CN111394153B - 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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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 two-dimensional layered nano material hexagonal boron nitride can reduce the friction coefficient to be below 0.01 under the condition of a few atomic layers. Zhang et al recently reported that hexagonal boron nitride nanosheet solutions obtained by using aqueous dispersion dots of Carbon Quanta (CQD) as debonding and stabilizing agents were used as aqueous lubricants with friction coefficients as low as 0.02 and even under certain working conditions achieved super lubricity (ACS appl.mater.interfaces.2016, DOI:10.1021/acsami.6b09752), and that "super-slip" state was also observed for heterostructures of hexagonal boron nitride/graphene obtained by Leven et al by CVD methods (j.phys.chem.lett.2013, DOI:10.1021/jz301758c), which studies have a milestone revolutionary significance in the field of tribology. The B, N element in the hexagonal boron nitride is an important element of the traditional friction reducer, and does not contain toxic elements such as S, P and the like. The material has an ultra-flat surface, and the low strength of the atomic shear surface of the material can provide low friction force during friction, and the hexagonal boron nitride is an ideal candidate material of a lubricating additive due to the excellent mechanical strength, high chemical inertness and thermal stability. Liu et al obtained 10 monolayers of boron nitride composite nanomaterial with a diameter greater than 200nm and a thickness by ball milling for 20 hours. In a friction experiment using the boron nitride composite nano material as a lubricating additive, the wear scar diameter and the friction coefficient are reduced by 30% and 13% compared with those of base oil (adv. Eng. Mater.2017, DOI: 10.1002/adem.201700488). Kumari et al prepared boron nitride nanosheets by ultrasound using N-methylpyrrolidone as the liquid stripper, h-BNNPs-ODA showed 35% and 25% reduction in coefficient of friction and wear scar width in the mineral base oil ball pan friction experiment (Phys. chem. Phys.2016, DOI: 10.1039/c6cp04741 f). Although hexagonal boron nitride materials have shown unprecedented super-lubricity and anti-friction properties, practical applications still face several key scientific and technical bottlenecks, such as: high cost, complex process, environment-friendliness, difficult scale-up, poor dispersibility and stability, undesirable macroscopic friction performance and the like.
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: taking lithium hydroxide as a raw material, preparing an alkaline solution from ethanol and deionized water according to the volume ratio of 1:1, controlling the concentration of the lithium hydroxide solution to be 0.12mg/ml, and adding 1 kg of hexagonal boron nitride into the alkaline solution under the condition of vigorous stirring to obtain a mixed solution; and (3) reacting the mixed solution in a reaction kettle at 300 ℃ for 2 hours, wherein the temperature rise rate is 100 ℃/h, and the rotation rate is 18 rpm/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 to a tubular furnace, heating to 600 ℃, reacting for 6 hours, and collecting; placing the collected sample in a Glanshi microwave oven (P70D20N1P) for heating treatment in a fire position for 1 hour, and then naturally cooling; immersing the cooled sample into 10L of liquid nitrogen for reaction, washing and drying to obtain a hexagonal boron nitride nanosheet; adding the collected hexagonal boron nitride nanosheets into Kunlun No. 2 white special lubricating grease in an adding amount of 0.05 wt.%, fully grinding for 15 minutes to achieve a state of no obvious white particles and uniform color, and performing a reciprocating friction experiment test. The blank grease, the picture of the reciprocating friction curve of the obtained boron nitride nanosheet and the picture of the friction and wear of the boron nitride nanosheet are shown in figures 1 and 2.
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: taking lithium hydroxide as a raw material, preparing an alkaline solution from ethanol and deionized water according to the volume ratio of 1:1, controlling the concentration of the solution of the lithium hydroxide to be 0.12mg/ml, and adding 1 kg of hexagonal boron nitride into the alkaline solution under the condition of vigorous stirring to obtain a mixed system; and (3) reacting the mixed solution in a reaction kettle at 300 ℃ for 2 hours, wherein the temperature rise rate is 100 ℃/h, and the rotation rate is 18 rpm/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 to a tubular furnace, heating to 600 ℃, reacting for 6 hours, and collecting; placing the collected sample in a Glanshi microwave oven (P70D20N1P) to be heated in a fire position for microwave treatment for 1 hour and then naturally cooling; immersing the cooled sample into 10L of liquid nitrogen for reaction, washing and drying to obtain a hexagonal boron nitride nanosheet; adding the collected hexagonal boron nitride nanosheets into Kunlun No. 2 white special lubricating grease in an amount of 0.05 wt.%, fully grinding for 15 minutes to reach a state of no obvious white particles and uniform color, and performing a reciprocating friction experiment test.
