CN113355146A - Preparation method of graphene-loaded copper nanoparticles for lubricating oil additive - Google Patents
Preparation method of graphene-loaded copper nanoparticles for lubricating oil additive Download PDFInfo
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- CN113355146A CN113355146A CN202110677481.XA CN202110677481A CN113355146A CN 113355146 A CN113355146 A CN 113355146A CN 202110677481 A CN202110677481 A CN 202110677481A CN 113355146 A CN113355146 A CN 113355146A
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- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 44
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 43
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 31
- 239000010949 copper Substances 0.000 title claims abstract description 31
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 28
- 239000010687 lubricating oil Substances 0.000 title claims abstract description 19
- 239000000654 additive Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 230000000996 additive effect Effects 0.000 title claims abstract description 9
- 239000000243 solution Substances 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 24
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 20
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 20
- 239000008367 deionised water Substances 0.000 claims abstract description 18
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 18
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 14
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 14
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000005485 electric heating Methods 0.000 claims abstract description 8
- 238000009777 vacuum freeze-drying Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 6
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 6
- 239000000047 product Substances 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 6
- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 22
- 238000007710 freezing Methods 0.000 claims description 12
- 230000008014 freezing Effects 0.000 claims description 12
- 239000002243 precursor Substances 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000004108 freeze drying Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 238000003760 magnetic stirring Methods 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 230000005496 eutectics Effects 0.000 claims description 3
- 229910000366 copper(II) sulfate Inorganic materials 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 11
- 238000005054 agglomeration Methods 0.000 abstract description 6
- 230000002776 aggregation Effects 0.000 abstract description 6
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 6
- 239000000843 powder Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 241000446313 Lamella Species 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000003879 lubricant additive Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/04—Elements
- C10M2201/041—Carbon; Graphite; Carbon black
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/04—Elements
- C10M2201/05—Metals; Alloys
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
Abstract
The invention discloses a preparation method of graphene-loaded copper nanoparticles for a lubricating oil additive, which solves the problems that the particle size of graphene cannot be regulated and controlled and hard agglomeration phenomenon exists in the prior art. The invention comprises the following steps: 1. dispersing graphene oxide into deionized water, and performing ultrasonic treatment by using an ultrasonic cleaning machine to obtain an aqueous solution of the graphene oxide; 2. dissolving copper sulfate pentahydrate and polyethylene glycol in deionized water, performing ultrasonic treatment, mixing with the solution obtained in the step 1, and performing ultrasonic treatment; 3. mixing hydrazine hydrate and ammonia water into a concentrated ammonia solution of hydrazine hydrate, adding the concentrated ammonia solution into the solution prepared in the step (2), and carrying out water bath stirring treatment; 4. reacting the solution prepared in the step 3 in an electric heating constant temperature drying oven environment, and then naturally cooling; 5. washing the reaction product for many times by using deionized water and absolute ethyl alcohol; 6. and (4) putting the solution collected in the step (5) into a container, and performing vacuum freeze drying to obtain a target product.
Description
The technical field is as follows:
the invention belongs to the technical field of preparation of nano powder materials, and relates to a preparation method of graphene-loaded copper nanoparticles for a lubricating oil additive.
Background art:
nanomaterials exhibit unique physical and chemical properties due to their atomic size and surface effects, and have been extensively studied in the field of tribology. The nano material as the lubricating oil additive can greatly improve the tribological performance of the lubricating oil and has obvious effects on reducing energy consumption and protecting environment. The graphene has a thin nano-layered structure, high mechanical strength, low interlaminar shear strength, a weak layered stacking structure and other excellent physical and chemical properties, and can be used as a lubricating oil additive to greatly improve the anti-wear performance of lubricating oil, so that the graphene has great attention in the aspects of lubricating and reinforced material anti-wear performance research and the like. In recent years, it is found that the nano copper particles loaded on the surface of graphene can not only inhibit the secondary agglomeration of graphene nanosheets, but also exert the synergistic friction-reducing and wear-resisting effects with graphene to the greatest extent. At present, the preparation methods of graphene-loaded copper nanoparticles mainly comprise a thermal decomposition method, a chemical vapor deposition method, a hydrothermal method, a chemical reduction method and the like. The preparation method has certain disadvantages: the powder is easy to agglomerate, the grain diameter is difficult to control, and the grain diameter of the prepared powder particles is not uniform.
Patent documents with publication numbers CN103113958A and CN108559576 both disclose methods for preparing graphene-supported copper nanoparticles used as lubricant additives, but the particle size of the prepared graphene-supported copper nanoparticles is not controllable, and the prepared graphene-supported copper nanoparticles have a certain agglomeration.
