CN106398802A - Rapid laser preparing method for composite with graphene loaded with spherical inorganic fullerene molybdenum disulfide - Google Patents
Rapid laser preparing method for composite with graphene loaded with spherical inorganic fullerene molybdenum disulfide Download PDFInfo
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
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Abstract
The invention discloses a preparing method for a composite with graphene loaded with spherical inorganic fullerene molybdenum disulfide. The preparing method includes the following steps that sheetlike molybdenum disulfide and an oxidized graphene solution are mixed, and the mixture is ultrasonically dispersed into a suspension; the mixed suspension is irradiated with pulse lasers and converted into an interlayer structure under the effect of the pulse lasers and a liquid-phase solution solvent, wherein the interlayer structure is formed by the reduced oxidized graphene and nanometer/submicron inorganic fullerene molybdenum disulfide small spheres loaded on the surface of the reduced oxidized graphene alternately; after irradiation, the suspension is centrifuged, the obtained sediment is dried, and the composite with the reduced oxidized graphene loaded with the spherical inorganic fullerene molybdenum disulfide is obtained. According to the preparing method, the mixed suspension is irradiated directly with a laser beam, suspended particles instantaneously (in the nanosecond order) obtain high energy and are ablated and rapidly (in the nanosecond order) cooled with a solution, and therefore reduction of the oxidized graphene and conversion of the structure of the sheetlike molybdenum disulfide into the spherical inorganic fullerene structure are achieved in a one-step mode; the method is easy to operate, low in cost and free of impurity pollution, and the obtained composite shows excellent friction reduction performance in the friction process.
Description
Technical field
The present invention relates to a kind of preparation method of graphene-supported inorganic spherical fullerene molybdenum disulfide is and in particular to one
Kind using pulse laser irradiation technology simple and quick realize the reduction of graphene oxide and flaky molybdenum disulfide to spherical inorganic
The transformation of similar Fuller olefin structure, belongs to the preparing technical field of micro-nano powder.
Background technology
The whole world accounts for 1/3rd of whole mechanical power loss because of the energy loss that fretting wear causes, and faces World Economics
Develop rapidly the tight demand with energy-saving and emission-reduction, the research of antiwear and antifriction material will make outstanding contributions for realizing energy-saving and emission-reduction.
The molybdenum bisuphide of layer structure（2H-MoS2）Additive as traditional kollag, lubricating oil, lubricating grease has obtained
Extensively apply；, as lubriation material, its performance difference is larger for the molybdenum bisuphide of diverse microcosmic structure and form.Inorganic fullerene
Molybdenum bisuphide（IF-MoS2）Spherical and outer shell enclosed construction make it have good chemical stability, in friction process
In can also become sliding friction into rolling friction, therefore, IF-MoS2Remain to show excellent under more harsh working environment
Tribological property.But, IF-MoS2Complicated production technology, the reaction environment of harshness, high cost, yield poorly so as to apply
It is very restricted.
Graphene is sp2The new carbon with monatomic thickness of hydridization, it has excellent mechanical performance, conduction
Heat conductivility, high intensity and larger specific surface area, easily occur sliding to be formed in surface of friction pair under shear action
Lubricating film.But, Graphene is general as the anti-wear effect of lubricant, and its preparation cost is higher, mechanical stripping low yield, liquid phase
Peel off（Hummers）Need to be reduced, cause Graphene defect to increase, affect its mechanical performance and electrical and thermal conductivity.
