CN111394153A - Hexagonal boron nitride nanosheet base lubricating grease and preparation method thereof - Google Patents
Hexagonal boron nitride nanosheet base lubricating grease and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
- C10M125/20—Compounds containing nitrogen
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- C10M177/00—Special methods of preparation of lubricating compositions; Chemical modification by after-treatment of components or of the whole of a lubricating composition, not covered by other classes
Abstract
The invention discloses hexagonal boron nitride nanosheet base lubricating grease and a preparation method thereof. The preparation method comprises the following steps: mixing boron nitride powder and strong alkaline solution, placing the mixture in a homogeneous reaction kettle for hydrothermal reaction, inserting an intercalation agent into a boron nitride layer by an impregnation method, performing thermal expansion stripping in a tubular furnace, and finally performing combined stripping treatment to further enlarge the interlayer spacing by the material thermal expansion damage interlayer acting force in the microwave process and the liquid nitrogen rapid volatilization in the liquid nitrogen process to obtain the final hexagonal boron nitride nanosheet. The nano sheet obtained by the invention has obvious antifriction and antiwear performances as a lubricating additive, and compared with lubricating grease in a friction test, the hexagonal boron nitride nano sheet base lubricating grease has the advantages that the wear volume is reduced by 30-50%, and the friction coefficient is reduced by 40-60%.
Description
Technical Field
The invention belongs to a lubricating material preparation technology, and particularly relates to hexagonal boron nitride nanosheet-based lubricating grease and a preparation method thereof.
Background
Friction and wear are widely seen in everyday life and in various industrial applications, and play an important role in achieving optimum operation, and friction-induced wear can lead to various problems including surface damage and degradation of equipment performance and reliability. Due to friction and abrasion, about one third of the global disposable energy is wasted in the friction process, about 80% of mechanical parts lose efficacy due to friction and abrasion, so that the economic loss of industrialized countries reaches 5% -7% of GDP (if the loss caused by friction is about 3.75 trillion to 5.25 trillion RMB calculated according to about 75 trillion RMB of GDP in 2015 of China), the industrial production is greatly influenced, and lubrication is the most effective method for controlling friction and abrasion. Lubricant additives are effective methods for improving performance, and currently, most commonly used friction reducing additives such as ZDDP (zinc bis diphosphate), MPZ (molybdenum-phosphorus-zinc) magnetic friction reducing additives and the like worldwide have increasingly limited use due to their own defects, such as the problem of easy decomposition of ZDDP at high temperature and the problem of corrosion of copper metal, and some additives have insignificant friction reducing properties and do not provide optimal lubricity. In addition, most of the additives contain sulfur, phosphorus, chlorine and heavy metal elements, and thus the environmental stress is high.
The hexagonal boron nitride nanosheet solution obtained by using a water dispersion point (CQD) of a carbon quantum as a stripping agent and a stabilizer is recently reported by Zhang et al to be used as an aqueous lubricant, the friction coefficient of the hexagonal boron nitride nanosheet solution is as low as 0.02, and super-lubricity can be realized even under certain working conditions (ACS Appl. Mater. Interfaces.2016, DOI:10.1021/acsami.6b09752), L even if the heterogeneous structure of the hexagonal boron nitride/graphene obtained by CVD method by the inventor et al is also observed to be in a super-slippery state (J.Phys.chem. L et.2013, DOI:10.1021/jz301758c), the research has a landmark significance in the tribology field, B, N element in the hexagonal boron nitride is an important element of a traditional friction reducer, and the hexagonal boron nitride has no super-smooth surface by itself, the hexagonal boron nitride nano material has low atomic shear strength in the atomic shear surface, the hexagonal boron nitride can provide a low mechanical strength in the hexagonal boron nitride surface, the chemical shear surface, the hexagonal boron nitride, the chemical shear surface, the boron nitride has a high friction coefficient of a chemical friction coefficient of a nano-nitride, the chemical friction coefficient of which is reduced by the chemical friction of a chemical additive, and the chemical additive, the chemical additive is not reduced by the chemical property of a chemical additive, the chemical additive is not reduced by the chemical additive, the chemical additive is more than the chemical additive, the chemical additive is not reduced by the chemical additive, the chemical additive is not reduced by the chemical additive.