The invention content is as follows:
the invention aims to provide a preparation method of graphene-loaded copper nanoparticles for a lubricating oil additive, which solves the problems that the particle size of graphene cannot be regulated and controlled and hard agglomeration phenomenon exists in the prior art, and the particle size of graphene-loaded copper nanoparticle powder prepared by the preparation method is controllable and has no hard agglomeration phenomenon.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of graphene loaded copper nanoparticles for a lubricating oil additive is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: dispersing 0.1-0.3 g of graphene oxide into deionized water according to the proportion of 1mg/mL, and performing ultrasonic treatment by using an ultrasonic cleaning machine to obtain an aqueous solution of the graphene oxide;
step two: dissolving 0.4g to 1.2g of blue vitriol and 0.01g to 0.03g of polyethylene glycol in a proper amount of deionized water, carrying out ultrasonic treatment for a certain time, mixing with the solution in the step one, and then carrying out ultrasonic treatment;
step three: mixing 3.5-10.5 mL of hydrazine hydrate and 7.0-21.0 mL of ammonia water into a concentrated ammonia solution of hydrazine hydrate, slowly adding the concentrated ammonia solution into the mixed solution prepared in the step two, and carrying out water bath stirring treatment in a magnetic stirring water bath;
step four: pouring the solution prepared in the step three into a high-pressure reaction kettle, reacting in an electric heating constant-temperature drying oven environment, and naturally cooling;
step five: and washing the reaction product for multiple times by using deionized water and absolute ethyl alcohol, wherein the solution obtained after washing is the precursor solution.
Step six: putting the solution collected in the fifth step into a container with the thickness of 3-8mm, and carrying out vacuum freeze drying, wherein the temperature of a water vapor condenser is below-50 ℃, the vacuum degree is below 0.5mbar, and the time is 10-15 h; and obtaining a target product after freeze-drying.
In the third step, the volume ratio of hydrazine hydrate to ammonia water is 1: 2.
Step six, before drying, putting the solution collected in the step five into a culture dish with the thickness of 3-8mm, and then putting the culture dish on a shelf of a vacuum freeze dryer; under the environment of vacuum low temperature, the temperature of the precursor solution is rapidly reduced to the eutectic point temperature of the solution.
In the first step, the ultrasonic treatment time is 60 min.
In the second step, the first ultrasonic treatment time is 20min, and the second ultrasonic treatment time is 15 min.
And in the fourth step, reacting for 3 hours in an electric heating constant-temperature drying oven at the temperature of 100 ℃, and then naturally cooling.
And step six, before drying, putting the solution collected in the step five into a culture dish according to the thickness of 3-8mm, respectively freezing by using liquid nitrogen, vacuumizing, and freezing at-20 ℃ in a refrigerator.
Compared with the prior art, the invention has the following advantages and effects:
1. according to the graphene-loaded copper nanoparticles prepared by the freeze-drying method, copper particles with the particle size of 100-200nm are uniformly attached to graphene, the transverse size of a graphene lamella is 0.7-4.4nm, the thickness of the graphene lamella is 2.8-3.2nm, and the particle size is uniform and controllable.
2. The invention is easy to disperse and has no hard agglomeration compared with other drying methods because the drying of the material is finished in a frozen state.
Description of the drawings:
FIG. 1 is an SEM electron micrograph of graphene-loaded copper nanoparticle powder;
FIG. 2 is an AFM photograph of nano-graphene loaded copper nanoparticle powder;
FIG. 3 is a graph of coefficient of friction versus time.
The specific implementation mode is as follows:
the present invention will be described in detail with reference to specific embodiments. These examples are intended to illustrate the invention and are not intended to limit the scope of the invention. The implementation conditions used in the examples can be further adjusted according to the specific experimental environment, and the implementation conditions not mentioned are generally the conditions in routine experiments.
Example 1
The method comprises the following steps: 0.1g of graphene oxide is dispersed into deionized water according to the proportion of 1mg/mL, and an ultrasonic cleaning machine is utilized to carry out ultrasonic treatment for 60min to obtain the aqueous solution of the graphene oxide.
Step two: dissolving 0.4g of blue vitriod and 0.01g of polyethylene glycol in deionized water, carrying out ultrasonic treatment for 20min, mixing with the solution in the step one, and carrying out ultrasonic treatment for 15 min.
Step three: and (3.5) mixing hydrazine hydrate and 7.0mL ammonia water to obtain a concentrated ammonia solution of hydrazine hydrate, slowly adding the concentrated ammonia solution into the mixed solution prepared in the step two, and carrying out water bath stirring treatment in a magnetic stirring water bath kettle.
