CN107686761B - In-situ rapid preparation method of noctilucent algae-like graphene-coated silicon carbide microspheres - Google Patents
In-situ rapid preparation method of noctilucent algae-like graphene-coated silicon carbide microspheres Download PDFInfo
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- 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
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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
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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
- C10M2201/10—Compounds containing silicon
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- 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
- C10N2030/04—Detergent property or dispersant property
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- 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 an in-situ rapid preparation method of noctilucent algae-like graphene-coated silicon carbide microspheres, which comprises the following steps: dispersing silicon carbide particles in a liquid phase medium to form a suspension with a certain concentration; pulse laser with certain energy density is focused and then irradiates the suspension liquid, so that silicon carbide particles realize the growth of silicon carbide epitaxial graphene, the stripping of partial multilayer graphene sheets and the spheroidization of irregular particles in situ under the dual actions of photo-thermal of laser irradiation and rapid cooling of a surrounding liquid environment; and after irradiation, centrifuging, separating and pickling the suspension, and drying the obtained precipitate to obtain the noctilucent algae-like graphene-coated silicon carbide microspheres with high dispersibility. The method is simple to operate, the preparation can be completed under the room temperature condition of normal temperature and normal pressure, the cost is low, the product purity is high, and the obtained graphene-coated silicon carbide microspheres show excellent dispersion stability and wear-resistant and antifriction properties in lubricating oil.
Description
Technical Field
The invention relates to an in-situ rapid preparation method of noctilucent algae-shaped graphene-coated silicon carbide microspheres, in particular to a method for forming noctilucent algae-shaped graphene-coated silicon carbide microspheres in situ by irradiating silicon carbide powder with simple liquid-phase laser, and belongs to the technical field of preparation of micro-nano powder.
Background
Mechanical friction and abrasion commonly exist in modern industrial production and life, and the existence of the friction and the abrasion not only causes a large amount of energy loss, but also damages the surfaces of parts and seriously reduces the service life of the device. The appearance of the nano material provides a new choice for the development of the lubricating oil additive and attracts people's extensive attention. Two-dimensional layered materials, such as graphene and molybdenum disulfide, are easy to slip under the shearing action and have low friction coefficient, and can form a transfer film on the surface of a friction pair as a lubricating oil additive, so that the abrasion is effectively reduced; the one-dimensional spherical particles, such as diamond, alumina and silicon oxide, can be used as lubricating oil additives to effectively change sliding friction into rolling friction, play the role of a micro bearing and effectively reduce the friction coefficient. Therefore, the flaky material and the spherical particles are combined, the synergistic effect is fully exerted, and excellent wear resistance and friction reduction performance are achieved at the same time.
At present, the graphene used as the lubricating oil additive is mostly prepared by a modified Hummers method (tribologyleters, 2011, 41(1): 209-. Silicon carbide, also called carborundum, still functions as an effective rolling bearing under high load due to its ultra-high hardness, but because of its ultra-high melting point and stability, the currently prepared silicon carbide nanoparticles mostly have sharp corners or hollow structures (Chemical Communications,2014, 50(9): 1070 and 1073), which cause scratches on the surfaces of friction pairs and are not studied as lubricating oil additives. Therefore, the preparation method of the composite material of the flake graphene and the smooth spherical silicon carbide, which is economic, simple and effective, still belongs to the technical blank.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides an in-situ rapid preparation method of noctilucent algae-shaped graphene-coated silicon carbide microspheres, which is simple to operate, short in flow, less in time consumption and capable of rapidly forming noctilucent algae-shaped graphene-coated silicon carbide microspheres.