At present, people to have solved low electric conductivity using the composite of flaky molybdenum disulfide/Graphene and to be easy to reunite
Problem（Number of patent application 201410711472.8；Adv. Mater. 2013, 25, 3979）；For spherical IF-MoS2/
The research of Graphene is less, and main preparation method is that liquid phase stripping method, vapour deposition process, calcination method and solvent-thermal method etc. are multiple
Method combines：Patent 201510155973.7 discloses a kind of composite lubricated solution additive of Graphene-fullerene molybdenum disulfide
And preparation method thereof, the reduction of graphene oxide adopts the hydrazine hydrate solution of high toxicity strong reducing property, IF-MoS2Preparation be
Reduce presoma molybdenum trisulfide under high temperature high-purity hydrogen and obtain.Patent 201510148981.9 discloses a kind of mineral-type fowler
Alkene molybdenum bisuphide/Graphene compounded lubricant and preparation method thereof, using high pressure resistant reactor, reaction temperature is 200 DEG C～600
DEG C, upper strata reaction atmosphere is the hydrogen of 0.2～3 MPa.However, the preparation method complex process of these reports, working environment will
Ask harsh, need using price, dangerous gas H2/H2S.A kind of more economical, simple, effective IF-MoS2/ Graphene
The preparation method of composite still falls within technological gap.
Content of the invention
In order to overcome the deficiencies in the prior art, the invention provides one kind has graphene-supported mineral-type fowler
The preparation method of alkene molybdenum bisuphide composite, the method is simple to operate, and flow process is short, without protective gas, Room pressure ring border
The reduction of graphene oxide and flaky molybdenum disulfide can quickly be realized down to the transformation of spherical inorganic similar Fuller olefin structure.
The present invention is directed to existing IF-MoS2The deficiency such as/graphene composite material preparation technology is loaded down with trivial details, condition is harsh, first
Propose to prepare graphene-supported inorganic spherical fullerene molybdenum disulfide composite by the way of pulse laser irradiation.Arteries and veins
Can be in contact interface moment after impulse light and material（Nanosecond order）Produce high temperature and high pressure environment, rapidly by sheet two sulphur
Change molybdenum ablation melting and be gradually converted into spherical, and be cooled rapidly under liquid phase medium environment around, realize molybdenum bisuphide from piece
Shape is to the fast transition of spherical similar Fuller olefin structure；Simultaneously under the strong reducing action of laser irradiation, graphene oxide is gone back
Former, finally give the inorganic spherical fullerene molybdenum disulfide composite of redox graphene load.The method operation letter
Single, reaction is quick, it is to avoid the deficiency such as vapor phase method and liquid phase method conditional are harsh, complex process is loaded down with trivial details, expensive.
Concrete technical scheme of the present invention is as follows：
A kind of preparation method of graphene-supported inorganic spherical fullerene molybdenum disulfide composite, the method includes following
Step：
（1）With sodium molybdate as molybdenum source, using thioacetamide as sulphur source, with polyethylene glycol, silico-tungstic acid or cetyl trimethyl
One of ammonium bromide, as dispersant, is 1 by the mol ratio between the sulphur in the molybdenum and sulphur source in molybdenum source, dispersant:（2～
2.8）∶（0～0.5）Ratio be added in deionized water, magnetic agitation, to being completely dissolved, is then transferred to autoclave
In, at 180～220 DEG C of temperature, insulation reaction 10～24h；After cooling, deionized water centrifuge washing 3～7 times, obtain all
Even dispersion flaky molybdenum disulfide suspension in aqueous；
（2）By graphene oxide solution（0.3～1.2 mg mL-1）Add in above-mentioned molybdenum bisuphide suspension, ultrasonic disperse 5～
30 min；
（3）Use pulse laser irradiation step（2）The mixing suspension obtaining, makes graphene oxide and flaky molybdenum disulfide powder exist
It is changed into the spherical fullerene molybdenum disulfide of redox graphene load in the presence of pulse laser；
（4）After irradiation is complete, suspension is centrifuged, separates, gained precipitates drying, obtain the spherical class of redox graphene load rich
Strangle alkene molybdenum bisuphide composite.
Step of the present invention（1）In, for the preparation of flaky molybdenum disulfide powder, the interpolation of dispersant or without meeting to it
Prototype micro pattern produces impact, and then influences whether the size of inorganic fullerene molybdenum disulfide produced by laser irradiation.
Preferably, step（1）In, dispersant selects in polyethylene glycol, silico-tungstic acid or cetyl trimethylammonium bromide
Zero kind or a kind of, finally can get inorganic fullerene molybdenum disulfide between 50～800 nm for the particle size range.
