CN113512449A - Composite lubricating material and preparation method thereof - Google Patents
Composite lubricating material and preparation method thereof Download PDFInfo
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- CN113512449A CN113512449A CN202110779791.2A CN202110779791A CN113512449A CN 113512449 A CN113512449 A CN 113512449A CN 202110779791 A CN202110779791 A CN 202110779791A CN 113512449 A CN113512449 A CN 113512449A
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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
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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
- C10M2201/06—Metal compounds
- C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
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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 belongs to the technical field of materials, and particularly relates to a composite lubricating material and a preparation method thereof. The method comprises the steps of preparing graphene oxide with manganese hydroxide nanoparticles attached to the surface under a strong alkaline condition by using potassium permanganate and concentrated sulfuric acid as oxidants in a water bath heating environment; dissolving the graphene oxide lamella attached with the manganese hydroxide nanoparticles and the strong base particles in absolute ethyl alcohol simultaneously to obtain a suspension; placing the suspension in a vacuum drying oven for evaporation treatment to obtain a graphene oxide lamella activated by strong alkali; and under the atmosphere of protective gas, placing the activated graphene oxide sheet layer in a tubular furnace for high-temperature calcination treatment, washing, filtering and vacuum drying to obtain the graphene loaded manganese oxide composite material. The method has the advantages of simple operation route, high and stable yield, and the obtained graphene loaded manganese oxide composite material has good lubricating and antifriction effects and can be applied to the fields of automobile industry, aerospace and the like.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a composite lubricating material, and particularly relates to a preparation method of the composite lubricating material.
Background
In all mechanical systems involving moving parts, there are problems of friction and wear of the interface. According to incomplete statistics, the annual energy loss due to friction accounts for 32% of the global energy consumption. Improving interfacial lubrication performance is the most direct way to improve the friction and wear resistance of mechanical systems. At present, the methods for improving the lubricating performance of the interface mainly comprise: self-lubricating coating, wear-resistant coating, surface strengthening treatment, surface texturing treatment, lubricating medium modification and the like.
Currently, the use of nano-lubricating additives is the most straightforward and effective method in modifying lubricating media. With the continuous deepening of the global green sustainable development concept, extremely strict requirements are put forward on the harmless treatment and the degradable property of the lubricating medium. The use of conventional wear and corrosion resistant additives containing harmful elements such as phosphorus and sulfur, as represented by zinc dialkyldithiophosphates (ZDDPs), is greatly limited.
Therefore, there is a need to develop a composite lubricating material that is environmentally friendly and has an excellent lubricating and friction reducing effect.
Disclosure of Invention
The present invention is based on the discovery and recognition by the inventors of the following facts and problems:
the graphene has ultrahigh normal bearing capacity, the theoretical Young modulus can reach 1Tpa, and the graphene has extremely low interlaminar shear stress and excellent heat conductivity, so that the graphene has great application prospect in the field of lubrication. However, the graphene sheet layer has stable chemical properties and is not easily adsorbed to form a film on the friction interface, so the effect of improving the abrasion resistance of the interface is to be improved. In addition, for graphene oxide, due to the fact that a large number of oxygen-containing functional groups with active properties are contained, the graphene sheet layers are prone to aggregation in a lubricating medium, and the lubricating and antifriction effects of graphene are greatly influenced. Therefore, the graphene is used as a carrier, and the surface of the graphene is loaded with nano particles, so that the chemical adsorption property between the graphene and a friction interface is enhanced, the lubricating property is improved, and the graphene is a research direction in the lubricating field.
The invention aims to provide a preparation method of a composite lubricating material, which comprises the steps of preparing graphene oxide with manganese hydroxide nanoparticles loaded on the surface in a strong alkaline environment by taking potassium permanganate and concentrated sulfuric acid as oxidants; the graphene oxide lamella is tightly coated by using excessive strong base solute, so that cavitation damage to the lamella caused by gas generated in the subsequent high-temperature calcination process is avoided; under the protection of inert gas or in a vacuum environment, reducing graphene oxide by using high-temperature heat, and decomposing manganese hydroxide nanoparticles to form manganese oxide particles. The preparation method has high repeatability, simple process and short production period, and the prepared composite lubricating material has excellent lubricating and antifriction effects.
The embodiment of the invention provides a composite lubricating material which is composed of graphene nanosheets and nano manganese oxide particles dispersed on the surfaces of the graphene nanosheets, wherein the graphene nanosheets are 5-10 nanometers thick, and the manganese oxide particles have an average particle size of 50-100 nanometers.
The embodiment of the invention provides a preparation method of a composite lubricating material, which comprises the following steps:
(1) mixing potassium permanganate and graphite powder into a sulfuric acid solution, heating to perform oxidation reaction to obtain a mixed solution containing graphene oxide;
(2) adding deionized water into the mixed solution containing graphene oxide in the step (1), adding a hydrogen peroxide solution, and stirring the mixed solution;
(3) adding an alkali solution into the mixed solution stirred in the step (2), and then filtering, washing and drying to obtain a graphene oxide sheet layer with the surface loaded with manganese hydroxide particles;
(4) dissolving the graphene oxide lamella obtained in the step (3) and solid alkali in an alcohol solution to obtain a suspension;
(5) evaporating the suspension obtained in the step (4) to obtain an alkali-activated graphene oxide lamella;
(6) and under the protection of inert gas or vacuum, carrying out high-temperature reduction treatment on the graphene oxide sheet layer after alkali activation, washing, filtering and drying to obtain the graphene-loaded manganese oxide nanoparticle composite lubricating material.
