CN110257128A - Nitrogen-doped graphene/silicon carbide microsphere nano composite material, preparation and application - Google Patents
Nitrogen-doped graphene/silicon carbide microsphere nano composite material, preparation and application Download PDFInfo
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- CN110257128A CN110257128A CN201910574495.1A CN201910574495A CN110257128A CN 110257128 A CN110257128 A CN 110257128A CN 201910574495 A CN201910574495 A CN 201910574495A CN 110257128 A CN110257128 A CN 110257128A
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- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
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- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
- C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
- C10M2205/028—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers containing aliphatic monomers having more than four carbon atoms
- C10M2205/0285—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers containing aliphatic monomers having more than four carbon atoms used as base material
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- 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 present invention discloses a kind of nitrogen-doped graphene/silicon carbide microsphere nano composite material, is grown on the nitrogen-doped graphene of silicon carbide microsphere surface including silicon carbide microballoon and in the form of sheets.It is microlayer model that the present invention, which is dissolved in the Polycarbosilane in petroleum ether by ultrasonic atomization technology atomization, it is brought into tube furnace by carrier gas, by Pintsch process, drop occurs cracking cross-linking shrinkage and is deposited in growth substrate, since silicon carbide crystallization process occurring inside microballoon, cause carbon extra in microballoon to surface enrichment, finally generates graphite microcrystal at high temperature.And the carbonaceous gas that microballoon cracking generates mushrooms out graphite microcrystal as multi-layer graphene.By the process, obtained graphene is firmly grown in microsphere surface.The phenomenon that after using acetonitrile, the carbon containing small molecule that acetonitrile cracks generation at high temperature is deposited in core surfaces, with high temperature graphitization, melts simultaneously, promotes growing up for nucleocapsid, and this graphene sheet layer increases, can promote the easy shear ability of graphene.
Description
Technical field
The present invention relates to a kind of nitrogen-doped graphene/silicon carbide microsphere nano composite material, preparation and applications, belong to compound
Material Field.
Background technique
Graphene relies on its unique layer structure, interlayer slip can occur in both macro and micro lubrication behavior, new
Huge application potential is shown in the research of emerging nano-lubricating material.However, because extremely strong point between layers of graphene
Interaction force is easy to promote to be overlapped between piece, reunite between son, influences its dispersibility in lubricating oil, influences the reality of graphene
With.The study found that its anti-wear and wear-resistant performance can be improved in graphene after N doping.Nitrogen-doped graphene synthetic method has
Preceding doping and rear two kinds of doping, the nitrogen-doped graphene that the above method is prepared still has dispersion limit in practical application.
Nitrogen-doped graphene can be significantly improved into its dispersion performance by forming composite material in conjunction with other materials, simultaneously
Also its anti-wear and wear-resistant performance can be improved.
Summary of the invention
In view of the above existing problems in the prior art, the present invention provides a kind of nitrogen-doped graphene/silicon carbide microsphere nanos
Composite material, can anti-agglomeration, have excellent anti-wear and wear-resistant performance.
The present invention also provides the nitrogen-doped graphene/silicon carbide microsphere nano composite material preparation method and answer
With.
To achieve the goals above, a kind of nitrogen-doped graphene/silicon carbide microsphere nano composite material that the present invention uses,
The composite material includes silicon carbide microballoon and is grown on the nitrogen-doped graphene of silicon carbide microsphere surface in the form of sheets.
As an improvement, the silicon carbide microballoon is solid construction, the diameter of silicon carbide microballoon is 1.55 μm -4.53 μm.
In addition, the present invention also provides a kind of nitrogen-doped graphene/silicon carbide microsphere nano composite material preparation method,
By the mixture for the carbon containing hydronitrogen of Polycarbosilane and liquid for being dissolved in petroleum ether, Pintsch process, preparation are negative in an inert atmosphere
Carry the silicon carbide microsphere nano composite material of nitrogen-doped graphene.
As an improvement, the carbon containing hydronitrogen of liquid uses any one of acetonitrile, pyridine.
