CN110229709A - SiC adulterates the preparation and application of onion shape graphitization carbon ball nanocomposite - Google Patents
SiC adulterates the preparation and application of onion shape graphitization carbon ball nanocomposite Download PDFInfo
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- CN110229709A CN110229709A CN201910574485.8A CN201910574485A CN110229709A CN 110229709 A CN110229709 A CN 110229709A CN 201910574485 A CN201910574485 A CN 201910574485A CN 110229709 A CN110229709 A CN 110229709A
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- sic
- carbon ball
- onion shape
- petroleum ether
- polycarbosilane
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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
- C10M125/26—Compounds containing silicon or boron, e.g. silica, sand
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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
- 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
- C10M2201/10—Compounds containing silicon
-
- 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 present invention discloses a kind of synthesis of controllable grain size SiC doping onion shape graphitization carbon ball nanocomposite, including fullerene structure three-dimensional nanometer material onion shape graphitization carbon ball and uniform doping SiC in situ and outer layer vertical direction grow graphene sheet layer.The present invention is using petroleum ether as carbon matrix precursor, micro Polycarbosilane is as structure directing agent, PCS is dissolved in wiring solution-forming in petroleum ether, stock dispersion is become to the microlayer model of uniform particle diameter with atomizing type, tube furnace is sent by carrier gas, volume polycondensation occurs for period each drop independent reaction, and the series reactions such as drop pyrolysis generate products therefrom.Wherein Polycarbosilane has the function of promoting product balling-up as structure directing agent, during the reaction steaming with surface solvent, and solute concentration increases and then surface lolute crystallization is caused to be precipitated, and forms spherical shell, and reaction is limited to ball interior after being allowed to.
Description
Technical field
The present invention relates to the preparations and application of a kind of SiC doping onion shape graphitization carbon ball nanocomposite, belong to multiple
Condensation material field.
Background technique
Recently as the development of nanotechnology, carbon nanomaterial is graduallyd mature, and has been had already appeared many different types of
Carbon nanomaterial is such as: graphene；Fullerene；Carbon nano-fiber；Nano carbon balls；Carbon nanotube etc..Three-dimensional nanometer material carbon nanometer
Ball, due to geometrical morphology of its rule and its can pass through graphitization, aromatization, many means such as atom doped carry out tables
Face is modified, just by the concern of scientists.With the maturation of technology, Nano carbon balls can be summarized as to sow at present
Class: carbon ball；Core-shell structure carbon ball；Hollow carbon sphere；Egg yolk structure hollow carbon sphere etc..Due to chemical and thermal stability and it is controllable
Geometrical characteristic and surface nature, they are just widely used in being catalyzed, absorption, and the conversion of energy is in storage, the neck such as biological medicine
Domain.
With the rise of nano lubricating, three-dimensional nanometer material is just gradually by the concern of scientists.It it is presently believed that
Nanometer lubricating additive (such as metal nanoparticle, inorganic compound nano particle, fullerene structure nano particle, polymer nano
Rice grain etc.) it can play the role of in lubrication " colloid action ", micro- axis of rolling or chemical films are formed in situ.WS2, MoS2, stone
The two-dimension nano materials such as black alkene are connected with each other by weak Van der Waals force between layers, have lower shear strength, and layer
Interior tensile strength is higher, is therefore widely used in lube oil additive, and shows good property.In the microcosmic of friction
Field, friction pair between contact with each other, rolling friction macroscopically is changed into microcosmic sliding friction.The addition of nanosphere body,
It can avoid contacting with each other between friction pair in microscopic fields, sliding friction is changed into rolling friction.In conjunction with the above advantage
Fullerene structure nano material has high application value.
In the preparation of onion shape carbon ball, it usually needs harsh conditions are such as heat-treated nanogold under 2000 DEG C of hot conditions
Hard rock, plasma enhanced chemical vapor precipitation method etc..And dispersibility of the lubricating additive in lubricating oil is also to discuss to add
An important factor for adding agent superiority, traditional three-dimensional nanometer material are difficult to stablize in lubricating oil due to the effect of gravitational settling
Dispersion.Luo etc. has synthesized suspension graphene package sphere, since its laminated structure to suspend can resist gravity, does
To the stable dispersion in lubricating oil, thinking is provided for the stable dispersion of nano particle in the oil.
Summary of the invention
In view of the above existing problems in the prior art, the present invention provides a kind of SiC doping onion shapes to be graphitized carbon ball nanometer
Composite material has good dispersion performance and excellent anti-wear and wear-resistant performance in lubricating oil.
The present invention also provides the preparation method of SiC doping onion shape graphitization carbon ball nanocomposite and answer
With.
