet
State stress strain curve comparison diagram.
Specific embodiment
With reference to specific embodiment, the present invention is further elaborated.
In following examples：
Graphene powder is made up of few layer graphene piece of purity ＞ 90%, and thickness is 1~1.7nm, and diameter is about 50 μ
M, is 1.06g/cm by the density for being calculated the Graphene3, the manufacturer of the graphene powder is Suzhou perseverance ballstone ink
Alkene Science and Technology Ltd..
Titanium valve：Density 4.51g/cm3, sale producer is that neat mechanical five ore deposit in Chengdu day imports and exports limited company.
The preparation of pure titanium：Titanium valve mix with absolute ethyl alcohol after 20~30min of ultrasonic disperse；Then, it is transferred in ball grinder,
Ball milling pearl is added, wherein, ball milling pearl is 5~6 with the mass ratio of titanium valve:1,0.4~2.5h of ball milling under 300~350r/min；
The absolute ethyl alcohol in ball milling disposed slurry is removed again, obtains powder；The powder that will be obtained is done in 90~120 DEG C of vacuum drying chamber
Dry 10~12h, obtains dried powder；Dried powder is loaded in graphite jig, mould inside pad graphite paper；Hot pressing
Lead to argon gas in stove, and apply the pressure of 2~2.12t to graphite jig, 900 are heated to the heating rate of 10~12 DEG C/min~
1300 DEG C, room temperature is naturally cooled to after 1~1.5h of insulation, the product in graphite jig is the pure titanium.Except without graphite
Outside alkene powder, the preparation of pure titanium strengthens other process conditions phases of titanium matrix composite with Graphene is prepared in corresponding embodiment
Together.
Graphite jig：The internal diameter of mould is 30mm, and pressure head diameter is 24.6mm, one layer of 0.2mm thickness of inner mast of mould
Coat the graphite paper of BN；
Hot pressing furnace：R-C-ZKQY-07, Shanghai Chen Rong electric furnaces Co., Ltd；
SEM：The HITACHI S-4800N Flied emission scanning electron microscopies of Japanese HITACHI companies production
Mirror；
Transmission electron microscope：The Tecnai G2F20 type transmission electron microscopes of FEI Co. of U.S. production.
Embodiment 1
Ultrasonic disperse after graphene powder that 0.11437g volume fractions are 1.80% and 200mL absolute ethyl alcohols are mixed
30min, then adds the titanium valve that 25.0376g volume fractions are 98.20% under agitation, obtains mixed slurry；It is mixed by what is obtained
Close slurry to be transferred in ball grinder, add 125.76g zirconia ceramics ball milling pearls, ball milling 0.4h under 300r/min, using rotation
Absolute ethyl alcohol of the evaporimeter in ball milling disposed slurry is removed at 75 DEG C of 65r/min, obtains powder；The powder that will be obtained is at 90 DEG C
Vacuum drying chamber in dry 12h, obtain dried powder；The dried powder that will be obtained loads in graphite jig, heat
Lead to argon gas in pressure stove, and apply the pressure of 2.12t to graphite jig, 900 DEG C, insulation are heated to the heating rate of 12 DEG C/min
Room temperature is naturally cooled to after 1h, the product in graphite jig is for volumeGraphene enhancing titanium-based composite wood
Material.
The sign and result carried out to the Graphene enhancing titanium matrix composite obtained by this implementation are as follows：
Fig. 1 is the high resolution transmission electron microscopy of the composite, from figure knowable to lattice distribution, the composite
In be clearly present two-phase, i.e., pure titanium phase and Graphene and pure titanium the spontaneous formation of high-temperature sintering process situ TiC phases, and
Two alternate interface cohesions are good.Knowable to from the SEM figures of the composite, the TiC particles that Graphene in-situ authigenic is formed are equal
It is even to be distributed in pure Titanium base.Fig. 2 is the SEM figures of the composite stretching fracture, and Graphene prepared as we know from the figure increases
There is a small amount of Graphene not reacted with pure titanium in strong titanium matrix composite inside, be TiC ceramic phases around it.The composite
There is the diffraction maximum of pure titanium and TiC in XRD diffraction patterns, can't see the diffraction maximum of Graphene.Can be with using universal testing machine
It is 21% to measure the elongation after fracture of the composite, and tensile strength is 630Mpa, than the tensile strength of pure titanium under same process
Improve 21.3%.