Disclosure of Invention
The invention aims to provide hexagonal boron nitride nanosheet base lubricating grease and a preparation method thereof.
The technical solution for realizing the purpose of the invention is as follows: a hexagonal boron nitride nanosheet base lubricating grease and a preparation method thereof, the method comprising the following steps:
(1) preparing an alkaline solution by using strong base as a raw material, and adding hexagonal boron nitride into the alkaline solution under the condition of vigorous stirring to obtain a white mixed solution;
(2) reacting the mixed solution in a homogeneous reaction kettle, and collecting and drying an obtained white sample after the reaction is finished;
(3) adding the intercalation agent into the sample obtained in the step (2) for 5-10 times by adopting an impregnation method, transferring the intercalation agent into a tubular furnace for reaction at the temperature of 600 ℃ and 800 ℃ for 6-12 hours, and collecting a gray sample with slightly expanded volume by a thermal expansion method after the reaction is finished;
(4) and (4) stripping the sample obtained in the step (3) by a microwave liquid nitrogen combination method, namely: placing a sample in a heat-resistant container, placing the heat-resistant container in a microwave oven, heating for a period of time, cooling to obtain fine white powder with reduced grayness, immersing the cooled sample in liquid nitrogen, reacting for 3-5 times, washing, and drying to obtain a white fluffy hexagonal boron nitride nanosheet;
(5) and (4) adding the hexagonal boron nitride nanosheet obtained in the step (4) into lubricating grease according to a certain proportion, and fully grinding to obtain a state of no obvious white particles and uniform color.
Preferably, in the step (1), the volume ratio of the solvents ethanol and deionized water in the alkaline solution is 1:1.
preferably, in the step (1), lithium hydroxide is used as strong base to prepare alkaline solution, the concentration of the alkaline solution is 0.12-0.17mg/ml, and the mass ratio of the strong base to the hexagonal boron nitride is 1: 1.5.
Preferably, in the step (2), the reaction temperature is 200-.
Preferably, in the step (3), the intercalation agent includes any one of urea, sodium bicarbonate, oxalic acid and the like, and the mass ratio of the intercalation agent to the hexagonal boron nitride is 3: 1.
Preferably, in the step (4), the power range of the microwave oven is 600-900W, the temperature is set at middle fire level or middle and high fire level when the microwave heating treatment is carried out, and the microwave treatment time is 0.5-1 hour.
Preferably, in the step (4), the volume of the liquid nitrogen immersed in each time is 50-100 ml.
Preferably, in the step (4), the size of the hexagonal boron nitride nanosheet is 300-800nm, and the thickness is 1.2-5.3 nm.
Preferably, in the step (5), the hexagonal boron nitride nanosheet obtained in the step (4) is added into lubricating grease according to the proportion of 0.05-0.15 wt.%; the time for full grinding in a mortar is 15-20 minutes.
Preferably, in the step (5), the grease includes any one of kunlun No. 2 white special grease, kunlun No. 3 white special grease, great wall No. 2 lithium-based grease, and the like.
Compared with the prior art, the invention has the advantages that:
1. low cost, avoids using toxic and harmful chemical reagents, and has no or little environmental pollution.
2. The invention solves the problem that the production of the hexagonal boron nitride nanosheet is difficult to scale, and is suitable for large-scale production.
3. The hexagonal boron nitride nanosheet prepared by the method has excellent dispersibility and stability, is excellent in macroscopic antifriction and wear resistance when being used as a lubricating additive, can be directly used as the lubricating additive without secondary treatment, and can greatly reduce the friction coefficient of lubricating grease.
4. The nanosheet obtained by the method is simple to operate from preparation to use as a lubricating additive, has high-efficiency process and has high application value.
Drawings
Fig. 1 is a picture of the back-and-forth friction curves of the blank grease of example 2 and the obtained boron nitride nanosheets.
Fig. 2 is a photograph of the frictional wear of the boron nitride nanosheets obtained in example 2.
Detailed Description
The invention is further illustrated with reference to the figures and the specific embodiments.
In the following examples, Kunlun No. 2 white specialty grease, Kunlun No. 3 white specialty grease were obtained from China Petroleum lubricating oil, and great wall No. 2 lithium-based grease was obtained from China petrochemical lubricating oil, using a microwave oven model of Greenwich microwave oven (P70D20N1P), using a medium fire grade.
