CN106221856A - A kind of nanometer MoS2/ graphene complex additive - Google Patents
A kind of nanometer MoS2/ graphene complex additive Download PDFInfo
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- CN106221856A CN106221856A CN201610592862.7A CN201610592862A CN106221856A CN 106221856 A CN106221856 A CN 106221856A CN 201610592862 A CN201610592862 A CN 201610592862A CN 106221856 A CN106221856 A CN 106221856A
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- Prior art keywords
- mos
- graphene
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- additive
- graphene complex
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Classifications
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- 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
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/04—Elements
- C10M2201/041—Carbon; Graphite; Carbon black
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/06—Metal compounds
- C10M2201/065—Sulfides; Selenides; Tellurides
- C10M2201/066—Molybdenum sulfide
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
Abstract
The invention discloses a kind of nanometer MoS2/ graphene complex additive, this additive is prepared by the following method and obtains: by graphene dispersion in the hydrous ethanol solution of molybdenum dithiophosphate acid amide, adds concentrated hydrochloric acid and makes molybdenum dithiophosphate acid amide resolve into MoS3Loading on Graphene, dispersion passes through membrane filtration, deionized water wash, and gained solid product is dried in atmosphere, puts into evacuation in tube furnace, then is passed through nitrogen protection, in 500 800 DEG C by MoS3Change into MoS2, form nanometer MoS2/ graphene complex (G MoS2).Nanometer additive of the present invention can show good anti-wear and wear-resistant performance 50 125 DEG C of temperature ranges in polyethers (PAG), Polyethylene Glycol (PEG) and synthesizing ester oil.
Description
Technical field
The present invention relates to a kind of nanometer MoS2/ graphene complex additive.
Background technology
Graphene (G) and molybdenum bisuphide (MoS2) be all there is lamellar structure lubriation material, substantial amounts of research report they i.e.
Again can be as the application of lube oil additive as solid lubricant.Graphene and MoS2Molecule interlayer there is Van der Waals
Power, therefore layer and interlayer are prone to slide.It addition, they easily form boundary lubricant film between friction pair, this is considered as them
There is the dominant mechanism of antifriction antiwear effect.Zhao Jun etc. reports Graphene, MoS2Nanometer sheet is respectively as hydraulic oil
Additive.Result of study shows MoS2Nanometer sheet have in hydraulic oil more preferable anti-wear and wear-resistant performance (J. Zhao etc.,
Tribology Internationa, 2016, l97,14 20).Xu Yufu etc. have studied Graphene, MoS2And not homogeneity
Graphene/the MoS of amount percentage ratio2Mixture as esterification bio oil additive (Y.F. Xu etc., Wear, 2015,342-343,
297 309).Result shows in these additives, and the antifriction antiwear effect of Graphene/molybdenum bisuphide mixture is better than individually
Add Graphene and molybdenum bisuphide, and add 0.3 wt% Graphene+0.2 wt% MoS2There is best lubricant effect.
But, MoS used in above research2Particle size is all micron order, is born by the molybdenum bisuphide (1-100 nm) of nano-scale
It is downloaded on Graphene, prepares nanometer MoS2/ graphene complex but has no report as the research of additive.
Along with science and technology and industrial expansion, modern industry just develops towards extreme severe rugged environment, such as at high speed, and heavy load
And high-temperature condition.Particularly hot environment has important impact to the rate of depreciation of friction pair under lubricating status.When lubrication temperature
During change, not only the viscosity characteristics of lubricant is changed, and the mechanical features of friction pair also can be changed.Lubrication in reality
Under agent applied environment, there are many actual condition temperature higher than 100◦C, such as Aero-Space, mining industry and iron and steel processing industry etc..This
Plant special operating mode and will cause lubricant deterioration and inefficacy so that lubricant and lubricating additive face the challenge.Have now
Many synthesizes basal liquid efficiently, and the most poly-a alkene (PAO), synthetic ester and polyethers (PAG) are developed to solve high temperature
Lubrication problem.But, these synthetic base oils at high temperature self anti-wear and wear-resistant performance is the most undesirable, needs to add antifriction and resists
Mill additive could meet industrial requirement, and it is the most necessary for therefore researching and developing the lube oil additive used in high temperature environments
's.
Summary of the invention
It is an object of the invention to provide a kind of nanometer MoS2/ graphene complex additive.