In laser irradiation process, the mixing suspension concentration of graphene oxide and flaky molybdenum disulfide be difficult excessive, dense
Spend all particles then cannot being uniformly irradiated with suspension greatly and make it receive identical energy and change, liquid phase simultaneously
The very few molybdenum bisuphide that also cannot make ablation melting of the content of medium quickly cools down.
Preferably, step（2）In, described molybdenum bisuphide with the effective mass percentage of Graphene is：（0.7～0.9）∶
（0.3～0.1）, both suspension mixed concentration are 0.8～20 mg mL-1.
Step of the present invention（3）In, the running parameter of pulse laser is as follows：Wavelength is 200～1600 nm, and frequency is 1～15
Hz, energy density is 100～800 mJ pulse-1cm-2, exposure time is 10～300 min.Being embodied as in the present invention
In mode, pulse laser is formed in the following ways：Laser beam is sent by laser instrument, then gathers through reflective mirror and convex lens
Jiao, the pulse laser beam of spot size needed for formation, adjust to required running parameter, you can carry out irradiation operations.
Preferably, step（3）In, during pulse laser irradiation, control the temperature of suspension to be 5 DEG C～20 DEG C；Pulse
The energy density of laser is 300～700 mJ pulse-1cm-2；Pulse laser irradiation 20～50 min can get preferable product
Product.
Further, in order that irradiation is evenly it is preferred that step（3）In, mixing suspension carries out arteries and veins under magnetic stirring
Impulse light irradiation, mixing speed is 500～1000 r min-1.
Preferably, step（4）In, the baking temperature of gained precipitation is 5 DEG C～15 DEG C.
Said method of the present invention can obtain the composite of graphene-supported inorganic spherical fullerene molybdenum disulfide,
This composite has more excellent subtracting than the mixed-powder of common graphene oxide/flaky molybdenum disulfide in friction process
The performance such as rub, the anti-friction agent as kollag, lubricating oil, lubricating grease has more preferable effect, and addition is left in 0.1 wt%
Right.
The solution of flaky molybdenum disulfide and graphene oxide is mixed by the present invention, ultrasonic disperse, forms suspension, through reflective
Laser beam after mirror and convex lens focus this suspension of direct irradiation, makes the molybdenum disulfide powder moment in solution（Nanosecond order）
The ablated melting of acquisition high-energy is simultaneously rapid by solution（Nanosecond order）Cooling, is produced with material using laser meanwhile
HTHP reducing atmosphere graphene oxide is reduced, thus realizing graphene-supported inorganic spherical fullerene curing
The preparation of the composite of molybdenum.Compared with prior art, this preparation method novelty, the pollution of product purity high free from admixture, gained stone
The inorganic spherical fullerene molybdenum disulfide composite of black alkene load has the excellent properties such as antifriction in friction process.This
Bright has the beneficial effect that：
（1）The present invention only needs to a step i.e. reduction of achievable graphene oxide and flaky molybdenum disulfide to spherical inorganic class fowler
The transformation of alkene structure, simple to operate, preparation cost is low；
（2）The present invention, by the selection use to different dispersants, can prepare different-grain diameter（50～800 nm）Spherical nothing
Machine fullerene molybdenum disulfide；
（3）Preparation process of the present invention only needs to laser irradiation dispersion flaky molybdenum disulfide in the solution and the mixing of Graphene is hanged
It is not necessary to other redox condition, reaction reagent and complex experiment device, condition is easily-controllable, process is simple, cost for supernatant liquid
Low, solve existing preparation process complexity and be difficult to the difficult problem produced in batches；
（4）Product purity that the inventive method obtains is high, and free from admixture pollutes, graphene-supported inorganic fullerene molybdenum disulfide
Composite has higher mechanical strength, toughness and stronger adsorptivity, as lubricating oil, lubricating oil, lubricating grease interpolation
Surface of friction pair can be adsorbed onto during agent, make separated from one another between metallic rubbing pairs, be effectively reduced friction, there is excellent subtracting
Rub performance.