To achieve the goals above, a kind of SiC doping onion shape that the present invention uses is graphitized carbon ball nanocomposite,
The composite material includes fullerene structure onion shape carbon ball, and uniform doping SiC in situ and the growth of outer layer vertical direction is floating
Swim flake graphite alkene.
As an improvement, onion shape carbon ball carbonization structure sequence is stablized, outer layer by vertical growth the sheet stone that swims
Black alkene package, particle size are 200nm-1.2 μm.
In addition, the present invention also provides a kind of preparation method of SiC doping onion shape graphitization carbon ball nanocomposite,
Micro Polycarbosilane and petroleum ether wiring solution-forming are taken, the spray pyrolysis under high temperature inert atmosphere prepares size tunable and partial size point
The uniform SiC doping onion shape of cloth is graphitized carbon ball nanocomposite.
As an improvement, the temperature of the high-temperature spray pyrolysis is 1300 DEG C -1400 DEG C, the high temperature pyrolysis time is 1.5h-3h.
As an improvement, the preparation method of the SiC doping onion shape graphitization carbon ball nanocomposite, specifically includes step
It is rapid:
1) Polycarbosilane is dissolved in petroleum ether, prepares 0.1g-1.5g/10ml PCS/ petroleum ether solution in proportion, takes
50ml is added in atomizer；
2) control tube furnace is heated up in 40sccm to tube furnace with the heating rate of 5 DEG C/min, nitrogen gas velocity whole-process control
To 850 DEG C -1000 DEG C, Polycarbosilane/petroleum ether solution is fed, into tube furnace by way of atomizer spray with syringe pump
Polycarbosilane/petroleum ether solution is supplemented into atomizer, the constant temperature 1.5h after the completion of feeding is cooled to room temperature to tube furnace, takes
Product out.
As an improvement, the atomizer feed rate is 0.3ml/min；The injection flow rate pump is 0.3ml/min.
Moisten finally, the present invention also provides a kind of SiC doping onion shape graphitization carbon ball nanocomposites as nanometer
The application of sliding additive.
As an improvement, by SiC doping onion shape graphitization carbon ball nanocomposite according to the mass ratio of 0.01-0.05%
It is added in base oil PAO-4, prepares lubricating oil.
Compared with prior art, the beneficial effects of the present invention are:
1. traditional fullerene structure onion shape carbon ball nanocomposite, generallys use 2000 DEG C of high-temperature heat treatment nanogold
Hard rock or Plasma Enhanced Chemical Vapor method etc. are synthesized, and process conditions are harsh and process is uncontrollable.The present invention is using atomization
Enhance chemical vapor infiltration (i.e. atomizer and chemical vapor infiltration are combined), having expanded charge raw material, (gas, solubility are solid
Body, liquid etc.) and process is simple, condition is controllable.Each micro- liquid serves as an independent reactor and exists during the preparation process
Reaction in furnace, and the introducing of the solutes such as Polycarbosilane, change the reaction mechanism mechanism of reaction, and product morphology is promoted to develop to chondritic.
2. products therefrom of the present invention, there is outer layer the flake graphite alkene of vertical growth to wrap up.The laminated structure swum, can
Gravitational settling is resisted in dispersion process, therefore there is good dispersion performance.
3. gained SiC doping onion shape of the invention is graphitized carbon ball nanocomposite, as nanometer lubricating additive
In the process, it can be realized in microscopic fields and become sliding friction as rolling friction, there is good friction-reducing and antiwear action.
Detailed description of the invention
Fig. 1 is to prepare SiC in the embodiment of the present invention 1 to adulterate the process flow that onion shape is graphitized carbon ball nanocomposite
Schematic diagram.
Fig. 2 is that SiC adulterates the growth mechanism figure that onion shape is graphitized carbon ball nanocomposite in the embodiment of the present invention 1.
Fig. 3 is that SiC adulterates onion shape and is graphitized sweeping for carbon ball nanocomposite and comparative experiments in the embodiment of the present invention 1
Retouch electron microscope picture.
Fig. 4 is that SiC adulterates onion shape graphitization carbon ball nanocomposite transmission electron microscope in the embodiment of the present invention 1
Scheme (10000 times of amplification factor).
Fig. 5 is that SiC adulterates onion shape graphitization carbon ball nanocomposite for nano lubricating material in the embodiment of the present invention 1
The dispersion performance figure of material.
Fig. 6 is that SiC adulterates onion shape graphitization carbon ball nanocomposite for greasy property survey in the embodiment of the present invention 1
The coefficient of friction and wear scar diameter figure 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.