Embodiment 2
Ultrasonic disperse after graphene powder that 0.11387g volume fractions are 1.90% and 200mL absolute ethyl alcohols are mixed
20min, then adds the titanium valve that 25.0186g volume fractions are 98.10% under agitation, obtains mixed slurry；It is mixed by what is obtained
Close slurry to be transferred in ball grinder, add 125.09g zirconia ceramics ball milling pearls, ball milling 2.5h under 350r/min, using rotation
Absolute ethyl alcohol of the evaporimeter in ball milling disposed slurry is removed at 75 DEG C of 65r/min, obtains powder；The powder that will be obtained is at 90 DEG C
Vacuum drying chamber in dry 12h, obtain dried powder；The dried powder that will be obtained loads in graphite jig, heat
Lead to argon gas in pressure stove, and apply the pressure of 2t to graphite jig, 1150 DEG C, insulation are heated to the heating rate of 10 DEG C/min
Room temperature is naturally cooled to after 1.5h, the product in graphite jig is for volumeGraphene enhancing titanium-based answer
Condensation material.
The sign and result carried out to the Graphene enhancing titanium matrix composite obtained by this implementation are as follows：
Fig. 3 is the SEM figures of the composite, from the figure, it can be seen that the TiC particles that Graphene in-situ authigenic is formed are uniform
It is distributed in pure Titanium base, strengthen particle is uniformly distributed the lifting for being conducive to composite overall mechanical properties.The composite wood
There is the diffraction maximum of pure titanium and TiC in the XRD diffraction patterns of material, can't see the diffraction maximum of Graphene.It is disconnected by composite stretching
The SEM figures of mouth understand, in the presence of a small amount of Graphene not reacted with pure titanium inside prepared Graphene enhancing titanium matrix composite,
It is TiC ceramic phases around it.The elongation percentage that can measure the composite using universal testing machine reaches 14%, and tension is strong
Degree reaches 750Mpa, and the tensile strength than pure titanium under same process improves 51.5%.
Embodiment 3
Ultrasonic disperse after graphene powder that 0.11437g volume fractions are 1.80% and 200mL absolute ethyl alcohols are mixed
30min, then adds the titanium valve that 25.0376g volume fractions are 98.20% under agitation, obtains mixed slurry；It is mixed by what is obtained
Close slurry to be transferred in ball grinder, add 150.912g zirconia ceramics ball milling pearls, ball milling 0.4h under 350r/min, using rotation
Absolute ethyl alcohol of the evaporimeter in ball milling disposed slurry is removed at 75 DEG C of 65r/min, obtains powder；The powder that will be obtained is at 120 DEG C
Vacuum drying chamber in dry 12h, obtain dried powder；The dried powder that will be obtained loads in graphite jig, heat
Lead to argon gas in pressure stove, and apply the pressure of 2.12t to graphite jig, 900 DEG C, insulation are heated to the heating rate of 10 DEG C/min
Room temperature is naturally cooled to after 1h, the product in graphite jig is for volumeGraphene enhancing titanium-based composite wood
Material.
The sign and result carried out to the Graphene enhancing titanium matrix composite obtained by this implementation are as follows：
Fig. 4 is the XRD spectra of the composite, the diffraction maximum of pure titanium and TiC is clear that from figure, due to graphite
The alkene number of plies is few, and content is low, so can't see the peak of Graphene.Knowable to from the SEM figures of the composite, Graphene is in situ certainly
The raw TiC particles for being formed are evenly distributed in pure Titanium base.Fig. 5 is the EDS energy spectrum analysis figures of the composite, according to 3 not
With region titanium atom and the atom content and mass percent of carbon atom, be shown in Table 1, it is known that region 1,2,3 be respectively pure Titanium base,
TiC, unreacted Graphene.The elongation after fracture that can measure the composite using universal testing machine is 22%, is resisted
Tensile strength is 650Mpa, and 30.5% is improve than the pure titanium tensile strength under same process.