Aiming at the technical blank that graphene prepared by the existing chemical solvent method is difficult to disperse in lubricating oil, solid silicon carbide spherical particles are difficult to prepare and the graphene and the solid silicon carbide spherical particles are compounded to be used as lubricating oil additives, the invention firstly proposes that noctilucent algae-shaped graphene-coated silicon carbide microspheres with high dispersibility in oil are prepared by adopting a liquid-phase laser irradiation mode. The pulse laser can generate an extreme non-equilibrium environment of ultrahigh temperature and ultrahigh pressure instantly (nanosecond magnitude), so that the growth of silicon carbide epitaxial graphene, the stripping of partial multilayer graphene sheets and the spheroidization of irregular silicon carbide particles are realized in situ under the dual actions of photo-thermal of laser irradiation and rapid cooling of a surrounding liquid environment, and the high-dispersity noctilucent algae-like graphene-coated silicon carbide microspheres can be obtained at room temperature and room pressure. The method is simple to operate, the reaction is rapid, a high-temperature and high-pressure environment is not needed, the graphene is obtained by directly decomposing the silicon carbide, the graphene and the silicon carbide are firmly combined, the suspension dispersion stability of the composite particles in the oil is obviously improved by the strip-shaped graphene, and the defects of harsh and complex processes for independently preparing the graphene and the spherical silicon carbide particles, uneven mechanical mixing, easy agglomeration in the oil and the like are overcome.
The specific technical scheme of the invention is as follows:
an in-situ rapid preparation method of noctilucent algae-like graphene-coated silicon carbide microspheres is characterized by comprising the following steps:
(1) ultrasonically dispersing silicon carbide powder in a liquid phase medium to form a suspension;
(2) under the condition of room temperature, the suspension is irradiated by pulse laser, so that the growth of silicon carbide epitaxial graphene, the stripping of partial outer layer graphene sheets and the spheroidization of irregular silicon carbide particles are realized under the dual functions of photo-thermal of laser irradiation and rapid cooling of the surrounding liquid environment of silicon carbide nanoparticles;
(3) and after irradiation, centrifuging, separating and pickling the suspension, and drying the obtained precipitate to obtain the noctilucent algae-shaped graphene coated silicon carbide microspheres.
The raw material used by the invention is silicon carbide powder, the granularity of the powder is required to be less than 1 mu m, and the focused laser beam can completely irradiate the whole particle and can rapidly enter between friction pairs as a lubricating oil additive. The raw silicon carbide powder may be monocrystalline or polycrystalline; the shape can be rod-shaped or sheet-shaped; the concentration of the extract in liquid phase medium is 0.01-10mg mL-1And each particle can be irradiated by laser, and the decomposition of silicon carbide, the generation of graphene and the spheroidization of irregular silicon carbide particles are completed.
According to the method, the graphene-coated silicon carbide structure is formed through the combined action of the pulse laser and the liquid phase solvent. In selecting the liquid phase medium, it is ensured that the particles are stably suspended and dispersed in the solvent throughout the laser irradiation process. When water is used as a liquid phase medium, graphene-coated silicon carbide particles formed after laser irradiation for a period of time can float on the water surface, so that irradiation on particles under the water surface is blocked, and finally, the conversion of all silicon carbide particles cannot be guaranteed. When absolute ethyl alcohol is selected as a dispersion medium, the dispersion medium can be completely and uniformly dispersed in a liquid phase medium from the beginning to the end of irradiation, so that uniform noctilucent algae-shaped graphene coated silicon carbide microspheres can be obtained.
In the step (2), the working parameters of the pulse laser are as follows: wavelength less than 310nm, frequency of 2-15Hz, and energy density of 0.4-1.8J pulse-1cm-2The irradiation time is 1-120 min. In a specific embodiment of the present invention, the pulsed laser beam is formed by: laser beams are emitted by a laser, then are focused by a reflector and a convex lens to form pulse laser beams with required light spot sizes, and the pulse laser beams are adjusted to required working parameters, so that the suspension dispersion liquid can be irradiated.
Preferably, in the step (2), the wavelength of the pulse laser is 193 nm, 248 nm, or 308 nm.
Preferably, in the step (2), the energy density of the pulse laser is 0.8 to 1.2J pulse-1cm-2。
Preferably, in the step (2), the better product can be obtained after the pulsed laser irradiation is carried out for 5-30 min.