Example 1, lithium hydroxide is used as a raw material, ethanol and deionized water are added into an alkaline solution according to a volume ratio of 1:1 to prepare an alkaline solution, the concentration of the lithium hydroxide solution is controlled to be 0.12mg/ml, 1 kg of hexagonal boron nitride is added into the alkaline solution under the condition of vigorous stirring to obtain a mixed solution, the mixed solution is reacted in a reaction kettle at 300 ℃ for 2 hours, the temperature rise rate is 100 ℃/h, the rotation rate is 18rpm/min, after the reaction is finished, a sample is collected and dried, 3 kg of urea is added into the collected sample as an intercalation agent, the sample is transferred into a tube furnace to be heated to 600 ℃ to react for 6 hours and then collected, the collected sample is placed into a Glassy microwave oven (P70D20N1P) for natural cooling after being heated for 1 hour at a medium fire gear, the cooled sample is immersed into 10L for reaction and then washed, the hexagonal boron nitride nanosheet is dried to obtain a hexagonal boron nitride nanosheet, the collected boron nitride nanosheet is added into Kunlun No. 2 white lubricating grease with an addition amount of 0.05 wt%, the boron nitride nanosheet is fully ground for 15 minutes, the boron nanosheet in a state, and a friction curve of a boron nitride nanosheet and a reciprocating friction test graph, wherein the boron nitride graph.
The size of the nano-sheet obtained by the method is 300-800nm, the thickness is 1.2-5.3nm, the yield is 26.32%, the wear volume in the lubricating grease is reduced by 43.20% compared with that in the base lubricating grease, and the friction coefficient is reduced by 42.19%.
Example 2, lithium hydroxide is used as a raw material, an alkaline solution is prepared by adding 1 kg of hexagonal boron nitride into the alkaline solution according to the volume ratio of ethanol to deionized water of 1:1, the concentration of the solution of the lithium hydroxide is controlled to be 0.12mg/ml, a mixed system is obtained by adding 1 kg of hexagonal boron nitride into the alkaline solution under the condition of vigorous stirring, the mixed solution is reacted in a reaction kettle at 300 ℃ for 2 hours, the temperature rise rate is 100 ℃/h, the rotation rate is 18rpm/min, after the reaction is finished, a sample is collected and dried, 3 kg of sodium bicarbonate is added into the collected sample as an intercalation agent, the sample is transferred into a tube furnace to be heated to 600 ℃ for reaction for 6 hours and then collected, the collected sample is placed into a Glanship microwave oven (P70D20N1P) to be heated at a medium fire gear for 1 hour for microwave treatment and then naturally cooled, the cooled sample is immersed into 10L liquid nitrogen for reaction and then washed, the hexagonal boron nitride nanosheet is obtained by drying, the collected boron nitride nanosheet is added into Kunlun No. 2 white special lubricating grease in 0.05 wt.%, and fully ground for 15 minutes to.
The size of the nano-sheet obtained by the method is 300-600nm, the thickness is 1.5-6.0nm, the yield is 25.42%, the wear volume in the lubricating grease is reduced by 32.41% compared with that in the base lubricating grease, the friction coefficient is reduced by 43.61%, and the picture of the friction and wear is shown in figure 2.
The picture of the reciprocating friction curve of Kunlun No. 2 white special grease (blank grease) and the obtained boron nitride nanosheets is shown in FIG. 1.
Example 3, using lithium hydroxide as a raw material, preparing an alkaline solution by using ethanol and deionized water in a volume ratio of 1:1, controlling the concentration of the solution of lithium hydroxide to be 0.12mg/ml, adding 1 kg of hexagonal boron nitride into the alkaline solution under a vigorous stirring condition to obtain a mixed system, reacting the mixed solution in a reaction kettle at 300 ℃ for 2 hours at a temperature rise rate of 100 ℃/h and a rotation rate of 18rpm/min, collecting and drying a sample after the reaction is finished, adding 3 kg of oxalic acid serving as an intercalation agent into the collected sample, transferring the mixture into a tubular furnace, heating the mixture to 600 ℃ for reaction for 6 hours, collecting the sample, placing the collected sample into a Glanship microwave oven (P70D20N1P) at a fire gear, heating the sample for 1 hour, naturally cooling the sample, immersing the cooled sample into 10L liquid nitrogen for reaction, washing the sample, drying the sample to obtain hexagonal boron nitride nanosheets, adding the collected hexagonal boron nitride nanosheets into Kunlun No. 2 white special lubricating grease in an amount of 0.05 wt.%, fully grinding the sample for 15 minutes to obtain a state without obvious white particles, performing a uniform color state, performing a friction test.