The preparation method of the composite lubricating material has the advantages that:
1. according to the method provided by the embodiment of the invention, manganese element is introduced in the graphene oxide preparation process, the graphene loaded manganese oxide nanoparticle composite lubricating material is prepared in situ by a high-temperature calcination method, the graphene is not required to be prepared first and then the manganese element is not required to be additionally introduced, the process is simple, the production period is short, the repeatability is high, and the large-scale industrial production is facilitated.
2. According to the method provided by the embodiment of the invention, before the graphene oxide with the manganese hydroxide loaded on the surface is calcined, the graphene sheet layer is coated with the strong alkaline solute. On one hand, the coating effect of the strong base solute is beneficial to reducing the cavitation effect of gas products generated in the calcining process on the graphene sheet layer and improving the surface quality; on the other hand, OH produced by pyrolysis of strongly basic solutes-And metal ions enter between graphene sheet layers, so that the sheet spacing is increased, and the graphene stripping degree is improved.
3. The graphene loaded manganese oxide nanoparticle composite lubricating material prepared by the method disclosed by the embodiment of the invention is composed of graphene nanosheets and nano manganese oxide particles dispersed on the surfaces of the graphene nanosheets, wherein the thickness of each graphene nanosheet is 5-10 nanometers, and the average particle size of the manganese oxide particles is about 50-100 nanometers.
4. According to the graphene loaded manganese oxide nanoparticle composite lubricating material prepared according to the embodiment of the invention, the unique two-dimensional structure and excellent lubricating property of graphene are fully utilized, and the hardness and chemical stability of manganese oxide particles are combined, so that excellent lubricating and antifriction effects are obtained, the lubricating effect of a lubricating medium under extreme working conditions such as high temperature, heavy load and high speed is remarkably improved, and the graphene loaded manganese oxide nanoparticle composite lubricating material has a wide application prospect in the fields of aerospace, mining machinery, military equipment and the like.
In some embodiments, in step (1), graphite powder, sulfuric acid, and potassium permanganate are mixed under ice bath conditions; the mass ratio of the graphite powder to the sulfuric acid to the potassium permanganate is as follows: graphite powder, sulfuric acid, potassium permanganate, 1, (20-40) and (3-5); the temperature of the oxidation reaction is 30-50 ℃, and the reaction time is 60-80 minutes; the particle size of the graphite powder is 1200-1800 meshes, and the mass concentration of the sulfuric acid is 95-98%.
In some embodiments, in the step (2), the mass ratio of deionized water to graphite powder is (80-100): 1, the mass concentration of the hydrogen peroxide solution is 30-50%, and the hydrogen peroxide solution is added until the mixed solution becomes golden yellow completely; the stirring time is 80-120 minutes.
In some embodiments, in the step (3), the alkali solution is at least one selected from a potassium hydroxide aqueous solution, a sodium hydroxide aqueous solution or a lithium hydroxide aqueous solution, and after the alkali solution is added, the pH value of the mixed solution is 10-13.
In some embodiments, in the step (4), the alcohol solution is one of methanol, ethanol or propanol; the mass ratio of the graphene oxide sheet layer to the solid alkali to the alcohol solution is (8-24) to (26-32), wherein the solid alkali is at least one selected from potassium hydroxide, sodium hydroxide or lithium hydroxide.
In some embodiments, in the step (5), a vacuum drying oven is used for evaporation treatment, the temperature of the evaporation treatment is 100-180 ℃, and the time of the evaporation treatment is 8-16 hours.
In some embodiments, in the step (6), the inert gas is nitrogen, argon or helium, the gas flow rate is 400-600 mL/min, and the vacuum degree under the vacuum condition is 50-100 Pa.
In some embodiments, in the step (6), the temperature of the reduction treatment is 400 to 700 ℃, and the reduction time is 4 to 7 hours.
The embodiment of the invention also provides a composite lubricating material prepared by the method according to the embodiment of the invention.
According to the composite lubricating material disclosed by the embodiment of the invention, the composite lubricating material is composed of graphene nanosheets and nano manganese oxide particles dispersed on the surfaces of the graphene nanosheets, wherein the thickness of the graphene nanosheets is 5-10 nanometers, and the average particle size of the manganese oxide particles is 50-100 nanometers.
The composite lubricating material provided by the embodiment of the invention has the following advantages:
1. according to the composite lubricating material disclosed by the embodiment of the invention, due to the intercalation of the manganese oxide particles among graphene sheet layers, the interlayer distance and the stripping degree of the graphene sheet layers are greatly increased, and the dispersion stability and uniformity of the lubricating material in a lubricating medium are enhanced.
2. According to the composite lubricating material disclosed by the embodiment of the invention, the unique two-dimensional structure and the excellent lubricating property of graphene are fully utilized, and the hardness and the chemical stability of manganese oxide particles are combined, so that the excellent lubricating and antifriction effects are obtained, the lubricating effect of a lubricating medium under extreme working conditions such as high temperature, heavy load and high speed is remarkably improved, and the composite lubricating material has great application prospects in the fields of aerospace, mining machinery, military equipment and the like.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It is obvious that the drawings in the following description are only some embodiments of the invention, and that for a person skilled in the art, other drawings can be derived from them without inventive effort.
Fig. 1 is an SEM scanning electron microscope image of the graphene-supported manganese oxide nanoparticle composite lubricating material prepared in example 1 of the present invention, where fig. a is an overall morphology view of composite graphene, and fig. b is a partially enlarged view of manganese oxide nanoparticles on the surface of a composite graphene sheet.
Fig. 2 is a Raman spectrum image of the graphene-supported manganese oxide nanoparticle composite lubricating material prepared in example 1 of the present invention.