Further, in order to make the irradiation more uniform, the suspension dispersion liquid is subjected to pulse laser irradiation under stirring, and the stirring speed is more than 200r min-1。
Further, in order to remove silicon particles obtained by decomposing silicon carbide, the centrifuged precipitate needs to be subjected to acid cleaning, and the acid solution used is a mixed acid solution comprising 5-10 wt% of hydrofluoric acid and 5-10 wt% of hydrogen peroxide.
According to the method, noctilucent algae-shaped graphene coated silicon carbide microspheres can be obtained, the core-shell structure improves the dispersion stability of composite particles in oil by using floating banded graphene, simultaneously gives full play to the advantages of two-dimensional layered materials and spherical particles as lubricating oil additives, shows excellent wear resistance and antifriction performance, and is added by about 0.06 wt%.
According to the invention, silicon carbide powder is dispersed in absolute ethyl alcohol to form a suspension, and the suspension is directly irradiated by a laser beam focused by a reflector and a convex lens, so that the silicon carbide powder in a solvent instantly obtains high energy (nanosecond level), is ablated and is rapidly cooled by the solution (nanosecond level), and the preparation of the noctilucent algae-shaped graphene coated silicon carbide microspheres is realized.
Compared with the prior art, the invention has the beneficial effects that: the preparation method is novel, the product purity is high, no impurity pollution is caused, and the obtained graphene-coated silicon carbide microspheres have excellent friction reducing and wear resisting properties in the friction process.
(1) The invention can be realized by only one step: in-situ epitaxial growth of graphene, stripping of partial graphene layers and spheroidization of irregular silicon carbide particles to obtain noctilucent algae-shaped graphene coated silicon carbide microspheres, and is simple to operate and low in preparation cost;
(2) the method can be suitable for the silicon carbide powder with different original appearances and different crystal forms, such as different appearances of blocks, rods and the like, different crystal forms of single crystals, polycrystal and the like, and has wide raw material selection range;
(3) in the preparation process, only laser irradiation is needed for the silicon carbide powder dispersed in the absolute ethyl alcohol, other redox atmospheres, reaction reagents and complex experimental devices are not needed, the conditions are easy to control, the process is simple, the cost is low, and the problems that the existing graphene preparation and silicon carbide spheroidization processes are complex and are difficult to apply to lubricating oil additives are solved;
(4) the product obtained by the method has high purity and no impurity pollution, the surface of the graphene-coated silicon carbide microsphere is provided with floating banded graphene which is like marine organism noctiluca, the graphene-coated silicon carbide microsphere can be stably dispersed in liquid, and can be quickly adsorbed to the surface of a friction pair when being used as a lubricating oil additive, and meanwhile, spherical particles can effectively change sliding friction into rolling friction, so that the double excellent performances of friction reduction and wear resistance are achieved.
Drawings
FIG. 1 is a transmission electron microscope image of a random silicon carbide powder feedstock;
FIG. 2 is a scanning electron microscope image of noctilucent algae-like graphene-coated silicon carbide microspheres formed after pulsed laser irradiation;
FIG. 3 is a transmission electron microscope image of noctilucent algae-like graphene-coated silicon carbide microspheres formed after pulsed laser irradiation;
FIG. 4 is a Raman spectrum of noctilucent algae-like graphene coated silicon carbide microspheres formed after pulsed laser irradiation;
FIG. 5 is a scanning electron microscope photograph of the product obtained in comparative example 1.
Detailed Description
The following examples are given for the purpose of illustrating the present invention, and are not to be construed as limiting the scope of the present invention.