Embodiment 4
Ultrasonic disperse after graphene powder that 0.11437g volume fractions are 1.80% and 200mL absolute ethyl alcohols are mixed
30min, then adds the titanium valve that 25.0376g volume fractions are 98.20% under agitation, obtains mixed slurry；It is mixed by what is obtained
Close slurry to be transferred in ball grinder, add 150.912g zirconia ceramics ball milling pearls, ball milling 2.5h under 350r/min, using rotation
Absolute ethyl alcohol of the evaporimeter in ball milling disposed slurry is removed at 75 DEG C of 65r/min, obtains powder；The powder that will be obtained is at 120 DEG C
Vacuum drying chamber in dry 10h, obtain dried powder；The dried powder that will be obtained loads in graphite jig, heat
Lead to argon gas in pressure stove, and apply the pressure of 2.12t to graphite jig, 1300 DEG C are heated to the heating rate of 10 DEG C/min, protect
Room temperature is naturally cooled to after warm 1h, the product in graphite jig is for volumeGraphene enhancing titanium-based answer
Condensation material.
The sign and result carried out to the Graphene enhancing titanium matrix composite obtained by this implementation are as follows：
Knowable to from the SEM figures of the composite, the TiC particles that Graphene in-situ authigenic is formed are evenly distributed on pure titanium-based
In body.There is the diffraction maximum of pure titanium and TiC in the XRD diffraction patterns of the composite, can't see the diffraction maximum of Graphene.Answered by this
The SEM figures of condensation material stretching fracture understand, without Graphene inside prepared Graphene enhancing titanium matrix composite, in the sintering
At a temperature of, Graphene reacts completely with pure titanium.Fig. 6 is prepared Graphene enhancing titanium matrix composite and system under same process
The quasi-static tensile curve comparison figure of standby pure titanium, as can be seen from Figure, the elongation after fracture of composite is 16%, tension
Intensity is 750Mpa, and the tensile strength compared to pure titanium increased 51.5%.
Graphene obtained in the embodiment 3 of table 1 strengthens the EDS gamma-spectrometric datas of titanium matrix composite
The present invention include but is not limited to above example, it is every carried out under the principle of spirit of the present invention it is any equivalent
Replace or local improvement, all will be regarded as within protection scope of the present invention.
Claims (2)
1. a kind of Graphene strengthens the preparation method of titanium matrix composite, it is characterised in that：Methods described step is as follows：
(1) weighing of raw material：First, the number of plies L of Graphene is gone out using transmission electron microscope or atomic force microscope observation, then
The thickness T of L layer graphenes is measured, so as to graphene film interlamellar spacing d=T/ (L-1) can be obtained, can be calculated according to following formula
Go out the density of Graphene：
Wherein, ρGNPsIt is the density of Graphene, unit is g/cm3；D is graphene film interlamellar spacing, and unit is nm；ρgraphiteIt is stone
The density of ink, is 2.25g/cm3；0.34nm is the piece interlamellar spacing of graphite；
Then, the quality of Graphene is weighed, and calculates its corresponding volume；Further according to the volume of Graphene, weigh corresponding
Titanium valve；
(2) mixing of powder：Graphene powder mix with absolute ethyl alcohol after 20~30min of ultrasonic disperse, then under agitation plus
Enter titanium valve, obtain mixed slurry；The mixed slurry that will be obtained is transferred in ball grinder, ball milling pearl is added, in 300~350r/min
0.4~2.5h of lower ball milling；Then, the absolute ethyl alcohol in ball milling disposed slurry is removed, powder is obtained；The powder that will be obtained 90~
10~12h is dried in 120 DEG C of vacuum drying chamber, dried powder is obtained；
Wherein, ball milling pearl and the mass ratio with graphene powder and titanium valve are 5~6:1；
(3) hot pressed sintering：Powder dried in step (2) is loaded in graphite jig, mould inside pad graphite paper, and to stone
Black mould applies the pressure of 2~2.12t, and 900~1300 DEG C are heated to the heating rate of 10~12 DEG C/min, and insulation 1~
Room temperature is naturally cooled to after 1.5h, the product in graphite jig is that the Graphene strengthens titanium matrix composite；
Counted as 100% with the volume of Graphene enhancing titanium matrix composite, the composition and volume fraction of its each composition：Graphite
Alkene powder 1.80~1.90%, titanium valve 98.10~98.20%.
2. a kind of Graphene according to claim 1 strengthens the preparation method of titanium matrix composite, it is characterised in that：It is described
The inner mast of graphite jig coats the graphite paper of boron nitride.
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