Fig. 3 is an X-ray polycrystalline diffraction pattern of the graphene-supported manganese oxide nanoparticle composite lubricating material prepared in example 1 of the present invention.
Fig. 4 is a tribological performance graph of the composite lubricating material of graphene-supported manganese oxide nanoparticles prepared in example 1 of the present invention and a related comparative material.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
(1) Mixing potassium permanganate and graphite powder into a sulfuric acid solution, heating to perform oxidation reaction to obtain a mixed solution containing graphene oxide;
(2) adding deionized water into the mixed solution containing graphene oxide in the step (1), adding a hydrogen peroxide solution, and stirring the mixed solution;
(3) adding an alkali solution into the mixed solution stirred in the step (2), and then filtering, washing and drying to obtain a graphene oxide sheet layer with the surface loaded with manganese hydroxide particles;
(4) dissolving the graphene oxide lamella obtained in the step (3) and solid alkali in an alcohol solution to obtain a suspension;
(5) evaporating the suspension obtained in the step (4) to obtain an alkali-activated graphene oxide lamella;
(6) and under the protection of inert gas or vacuum, carrying out high-temperature reduction treatment on the graphene oxide sheet layer after alkali activation, washing, filtering and drying to obtain the graphene-loaded manganese oxide nanoparticle composite lubricating material.
According to the preparation method of the composite lubricating material, the manganese element is introduced in the graphene oxide preparation process, the graphene loaded manganese oxide nanoparticle composite lubricating material is prepared in situ by a high-temperature calcination method, the graphene is not required to be prepared first, and then the manganese element is not required to be additionally introduced, so that the process is simpleThe production period is short, the repeatability is high, and the large-scale industrial production is facilitated; according to the method, before the graphene oxide with the manganese hydroxide loaded on the surface is calcined, the graphene sheet layer is coated with the strong alkali solute, so that on one hand, the coating effect of the strong alkali solute is beneficial to reducing the cavitation effect of a gas product generated in the calcining process on the graphene sheet layer, and the surface quality is improved; on the other hand, OH produced by pyrolysis of strongly basic solutes-And metal ions enter between the graphene sheet layers, so that the distance between the sheet layers is increased, and the stripping degree of the graphene is improved.
The graphene loaded manganese oxide nanoparticle composite lubricating material prepared by the method is composed of graphene nanosheets and nano manganese oxide particles dispersed on the surfaces of the graphene nanosheets, wherein the thickness of each graphene nanosheet is 5-10 nanometers, and the average particle size of the manganese oxide particles is about 50-100 nanometers; the graphene-loaded manganese oxide nanoparticle composite lubricating material prepared by the method provided by the invention fully utilizes the unique two-dimensional structure and excellent lubricating property of graphene, and combines the hardness and chemical stability of manganese oxide particles, so that an excellent lubricating and antifriction effect is obtained, the lubricating effect of a lubricating medium under extreme working conditions such as high temperature, heavy load and high speed is remarkably improved, and the graphene-loaded manganese oxide nanoparticle composite lubricating material has a wide application prospect in the fields of aerospace, mining machinery, military equipment and the like.
According to the preparation method of the composite lubricating material, in the step (1), graphite powder, sulfuric acid and potassium permanganate are mixed under an ice bath condition; the mass ratio of the graphite powder to the sulfuric acid to the potassium permanganate is as follows: graphite powder, sulfuric acid, potassium permanganate, 1, (20-40) and (3-5); the temperature of the oxidation reaction is 30-50 ℃, and the reaction time is 60-80 minutes; the particle size of the graphite powder is 1200-1800 meshes, and the mass concentration of the sulfuric acid is 95-98%. According to the method provided by the embodiment of the invention, the preferable mass ratio of the graphite powder, the sulfuric acid and the potassium permanganate is as follows: the graphite powder comprises (1), (25-35) and (3.5-4) potassium permanganate, and if the addition amount of the sulfuric acid and the potassium permanganate is too large, the surface defects of the graphene are too many, and the lubricating performance of the composite material is influenced.
According to the preparation method of the composite lubricating material, in the step (2), the mass ratio of deionized water to graphite powder is (80-100): 1, the mass concentration of the hydrogen peroxide solution is 30-50%, and the hydrogen peroxide solution is added until the mixed solution is completely golden yellow and is stopped; the stirring time is 80-120 minutes. The stirring purpose is two: firstly, the oxidation stripping degree of graphite is improved, and graphene with better lamellar quality is obtained; and secondly, sufficient reaction time is provided for hydrogen peroxide and permanganate to fully reduce excessive permanganate ions, so that the content of low-valence manganese elements in the solution is increased, and the manganese hydroxide adhesion effect under the subsequent strong alkali condition is improved.
According to the method provided by the embodiment of the invention, a large amount of deionized water is added to improve the dispersion uniformity of the solute; the hydrogen peroxide solution is added to reduce the excessive potassium permanganate to obtain low-valence manganese element.
In some embodiments, the alkali solution in the step (3) is at least one selected from a potassium hydroxide aqueous solution, a sodium hydroxide aqueous solution or a lithium hydroxide aqueous solution, and the alkali solution is added to adjust the pH value of the mixed solution to 10-13. Under the condition of an alkaline solution, the low-valence manganese element reduced by hydrogen peroxide in the mixed solution forms insoluble manganese hydroxide, and manganese hydroxide nanoparticles are formed on the surface of the graphene large sheet layer.