Embodiment 1
A kind of preparation method of SiC doping onion shape graphitization carbon ball nanocomposite, specifically includes step:
1) Polycarbosilane and petroleum ether are made into following ratio solution: 0.1g/10ml, 0.3g/10ml, 1.0g/10ml,
1.5g/10.ml, and control group (pure petroleum ether) is set, above-mentioned solution or petroleum ether are respectively placed in atomizer；
2) control tube furnace is heated up with the rate of 5 DEG C/min, and nitrogen gas velocity is controlled in 40sccm, 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
(Polycarbosilane/petroleum ether is homogeneous solution, and consumption is identical, flow velocity and atomizer frequency, flow rate of carrier gas, SOLUTION PROPERTIES
It is related, according to actual measurement convert flow velocity be 0.3ml/min), feed 3h, pass through syringe pump supplement raw material, the syringe pump
Flow velocity be 0.3mL/min, ejection of syringe pump 90min, after the completion of charging in 1300 DEG C of holdings 1.5h, press 5 DEG C/min later
After speed is cooled to 500 DEG C, Temperature fall is graphitized carbon ball nanocomposite up to SiC doping onion shape.
SiC doping onion shape graphitization carbon ball nanocomposite obtained includes that onion shape is graphitized carbon ball and original position
One doping SiC and outer layer swim flake graphite alkene, and the partial size of carbon ball is 200nm-1.5 μm.
Fig. 1 shows the preparation process of the technique, and Polycarbosilane/petroleum ether solution is atomized into the mist of uniform particle diameter by atomizer
Drop, droplet is with N2Carrier gas enters in furnace, and each droplet independent reaction is simultaneously deposited in furnace.Fig. 2 illustrates the growth of product
Journey, the solvent in the droplet of high-temperature region from surface evaporation and are diffused into ambient gas, and with the reduction of quantity of solvent, droplet is shunk
Volume is reduced.The evaporation of surface solvent causes the concentration on solute surface to increase, as the increase solute of surface concentration can satisfy
With, be precipitated on surface, the crystal of precipitation forms complete sphere in droplet surface and covers entire droplet, droplet in ball further
Condensation curing is changed into micro silicon carbide and sorts stable " onion carbon ball ", under the high temperature conditions in graphene growth process
In reduce with droplet surface carbon source, lead to graphene growth defect and the carbon source in ambient gas causes graphene from defect
In grown along other directions, and then result in surface and produce the flake graphite alkene that swims.
In order to which the effect to its growth mechanism and Polycarbosilane is further studied, we are to the pure stone for being added without Polycarbosilane
Oily ether liquid, Polycarbosilane/petroleum ether solution (0.1-1.5g/10ml Polycarbosilane/petroleum ether) of various concentration and one pot
Pyrolysis PCS/ petroleum ether is compared in method furnace.
Fig. 3 presents the scanning of pure petroleum ether, various concentration Polycarbosilane/petroleum ether solution and one kettle way feed product
(Fig. 3 a is pure petroleum ether control experiment to Electronic Speculum；Fig. 3 b-e is respectively 0.1g/10ml, 0.3g/10ml, 1.0g/10ml, 1.5g/
10ml Polycarbosilane/petroleum ether acquired solution；Fig. 3 f is to be pyrolyzed Polycarbosilane/petroleum ether solution using one kettle way).It can from figure
To find out that pure petroleum ether products therefrom as geometry irregular particle, and adds and regular spherical is presented after Polycarbosilane, and periphery
There are sheet packages, therefore Polycarbosilane has very big influence to product morphology.Compare atomized feed, the pyrolysis of Fig. 3 f one kettle way
Products therefrom geometry is irregular, is melted by several spherulas and agglomerating, therefore illustrates that atomizer atomized feed improves and reacted
Journey, when droplet carries out chemical gaseous phase deposition, each droplet independent reaction serves as a miniature reactor and independently carries out heat
Solve a series of processes such as polycondensation, product sedimentation.
Fig. 4 is the transmission electron microscope picture of 0.3g/10ml solution products therefrom, it can be seen from the figure that particle size about 200nm
Balling-up is wrapped up in onion shape and outer layer vertical growth goes out the flake graphite alkene that swims.
The dispersion performance of the nanometer lubricating additive is assessed by ultraviolet-visible spectrophotometer.First
SiC doping onion shape graphitization carbon ball nanocomposite in embodiment 1 is dispersed in by the basis PAO-4 using the method for ultrasound
In oil, and make the lubricating oil (0.01,0.025 and 0.05wt%) of various concentration.Gained lubricating oil ultrasonic disperse 40min
Afterwards, absorbance test is carried out, in the case where 600nm standing wave is long, records the absorbance of its 0-36h different time.