Step four: pouring the solution prepared in the third step into a high-pressure reaction kettle, reacting for 3 hours in an electric heating constant-temperature drying oven at the temperature of 100 ℃, and naturally cooling.
Step five: and washing the reaction product for multiple times by using deionized water and absolute ethyl alcohol to obtain a solution, namely the precursor solution.
Step six: and (4) filling the solution collected in the fifth step into a culture dish with the thickness of 5mm, then pouring a proper amount of liquid nitrogen into the culture dish, and completely freezing the precursor solution at an extremely high speed in an environment of-196 ℃. And (3) carrying out vacuum freeze drying on the precursor frozen object in a freeze dryer, wherein the temperature of a water vapor condenser is below 50 ℃ below zero, and the vacuum degree is below 30 pa. And obtaining a target product after freeze-drying.
Example 2
The method comprises the following steps: 0.2g of graphene oxide is dispersed into deionized water according to the proportion of 1mg/mL, and an ultrasonic cleaning machine is utilized to carry out ultrasonic treatment for 60min to obtain the aqueous solution of the graphene oxide.
Step two: dissolving 0.8g of blue vitriod and 0.02g of polyethylene glycol in deionized water, carrying out ultrasonic treatment for 20min, mixing with the solution in the step one, and carrying out ultrasonic treatment for 15 min.
Step three: and (3) mixing 7.0mL of hydrazine hydrate and 14.0mL of ammonia water to obtain a concentrated ammonia solution of the hydrazine hydrate, slowly adding the concentrated ammonia solution into the mixed solution prepared in the step two, and carrying out water bath stirring treatment in a magnetic stirring water bath kettle.
Step four: pouring the solution prepared in the third step into a high-pressure reaction kettle, reacting for 3 hours in an electric heating constant-temperature drying oven at the temperature of 100 ℃, and naturally cooling.
Step five: and washing the reaction product for many times by using deionized water and absolute ethyl alcohol.
Step six: and (4) filling the solution collected in the fifth step into a culture dish with the thickness of 8mm, then putting the culture dish on a shelf of a vacuum freeze dryer, wherein the precursor solution can be quickly evaporated under the vacuum low-temperature environment, the evaporation is a heat absorption process, and a large amount of heat is taken away in the evaporation process, so that the temperature of the precursor solution is quickly reduced to the eutectic point temperature of the solution, the water contained in the solution is changed into ice, and the residual liquid is frozen. And (3) carrying out vacuum freeze drying on the precursor frozen object in a freeze dryer, wherein the temperature of a water vapor condenser is below 50 ℃ below zero, and the vacuum degree is below 30 pa. And obtaining a target product after freeze-drying.
Example 3
The method comprises the following steps: 0.2g of graphene oxide is dispersed into deionized water according to the proportion of 1mg/mL, and an ultrasonic cleaning machine is utilized to carry out ultrasonic treatment for 60min to obtain the aqueous solution of the graphene oxide.
Step two: dissolving 0.4g of blue vitriod and 0.02g of polyethylene glycol in deionized water, carrying out ultrasonic treatment for 20min, mixing with the solution in the step one, and carrying out ultrasonic treatment for 15 min.
Step three: and (3) mixing 7.0mL of hydrazine hydrate and 14.0mL of ammonia water to obtain a concentrated ammonia solution of the hydrazine hydrate, slowly adding the concentrated ammonia solution into the mixed solution prepared in the step two, and carrying out water bath stirring treatment in a magnetic stirring water bath kettle.
Step four: pouring the solution prepared in the third step into a high-pressure reaction kettle, reacting for 3 hours in an electric heating constant-temperature drying oven at the temperature of 100 ℃, and naturally cooling.
Step five: and washing the reaction product for many times by using deionized water and absolute ethyl alcohol.
Step six: putting the solution collected in the fifth step into a culture dish with the thickness of 3mm, and then putting the culture dish into a refrigerator to freeze at (-20 ℃); and (3) putting the precursor frozen substance into a freeze dryer for vacuum freeze drying, wherein the temperature of a water vapor condenser is below 50 ℃ below zero, and the vacuum degree is below 30 pa. And obtaining a target product after freeze-drying.
Experimental example:
fig. 1 shows an SEM photograph of the graphene-supported copper nanoparticles prepared by the vacuum freeze-drying method in example 1, from which it can be seen that the graphene sheet layers are substantially separated, a small amount of stacking exists, the surface has obvious wrinkles, and the nano copper particles with the particle size of 100-200nm are uniformly and dispersedly supported on the graphene sheet layers.