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: taking lithium hydroxide as a raw material, preparing an alkaline solution from ethanol and deionized water according to the volume ratio of 1:1, controlling the concentration of the solution of the lithium hydroxide to be 0.12mg/ml, and adding 1 kg of hexagonal boron nitride into the alkaline solution under the condition of vigorous stirring to obtain a mixed system; and (3) reacting the mixed solution in a reaction kettle at 300 ℃ for 2 hours, wherein the temperature rise rate is 100 ℃/h, and the rotation rate is 18 rpm/min. Collecting and drying a sample after the reaction is finished; adding 3 kg of oxalic acid serving as an intercalating agent into the collected sample, transferring the sample to a tubular furnace, heating to 600 ℃, reacting for 6 hours, and collecting; placing the collected sample in a Glanshi microwave oven (P70D20N1P) to be heated in a fire position for microwave treatment for 1 hour and then naturally cooling; immersing the cooled sample into 10L of liquid nitrogen for reaction, washing and drying to obtain a hexagonal boron nitride nanosheet; adding the collected hexagonal boron nitride nanosheets into Kunlun No. 2 white special lubricating grease in an amount of 0.05 wt.%, fully grinding for 15 minutes to obtain a state without obvious white particles and uniform color, and performing a reciprocating friction experiment 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: taking lithium hydroxide as a raw material, preparing an alkaline solution from ethanol and deionized water according to the volume ratio of 1:1, controlling the concentration of the solution of the lithium hydroxide to be 0.14mg/ml, and adding 1 kg of hexagonal boron nitride into the alkaline solution under the condition of vigorous stirring to obtain a mixed system; and (3) reacting the mixed solution in a reaction kettle at 300 ℃ for 2 hours, wherein the temperature rise rate is 100 ℃/h, and the rotation rate is 18 rpm/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 to a tubular furnace, heating to 600 ℃, reacting for 6 hours, and collecting; placing the collected sample in a Glanshi microwave oven (P70D20N1P) to be heated in a fire gear for microwave treatment for 1 hour and then naturally cooling; immersing the cooled sample into 10L of liquid nitrogen for reaction, washing and drying to obtain a hexagonal boron nitride nanosheet; adding the collected hexagonal boron nitride nanosheets into Kunlun No. 2 white special lubricating grease in an amount of 0.05 wt.%, fully grinding for 15 minutes to obtain a state without obvious white particles and uniform color, and performing a reciprocating friction experiment test.
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: taking lithium hydroxide as a raw material, preparing an alkaline solution from ethanol and deionized water according to the volume ratio of 1:1, controlling the concentration of the solution of the lithium hydroxide to be 0.16mg/ml, and adding 1 kg of hexagonal boron nitride into the alkaline solution under the condition of vigorous stirring to obtain a mixed system; and (3) reacting the mixed solution in a reaction kettle at 300 ℃ for 2 hours, wherein the temperature rise rate is 100 ℃/h, and the rotation rate is 18 rpm/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 to a tubular furnace, heating to 600 ℃, reacting for 6 hours, and collecting; placing the collected sample in a Glanshi microwave oven (P70D20N1P) to be heated in a fire gear for microwave treatment for 1 hour and then naturally cooling; immersing the cooled sample into 10L of liquid nitrogen for reaction, washing and drying to obtain a hexagonal boron nitride nanosheet; adding the collected hexagonal boron nitride nanosheets into Kunlun No. 2 white special lubricating grease in an amount of 0.05 wt.%, fully grinding for 15 minutes to obtain a state without obvious white particles and uniform color, and performing a reciprocating friction experiment test.
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: taking lithium hydroxide as a raw material, preparing an alkaline solution from ethanol and deionized water according to the volume ratio of 1:1, controlling the concentration of the solution of the lithium hydroxide to be 0.18mg/ml, and adding 1 kg of hexagonal boron nitride into the alkaline solution under the condition of vigorous stirring to obtain a mixed system; and (3) reacting the mixed solution in a reaction kettle at 300 ℃ for 2 hours, wherein the temperature rise rate is 100 ℃/h, and the rotation rate is 18 rpm/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 to a tubular furnace, heating to 600 ℃, reacting for 6 hours, and collecting; placing the collected sample in a Glanshi microwave oven (P70D20N1P) to be heated in a fire gear for microwave treatment for 1 hour and then naturally cooling; immersing the cooled sample into 10L of liquid nitrogen for reaction, washing and drying to obtain a hexagonal boron nitride nanosheet; adding the collected hexagonal boron nitride nanosheets into Kunlun No. 2 white special lubricating grease in an amount of 0.05 wt.%, fully grinding for 15 minutes to obtain a state without obvious white particles and uniform color, and performing a reciprocating friction experiment 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: preparing an alkaline solution from lithium hydroxide serving as a raw material by using ethanol and deionized water in a volume ratio of 1:1, controlling the concentration of the solution of the lithium hydroxide to be 0.2mg/ml, and adding 1 kg of hexagonal boron nitride into the alkaline solution under the condition of vigorous stirring to obtain a mixed system; and (3) reacting the mixed solution in a reaction kettle at 300 ℃ for 2 hours, wherein the temperature rise rate is 100 ℃/h, and the rotation rate is 18 rpm/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 to a tubular furnace, heating to 600 ℃, reacting for 6 hours, and collecting; placing the collected sample in a Glanshi microwave oven (P70D20N1P) to be heated in a fire gear for microwave treatment for 1 hour and then naturally cooling; immersing the cooled sample into 10L of liquid nitrogen for reaction, washing and drying to obtain a hexagonal boron nitride nanosheet; adding the collected hexagonal boron nitride nanosheets into Kunlun No. 2 white special lubricating grease in an amount of 0.05 wt.%, fully grinding for 15 minutes to obtain a state without obvious white particles and uniform color, and performing a reciprocating friction experiment test.