Brief description
Fig. 1 is the transmission electron microscope figure of laser predose flaky molybdenum disulfide and graphene oxide mixed-powder；
Fig. 2 is the scanning of the graphene-supported inorganic spherical fullerene molybdenum disulfide composite being formed after pulse laser irradiation
Electron microscope picture；
Fig. 3 is the high score of the graphene-supported inorganic spherical fullerene molybdenum disulfide composite being formed after pulse laser irradiation
Distinguish transmission electron microscope figure.
Specific embodiment
For the ease of understanding the present invention, in the form of embodiment, the present invention is elaborated below, following embodiments are
Implemented under premised on the technology of the present invention, given detailed embodiment and specific operating process, but the present invention
Protection domain be not limited to following embodiments.
Embodiment 1
（1）Weigh 0.24 g sodium molybdate（Purity 99%）With 0.15 g thioacetamide（Purity 98%）Put in beaker, add 50
ML deionized water, magnetic agitation is completely dissolved to powder；Then solution is moved into reactor, be incubated 24h at 180 DEG C；Cooling
Afterwards, deionized water centrifuge washing 7 times, obtain dispersed flaky molybdenum disulfide suspension in aqueous；
（2）Graphene oxide solution by 2.0 mL（0.8 mg mL-1）Add in above-mentioned molybdenum bisuphide suspension, both mixing
Concentration afterwards is 0.8 mg mL-1, ultrasonic disperse 5 min；
（3）By the krypton fluorine laser bundle after reflective mirror and convex lens focus（248 nm）Irradiation above-mentioned steps（2）Prepared is mixed
Close suspension, laser energy density is 300 mJ pulse-1cm-1, frequency is 15 Hz, and exposure time is 20 min.Laser beam
In irradiation process, with magnetic stirrer with 1000 r min-1Rotating speed is stirred continuously suspension, and suspension temperature is 5 DEG C；
（4）After irradiation is complete, centrifuged suspension, then dried powder at 5 DEG C, obtain the spherical class of redox graphene load rich
Strangle alkene molybdenum bisuphide composite.
Fig. 1 is step（2）Middle laser predose flaky molybdenum disulfide and the transmission electron microscope picture of graphene oxide mixed-powder,
It can be seen that flaky molybdenum disulfide agglomerates are got together.The graphene-supported ball being formed after Fig. 2 pulse laser irradiation
The surface sweeping electron microscope of shape inorganic fullerene molybdenum disulfide composite, it can be seen that equably bear on graphene film
Carry spherical molybdenum disulfide particles, both form sandwich, Microsphere Size is more uniform, particle diameter is 100～200 nm.Fig. 3
It is the transmission electron microscope picture of products obtained therefrom after irradiation, as can be seen from the figure microballoon edge（002）The spacing in face（0.62 nm）Occur
1% lattice dilatation, illustrates that marginal portion crimps, and stress becomes and leads to greatly interlamellar spacing to become big, occurs in that inorganic fullerene
Structure, effectively eliminates the dangling bond of sheet-like particle edge.So, in friction process, this composite can be effectively
Suppression molybdenum disulfide powder makes the bad phenomenon that coefficient of friction raises because high temperature is oxidized, thus showing excellent frictional property
Energy.
Embodiment 2
（1）Weigh 0.24 g sodium molybdate（Purity 99%）, 0.19 g thioacetamide（Purity 98%）With 0.15 g silico-tungstic acid（Purity
98%）Put in beaker, add 50 mL deionized waters, magnetic agitation is completely dissolved to powder；Then solution is moved into reactor
In, it is incubated 10 h at 220 DEG C；After cooling, deionized water centrifuge washing 7 times, obtain dispersed piece in aqueous
Shape molybdenum bisuphide suspension；
（2）Graphene oxide solution by 2 mL（0.8 mg mL-1）Add in above-mentioned molybdenum bisuphide suspension, after both mixing
Concentration be 5 mg mL-1, ultrasonic disperse 15 min；
（3）By the krypton fluorine laser bundle after reflective mirror and convex lens focus（248 nm）Irradiation above-mentioned steps（2）Prepared is mixed
Close suspension, laser energy density is 500 mJ pulse-1cm-1, frequency is 10 Hz, and exposure time is 40 min.Laser beam
In irradiation process, with magnetic stirrer with 800 r min-1Rotating speed is stirred continuously suspension, and suspension temperature is 10 DEG C；
（4）After irradiation is complete, centrifuged suspension, then dried powder at 15 DEG C, obtain redox graphene and load spherical class
Fullerene molybdenum disulphide composite.Products obtained therefrom microscopic appearance is similar to Example 1, but inorganic spherical fullerene two sulphur
The particle diameter changing molybdenum is 50～100 nm.