A kind of nanometer MoS2/ graphene complex additive, it is characterised in that this additive is prepared by the following method
Arrive: by graphene dispersion at molybdenum dithiophosphate acid amide ((NH4)2MoS4) water-ethanol solution in, add concentrated hydrochloric acid make molybdenum dithiophosphate acid amide
Resolve into MoS3Loading on Graphene, dispersion passes through membrane filtration, deionized water wash, and gained solid product is at air
In be dried, put into evacuation in tube furnace, then be passed through nitrogen protection, in 500-800 DEG C by MoS3Change into MoS2, form nanometer
MoS2/ graphene complex (G-MoS2).
Described Graphene and (NH4)2MoS4Mass ratio be 1:1;Described (NH4)2MoS4Mass volume ratio with concentrated hydrochloric acid
It is 0.2 g/mL;Described concentrated hydrochloric acid is 1:40 with the volume ratio of water-ethanol solvent.
In described water-ethanol solvent, the volume ratio of water and ethanol is 1:1.
Nanometer MoS as mentioned above2/ graphene complex additive is as Esters oil, polyethers, the additive of Polyethylene Glycol
Application.
Nanometer MoS of the present invention2/ graphene complex (G-MoS2) add polyethers (PAG), Polyethylene Glycol (PEG) to
With in synthesizing ester oil, all showing the anti-wear and wear-resistant performance of excellence in temperature 50-125 DEG C, their tribological property is intended to
It is better than respectively by Graphene, MoS2(business product, particle diameter 0.5 is m) and Graphene/MoS2Mixture adds in these base oils
Tribological property.
Accompanying drawing explanation
Fig. 1 is nanometer MoS described in embodiment 12/ graphene complex (G-MoS2) high resolution scanning electronic image
(a, b) and transmission electron microscope image (c, d).
Fig. 2 is polyethers (PAG), 0.5% G, 0.5% MoS2, 0.3% G+0.2% MoS2With 0.5% G-MoS2(embodiment 1
Prepared by) at 100 DEG C, frequency 25 Hz, load is respectively 25 N(a), 50 N(b), 75N(c) and 100 N(d) duration mill
The friction coefficient curve of 30 min.
Fig. 3 is polyethers (PAG), 0.5% G, 0.5% MoS2, 0.3% G+0.2% MoS2With 0.5% G-MoS2(embodiment 1
Prepared by) at 100 DEG C, frequency 25 Hz, load is respectively 25 N, 50 N, 75N and 100 N durations and grinds 30 min mill speckles
Wear extent.
Fig. 4 is polyethers (PAG), 0.5% G, 0.5% MoS2, 0.3% G+0.2% MoS2With 0.5% G-MoS2(embodiment 1
Prepared by) at 50 N, frequency 25 Hz, temperature is respectively 25 DEG C (a), 50 DEG C (b), 75 DEG C (c), 100 DEG C (d) and 125
DEG C duration grinds the friction coefficient curve of 30 min.
Fig. 5 is polyethers (PAG), 0.5% G, 0.5% MoS2, 0.3% G+0.2% MoS2With 0.5% G-MoS2(embodiment 1
Prepared by) at 50 N, frequency 25 Hz, temperature is respectively 25 DEG C, 50 DEG C, 75 DEG C, 100 DEG C and 125 DEG C of durations mills 30
The wear extent of min mill speckle.
Detailed description of the invention
Embodiment 1
100 mg Graphenes are joined in water-ethanol (v:v=1:1) solution that 20 mL contain 100 mg molybdenum dithiophosphate acid amides, it
Rear addition 0.5 mL concentrated hydrochloric acid, with membrane filtration after being sufficiently stirred for, deionized water wash, it is dried in atmosphere.Dried powder
End solid is put in tube furnace, and evacuation is protected by high pure nitrogen afterwards, is warming up to 500 DEG C and keeps 1 h.After cooling
To nanometer MoS2/ Graphene (G-MoS2) additive.
Nanometer MoS by above-mentioned preparation2/ Graphene (G-MoS2), commercial graphite alkene (G) and commodity MoS2(0.5 m) point
Do not add in polyethers (PAG), after being sufficiently stirred for, disperse 2 h with ultrasound wave, obtain 0.5% G-MoS2, 0.5% G, 0.5%
MoS2With 0.3%G+ 0.2%MoS2Dispersion.