In some embodiments, in the step (4), the mass ratio of the graphene oxide lamella to the solid base to the absolute ethyl alcohol is 1 (8-24) to (26-32), wherein the solid base is at least one selected from potassium hydroxide, sodium hydroxide or lithium hydroxide. In the method, after the graphene oxide lamella with the surface loaded with the manganese hydroxide particles is obtained in the step (3), solid alkali particles are continuously added, the graphene lamella is coated with the strong alkali solute, the cavitation of gas generated in the subsequent calcining process on the graphene lamella is reduced under the coating action of the strong alkali solute, the surface quality is improved, and the strong alkali solute is at high temperature in the calcining processOH formed by decomposition-And metal ions can enter between graphene sheet layers, so that the distance between the sheet layers is increased, the stripping degree of the graphene is improved, the addition amount of solid alkali is further optimized, and the lubricating and anti-wear effects of the composite lubricating material are effectively improved. According to the method provided by the embodiment of the invention, the alcohols are used as the solvent, so that the dispersion uniformity of the graphene in the solvent can be increased, and the volatility of the solute can be improved.
In some embodiments, in the step (5), a vacuum drying oven is used for evaporation treatment, the temperature of the evaporation treatment is 100-180 ℃, and the time of the evaporation treatment is 8-16 hours. According to the method provided by the embodiment of the invention, the turbid liquid obtained in the step (4) is subjected to evaporation treatment, so that the strong base solute is used for activating the graphene oxide lamellar layer, the cavitation damage effect of a gas product generated in the subsequent calcination process on the graphene lamellar layer is favorably reduced under the coating of the strong base solute, and OH generated by high-temperature decomposition of the strong base solute in the calcination process is simultaneously reduced-And metal ions can enter between graphene lamella, so that the lamella spacing is increased, and the lubricating performance of the composite lubricating material is improved.
In some embodiments, in the step (6), the inert gas is nitrogen, argon or helium, the gas flow rate is 400 to 600 mL/min, the vacuum degree under the vacuum condition is 50 to 100Pa, the temperature of the reduction treatment is 400 to 700 ℃, and the reduction time is 4 to 7 hours. According to the method provided by the embodiment of the invention, the graphene oxide lamella activated by alkali is calcined at high temperature in an inert atmosphere or a vacuum environment, so that the composite lubricating material with excellent performance is prepared.
According to the composite lubricating material disclosed by the embodiment of the invention, due to the intercalation of the manganese oxide particles among graphene sheet layers, the interlayer distance and the stripping degree of the graphene sheet layers are greatly increased, and the dispersion stability and uniformity of the lubricating material in a lubricating medium are enhanced; the composite lubricating material provided by the invention fully utilizes the unique two-dimensional structure and excellent lubricating property of graphene, and combines the hardness and chemical stability of manganese oxide particles, so that an excellent lubricating and antifriction effect is obtained, the lubricating effect of a lubricating medium under extreme working conditions such as high temperature, heavy load and high speed is remarkably improved, and the composite lubricating material has a great application prospect in the fields of aerospace, mining machinery, military equipment and the like.
Specific examples of the method for producing the composite lubricating material according to the embodiment of the invention are described in detail below.
Example 1
(1) Under the ice-bath condition, 40 g of potassium permanganate solid is slowly and uniformly added into 300 g of concentrated sulfuric acid solution, and then 10 g of 1400-mesh graphite powder is slowly added; and then heating the water bath environment to 40 ℃, electromagnetically stirring, and carrying out heat preservation treatment for 60 minutes to obtain a mixed solution containing graphene oxide.
(2) Slowly adding 1000 ml of deionized water into the mixed solution containing the graphene oxide; after electromagnetic stirring for 10 minutes, dropwise adding a 50% hydrogen peroxide aqueous solution until the solution is completely golden yellow, and then performing electromagnetic stirring treatment on the mixed solution for 120 minutes.
(3) Slowly dropwise adding a sodium hydroxide aqueous solution with the mass concentration of 50% into the mixed solution after electromagnetic stirring until the pH value of the solution is 12; and then, carrying out suction filtration, washing and drying treatment on the mixed solution for multiple times to obtain a graphene oxide lamellar layer with the surface loaded with the manganese hydroxide particles.
(4) Simultaneously dissolving the graphene oxide lamella obtained in the step (3) and sodium hydroxide particles in an absolute ethyl alcohol solution to obtain a suspension containing the graphene oxide lamella; the mass ratio of the graphene oxide to the sodium hydroxide to the absolute ethyl alcohol is 1:12: 32.
(5) And (5) placing the suspension obtained in the step (4) in a vacuum drying oven at 120 ℃, and carrying out evaporation drying treatment for 12 hours to obtain the graphene oxide lamella activated by sodium hydroxide strong base.
(6) Under the protection of nitrogen, placing the paste obtained in the step (5) in a tube furnace at 600 ℃ for high-temperature reduction for 5 hours; and fully washing, filtering and drying the product after high-temperature reduction to obtain the graphene-loaded manganese oxide nanoparticle composite lubricating material.
Morphology and crystallography analysis were performed on the graphene-supported manganese oxide nanoparticle composite lubricating material prepared in example 1 using a TESCAN Magna field emission scanning electron microscope, an HR8001 Raman spectrometer, and a Bruker D8X-ray diffractometer, and the detection results are shown in fig. 1, fig. 2, and fig. 3, respectively. The figure 1 is an SEM (scanning electron microscope) morphology of the graphene-loaded manganese oxide nanoparticle composite material, wherein the size of a sheet layer of the composite graphene is 5-8 micrometers, and the particle size of manganese oxide particles is 50-100 nanometers. Fig. 2 is a Raman spectrum of the composite material, and it can be seen that the prepared composite lubricating material has typical characteristic D peak and G peak of graphene. FIG. 3 is an X-ray diffraction pattern of the composite material, and compared with the X-ray diffraction pattern (PDF #07-0230) of the graphene-loaded manganese oxide nanoparticle composite material and the standard manganese oxide, characteristic peaks of the two are completely matched, which proves that the manganese oxide nanoparticles exist in the composite material. Wherein, the 2 theta is 34.910 degrees, 40.547 degrees, 58.722 degrees, 70.176 degrees, 73.793 degrees and 87.767 degrees, which respectively correspond to the (111), (200), (220), (311), (222) and (400) crystal planes of the manganese oxide crystal.