The size of the nano-sheet obtained by the method is 200-600nm, the thickness is 2.1-6.8nm, the yield is 22.36%, the wear volume in the lubricating grease is reduced by 38.62% compared with that in the base lubricating grease, and the friction coefficient is reduced by 50.73%.
Example 4, using lithium hydroxide as a raw material, preparing an alkaline solution by using ethanol and deionized water in a volume ratio of 1:1, controlling the concentration of the solution of lithium hydroxide to be 0.14mg/ml, adding 1 kg of hexagonal boron nitride into the alkaline solution under a vigorous stirring condition to obtain a mixed system, reacting the mixed solution in a reaction kettle at 300 ℃ for 2 hours at a temperature rise rate of 100 ℃/h and a rotation rate of 18rpm/min, collecting and drying a sample after the reaction is finished, adding 3 kg of sodium bicarbonate as an intercalating agent into the collected sample, transferring the sample into a tubular furnace, heating the sample to 600 ℃ for reaction for 6 hours, collecting the sample, placing the collected sample into a Glanship microwave oven (P70D20N1P) for heating and microwave treatment at a medium fire position for 1 hour, naturally cooling the sample, immersing the cooled sample into 10 g of liquid nitrogen for reaction, washing the sample, drying the sample to obtain hexagonal boron nitride nanosheets, adding the collected boron nitride nanosheets into Kunlun No. 2 white special lubricating grease in an amount of 0.05 wt.%, fully grinding the sample for 15 minutes to obtain a state without obvious white particles, performing a 10L uniform state, and performing a reciprocating.
The size of the nano-sheet obtained by the method is 200-600nm, the thickness is 2.2-6.5nm, the yield is 23.19%, the wear volume in the lubricating grease is reduced by 43.47% compared with that in the base lubricating grease, and the friction coefficient is reduced by 48.25%.
Example 5, using lithium hydroxide as a raw material, preparing an alkaline solution by using ethanol and deionized water in a volume ratio of 1:1, controlling the concentration of the solution of lithium hydroxide to be 0.16mg/ml, adding 1 kg of hexagonal boron nitride into the alkaline solution under a vigorous stirring condition to obtain a mixed system, reacting the mixed solution in a reaction kettle at 300 ℃ for 2 hours at a temperature rise rate of 100 ℃/h and a rotation rate of 18rpm/min, collecting and drying a sample after the reaction is finished, adding 3 kg of sodium bicarbonate serving as an intercalating agent into the collected sample, transferring the sample into a tubular furnace, heating the sample to 600 ℃ for reaction for 6 hours, collecting the sample, placing the collected sample into a Glanship microwave oven (P70D20N1P) for heating and microwave treatment at a medium fire gear for 1 hour, naturally cooling the sample, immersing the cooled sample into 10L liquid nitrogen for reaction, washing the sample, drying the sample to obtain hexagonal boron nitride nanosheets, adding the collected boron nitride nanosheets into Kunlun No. 2 white special lubricating grease in an amount of 0.05 wt.%, fully grinding the sample for 15 minutes to obtain a state without obvious white particles, performing a uniform state, and performing a reciprocating friction.
The size of the nano-sheet obtained by the method is 200-500nm, the thickness is 1.5-5.3nm, the yield is 27.28%, the wear volume in the lubricating grease is reduced by 31.52% compared with that in the base lubricating grease, and the friction coefficient is reduced by 51.36%.