Embodiment 3
（1）Weigh 0.24 g sodium molybdate（Purity 99%）, 0.21g thioacetamide（Purity 98%）With 0.15 g polyethylene glycol（Pure
Degree 98%）Put in beaker, add 50 mL deionized waters, magnetic agitation is completely dissolved to powder；Then solution is moved into reaction
In kettle, it is incubated 16 h at 200 DEG C；After cooling, deionized water centrifuge washing 5 times, obtain dispersed in aqueous
Flaky molybdenum disulfide suspension；
（2）Graphene oxide solution by 3 mL（0.8 mg mL-1）Add in above-mentioned molybdenum bisuphide suspension, after both mixing
Concentration be 15 mg mL-1, ultrasonic disperse 30 min；
（3）By the krypton fluorine laser bundle after reflective mirror and convex lens focus（248 nm）Irradiation above-mentioned steps（2）Prepared is mixed
Close suspension, laser energy density is 700 mJ pulse-1cm-1, frequency is 5 Hz, and exposure time is 60 min；Laser beam
In irradiation process, with magnetic stirrer with 500 r min-1Rotating speed is stirred continuously suspension, and suspension temperature is 15 DEG C；
（4）After irradiation is complete, centrifuged suspension, then dried powder at 20 DEG C, obtain redox graphene and load spherical class
Fullerene molybdenum disulphide composite.Products obtained therefrom microscopic appearance is similar to Example 1, but inorganic spherical fullerene two sulphur
The particle diameter changing molybdenum is 300～500nm.
Embodiment 4
（1）Weigh 0.24 g sodium molybdate（Purity 99%）, 0.15 g thioacetamide（Purity 98%）With 0.15 g cetyl three
Methyl bromide ammonium（Purity 98%）Put in beaker, add 50 mL deionized waters, magnetic agitation is completely dissolved to powder；Then will
Solution moves in reactor, is incubated 10 h at 220 DEG C；After cooling, deionized water centrifuge washing 7 times, obtain dispersed
Flaky molybdenum disulfide suspension in aqueous；
（2）Graphene oxide solution by 2 mL（0.8 mg mL-1）Add in above-mentioned molybdenum bisuphide suspension, after both mixing
Concentration be 20 mg mL-1, ultrasonic disperse 30 min；
（3）By the krypton fluorine laser bundle after reflective mirror and convex lens focus（248 nm）Irradiation above-mentioned steps（2）Prepared is mixed
Close suspension, laser energy density is 700 mJ pulse-1cm-1, frequency is 15 Hz, and exposure time is 60 min, laser beam
In irradiation process, with magnetic stirrer with 700 r min-1Rotating speed is stirred continuously suspension, and suspension temperature is 20 DEG C；
（4）After irradiation is complete, centrifuged suspension, then dried powder at 20 DEG C, obtain redox graphene and load spherical class
Fullerene molybdenum disulphide composite, products obtained therefrom microscopic appearance is similar to Example 1, but inorganic spherical fullerene two sulphur
The particle diameter changing molybdenum is 700～800 nm.