Fig. 2 shows AFM photographs of graphene-supported copper nanoparticles prepared by vacuum freeze-drying methods in examples 1, 2 and 3. Wherein, FIG. 2(a) shows sample 1 obtained under the condition that the freezing mode is liquid nitrogen freezing; FIG. 2(b) shows the freezing mode of sample 2 obtained under vacuum freezing conditions; FIG. 2(c) shows sample 3 obtained under freezing conditions at-20 ℃. It can be seen from the figure that the lateral dimensions and shapes of graphene in the graphene-loaded copper nanoparticles prepared by the three preparation processes are obviously different, the higher the freezing rate is, the smaller the lateral dimension of the graphene is, the larger the lateral dimension of the graphene-loaded copper nanoparticles prepared by freezing at-20 ℃ is, and the more complete the sheet layer is.
Fig. 3 shows the average friction coefficient of graphene-loaded copper nanoparticles as lubricant additives at different addition concentrations. The figure shows that the friction performance of the lubricating oil can be improved by adding a proper amount of graphene-loaded copper nanoparticles, and when the addition amount of the graphene-loaded copper nanoparticles is 0.10 wt%, the friction coefficient of an oil sample is minimum, and the lubricating oil has a better antifriction effect than that of a graphene single agent.
The above embodiment 3 is the most preferable embodiment.
The above embodiments are merely illustrative of the principles and effects of the present invention, and it will be apparent to those skilled in the art that various changes and modifications can be made without departing from the inventive concept of the present invention, and the scope of the present invention is defined by the appended claims.
Claims (7)
1. A preparation method of graphene loaded copper nanoparticles for a lubricating oil additive is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: dispersing 0.1-0.3 g of graphene oxide into deionized water according to the proportion of 1mg/mL, and performing ultrasonic treatment by using an ultrasonic cleaning machine to obtain an aqueous solution of the graphene oxide;
step two: dissolving 0.4g to 1.2g of blue vitriol and 0.01g to 0.03g of polyethylene glycol in a proper amount of deionized water, carrying out ultrasonic treatment for a certain time, mixing with the solution in the step one, and then carrying out ultrasonic treatment;
step three: mixing 3.5-10.5 mL of hydrazine hydrate and 7.0-21.0 mL of ammonia water into a concentrated ammonia solution of hydrazine hydrate, slowly adding the concentrated ammonia solution into the mixed solution prepared in the step two, and carrying out water bath stirring treatment in a magnetic stirring water bath;
step four: pouring the solution prepared in the step three into a high-pressure reaction kettle, reacting in an electric heating constant-temperature drying oven environment, and naturally cooling;
step five: and washing the reaction product for multiple times by using deionized water and absolute ethyl alcohol, wherein the solution obtained after washing is the precursor solution.
Step six: putting the solution collected in the fifth step into a container with the thickness of 3-8mm, and carrying out vacuum freeze drying, wherein the temperature of a water vapor condenser is below-50 ℃, the vacuum degree is below 0.5mbar, and the time is 10-15 h; and obtaining a target product after freeze-drying.
2. The method for preparing graphene-supported copper nanoparticles for lubricating oil additives according to claim 1, wherein: in the third step, the volume ratio of hydrazine hydrate to ammonia water is 1: 2.
3. The method for preparing graphene-supported copper nanoparticles for lubricating oil additives according to claim 1, wherein: step six, before drying, putting the solution collected in the step five into a culture dish with the thickness of 3-8mm, and then putting the culture dish on a shelf of a vacuum freeze dryer; under the environment of vacuum low temperature, the temperature of the precursor solution is rapidly reduced to the eutectic point temperature of the solution.
4. The method for preparing graphene-supported copper nanoparticles for lubricating oil additives according to claim 1, wherein: in the first step, the ultrasonic treatment time is 60 min.
5. The method for preparing graphene-supported copper nanoparticles for lubricating oil additives according to claim 1, wherein: in the second step, the first ultrasonic treatment time is 20min, and the second ultrasonic treatment time is 15 min.
6. The method for preparing graphene-supported copper nanoparticles for lubricating oil additives according to claim 1, wherein: and in the fourth step, reacting for 3 hours in an electric heating constant-temperature drying oven at the temperature of 100 ℃, and then naturally cooling.
7. The method for preparing graphene-supported copper nanoparticles for lubricating oil additives according to claim 1, wherein: and step six, before drying, putting the solution collected in the step five into a culture dish according to the thickness of 3-8mm, respectively freezing by using liquid nitrogen, vacuumizing, and freezing at-20 ℃ in a refrigerator.
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