Example 6, using lithium hydroxide as a raw material, preparing an alkaline solution from ethanol and deionized water in a volume ratio of 1:1, controlling the concentration of the solution of lithium hydroxide to be 0.18mg/ml, adding 1 kg of hexagonal boron nitride into the alkaline solution under a vigorous stirring condition to obtain a mixed system, reacting the mixed solution in a reaction kettle at 300 ℃ for 2 hours at a temperature rise rate of 100 ℃/h and a rotation rate of 18rpm/min, collecting and drying a sample after the reaction is finished, adding 3 kg of sodium bicarbonate as an intercalating agent into the collected sample, transferring the sample into a tube furnace, heating the sample to 600 ℃ for reaction for 6 hours, collecting the sample, placing the collected sample into a Glanship microwave oven (P70D20N1P) at a fire gear, heating the sample for 1 hour, naturally cooling the sample, immersing the cooled sample into 10L liquid nitrogen, reacting, washing the sample, drying the sample to obtain hexagonal boron nitride nanosheets, adding the collected hexagonal boron nitride nanosheets into Kunlun No. 2 white special lubricating grease in an amount of 0.05 wt.%, fully grinding the sample for 15 minutes to obtain a state without obvious white particles, performing a uniform color and performing a reciprocating friction test.
The size of the nano-sheet obtained by the method is 250-600nm, the thickness is 1.4-4.2nm, the yield is 24.93%, the wear volume in the lubricating grease is reduced by 30.10% compared with that in the base lubricating grease, and the friction coefficient is reduced by 55.8%.
Example 7, using lithium hydroxide as a raw material, preparing an alkaline solution from ethanol and deionized water in a volume ratio of 1:1, controlling the concentration of the solution of lithium hydroxide to be 0.2mg/ml, adding 1 kg of hexagonal boron nitride into the alkaline solution under a vigorous stirring condition to obtain a mixed system, reacting the mixed solution in a reaction kettle at 300 ℃ for 2 hours at a temperature rise rate of 100 ℃/h and a rotation rate of 18rpm/min, collecting and drying the sample after the reaction is finished, adding 3 kg of sodium bicarbonate as an intercalating agent into the collected sample, transferring the sample into a tubular furnace, heating the sample to 600 ℃ for reaction for 6 hours, collecting the sample, placing the collected sample into a Glanship microwave oven (P70D20N1P) for heating and microwave treatment at a medium fire position for 1 hour, naturally cooling the sample, immersing the cooled sample into 10 g of liquid nitrogen for reaction, washing the sample, drying the sample to obtain hexagonal boron nitride nanosheets, adding the collected boron nitride nanosheets into Kunlun No. 2 white special lubricating grease in an amount of 0.05 wt.%, fully grinding the sample for 15 minutes to obtain a state without obvious white particles, performing a 10L uniform state, and performing a reciprocating friction.
The size of the nano-sheet obtained by the method is 300-500nm, the thickness is 1.8-6.4nm, the yield is 25.24%, the wear volume in the lubricating grease is reduced by 37.62% compared with that in the base lubricating grease, and the friction coefficient is reduced by 43.55%.
Example 8, using lithium hydroxide as a raw material, preparing an alkaline solution by using ethanol and deionized water in a volume ratio of 1:1, controlling the concentration of the solution of lithium hydroxide to be 0.1mg/ml, adding 1 kg of hexagonal boron nitride into the alkaline solution under a vigorous stirring condition to obtain a mixed system, reacting the mixed solution in a reaction kettle at 300 ℃ for 2 hours at a temperature rise rate of 100 ℃/h and a rotation rate of 18rpm/min, collecting and drying a sample after the reaction is finished, adding 3 kg of sodium bicarbonate as an intercalating agent into the collected sample, transferring the sample into a tubular furnace, heating the sample to 600 ℃ for reaction for 6 hours, collecting the sample, placing the collected sample into a Glanship microwave oven (P70D20N1P) for heating and microwave treatment at a medium fire position for 1 hour, naturally cooling the sample, immersing the cooled sample into 10 g of liquid nitrogen for reaction, washing the sample, drying the sample to obtain hexagonal boron nitride nanosheets, adding the collected boron nitride nanosheets into Kunlun No. 2 white special lubricating grease in an amount of 0.05 wt.%, fully grinding the sample for 15 minutes to obtain a state without obvious white particles, performing a 10L uniform state, and performing a reciprocating.
The size of the nano-sheet obtained by the method is 300-550nm, the thickness is 2.2-5.4nm, the yield is 26.19%, the wear volume in the lubricating grease is reduced by 35.48% compared with that in the base lubricating grease, and the friction coefficient is reduced by 47.18%.