As an improvement, the temperature of the Pintsch process is 1300-1400 DEG C, the Pintsch process time is 1.5-2.5h.
As an improvement, the nitrogen-doped graphene/silicon carbide microsphere nano composite material preparation method, specifically includes step
It is rapid:
1) Polycarbosilane/petroleum ether is prepared according to the ratio of 0.5g/10mL, and adds to atomizer；
2) control tube furnace is heated up with the rate of 5 DEG C/min, and the control of nitrogen gas velocity heats up in 10-20sccm to tube furnace
When to 850 DEG C, Polycarbosilane/petroleum ether is added by atomizer into tube furnace, passes through syringe pump and acetonitrile, nitrogen gas velocity is added
In 1300 DEG C of holding 1.5h after the completion of 40sccm, charging, nitrogen gas velocity drops to 10-20sccm later by the speed of 5 DEG C/min
After being cooled to 500 DEG C, Temperature fall is up to the nitrogen-doped graphene/silicon carbide microsphere nano composite material.
As an improvement, the charging rate of the atomizer is 0.3mL/min, 3h is fed；The flow velocity of the syringe pump is
0.1mL/min feeds 0.5h.
Finally, the present invention also provides a kind of nitrogen-doped graphene/silicon carbide microsphere nano composite materials as lubricating oil
The application of additive.
As an improvement, by nitrogen-doped graphene/silicon carbide microsphere nano composite material according to the quality of 0.01%-0.05%
Ratio adds in base oil PAO-4, prepares lubricating oil.
Compared with prior art, the beneficial effects of the present invention are:
1. nitrogen-doped graphene of the invention/silicon carbide microsphere nano composite material, including solid silicon carbide microballoon and it is in
In the nitrogen-doped graphene of microsphere surface, the growth course of the structure is that the Polycarbosilane being dissolved in petroleum ether leads to for lamellar growth
Crossing ultrasonic atomization technology atomization is microlayer model, is brought into tube furnace by carrier gas, and by Pintsch process, cracking crosslinking occurs for drop
It shrinks and is deposited in growth substrate (growth substrate refers to commercially available porcelain boat), since silicon carbide crystallization process occurring inside microballoon, lead
It causes carbon extra in microballoon to surface enrichment, finally generates graphite microcrystal at high temperature.And the carbon containing gas that microballoon cracking generates
Body mushrooms out graphite microcrystal as multi-layer graphene.By the process, obtained graphene is firmly grown in microballoon
Surface.After using acetonitrile, the carbon containing small molecule that acetonitrile cracks generation at high temperature is deposited in core surfaces, with pyrographite
Change, it is molten simultaneously promote growing up for nucleocapsid, the phenomenon that this graphene sheet layer increases, can promote graphene to be easy to shear energy
Power.
2. the preparation method is that being fed using misted chemical vapour deposition process by ultrasonic atomization technology, ultrasound
The high energy dispersion mechanism of ultrasonic energy generation is utilized in atomization, when the incoming liquid of ultrasound, can be partially formed negative pressure, liquid in liquid
Internal portion will generate hole and bubble, lead to liquid crushing, be embodied in when ultrasonic wave passes to liquid level, in wave crest
Liquid can be shaken into droplet, and droplet continues by ultrasound vibration after flying up again into smaller drop, and so circulation forms minimum mist
It drips and is pulled away.The method of the present invention can prepare by a Pintsch process process and be grown on silicon carbide microsphere surface in the form of sheets
Multi-layer graphene is prepared for multi-layer graphene and silicon carbide core simultaneously, and the two is firmly combined.
3. nitrogen-doped graphene of the invention/silicon carbide microsphere nano composite material can be widely applied to lubricating additive
In, play antifriction antiwear effect.
Detailed description of the invention
Fig. 1 is to prepare nitrogen-doped graphene/silicon carbide microsphere nano composite material atomising device in the embodiment of the present invention 1
Schematic diagram.
Fig. 2 is nitrogen-doped graphene/silicon carbide microsphere nano composite material x-ray photoelectron spectroscopy in the embodiment of the present invention 1
Figure.
