CN115558926A - High-temperature liquid super-smooth borate nano-film and construction method and use method thereof - Google Patents

High-temperature liquid super-smooth borate nano-film and construction method and use method thereof Download PDF

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CN115558926A
CN115558926A CN202210469388.4A CN202210469388A CN115558926A CN 115558926 A CN115558926 A CN 115558926A CN 202210469388 A CN202210469388 A CN 202210469388A CN 115558926 A CN115558926 A CN 115558926A
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dimensional material
smooth
film
borate
workpiece
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吴红星
尹绍冲
花珂
史俊勤
王海丰
周峰
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Northwestern Polytechnical University
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Northwestern Polytechnical University
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C26/00Coating not provided for in groups C23C2/00 - C23C24/00
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/60Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using solids, e.g. powders, pastes
    • C23C8/62Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using solids, e.g. powders, pastes only one element being applied
    • C23C8/68Boronising
    • C23C8/70Boronising of ferrous surfaces
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/028Borodising,, i.e. borides formed electrochemically

Abstract

The invention discloses a construction method of a high-temperature liquid super-smooth borate nano film, which comprises the following steps of adding a two-dimensional material into deionized water; dissolving a liquid lubricant in deionized water; adding a liquid lubricant mixed solution into a two-dimensional material mixed solution to obtain a uniformly dispersed two-dimensional material suspension, wherein the two-dimensional material accounts for 0.01-1 wt%, and the liquid lubricant accounts for 5-50 wt%; coating the two-dimensional material suspension on the surface of a workpiece containing a boron-based coating to form a compound, mounting the workpiece on an abrasion tester to grind the compound, applying a load of 5-30N, wherein the grinding speed is not less than 10mm/s, and after grinding for 5-60 min, cleaning residual liquid to obtain the borate nano film. The borate nano film disclosed by the invention not only can realize super-lubricity at a high temperature of 70-200 ℃ (far higher than the super-lubricity ambient temperature of the mainstream), and reduce the loss of key parts, but also has the characteristics of convenience and rapidness in processing, low requirement on equipment in the forming process, and capability of effectively improving the production efficiency and reducing the production cost.