The graphene-supported manganese oxide composite lubricating material (MnO # G) prepared in example 1 and a related comparison material were subjected to a tribological performance test, and the test results are shown in fig. 4 and table 1. The graphene loaded manganese oxide nanoparticle composite lubricating material prepared by the invention has excellent lubricating and antifriction properties.
Table 1 example 1 comparison of lubricating properties of graphene-loaded manganese oxide nanoparticle composites and other comparative materials
Note:
1. the commercial graphene is purchased from Nanjing Xiancheng nanotechnology Limited, and the size of a commercial graphene sheet layer is 5-10 mu m;
2. in the comparative material, commercial graphene + MnO refers to mechanical mixing of commercial graphene and commercial manganese oxide nanoparticles. The mixing mass ratio of the two is as follows: commercial graphene commercial manganese oxide particles are 9:1, wherein the particle size of the commercial manganese oxide is 50-60 nanometers.
3. The base grease was purchased from China petrochemical lubricating oil Co., Ltd., and was Shangbo No. 0 Universal grease.
4. The mass concentration of all the lubricating materials was 5 wt%.
Example 2
(1) Under the ice bath condition, slowly and uniformly adding 35 g of potassium permanganate solid into 250 g of concentrated sulfuric acid solution, and then slowly adding 10 g of 1400-mesh graphite powder; and then heating the water bath environment to 50 ℃, electromagnetically stirring, and carrying out heat preservation treatment for 60 minutes to obtain a mixed solution containing graphene oxide.
(2) Slowly adding 800 ml of deionized water into the mixed solution containing the graphene oxide; after electromagnetic stirring for 10 minutes, dropwise adding aqueous hydrogen peroxide solution with the mass concentration of 40% until the solution is completely golden yellow, and then performing electromagnetic stirring treatment on the mixed solution for 80 minutes.
(3) Slowly dropwise adding a sodium hydroxide aqueous solution with the mass concentration of 50% into the mixed solution after electromagnetic stirring until the pH value of the solution is 13; and then, carrying out suction filtration, washing and drying treatment on the mixed solution for multiple times to obtain a graphene oxide lamellar layer with the surface loaded with the manganese hydroxide particles.
(4) Simultaneously dissolving the graphene oxide lamella obtained in the step (3) and sodium hydroxide particles in an absolute ethyl alcohol solution to obtain a suspension containing the graphene oxide lamella; the mass ratio of the graphene oxide to the sodium hydroxide to the absolute ethyl alcohol is 1:16: 32.
(5) And (5) putting the suspension obtained in the step (4) into a vacuum drying oven at 120 ℃, and carrying out evaporation drying treatment for 12 hours to obtain the graphene oxide lamellar paste activated by sodium hydroxide strong base.
(6) Under the protection of nitrogen, placing the paste obtained in the step (5) in a tubular furnace at 500 ℃ for high-temperature reduction for 7 hours; and fully washing, filtering and drying the product after high-temperature reduction to obtain the graphene-loaded manganese oxide nanoparticle composite lubricating material.
The graphene-supported manganese oxide composite lubricating material (MnO # G) prepared in example 2 and a related contrast material were subjected to a tribological performance test, and the test results are shown in table 2. The graphene loaded manganese oxide nanoparticle composite lubricating material prepared by the invention has excellent lubricating and antifriction properties.
Table 2 example 2 comparison of lubricating properties of graphene-loaded manganese oxide nanoparticle composites and other comparative materials
Example 3
(1) Under the ice bath condition, 50 g of potassium permanganate solid is slowly and uniformly added into 400 g of concentrated sulfuric acid solution, and then 10 g of 1800-mesh graphite powder is slowly added; and then heating the water bath environment to 50 ℃, electromagnetically stirring, and carrying out heat preservation treatment for 70 minutes to obtain a mixed solution containing graphene oxide.
(2) Slowly adding 900 ml of deionized water into the mixed solution containing the graphene oxide; after electromagnetic stirring for 10 minutes, adding a hydrogen peroxide aqueous solution with the mass concentration of 30% dropwise until the solution is completely golden yellow, and then performing electromagnetic stirring treatment on the mixed solution for 100 minutes.
(3) Slowly dropwise adding a potassium hydroxide aqueous solution with the mass concentration of 40% into the mixed solution after electromagnetic stirring until the pH value of the solution is 11; and then, carrying out suction filtration, washing and drying treatment on the mixed solution for multiple times to obtain a graphene oxide lamellar layer with the surface loaded with the manganese hydroxide particles.
(4) Simultaneously dissolving the graphene oxide lamella obtained in the step (3) and potassium hydroxide particles in an absolute ethyl alcohol solution to obtain a suspension containing the graphene oxide lamella; the mass ratio of the graphene oxide to the sodium hydroxide to the absolute ethyl alcohol is 1:20: 32.
(5) And (5) putting the suspension obtained in the step (4) into a vacuum drying oven at 140 ℃, and carrying out evaporation drying treatment for 16 hours to obtain the graphene oxide lamellar paste activated by sodium hydroxide strong base.