Fig. 3 is nitrogen-doped graphene/silicon carbide microsphere nano composite material scanning electron microscopy in the embodiment of the present invention 1
Mirror figure (3500 times of amplification factor).
Fig. 4 is nitrogen-doped graphene/silicon carbide microsphere nano composite material scanning electron microscopy in the embodiment of the present invention 1
Mirror figure (10000 times of amplification factor).
Fig. 5 is that nitrogen-doped graphene/silicon carbide microsphere nano composite material is surveyed for greasy property in the embodiment of the present invention 2
The coefficient of friction and wear scar diameter figure of examination.
Fig. 6 is that nitrogen-doped graphene/silicon carbide microsphere nano composite material is surveyed for greasy property in the embodiment of the present invention 2
The mill spot optical microscope of examination.
Fig. 7 is that nitrogen-doped graphene/silicon carbide microsphere nano composite material is surveyed for greasy property in the embodiment of the present invention 4
The coefficient of friction and wear scar diameter figure of examination.
Fig. 8 is that nitrogen-doped graphene/silicon carbide microsphere nano composite material is surveyed for greasy property in the embodiment of the present invention 4
The mill spot optical microscope of examination.
Specific embodiment
In order to make the objectives, technical solutions and advantages of the present invention clearer, the present invention is carried out below further detailed
It describes in detail bright.However, it should be understood that the specific embodiments described herein are merely illustrative of the present invention, it is not limited to this hair
Bright range.
Unless otherwise defined, all technical terms and scientific terms used herein are led with technology of the invention is belonged to
The normally understood meaning of the technical staff in domain is identical, and term as used herein in the specification of the present invention is intended merely to retouch
State the purpose of specific embodiment, it is not intended that in the limitation present invention.
Embodiment 1
A kind of preparation method of nitrogen-doped graphene/silicon carbide microsphere nano composite material, specifically includes step:
1) Polycarbosilane/petroleum ether is prepared according to the ratio of 0.5g/10mL, and adds to atomizer as shown in Figure 1；
2) control tube furnace is heated up with the rate of 5 DEG C/min, and nitrogen gas velocity is controlled in 10sccm, is warming up to tube furnace
At 850 DEG C, Polycarbosilane/petroleum ether is added by atomizer into tube furnace, the charging rate of atomizer is 0.3mL/min,
3h is fed, acetonitrile is added by syringe pump, the flow velocity of syringe pump is 0.1mL/min, ejection of syringe pump 30min, and nitrogen gas velocity exists
40sccm, in 1300 DEG C of holding 1.5h after the completion of charging, nitrogen gas velocity is cooled to after dropping to 10sccm by the speed of 5 DEG C/min
After 500 DEG C, Temperature fall is up to the nitrogen-doped graphene/silicon carbide microsphere nano composite material.
Nitrogen-doped graphene obtained/silicon carbide microsphere nano composite material includes solid silicon carbide microballoon and gives birth in the form of sheets
It is longer than the nitrogen-doped graphene of microsphere surface, the diameter of silicon carbide microballoon is 1.55 μm -2.71 μm.
The x-ray photoelectron spectroscopy of nitrogen-doped graphene/silicon carbide microsphere nano composite material as shown in Figure 2, it is shown in figure
Peak position everywhere respectively represent oxygen, nitrogen, carbon, silicon, content can also be provided by x-ray photoelectron spectroscopy, respectively atomic percent
7.34%, 2.28%, 89.42%, 0.96%.Fig. 3 and Fig. 4 is nitrogen-doped graphene/silicon carbide microsphere nano composite material
Scanning electron microscope diagram, it may be clearly seen that, silicon carbide microsphere surface covers the nitrogen-doped graphene of vertical growth in figure.