In order to verify the antifriction performance of products obtained therefrom, carry out following experiment：
1st, the mixed-powder of the Graphene after laser predose in the various embodiments described above and molybdenum bisuphide is respectively added to liquid
In paraffin oil, carry out frictional behaviour test, addition is 0.1 wt% of atoleine oil quality；
2nd, frictional behaviour method of testing：Four-ball friction and wear is tested, meanwhile, with paraffin refined wax oil as blank；
3rd, result：The frictional property test result of each embodiment and comparative example product, see table 1.
Table 1
It can thus be seen that the graphene-supported inorganic spherical fullerene molybdenum disulfide composite that the inventive method is obtained exists
Good lifting is had on antifriction performance hence it is evident that being higher than the mixed-powder of laser predose Graphene and flaky molybdenum disulfide.Point
The condition on production performances such as the species of powder, suspension mixed concentration, the energy density in irradiation for the suspension have larger shadow
Ring.
Claims (9)
1. a kind of preparation method of graphene-supported inorganic spherical fullerene molybdenum disulfide composite is it is characterised in that be somebody's turn to do
Composite is by redox graphene and in its area load nano/submicron inorganic fullerene molybdenum disulfide bead phase
Between formed sandwich；Using liquid-phase pulse laser irradiation technique, going back of graphene oxide can quickly be realized by a step
Former and flaky molybdenum disulfide is to the transformation of spherical inorganic similar Fuller olefin structure, wherein, inorganic spherical fullerene molybdenum disulfide
Particle diameter is 50～800 nm.
2. a kind of preparation side of graphene-supported as claimed in claim 1 inorganic spherical fullerene molybdenum disulfide composite
Method is it is characterised in that comprise the following steps：
（1）With sodium molybdate as molybdenum source, with thioacetamide as sulphur source, with polyethylene glycol, silico-tungstic acid or cetyl trimethyl bromine
Change one of ammonium as dispersant, be 1 by the mol ratio between the sulphur in the molybdenum and sulphur source in molybdenum source, dispersant:（2～
2.8）∶（0～0.5）Ratio be added in deionized water, magnetic agitation, to being completely dissolved, is then transferred to autoclave
In, at 180～220 DEG C of temperature, insulation reaction 10～24 h；After cooling, deionized water centrifuge washing 3～7 times, obtain all
Even dispersion flaky molybdenum disulfide suspension in aqueous；
（2）Graphene oxide solution is added in above-mentioned molybdenum bisuphide suspension, ultrasonic disperse 5～30 min；
（3）Use pulse laser irradiation step（2）The mixing suspension obtaining, makes graphene oxide and flaky molybdenum disulfide powder exist
It is changed into the composite of the spherical fullerene molybdenum disulfide of redox graphene load in the presence of pulse laser；
（4）After irradiation terminates, suspension is centrifuged, separates, gained is precipitated drying, obtain redox graphene load spherical
Fullerene molybdenum disulfide composite.
3. preparation method according to claim 2, is characterized in that：Step（2）In, described molybdenum bisuphide is had with Graphene
Imitating mass percent is：（0.7～0.9）∶（0.3～0.1）.
4. preparation method according to claim 2, is characterized in that：Step（2）In, described graphene oxide solution concentration is
0.3～1.2 mg mL-1.
5. preparation method according to claim 2, is characterized in that：Step（2）In, by described graphene oxide solution and institute
Stating the suspension mixed concentration that flaky molybdenum disulfide suspension is mixed to get is 0.8～20 mg mL-1.
6. preparation method according to claim 2, is characterized in that：Step（3）In, the wavelength of described pulse laser is 200
～1600 nm, frequency is 1～15 Hz, and energy density is 100～800 mJ pulse-1cm-2, exposure time is 10～300
min.
7. preparation method according to claim 2, is characterized in that：Step（3）In, during pulse laser irradiation, control
The temperature of suspension is 5 DEG C～20 DEG C.
8. preparation method according to claim 2, is characterized in that：Step（3）In, suspension carries out arteries and veins under magnetic stirring
Impulse light irradiation, mixing speed is 300～2000 r min-1.
9. preparation method according to claim 2, is characterized in that：Step（4）In, the baking temperature of described precipitation is 5 DEG C
～30 DEG C.
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