(6) Under the protection of argon, placing the paste obtained in the step (5) in a tube furnace at 600 ℃ for high-temperature reduction for 7 hours; and fully washing, filtering and drying the product after high-temperature reduction to obtain the graphene-loaded manganese oxide nanoparticle composite lubricating material.
The graphene-supported manganese oxide composite lubricating material (MnO # G) prepared in example 3 and a related contrast material were subjected to a tribological performance test, and the test results are shown in table 3. The graphene loaded manganese oxide nanoparticle composite lubricating material prepared by the invention has excellent lubricating and antifriction properties.
Table 3 example 3 comparison of lubricating properties of graphene-loaded manganese oxide nanoparticle composites and other comparative materials
Example 4
(1) Under the ice bath condition, 30 g of potassium permanganate solid is slowly and uniformly added into 200 g of concentrated sulfuric acid solution, and then 10 g of 1800-mesh graphite powder is slowly added; and then heating the water bath environment to 30 ℃, electromagnetically stirring, and carrying out heat preservation treatment for 60 minutes to obtain a mixed solution containing graphene oxide.
(2) Slowly adding 800 ml of deionized water into the mixed solution containing the graphene oxide; after electromagnetic stirring for 10 minutes, dropwise adding a hydrogen peroxide aqueous solution with the mass concentration of 30% until the solution is completely golden yellow, and then performing electromagnetic stirring treatment on the mixed solution for 120 minutes.
(3) Slowly dropwise adding a lithium hydroxide aqueous solution with the mass concentration of 40% into the mixed solution after electromagnetic stirring until the pH value of the solution is 10; and then, carrying out suction filtration, washing and drying treatment on the mixed solution for multiple times to obtain a graphene oxide lamellar layer with the surface loaded with the manganese hydroxide particles.
(4) Simultaneously dissolving the graphene oxide lamella obtained in the step (3) and potassium hydroxide particles in an absolute ethyl alcohol solution to obtain a suspension containing the graphene oxide lamella; the mass ratio of the graphene oxide to the sodium hydroxide to the absolute ethyl alcohol is 1:24: 32.
(5) And (5) putting the suspension obtained in the step (4) into a vacuum drying oven at 180 ℃, and carrying out evaporation drying treatment for 8 hours to obtain the graphene oxide lamellar paste activated by sodium hydroxide strong base.
(6) Under the protection of helium, placing the paste obtained in the step (5) in a tube furnace at 700 ℃ for high-temperature reduction for 7 hours; and fully washing, filtering and drying the product after high-temperature reduction to obtain the graphene-loaded manganese oxide nanoparticle composite lubricating material.
The graphene-supported manganese oxide composite lubricating material (MnO # G) prepared in example 4 and a related contrast material were subjected to a tribological performance test, and the test results are shown in table 4. The graphene loaded manganese oxide nanoparticle composite lubricating material prepared by the invention has excellent lubricating and antifriction properties.
Table 4 example 4 comparison of lubricating properties of graphene-loaded manganese oxide nanoparticle composites and other comparative materials
Example 5
(1) Under the ice bath condition, slowly and uniformly adding 30 g of potassium permanganate solid into 300 g of concentrated sulfuric acid solution, and then slowly adding 10 g of 1200-mesh graphite powder; and then heating the water bath environment to 40 ℃, electromagnetically stirring, and carrying out heat preservation treatment for 60 minutes to obtain a mixed solution containing graphene oxide.
(2) Slowly adding 1000 ml of deionized water into the mixed solution containing the graphene oxide; after electromagnetic stirring for 10 minutes, adding a hydrogen peroxide aqueous solution with the mass concentration of 30% dropwise until the solution is completely golden yellow, and then performing electromagnetic stirring treatment on the mixed solution for 100 minutes.
(3) Slowly dropwise adding a mixed aqueous solution of sodium hydroxide and potassium hydroxide with the mass concentration of 40% into the mixed solution after electromagnetic stirring until the pH value of the solution is 12; and then, carrying out suction filtration, washing and drying treatment on the mixed solution for multiple times to obtain a graphene oxide lamellar layer with the surface loaded with the manganese hydroxide particles.
(4) Simultaneously dissolving the graphene oxide lamella obtained in the step (3) and potassium hydroxide particles in an absolute ethyl alcohol solution to obtain a suspension containing the graphene oxide lamella; the mass ratio of the graphene oxide to the sodium hydroxide to the absolute ethyl alcohol is 1:8: 32.
(5) And (5) putting the suspension obtained in the step (4) into a vacuum drying oven at 100 ℃, and carrying out evaporation drying treatment for 12 hours to obtain the graphene oxide lamellar paste activated by sodium hydroxide strong base.
(6) Under the protection of helium, placing the paste obtained in the step (5) in a tubular furnace at 500 ℃ for high-temperature reduction for 7 hours; and fully washing, filtering and drying the product after high-temperature reduction to obtain the graphene-loaded manganese oxide nanoparticle composite lubricating material.
The graphene-supported manganese oxide composite lubricating material (MnO # G) prepared in example 5 and a related contrast material were subjected to a tribological property test, and the test results are shown in table 5. The graphene loaded manganese oxide nanoparticle composite lubricating material prepared by the invention has excellent lubricating and antifriction properties.
Table 5 example 5 comparison of lubricating properties of graphene-loaded manganese oxide nanoparticle composites and other comparative materials
Example 6
(1) Under the ice bath condition, 30 g of potassium permanganate solid is slowly and uniformly added into 400 g of concentrated sulfuric acid solution, and then 10 g of 1400-mesh graphite powder is slowly added; and then heating the water bath environment to 40 ℃, electromagnetically stirring, and carrying out heat preservation treatment for 60 minutes to obtain a mixed solution containing graphene oxide.