Embodiment 2
100 mg Graphenes are joined in water-ethanol (v:v=1:1) solution that 20 mL contain 100 mg molybdenum dithiophosphate acid amides, it
Rear addition 0.5 mL concentrated hydrochloric acid, with membrane filtration after being sufficiently stirred for, deionized water wash, it is dried in atmosphere.Dried powder
End solid is put in tube furnace, and evacuation is protected by high pure nitrogen afterwards, is warming up to 600 DEG C and keeps 1 h.After cooling
To nanometer MoS2/ Graphene (G-MoS2) additive.
Nanometer MoS by above-mentioned preparation2/ Graphene (G-MoS2), commercial graphite alkene (G) and commodity MoS2(0.5 m) point
Do not add in polyethers (PAG), after being sufficiently stirred for, disperse 2 h with ultrasound wave, obtain 0.5% G-MoS2, 0.5% G, 0.5%
MoS2With 0.3%G+ 0.2%MoS2Dispersion.
Embodiment 3
100 mg Graphenes are joined in water-ethanol (v:v=1:1) solution that 20 mL contain 100 mg molybdenum dithiophosphate acid amides, it
Rear addition 0.5 mL concentrated hydrochloric acid, with membrane filtration after being sufficiently stirred for, deionized water wash, it is dried in atmosphere.Dried powder
End solid is put in tube furnace, and evacuation is protected by high pure nitrogen afterwards, is warming up to 800 DEG C and keeps 1 h.After cooling
To nanometer MoS2/ Graphene (G-MoS2) additive.
Nanometer MoS by above-mentioned preparation2/ Graphene (G-MoS2), commercial graphite alkene (G) and commodity MoS2(0.5 m) point
Do not add in polyethers (PAG), after being sufficiently stirred for, disperse 2 h with ultrasound wave, obtain 0.5% G-MoS2, 0.5% G, 0.5%
MoS2With 0.3%G+ 0.2%MoS2Dispersion.
Structural analysis: be dispersed in dehydrated alcohol by the product of embodiment 1, is swept by JSM-6701F cold field emission type
Retouch Electronic Speculum and its exterior appearance of JEM-1200EX determination of transmission electron microscopy, as shown in Figure 1.Result shows in embodiment 1
Prepared nanometer MoS2In/graphene complex, load to the MoS on Graphene2Nanoparticle size is less than 50 nm.
The tribological property evaluation of product
1. in SRV-IV micro-vibration friction abrasion testing machine testing example 1 that employing Germany Optimol oils and fats company produces
0.5% G-MoS of preparation2, 0.5% G, 0.5% MoS2And 0.3%G+0.2%Mo2In polyethers (PAG), temperature 100 DEG C, frequently
Rate 25 Hz, amplitude 1 mm, load is respectively 25 N, 50 N, 75 N, and coefficient of friction f when 100 N durations grind 30 min, examination
Testing the GCr15 bearing steel that steel ball used is F=10 mm, lower sample is the GCr15 bloom of F24 × 7.9 mm.Result is shown in accompanying drawing 2.
As seen from the figure, at 100 DEG C, 0.5% G-MoS2The coefficient of friction of PAG all can be significantly reduced under different loads.It addition, receive
Rice MoS2/ graphene complex antifriction performance in PAG is also significantly better than Graphene, micron-sized MoS2With Graphene/MoS2
Mixture.
2. use 0.5% G-MoS of preparation in MicroXAM 3D non-contacting Surface Tester testing example 12,
0.5%G, 0.5%MoS2, 0.3%G+0.2%Mo2In polyethers (PAG), 100 DEG C, frequency 25 Hz, amplitude 1 mm, load is respectively
25 N, 50 N, 75 N, and the wear volume of mill speckle when 100 N durations grind 30 min, as shown in Figure 3.Result shows, 100
DEG C, 0.5% G-MoS2The abrasion volume of PAG all can be significantly reduced under different loads.It addition, nanometer MoS2/ graphene complex
In PAG, the abrasion resistance under different loads is also significantly better than Graphene, micron-sized MoS2With Graphene/MoS2Mixing
Thing.