Example 1
(1) Weighing 500 mg of nano silicon carbide powder (with the purity of 99.9 percent and the particle size of less than 0.04-0.2 mu m) in a beaker, adding 50 mL of absolute ethyl alcohol, and performing ultrasonic dispersion until no precipitate exists at the bottom of the beaker to form a uniform suspension;
(2) irradiating the suspension prepared in the step (1) with argon-fluorine laser beam (193 nm) focused by a reflector and a convex lens, wherein the laser energy density is 0.8J pulse-1cm-1The frequency is 2 Hz, and the irradiation time is 20 min. In the laser beam irradiation process, the magnetic stirrer is used for 300 r min-1Continuously stirring the suspension at a rotating speed;
(3) after the irradiation is finished, centrifuging the suspension, then washing the suspension for three times by using mixed acid liquid (5 wt% hydrofluoric acid and 5 wt% hydrogen peroxide) and deionized water respectively, and drying the powder to obtain the product.
FIG. 1 is a transmission electron microscope photograph of the raw silicon carbide powder in step (1), from which it can be seen that the morphology of the silicon carbide in the raw material is various and disordered. FIG. 2 is a scanning electron microscope image of the product obtained after irradiation, from which it can be seen that the product has a single morphology, is spherical and has a particle size of 0.1-0.2. mu.m. Fig. 3 is a transmission electron microscope image of the product obtained after irradiation, from which it can be seen that the silicon carbide microspheres are coated by graphene, and part of the graphene is stripped to form a floating belt-like structure, like marine organism noctiluca, so that a large suspending force is shown in the liquid, and the silicon carbide microspheres can be stably dispersed in the lubricating oil.
Fig. 4 is a raman spectrum of the graphene-coated silicon carbide particles obtained after irradiation, and from three characteristic peaks (D, G and 2D) in the spectrum, successful preparation of epitaxial graphene can be proved.
Example 2
(1) Weighing 250 mg of superfine silicon carbide powder (with the purity of 99 percent and the particle size of 0.5-0.7 mu m) into a beaker, adding 50 mL of absolute ethyl alcohol, and performing ultrasonic dispersion until no precipitate is left at the bottom of the beaker to form uniform suspension;
(2) irradiating the suspension prepared in the step (1) by krypton-fluorine laser beam (248 nm) focused by a reflector and a convex lens, wherein the laser energy density is 1.0J pulse-1cm-1The frequency is 10 Hz, and the irradiation time is 10 min. In the laser beam irradiation process, a magnetic stirrer is used for 700 r min-1Continuously stirring the suspension at a rotating speed;
(3) after the irradiation is finished, centrifuging the suspension, then washing the suspension for three times by using mixed acid liquid (10 wt% hydrofluoric acid and 10 wt% hydrogen peroxide) and deionized water respectively, and drying the powder to obtain the product. The morphology of the product obtained is similar to that of example 1, the particle size being from 0.3 to 0.5. mu.m.
Example 3
(1) Weighing 5 mg of nano silicon carbide powder (with the purity of 99.9 percent and the particle size of less than 0.04-0.2 mu m) into a beaker, adding 50 mL of absolute ethyl alcohol, and performing ultrasonic dispersion until no precipitate exists at the bottom of the beaker to form a uniform suspension;
(2) irradiating the suspension prepared in the step (1) by xenon-chlorine laser beams (308 nm) focused by a reflector and a convex lens, wherein the laser energy density is 1.2J pulse-1cm-1The frequency is 15Hz, and the irradiation time is 5 min. In the laser beam irradiation process, a magnetic stirrer is used for 1000 r min-1Continuously stirring the suspension at a rotating speed;
(3) after the irradiation is finished, centrifuging the suspension, then washing the suspension for three times by using mixed acid liquid (5 wt% hydrofluoric acid and 10 wt% hydrogen peroxide) and deionized water respectively, and drying the powder to obtain the product. The morphology of the product obtained is similar to that of example 1, the particle size being from 0.1 to 0.2. mu.m.