Fig. 5 illustrates the lubricating oil Relative Absorbance versus time curve of various concentration.As can be seen from Figure 5 every
The increase at any time of the Relative Absorbance of kind of lubricating oil and decline, but the fall of every kind of lubricating oil be it is different,
Therefore dispersed quality: 0.01wt% > 0.025wt% > 0.05wt% can be summed up.It is inhaled even if 0.05wt% lubricating oil is opposite
Luminosity fall decline compared to other concentration it is more obvious, but still kept after 36h higher horizontal (being greater than 0.4) and it
Trend afterwards tends towards stability, it can therefore be concluded that SiC doping onion shape graphitization carbon ball nanocomposite is as nano lubricating
Additive has good dispersion performance.
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.
The lubricating oil of above-mentioned different content SiC doping onion shape carbon ball nanocomposite, under by 30min test,
Show good anti-wear and wear-resistant performance.Fig. 6 presents coefficient of friction, wear scar diameter comparison diagram.
For the present invention using petroleum ether as carbon matrix precursor, micro Polycarbosilane (PCS) is used as structure directing agent, and PCS is dissolved
Stock dispersion is become the microlayer model of uniform particle diameter with atomizing type, is sent into tubular type by carrier gas by the wiring solution-forming in petroleum ether
Furnace, during which volume polycondensation occurs for each drop independent reaction, and the series reactions such as drop pyrolysis generate products therefrom.Wherein poly- carbon
Silane has the function of promotion product balling-up as structure directing agent, during the reaction steaming with surface solvent, solute
Concentration increases and then surface lolute crystallization is caused to be precipitated, and forms spherical shell, and reaction is limited to ball interior after being allowed to.
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 (8)
1. a kind of SiC doping onion shape is graphitized carbon ball nanocomposite, which is characterized in that the composite material includes fullerene
Structure onion shape carbon ball, and the flake graphite alkene that swims of uniform doping SiC and the growth of outer layer vertical direction in situ.
2. SiC adulterates onion shape and is graphitized carbon ball nanocomposite according to claim 1, which is characterized in that the ocean
The sequence of green onion shape carbon ball carbonization structure is stablized, and outer layer is wrapped up by the flake graphite alkene that swims of vertical growth, and particle size is
200nm-1.2μm。
3. a kind of preparation method of any one of claim 1-2 SiC doping onion shape graphitization carbon ball nanocomposite,
It is characterized in that, taking micro Polycarbosilane and petroleum ether wiring solution-forming, the spray pyrolysis under high temperature inert atmosphere, preparing partial size can
Control and particle diameter distribution it is uniform SiC doping onion shape be graphitized carbon ball nanocomposite.
4. SiC adulterates the preparation method of onion shape graphitization carbon ball nanocomposite according to claim 3, feature exists
In the temperature of the high-temperature spray pyrolysis is 1300 DEG C -1400 DEG C, and the high temperature pyrolysis time is 1.5h-3h.
5. SiC adulterates the preparation method of onion shape graphitization carbon ball nanocomposite according to claim 3, feature exists
In specific steps include:
1) Polycarbosilane is dissolved in petroleum ether, prepares 0.1g-1.5g/10ml PCS/ petroleum ether solution in proportion, takes 50ml
It is added in atomizer；
2) tube furnace is controlled with the heating rate of 5 DEG C/min, and nitrogen gas velocity whole-process control is warming up in 40sccm to tube furnace
850 DEG C -1000 DEG C, by way of atomizer spray into tube furnace feed Polycarbosilane/petroleum ether solution, with syringe pump to
Polycarbosilane/petroleum ether solution is supplemented in atomizer, the constant temperature 1.5h after the completion of feeding is cooled to room temperature to tube furnace, is taken out
Product.
6. SiC adulterates the preparation method of onion shape graphitization carbon ball nanocomposite according to claim 5, feature exists
In the atomizer feed rate is 0.3ml/min；The injection flow rate pump is 0.3ml/min.
7. described in a kind of any one of claim 1-2 or any one of the claim 3-6 preparation method is made SiC and adulterates onion
Shape is graphitized application of the carbon ball nanocomposite as nanometer lubricating additive.
8. application according to claim 7, which is characterized in that SiC doping onion shape is graphitized the nano combined material of carbon ball
Material is added in base oil PAO-4 according to the mass ratio of 0.01-0.05%, prepares lubricating oil.
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| CN114058075A (en) * | 2021-10-13 | 2022-02-18 | 河北大学 | Reed-based flame retardant and flame-retardant epoxy resin |
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