Example 9, using lithium hydroxide as a raw material, preparing an alkaline solution from ethanol and deionized water according to a volume ratio of 1:1, controlling the concentration of the lithium hydroxide solution to be 0.12mg/ml, adding 1 kg of hexagonal boron nitride into the alkaline solution under a vigorous stirring condition to obtain a mixed solution, reacting the mixed solution in a reaction kettle at 300 ℃ for 2 hours at a temperature rise rate of 100 ℃/h and a rotation rate of 18rpm/min, collecting and drying a sample after the reaction is finished, adding 3 kg of urea as an intercalating agent into the collected sample, transferring the sample into a tube furnace, heating to 600 ℃ for reaction for 6 hours, collecting the sample, placing the collected sample in a Glan microwave oven (P70D20N1P) at a medium fire position, heating for 1 hour, naturally cooling, immersing the cooled sample in 10 kg of liquid nitrogen, washing, drying to obtain hexagonal boron nitride nanosheets, adding the collected boron nitride nanosheets into Kunlun No. 3 white lubricating grease at an addition amount of 0.05 wt%, fully grinding for 15 minutes to obtain white particles, performing a 10L liquid nitrogen reaction, performing a reciprocating friction test on the hexagonal boron nitride nanosheets.
The size of the nano-sheet obtained by the method is 300-600nm, the thickness is 1.9-6.5nm, the yield is 26.37%, the wear volume in the lubricating grease is reduced by 32.95% compared with that in the base lubricating grease, and the friction coefficient is reduced by 50.23%.
Example 10, using lithium hydroxide as a raw material, preparing an alkaline solution from ethanol and deionized water according to a volume ratio of 1:1, controlling the concentration of the lithium hydroxide solution to be 0.12mg/ml, adding 1 kg of hexagonal boron nitride into the alkaline solution under a vigorous stirring condition to obtain a mixed solution, reacting the mixed solution in a reaction kettle at 300 ℃ for 2 hours at a temperature rise rate of 100 ℃/h and a rotation rate of 18rpm/min, collecting and drying a sample after the reaction is finished, adding 3 kg of urea as an intercalating agent into the collected sample, transferring the sample into a tube furnace, heating to 600 ℃ for reaction for 6 hours, collecting the sample, placing the collected sample in a Glan microwave oven (P70D20N1P) at a medium fire position for heating treatment for 1 hour, naturally cooling, immersing the cooled sample in 10 kg of liquid nitrogen for reaction, washing, drying to obtain hexagonal boron nitride nanosheets, adding the collected boron nitride nanosheets into No. 2 lithium base in an amount of 0.05 wt.%, fully grinding for 15 minutes to obtain a state without 10L obvious white particles, performing a friction test, and performing a reciprocating friction test on the hexagonal boron nitride nanosheets.
The size of the nano-sheet obtained by the method is 400-600nm, the thickness is 1.8-5.0nm, the yield is 25.94%, the wear volume in the lubricating grease is reduced by 33.69% compared with that in the base lubricating grease, and the friction coefficient is reduced by 52.18%.
Table 1 is a comparison table of the quality of the nanosheets prepared in examples 1-10 and their improved tribological properties.
Description of the test conditions: the white special lubricating grease of Kunlun No. 2, the white special lubricating grease of Kunlun No. 3 and the lithium-based lubricating grease of great wall No. 2 are used as blank lubricating greases, and the tribological performance of the lubricating grease is carried out by a reciprocating sliding friction pair test system (MFT-5000). The test conditions were as follows: the frequency was 5Hz, the load was 20N, the amplitude was 5mm, the time was 120min, and each test was repeated at least 3 times.
Comparative example 1
Preparing the nano-sheet by liquid phase stripping, wherein the reference document comprises: aideen Griffin, Andrew Harvey, BrianCunningham, Declan Scullion, Tian Tian, Chih-Jen Shih, Myrta Gruening, John FDonegan, Elton J.G.Santos, Claudia Backes, Jonathan N.Coleman.Spectroscopic sizing and thickness metrics for liquid-enriched h-BN.chemical materials.30(2018)1998-2005 the nanosheets produced by this method have a size of 100-1000nm and a thickness of 1-20 layers.