(2) Slowly adding 1000 ml of deionized water into the mixed solution containing the graphene oxide; after electromagnetic stirring for 10 minutes, adding a hydrogen peroxide aqueous solution with the mass concentration of 30% dropwise until the solution is completely golden yellow, and then performing electromagnetic stirring treatment on the mixed solution for 80 minutes.
(3) Slowly dripping a sodium hydroxide aqueous solution with the mass concentration of 40% into the mixed solution after electromagnetic stirring until the pH value of the solution is 10; and then, carrying out suction filtration, washing and drying treatment on the mixed solution for multiple times to obtain a graphene oxide lamellar layer with the surface loaded with the manganese hydroxide particles.
(4) Simultaneously dissolving the graphene oxide lamella obtained in the step (3) and potassium hydroxide particles in an absolute ethyl alcohol solution to obtain a suspension containing the graphene oxide lamella; the mass ratio of the graphene oxide to the sodium hydroxide to the absolute ethyl alcohol is 1:12: 32.
(5) And (5) putting the suspension obtained in the step (4) into a vacuum drying oven at 140 ℃, and carrying out evaporation drying treatment for 12 hours to obtain the graphene oxide lamellar paste activated by sodium hydroxide strong base.
(6) Placing the paste obtained in the step (5) in a tubular furnace at 500 ℃ under the vacuum condition of 50Pa for high-temperature reduction for 7 hours; and fully washing, filtering and drying the product after high-temperature reduction to obtain the graphene-loaded manganese oxide nanoparticle composite lubricating material.
The graphene-supported manganese oxide composite lubricating material (MnO # G) prepared in example 6 and a related contrast material were subjected to a tribological property test, and the test results are shown in table 6. The graphene loaded manganese oxide nanoparticle composite lubricating material prepared by the invention has excellent lubricating and antifriction properties.
Table 6 example 6 comparison of lubricating properties of graphene-loaded manganese oxide nanoparticle composites and other comparative materials
Example 7
(1) Under the ice bath condition, 30 g of potassium permanganate solid is slowly and uniformly added into 400 g of concentrated sulfuric acid solution, and then 10 g of 1600-mesh graphite powder is slowly added; and then heating the water bath environment to 30 ℃, electromagnetically stirring, and carrying out heat preservation treatment for 60 minutes to obtain a mixed solution containing graphene oxide.
(2) Slowly adding 900 ml of deionized water into the mixed solution containing the graphene oxide; after electromagnetic stirring for 10 minutes, dropwise adding aqueous hydrogen peroxide solution with the mass concentration of 40% until the solution is completely golden yellow, and then performing electromagnetic stirring treatment on the mixed solution for 80 minutes.
(3) Slowly dripping a sodium hydroxide aqueous solution with the mass concentration of 40% into the mixed solution after the electromagnetic stirring until the pH value of the solution is 13; and then, carrying out suction filtration, washing and drying treatment on the mixed solution for multiple times to obtain a graphene oxide lamellar layer with the surface loaded with the manganese hydroxide particles.
(4) Simultaneously dissolving the graphene oxide lamella obtained in the step (3) and potassium hydroxide particles in an absolute ethyl alcohol solution to obtain a suspension containing the graphene oxide lamella; the mass ratio of the graphene oxide to the sodium hydroxide to the absolute ethyl alcohol is 1:18: 32.
(5) And (5) putting the suspension obtained in the step (4) into a vacuum drying oven at 160 ℃, and carrying out evaporation drying treatment for 14 hours to obtain the graphene oxide lamellar paste activated by sodium hydroxide strong base.
(6) Placing the paste obtained in the step (5) in a tubular furnace at 500 ℃ under the vacuum condition of 80Pa for high-temperature reduction for 7 hours; and fully washing, filtering and drying the product after high-temperature reduction to obtain the graphene-loaded manganese oxide nanoparticle composite lubricating material.
The graphene-supported manganese oxide composite lubricating material (MnO # G) prepared in example 7 and a related comparative material were subjected to a tribological property test, and the test results are shown in table 7. The graphene loaded manganese oxide nanoparticle composite lubricating material prepared by the invention has excellent lubricating and antifriction properties.
Table 7 example 7 comparison of lubricating properties of graphene-loaded manganese oxide nanoparticle composites and other comparative materials
Example 8
(1) Under the ice bath condition, 30 g of potassium permanganate solid is slowly and uniformly added into 300 g of concentrated sulfuric acid solution, and then 10 g of 1800-mesh graphite powder is slowly added; and then heating the water bath environment to 30 ℃, electromagnetically stirring, and carrying out heat preservation treatment for 60 minutes to obtain a mixed solution containing graphene oxide.
(2) Slowly adding 900 ml of deionized water into the mixed solution containing the graphene oxide; after electromagnetic stirring for 10 minutes, dropwise adding a 40% hydrogen peroxide aqueous solution until the solution is completely golden yellow, and then performing electromagnetic stirring treatment on the mixed solution for 120 minutes.
(3) Slowly dripping a sodium hydroxide aqueous solution with the mass concentration of 40% into the mixed solution after electromagnetic stirring until the pH value of the solution is 10; and then, carrying out suction filtration, washing and drying treatment on the mixed solution for multiple times to obtain a graphene oxide lamellar layer with the surface loaded with the manganese hydroxide particles.
(4) Simultaneously dissolving the graphene oxide lamella obtained in the step (3) and potassium hydroxide particles in an absolute ethyl alcohol solution to obtain a suspension containing the graphene oxide lamella; the mass ratio of the graphene oxide to the sodium hydroxide to the absolute ethyl alcohol is 1:18: 32.