Example 4
(1) Weighing 100 mg of nano silicon carbide powder (with the purity of 99.9 percent and the particle size of less than 0.04-0.2 mu m) in a beaker, adding 50 mL of absolute ethyl alcohol, and performing ultrasonic dispersion until no precipitate exists at the bottom of the beaker to form a uniform suspension;
(2) irradiating the suspension prepared in the step (1) by krypton-fluorine laser beam (248 nm) focused by a reflector and a convex lens, wherein the laser energy density is 0.9J pulse-1cm-1The frequency is 8 Hz, and the irradiation time is 30 min. In the laser beam irradiation process, a magnetic stirrer is used for 1200 r min-1Continuously stirring the suspension at a rotating speed;
(3) after the irradiation is finished, centrifuging the suspension, then washing the suspension for three times by using mixed acid liquid (10 wt% hydrofluoric acid and 5 wt% hydrogen peroxide) and deionized water respectively, and drying the powder to obtain the product. The morphology of the product obtained is similar to that of example 1, the particle size being from 0.1 to 0.2. mu.m.
Comparative example 1
The method of example 1 was used to prepare graphene-coated silicon carbide microspheres except that: the silicon carbide particles used have a diameter of 0.4 to 3 μm. And after the irradiation is finished, centrifuging, separating, pickling and drying to obtain the product. The scanning electron microscope tests show that the obtained product has various particle shapes, large particles are still polygons with sharp corners and are difficult to be sphericized, and only particles with the particle size smaller than 1 mu m are converted into spheres, as shown in figure 5, the irregular particles serving as the lubricating oil additive are easy to scratch the surfaces of friction pairs.
Comparative example 2
The method of example 2 was used to prepare graphene-coated silicon carbide microspheres, except that: laser energy density of 0.2 Jpulse-1cm-1. And after the irradiation is finished, centrifuging, separating and pickling to obtain the product. The scanning electron microscope test of the obtained product shows that the shape of the silicon carbide particles is basically unchanged and still polygonal, which indicates that the laser energy is too low to melt the silicon carbide particles with high melting point into balls.
To verify the antifriction properties of the resulting product, the following experiment was performed.
1. Respectively adding the products prepared in the embodiments and the comparative examples into paraffin base oil, and carrying out friction performance test, wherein the addition amount is 0.06 wt% of the base oil;
2. the friction performance test method comprises the following steps: four-ball friction and wear test, and meanwhile, taking pure paraffin oil as a blank control;
3. and (6) obtaining the result. The results of the tribological tests on the various examples and comparative products are given in table 1 below.
TABLE 1
Therefore, the noctilucent algae-shaped graphene-coated silicon carbide microspheres prepared by the method have the advantages that the antifriction and wear resistance performance is well improved and is obviously higher than that of comparative products. The product performance is greatly influenced by the granularity and concentration of raw materials, parameters of laser irradiation and other conditions.
Claims (4)
1. An in-situ rapid preparation method of noctilucent algae-like graphene-coated silicon carbide microspheres is characterized by comprising the following steps:
(1) ultrasonically dispersing silicon carbide powder with the particle size of less than 1 mu m in absolute ethyl alcohol to form a silicon carbide powder with the concentration of 0.1-10mgmL-1The suspension of (a);
(2) under the condition of room temperature, selecting laser with wavelength less than 310nm, and focusing laser beam by convex lens to make laser energy density be 0.4-1.8J pulse-1cm-2Irradiating the suspension for 1-120min at the laser frequency of 2-15Hz, and realizing the growth of silicon carbide epitaxial graphene, the stripping of partial outer graphene sheets and the spheroidization of irregular particles by the silicon carbide nanoparticles under the dual actions of the photothermal of laser irradiation and the rapid cooling of the surrounding liquid environment;
(3) and after irradiation, centrifuging, separating and pickling the suspension, and drying the obtained precipitate to obtain the noctilucent algae-shaped graphene coated silicon carbide microspheres.
2. The method of claim 1, wherein: in the step (1), the silicon carbide particles are polycrystalline or single crystal.
3. According toThe method of claim 1, wherein: in the step (2), the suspension is irradiated by pulse laser under stirring, and the stirring speed is more than 200r min-1。
4. The method of claim 1, wherein: in the step (3), the acid cleaning is carried out by using a mixed acid solution which comprises 5-10 wt% of hydrofluoric acid and 5-10 wt% of hydrogen peroxide.
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