Comparative example 2
The nanosheets were prepared by ball milling, as described in Chaochao Cao, Yanming Xue, Zhenya L iu, Zheng Zhou, Jianwei Ji, Qianqian Song, Qi Hu, Yi Fan, Chengchun Tang, scalable and gradable segmentation of boundary-acid functionalized nanoparticles materials.2D materials.6(2019)035014. the nanosheets prepared by this method had a size of 2.0 μm and a thickness of 2.0 nm.
Comparative example 3
Nanosheets were prepared by chemical exfoliation, reference: du Miao, Yongzhong Wu, Xiaoope chemical evolution method to object large size boron nitride semiconductors.15 (2013)1782-1786 the size of the nano-sheet prepared by the method is about 4 μm and the thickness is 1.44 nm.
Comparative example 4
The nanosheet is prepared by adopting a combined stripping method, and the reference documents are as follows: guingyong Wu, Mingdong Yi, Guingchun Xiao, Zooqiang Chen, Jingjie Zhang, Chonghai xu. A novel method for producing boron nitride semiconductors with synthesis and purification with pure moisture International 45(2019)23841 23848. the size of the nanoplate prepared by this method is 200nm for 100 and the thickness is 2-3 nm.
Table 2 shows the existing composite lubricant prepared by hexagonal boron nitride nanosheets and the performance or contrast table thereof
Description of the test conditions: comparative examples friction tests all use Kunlun No. 2 white specialty grease as a blank grease and the other conditions are the same as the test conditions in Table 1.
Claims (10)
1. A preparation method of hexagonal boron nitride nanosheet base grease is characterized by comprising the following steps:
(1) adding hexagonal boron nitride into the alkaline solution under the condition of vigorous stirring to obtain a mixed solution;
(2) reacting the mixed solution obtained in the step (1) in a homogeneous reaction kettle, and drying the obtained sample;
(3) adding the intercalation agent into the sample obtained in the step (2) for 5-10 times by adopting an impregnation method, and reacting for 6-12 hours at the temperature of 600-;
(4) and (4) stripping the sample obtained in the step (3) by a microwave liquid nitrogen combination method, namely: heating the sample in a microwave oven for a period of time, cooling, immersing the cooled sample in liquid nitrogen, reacting for 3-5 times, washing, and drying to obtain hexagonal boron nitride nanosheets;
(5) and (4) adding the hexagonal boron nitride nanosheet obtained in the step (4) into lubricating grease according to a certain proportion, and fully grinding.
2. The method of claim 1, wherein in step (1), the ratio of the solvents ethanol and deionized water in the alkaline solution is 1:1.
3. the method of claim 1, wherein in step (1), the alkaline solution is prepared with lithium hydroxide as the strong base, the concentration of the alkaline solution is 0.12-0.17mg/ml, and the mass ratio of the strong base to the hexagonal boron nitride is 1: 1.5.
4. The method as claimed in claim 1, wherein in the step (2), the reaction temperature is 200 ℃ to 300 ℃, the temperature rise rate is 80 to 100 ℃/h, and the rotation rate of the homogeneous reaction kettle is 10 to 18 rpm.
5. The method of claim 1, wherein in step (3), the intercalating agent comprises any one of urea, sodium bicarbonate, and oxalic acid, and the mass ratio of the intercalating agent to the hexagonal boron nitride is 3: 1.
6. The method according to claim 1, wherein in the step (4), the power of the microwave oven is in the range of 600-900W, the temperature is set at middle fire or middle fire, and the microwave treatment time is 0.5-1 hour.
7. The method according to claim 1, wherein in step (4), the volume of liquid nitrogen per immersion is 50-100 ml.
8. The method of claim 1, wherein in step (5), the hexagonal boron nitride nanosheets obtained in step (4) are added to a lubricating grease in a proportion of 0.05 to 0.15 wt.%; the time for full grinding in a mortar is 15-20 minutes.
9. The method of claim 1, wherein in step (5), the grease comprises any one of Kunlun No. 2 white specialty grease, Kunlun No. 3 white specialty grease, and great wall No. 2 lithium-based grease.
10. A hexagonal boron nitride nanoplatelet-based grease prepared according to the method of any of claims 1-9.
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