3. SRV-IV micro-vibration friction abrasion testing machine testing example that employing Germany Optimol oils and fats company produces
0.5% G-MoS of preparation in 12And 0.5%G, 0.5%MoS2, 0.3%G+0.2%Mo2In polyethers (PAG), load 50 N, frequently
Rate 25 Hz, amplitude 1 mm, temperature is respectively 25 DEG C, 50 DEG C, 75 DEG C, friction when 100 DEG C and 125 DEG C of long mill 30 min
Coefficient f, test steel ball used is the GCr15 bearing steel of F=10 mm, and lower sample is the GCr15 bloom of F24 × 7.9 mm.Result
See accompanying drawing 4.As seen from the figure, room temperature 25 DEG C, various additives the most do not show obvious antifriction performance.And along with temperature
The rising of degree, 0.5% G-MoS2Antifriction performance significantly improves, and significantly better than Graphene, micron-sized MoS2With Graphene/
MoS2Mixture.When temperature is raised to 125 DEG C, G-MoS2Antifriction performance can increase over time and lose efficacy.
4. use 0.5% G-MoS of preparation in MicroXAM 3D non-contacting Surface Tester testing example 12
And 0.5%G, 0.5%MoS2, 0.3%G+0.2%Mo2In polyethers (PAG), load 50 N, frequency 25 Hz, amplitude 1 mm, temperature
It is respectively 25 DEG C, 50 DEG C, 75 DEG C, when 100 DEG C and 125 DEG C of long mill 30 min, grinds the wear extent of speckle.Result is shown in accompanying drawing 5.By
Figure is not it can be seen that room temperature 25 DEG C, the abrasion resistance of various additives is clearly.And along with the rising of temperature, 0.5% G-
MoS2Abrasion resistance significantly improves, and significantly better than Graphene, micron-sized MoS2With Graphene/MoS2Mixture.
Claims (4)
1. nanometer MoS2/ graphene complex additive, it is characterised in that this additive is prepared by the following method and obtains:
By graphene dispersion in the water-ethanol solution of molybdenum dithiophosphate acid amide, add concentrated hydrochloric acid and make molybdenum dithiophosphate acid amide resolve into MoS3Load
On Graphene, dispersion passes through membrane filtration, deionized water wash, and gained solid product is dried in atmosphere, puts into pipe
Evacuation in formula stove, then it is passed through nitrogen protection, in 500-800 DEG C by MoS3Change into MoS2, form nanometer MoS2/ Graphene is multiple
Compound.
2. nanometer MoS as claimed in claim 12/ graphene complex, it is characterised in that described Graphene and (NH4)2MoS4's
Mass ratio is 1:1;Described (NH4)2MoS4It is 0.2 g/mL with the mass volume ratio of concentrated hydrochloric acid;Described concentrated hydrochloric acid and water-ethanol
The volume ratio of solvent is 1:40.
3. nanometer MoS as claimed in claim 1 or 22/ graphene complex, it is characterised in that water in described water-ethanol solvent
It is 1:1 with the volume ratio of ethanol.
4. nanometer MoS as claimed in claim 12/ graphene complex resists as the high-temperature antifriction of Esters oil, polyethers, Polyethylene Glycol
The application of mill additive.
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Cited By (2)
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CN110041983A (en) * | 2019-04-11 | 2019-07-23 | 中国科学院兰州化学物理研究所 | A kind of carbon material supported nanometer MoS2The preparation method and application of compound |
CN110041981A (en) * | 2019-04-11 | 2019-07-23 | 中国科学院兰州化学物理研究所 | Surface-functionalized nanometer carbon material supported MoS2The preparation method and application of compound |
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US20130045427A1 (en) * | 2011-08-19 | 2013-02-21 | Nanoteck Instruments, Inc. | Prelithiated current collector and secondary lithium cells containing same |
CN102807907A (en) * | 2012-08-24 | 2012-12-05 | 江苏大学 | Graphene/metal oxide semiconductor (MoS2) nano self-lubricating composite material and preparation method thereof |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110041983A (en) * | 2019-04-11 | 2019-07-23 | 中国科学院兰州化学物理研究所 | A kind of carbon material supported nanometer MoS2The preparation method and application of compound |
CN110041981A (en) * | 2019-04-11 | 2019-07-23 | 中国科学院兰州化学物理研究所 | Surface-functionalized nanometer carbon material supported MoS2The preparation method and application of compound |
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Application publication date: 20161214 |