Embodiment 2
Nitrogen-doped graphene/silicon carbide microsphere nano composite material is made as lube oil additive in a kind of embodiment 1
Using, by nitrogen-doped graphene/silicon carbide microsphere nano composite material according to 0.01%, 0.025%, 0.05% mass ratio
It adds in base oil PAO-4, prepares lubricating oil；
Prepared lubricating oil is subjected to ultrasonic disperse 40min；
The coefficient of friction of each lubricating oil, grinding defect diameter are tested using four ball tester for friction between of lever, according to GB/T
12583 experiments, time 30min, load 294N.Its maximum nonseizure load is tested using four ball frictional testing machine of fluid pressure type.It is real
In testing, consumption of lubricating oil is both needed to submergence steel ball to being higher than 1~2mm of steel ball surface.
In above-mentioned different content nitrogen-doped graphene/silicon carbide microsphere nano composite material lubricating oil, passing through 30min
Under test, which shows good anti-wear and wear-resistant performance.
Wherein, base oil is tested by 30min, coefficient of friction 0.0550, grinding defect diameter 0.4673mm；
Such as Fig. 5, Fig. 6 (wherein (a) PAO-4；(b) NG30.01wt%；(c) NG30.025wt%；(d) NG30.05wt%)
It is shown, in the lubricating oil for making additive using nitrogen-doped graphene/silicon carbide microsphere nano composite material, 0.01wt%,
The coefficient of friction of 0.025wt%, 0.05wt% are followed successively by 0.04576,0.05048,0.05224, successively reduce 16.80%,
8.22%, 5.02%, grinding defect diameter is followed successively by 0.4207mm, 0.429mm, 0.4243mm, successively reduce 9.97%,
8.20%, 9.20%.Corresponding maximum nonseizure load increases by 15.67%, 10.39%, 16.67%.
Embodiment 3
A kind of preparation method of nitrogen-doped graphene/silicon carbide microsphere nano composite material, specifically includes step:
1) Polycarbosilane/petroleum ether is prepared according to the ratio of 0.5g/10mL, and adds to atomizer as shown in Figure 1；
2) control tube furnace is heated up with the rate of 5 DEG C/min, and nitrogen gas velocity is controlled in 20sccm, is warming up to tube furnace
At 850 DEG C, Polycarbosilane/petroleum ether is added by atomizer into tube furnace, the charging rate of the atomizer is 0.3mL/
(Polycarbosilane/petroleum ether is homogeneous solution to min, and digestion amount is identical, and flow velocity has with atomizer power, inert gas flow velocity
Close), 3h is fed, acetonitrile is added by syringe pump into tube furnace, the flow velocity of the syringe pump is 0.1mL/min, syringe pump note
30min is penetrated, in 1300 DEG C of holding 1.5h after the completion of 40sccm, charging, nitrogen gas velocity drops to after 20sccm by 5 nitrogen gas velocity
DEG C/after the speed of min is cooled to 500 DEG C, Temperature fall is up to the nitrogen-doped graphene/silicon carbide microsphere nano composite wood
Material.
Nitrogen-doped graphene obtained/silicon carbide microsphere nano composite material includes solid silicon carbide microballoon and gives birth in the form of sheets
It is longer than the nitrogen-doped graphene of microsphere surface, the diameter of silicon carbide microballoon is 2.28 μm -4.53 μm.
Embodiment 4
Nitrogen-doped graphene/silicon carbide microsphere nano composite material is made as lube oil additive in a kind of embodiment 3
Using, by nitrogen-doped graphene/silicon carbide microsphere nano composite material according to 0.01%, 0.025%, 0.05% mass ratio
It adds in base oil PAO-4, prepares lubricating oil；
Prepared lubricating oil is subjected to ultrasonic disperse 40min；
The coefficient of friction of each lubricating oil, grinding defect diameter are tested using four ball tester for friction between of lever, according to GB/T
12583 experiments, time 30min, load 294N.Its maximum nonseizure load is tested using four ball frictional testing machine of fluid pressure type.It is real
In testing, consumption of lubricating oil is both needed to submergence steel ball to being higher than 1~2mm of steel ball surface.
In the lubricating oil of above-mentioned difference nitrogen-doped graphene/silicon carbide microsphere nano composite material content, passing through 30min
Under test, which shows good anti-wear and wear-resistant performance.