Description

High-temperature liquid ultra-smooth borate nano-film and construction method and use method thereof
Technical Field
The invention relates to a high-temperature liquid super-smooth borate nano-film, a construction method and a use method thereof, belonging to the technical field of lubricating materials.
Background
In the course of various sports in nature and human production life, friction consumes 1/3-1/2 of the primary energy source all over the world, about 80% of machine part failures are caused by friction-induced wear, and about more than 50% of the vicious accidents of mechanical equipment are caused by lubrication failure and excessive wear. According to statistics, 85% of airplane plunger pumps fail due to abrasion, and the abrasion failure of key parts becomes a bottleneck limiting the service reliability and service life of new-generation high-end equipment in China.
The ultra-smooth technology is hopeful to overcome frictional wear, and is expected to solve the problems of failure, reliability reduction and the like of key parts of important equipment caused by wear. At present, although a system for realizing super-lubricity under a room-temperature working condition is available, the feasibility of super-lubricity is proved, but the practical application environment temperature of the super-lubricity is often over 100 ℃, for example: the working temperature of the plunger pump for the airplane is about 100 ℃, the lubricating agent for the rolling bearing of the aircraft engine can reach 150-200 ℃, and the service temperature of the lubricating agent is far higher than that of the current ultra-slip system.
Meanwhile, the current key parts mainly take metal products as main parts, and the ultra-smooth system mainly relying on diamond-like carbon coating (DLC) has higher requirements on coating preparation equipment and high cost.
Disclosure of Invention
The invention aims to provide a high-temperature liquid ultra-smooth borate nano film, a construction method and a use method thereof, the film and the construction method not only make up the defect that an ultra-smooth system in the prior art cannot work in a high-temperature environment and reduce the loss of key parts, but also solve the problems of complex preparation, high requirement on equipment by a forming process and high cost of the ultra-smooth system in the prior art.
In order to achieve the purpose, the invention adopts the technical scheme that: a construction method of a high-temperature liquid super-smooth borate nano-film comprises the following steps:
preparing a boronizing layer on the surface of a workpiece, cleaning the boronized workpiece in boiling water, and drying to remove residual substances on the surface of the workpiece;
adding a two-dimensional material into deionized water; dissolving a liquid lubricant in deionized water; adding a liquid lubricant solution into a two-dimensional material solution, and carrying out ultrasonic treatment to obtain a uniformly dispersed two-dimensional material suspension, wherein the two-dimensional material accounts for 0.01-1 wt%, and the liquid lubricant accounts for 5-50 wt%;
coating the two-dimensional material suspension on the surface of a workpiece containing a boron-based coating to form a compound, mounting the workpiece on an abrasion tester to grind the compound, applying a load not greater than 30N, wherein the grinding speed is not less than 10mm/s, and after grinding for 5-60 min, cleaning the residual two-dimensional material suspension to obtain the borate nano film.
Further, the two-dimensional material is one or more of graphene oxide, graphene, molybdenum disulfide, tungsten disulfide and hexagonal boron nitride.
Further, the liquid lubricant is one or more of R-OH.
Furthermore, the thickness of the borate nano film is 3-100 nm.
Further, when the two-dimensional material solution is prepared, the two-dimensional material solution is subjected to ultrasonic treatment, the frequency of the ultrasonic treatment is 40-60 kHz, the power is 100-200W, and the treatment time is 15-60 min.
Further, when the liquid lubricant solution is prepared, the liquid lubricant solution is subjected to ultrasonic treatment at the temperature of 40-60 ℃, the frequency of 40-60 kHz, the power of 100-150W and the treatment time of 10-20 min.
Furthermore, when preparing the two-dimensional material suspension, the ultrasonic treatment frequency is 40-60 kHz, the power is 30-500W, and the treatment time is 10-120 min.
Further, the residual liquid was washed with anhydrous ethanol.
The invention also provides a technical scheme that: a borate nano-film is prepared according to the method.
The invention also provides a technical scheme that: a method for using a high-temperature liquid ultra-smooth borate nano film comprises the steps of adding a liquid lubricant to the surface of the borate nano film prepared by the method, heating the borate nano film to 70-200 ℃, and applying a working load and speed.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
1. the invention relates to a high-temperature liquid super-smooth borate nano film, a construction method and a use method thereof.A two-dimensional material liquid lubricant suspension is prepared and coated on the surface of a boron-based coating workpiece, a friction tester is used for running-in, and a layer of nano borate film is constructed and formed by utilizing a friction chemical reaction.
2. According to the high-temperature liquid ultra-smooth borate nano-film and the construction method and the using method thereof, the borate nano-film is constructed by preparing the two-dimensional material suspension, so that the grinding-in surface is protected, and the surface abrasion in the construction process is reduced.
3. The high-temperature liquid super-smooth borate nano film can realize super-smooth behavior in an atmospheric environment, does not need special inert atmosphere, has wide temperature range application range, covers the temperature range of common gear oil, the service temperature of an automobile engine and is close to the temperature limit of a liquid lubricant, and has excellent industrial application value.
4. According to the high-temperature liquid super-smooth borate nano film, the construction method and the using method thereof, the addition of the two-dimensional material can further improve the forming quality and the high-temperature super-smooth effect of the borate nano film.
Drawings
FIG. 1 is a TEM (transmission electron microscope) cross-section of a borate nano-film constructed by the invention, wherein a light-colored part is the film, and an adjacent dark-colored part is a boronizing layer;