(5) And (5) putting the suspension obtained in the step (4) into a vacuum drying oven at 180 ℃, and carrying out evaporation drying treatment for 12 hours to obtain the graphene oxide lamellar paste activated by sodium hydroxide strong base.
(6) Placing the paste obtained in the step (5) in a tubular furnace at 700 ℃ under the vacuum condition of 100Pa for high-temperature reduction for 5 hours; and fully washing, filtering and drying the product after high-temperature reduction to obtain the graphene-loaded manganese oxide nanoparticle composite lubricating material.
The graphene-supported manganese oxide composite lubricating material (MnO # G) prepared in example 8 and a related contrast material were subjected to a tribological property test, and the test results are shown in table 8. The graphene loaded manganese oxide nanoparticle composite lubricating material prepared by the invention has excellent lubricating and antifriction properties.
Table 8 example 8 comparison of lubricating properties of graphene-loaded manganese oxide nanoparticle composites and other comparative materials
Comparative example 1
The same procedure as in example 1 according to the invention, except that step (4) is eliminated.
The composite lubricating material obtained in comparative example 1 was subjected to a friction test, and the lubricating property data are shown in Table 9. It can be seen that the lubricating performance of the graphene-loaded manganese oxide nanoparticle material prepared by omitting the step (4) is slightly reduced, so that the step 4 is very important for the lubricating performance of the composite lubricating material. The reason for this is that: under the coating action of the strong base solute, the method is favorable for reducing the cavitation of gas generated in the subsequent calcining process on the graphene sheet layer and improving the surface quality, and OH generated by high-temperature decomposition of the strong base solute in the calcining process-And metal ions can enter between the graphene sheet layers, so that the distance between the graphene sheet layers is increased, the stripping degree of the graphene is improved, and the lubricating and anti-wear effects of the composite lubricating material are effectively improved.
Table 9 comparative example 1 comparison table of lubricating properties of graphene-supported manganese oxide nanoparticle composite and other comparative materials
Claims (10)
1. The composite lubricating material is characterized by consisting of graphene nanosheets and nano manganese oxide particles dispersed on the surfaces of the graphene nanosheets, wherein the graphene nanosheets are 5-10 nanometers thick, and the manganese oxide particles have an average particle size of 50-100 nanometers.
2. A preparation method of a composite lubricating material is characterized by comprising the following steps:
(1) mixing potassium permanganate and graphite powder into a sulfuric acid solution, heating to perform oxidation reaction to obtain a mixed solution containing graphene oxide;
(2) adding deionized water into the mixed solution containing graphene oxide in the step (1), adding a hydrogen peroxide solution, and stirring the mixed solution;
(3) adding an alkali solution into the mixed solution stirred in the step (2), and then filtering, washing and drying to obtain a graphene oxide sheet layer with the surface loaded with manganese hydroxide particles;
(4) dissolving the graphene oxide lamella obtained in the step (3) and solid alkali in an alcohol solution to obtain a suspension;
(5) evaporating the suspension obtained in the step (4) to obtain an alkali-activated graphene oxide lamella;
(6) and under the protection of inert gas or vacuum, carrying out high-temperature reduction treatment on the graphene oxide sheet layer after alkali activation, washing, filtering and drying to obtain the graphene-loaded manganese oxide nanoparticle composite lubricating material.
3. The method for preparing a composite lubricating material according to claim 2, wherein in the step (1), graphite powder, sulfuric acid and potassium permanganate are mixed under ice bath conditions; the mass ratio of the graphite powder to the sulfuric acid to the potassium permanganate is as follows: graphite powder, sulfuric acid, potassium permanganate, 1, (20-40) and (3-5); the temperature of the oxidation reaction is 30-50 ℃, and the reaction time is 60-80 minutes; the particle size of the graphite powder is 1200-1800 meshes, and the mass concentration of the sulfuric acid is 95-98%.
4. The preparation method of the composite lubricating material, according to the claim 2, characterized in that in the step (2), the mass ratio of the deionized water to the graphite powder is (80-100): 1, the mass concentration of the hydrogen peroxide solution is 30-50%, and the hydrogen peroxide solution is added until the mixed solution turns golden yellow completely and is stopped; the stirring time is 80-120 minutes.
5. The method for preparing a composite lubricating material according to claim 2, wherein in the step (3), the alkali solution is at least one selected from the group consisting of an aqueous potassium hydroxide solution, an aqueous sodium hydroxide solution and an aqueous lithium hydroxide solution, and after the alkali solution is added, the pH value of the mixed solution is 10 to 13.
6. The method for preparing a composite lubricating material according to claim 2, wherein in the step (4), the alcohol solution is one of methanol, ethanol or propanol; the mass ratio of the graphene oxide sheet layer to the solid alkali to the alcohol solution is (8-24) to (26-32), wherein the solid alkali is at least one selected from potassium hydroxide, sodium hydroxide or lithium hydroxide.
7. The method for preparing the composite lubricating material according to claim 2, wherein in the step (5), the evaporation treatment is performed by using a vacuum drying oven, the temperature of the evaporation treatment is 100-180 ℃, and the time of the evaporation treatment is 8-16 hours.
8. The method for preparing the composite lubricating material according to claim 2, wherein in the step (6), the inert gas is nitrogen, argon or helium, the gas flow rate is 400 to 600 mL/min, and the vacuum degree under the vacuum condition is 50 to 100 Pa.
9. The method for preparing the composite lubricating material according to claim 2, wherein in the step (6), the temperature of the reduction treatment is 400 to 700 ℃ and the reduction time is 4 to 7 hours.
10. A composite lubricating material, characterized in that it is produced by the method according to any one of claims 2 to 9.
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