Wherein, base oil is tested by 30min, coefficient of friction 0.055, grinding defect diameter 0.4673mm；
Such as Fig. 7, Fig. 8 (wherein, (a) PAO-4；(b) NG50.01wt%；(c) NG50.025wt%；(d)
NG50.05wt% shown in), in the lubricating oil for making additive using nitrogen-doped graphene/silicon carbide microsphere nano composite material,
The coefficient of friction of 0.01wt%, 0.025wt%, 0.05wt% are followed successively by 0.05033,0.04553,0.03655, successively reduce
8.49%, 17.22%, 33.55%, grinding defect diameter is followed successively by 0.4313mm, 0.433mm, 0.343mm, successively reduces
7.7%, 7.34%, 26.60%.Corresponding maximum nonseizure load increases by 10.39%, 10.39%, 5.28%.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modification, equivalent replacement or improvement etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (9)
1. a kind of nitrogen-doped graphene/silicon carbide microsphere nano composite material, which is characterized in that the composite material includes silicon carbide
Microballoon and the nitrogen-doped graphene for being grown on silicon carbide microsphere surface in the form of sheets.
2. a kind of nitrogen-doped graphene according to claim 1/silicon carbide microsphere nano composite material, which is characterized in that
The silicon carbide microballoon is solid construction, and the diameter of silicon carbide microballoon is 1.55 μm -4.53 μm.
3. a kind of any one of claim 1-2 nitrogen-doped graphene/silicon carbide microsphere nano composite material preparation method,
It is characterized in that, by the mixture for the carbon containing hydronitrogen of Polycarbosilane and liquid for being dissolved in petroleum ether high temperature in an inert atmosphere
Cracking, the silicon carbide microsphere nano composite material of preparation load nitrogen-doped graphene.
4. nitrogen-doped graphene/silicon carbide microsphere nano composite material preparation method, feature exist according to claim 3
In the carbon containing hydronitrogen of liquid uses any one of acetonitrile, pyridine.
5. nitrogen-doped graphene/silicon carbide microsphere nano composite material preparation method, feature exist according to claim 3
In the temperature of the Pintsch process is 1300-1400 DEG C, and the Pintsch process time is 1.5-2.5h.
6. nitrogen-doped graphene/silicon carbide microsphere nano composite material preparation method, feature exist according to claim 3
In specifically including step:
1) Polycarbosilane/petroleum ether is prepared according to the ratio of 0.5g/10mL, and adds to atomizer；
2) control tube furnace is heated up with the rate of 5 DEG C/min, and nitrogen gas velocity is controlled in 10-20sccm, is warming up to 850 to tube furnace
DEG C when, Polycarbosilane/petroleum ether is added by atomizer into tube furnace, acetonitrile is added by syringe pump, nitrogen gas velocity exists
40sccm, in 1300 DEG C of holding 1.5h after the completion of charging, nitrogen gas velocity is dropped after dropping to 10-20sccm by the speed of 5 DEG C/min
Temperature is to after 500 DEG C, and Temperature fall is up to the nitrogen-doped graphene/silicon carbide microsphere nano composite material.
7. nitrogen-doped graphene/silicon carbide microsphere nano composite material preparation method, feature exist according to claim 6
In the charging rate of the atomizer is 0.3mL/min, feeds 3h；The flow velocity of the syringe pump is 0.1mL/min, charging
0.5h。
8. described in a kind of any one of claim 1-2 or N doping stone made from any one of the claim 3-7 preparation method
Black alkene/application of the silicon carbide microsphere nano composite material as lube oil additive.
9. application according to claim 8, which is characterized in that by nitrogen-doped graphene/silicon carbide microsphere nano composite wood
Material adds in base oil PAO-4 according to the mass ratio of 0.01%-0.05%, prepares lubricating oil.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111892982A (en) * | 2020-08-21 | 2020-11-06 | 北京化工大学 | Preparation method of nitrogen-doped nano lubricating material |
| CN115627157A (en) * | 2022-03-24 | 2023-01-20 | 中石化石油工程技术服务有限公司 | Application of high-nitrogen-doped graphene nanosheet in oil-based drilling fluid |
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