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: preparing an alkaline solution from lithium hydroxide serving as a raw material by using ethanol and deionized water in a volume ratio of 1:1, controlling the concentration of the solution of the lithium hydroxide to be 0.1mg/ml, and adding 1 kg of hexagonal boron nitride into the alkaline solution under the condition of vigorous stirring to obtain a mixed system; and (3) reacting the mixed solution in a reaction kettle at 300 ℃ for 2 hours, wherein the temperature rise rate is 100 ℃/h, and the rotation rate is 18 rpm/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 to a tubular furnace, heating to 600 ℃, reacting for 6 hours, and collecting; placing the collected sample in a Glanshi microwave oven (P70D20N1P) to be heated in a fire gear for microwave treatment for 1 hour and then naturally cooling; immersing the cooled sample into 10L of liquid nitrogen for reaction, washing and drying to obtain a hexagonal boron nitride nanosheet; adding the collected hexagonal boron nitride nanosheets into Kunlun No. 2 white special lubricating grease in an amount of 0.05 wt.%, fully grinding for 15 minutes to obtain a state without obvious white particles and uniform color, and performing a reciprocating friction experiment test.
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: taking lithium hydroxide as a raw material, preparing an alkaline solution from ethanol and deionized water according to the volume ratio of 1:1, controlling the concentration of the lithium hydroxide solution to be 0.12mg/ml, and adding 1 kg of hexagonal boron nitride into the alkaline solution under the condition of vigorous stirring to obtain a mixed solution; and (3) reacting the mixed solution in a reaction kettle at 300 ℃ for 2 hours, wherein the temperature rise rate is 100 ℃/h, and the rotation rate is 18 rpm/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 to a tubular furnace, heating to 600 ℃, reacting for 6 hours, and collecting; placing the collected sample in a Glanshi microwave oven (P70D20N1P) for heating treatment in a fire position for 1 hour, and then naturally cooling; immersing the cooled sample into 10L of liquid nitrogen for reaction, washing and drying to obtain a hexagonal boron nitride nanosheet; adding the collected hexagonal boron nitride nanosheets into Kunlun No. 3 white special lubricating grease in an adding amount of 0.05 wt.%, fully grinding for 15 minutes to achieve a state of no obvious white particles and uniform color, and performing a reciprocating friction experiment test.
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: taking lithium hydroxide as a raw material, preparing an alkaline solution from ethanol and deionized water according to the volume ratio of 1:1, controlling the concentration of the lithium hydroxide solution to be 0.12mg/ml, and adding 1 kg of hexagonal boron nitride into the alkaline solution under the condition of vigorous stirring to obtain a mixed solution; and (3) reacting the mixed solution in a reaction kettle at 300 ℃ for 2 hours, wherein the temperature rise rate is 100 ℃/h, and the rotation rate is 18 rpm/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 to a tubular furnace, heating to 600 ℃, reacting for 6 hours, and collecting; placing the collected sample in a Glanshi microwave oven (P70D20N1P) for heating treatment in a fire position for 1 hour, and then naturally cooling; immersing the cooled sample into 10L of liquid nitrogen for reaction, washing and drying to obtain a hexagonal boron nitride nanosheet; adding the collected hexagonal boron nitride nanosheets into the great wall No. 2 lithium-based lubricating grease in an adding amount of 0.05 wt.%, fully grinding for 15 minutes to achieve a state of no obvious white particles and uniform color, and performing a reciprocating friction experiment test.
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, Brian Cunningham, Declan Scullion, Tian Tian, Chih-Jen Shih, Myrta Gruening, John F Donegan, Elton J.G.Santos, Claudia Backes, Jonathan N.Coleman.Spectroscopic size 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
Preparing a nano sheet by adopting a ball milling method, wherein the reference document comprises the following steps: chaochao Cao, Yanming Xue, Zhenya Liu, Zheng Zhou, Jianwei Ji, Qianqian Song, Qi Hu, Yi Fan, Chengchun Tang. scalable enhancement and gradable segmentation of boron-acid-functionalized boron nitride materials.2D materials.6(2019)035014 the size of the nanosheets produced by this method was 2.0 μm and the thickness was 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 nanosheets.15 (2013)1782-1786 the size of the nanosheet 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, Zhaoqiang Chen, Jingjie Zhang, Chonghai xu. A novel method for producing boron nitride films with a synthesis of synthesis and synthesis with pure moisture center 45(2019)23841 23848. the size of the nanoplate prepared by this method is 200nm 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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