FIG. 2 is a graph of the ultra-low friction coefficient at 70 ℃ of the borate ester constructed in example 1;
FIG. 3 is a surface composition diagram of a borate workpiece constructed in example 2;
FIG. 4 is a graph of the ultra-low friction coefficient at 175 ℃ of the boronic ester constructed in example 4;
FIG. 5 is a plot of the coefficient of friction of the borate-free film on the boriding work piece of comparative example 2.
Detailed Description
Example 1: the construction method of the high-temperature liquid super-smooth borate nano film comprises the following steps:
s1: preparing a boron-based coating, namely putting a bearing steel disc workpiece with the diameter of 30mm and the thickness of 5mm into a salt bath boronizing in an electrolytic molten salt furnace, and treating for 30min at the temperature of 900 ℃ under the current of 20A to obtain a workpiece coated by the boron-based coating; and after the workpiece is cooled, putting the workpiece into boiled hot water, heating for 2 hours to remove residual substances on the surface, and then putting the workpiece into an oven at 80 ℃ for drying to obtain the workpiece with the boron-based coating and the clean surface.
The boronizing method can also be solid boronizing or gas boronizing, the specific boronizing operation is not limited to the method mentioned in the embodiment, and after boronizing, the hardness of the boronized layer can reach HV1800.
S2: preparing a two-dimensional material solution, namely adding 0.1g of a two-dimensional material into 10g of deionized water, starting an ultrasonic cleaner, deagglomerating the two-dimensional material with the working frequency of 50kHz, the ultrasonic power of 100W and the oscillation time of 20min, and uniformly dispersing the two-dimensional material in the deionized water to obtain the 1wt% two-dimensional material solution.
The two-dimensional material is one or more of graphene oxide, graphene, molybdenum disulfide, tungsten disulfide and hexagonal boron nitride, wherein the graphene oxide is selected.
S3: liquid lubricant solution preparation-0.4 g of liquid lubricant is dissolved in deionized water, an ultrasonic cleaner is started, the working frequency is 50kHz, the ultrasonic power is 100W, the oscillation time is 10min, and the liquid temperature is 50 ℃, so that a uniformly dispersed 40wt% liquid lubricant solution is obtained.
The liquid lubricant R-OH is preferably one or more of hydroxyl-containing substances such as methanol, ethylene glycol, glycerol, glucose, sucrose, polyethylene glycol, etc., wherein ethylene glycol is selected.
S4: and (3) suspension preparation, namely adding the liquid lubricant solution obtained in 5g of S3 into the two-dimensional material solution prepared in 5g of S2, and performing ultrasonic treatment to obtain a suspension containing 0.5wt% of two-dimensional material and 20wt% of liquid lubricant.
S5: forming, namely coating the suspension obtained in the step S4 on the surface of a workpiece by using a spin coating instrument, so that the surface of the workpiece is simultaneously provided with a compound of a boronizing layer, a two-dimensional material, a liquid lubricant and water;
opening the RTEC multifunctional friction wear testing machine, placing the composite side of the workpiece on the testing machine for running-in treatment, applying 5N load and 10mm/s running-in speed, wiping off residual liquid on the surface by using absolute ethyl alcohol after running-in for 20min, and constructing a layer of nanoscale borate film in a friction area.
The nano-scale borate film prepared by the above method was obtained, FIB sampling was performed, the thickness was 30nm after detection by a Transmission Electron Microscope (TEM), and a cross-sectional picture was shown in fig. 1.
And (3) testing: as shown in figure 2, a glycerol liquid lubricant is added on the surface of a borate film, an RTEC multifunctional friction and wear testing machine is adopted, a heating program is started, the temperature is raised to 70 ℃, the load is 5N, the linear velocity is 10mm/s, the friction coefficient in a stable stage is 0.004, and the ultra-smooth state is achieved at high temperature.
Example 2: the construction method of the high-temperature liquid super-smooth borate nano film comprises the following steps:
s1: preparing a boron-based coating, namely putting a bearing steel disc workpiece with the diameter of 40mm and the thickness of 5mm into a salt bath boronizing in an electrolytic molten salt furnace, and treating for 15min at the temperature of 900 ℃ under the current of 20A to obtain a workpiece coated with the boron-based coating; and after the workpiece is cooled, putting the workpiece into boiling hot water, heating for 1h, removing residual substances on the surface, and then putting the workpiece into a 100 ℃ oven for drying to obtain the boron-based coating workpiece with a clean surface.
The boronizing method can also be solid boronizing or gas boronizing, the specific boronizing operation is not limited to the method mentioned in the embodiment, and after boronizing, the hardness of the boronized layer can reach HV1800.
S2: preparing a two-dimensional material solution, namely adding 0.08g of a two-dimensional material into 10g of deionized water, starting an ultrasonic cleaner, deagglomerating the two-dimensional material and uniformly dispersing the two-dimensional material in the deionized water to obtain a 1wt% two-dimensional material solution, wherein the working frequency is 50kHz, the ultrasonic power is 150W, and the oscillation time is 15 min.
The two-dimensional material is one or more of graphene oxide, graphene, molybdenum disulfide, tungsten disulfide and hexagonal boron nitride, wherein the graphene oxide is selected.
S3: preparing a liquid lubricant solution, namely dissolving 0.4g of liquid lubricant in deionized water, starting an ultrasonic cleaner, wherein the working frequency is 50kHz, the ultrasonic power is 150W, the oscillation time is 15min, and the liquid temperature is 60 ℃, so as to obtain a uniformly dispersed 40wt% liquid lubricant solution.
The liquid lubricant R-OH is preferably one or more of hydroxyl-containing substances such as methanol, ethylene glycol, glycerol, glucose, sucrose, and polyethylene glycol, wherein glycerol is used.
S4: and (3) suspension preparation, namely adding the liquid lubricant solution obtained in 5g of S3 into the two-dimensional material solution prepared in 5g of S2, and performing ultrasonic treatment to obtain a suspension containing 0.4wt% of two-dimensional material and 20wt% of liquid lubricant.
S5: forming, namely coating the suspension obtained in the step S4 on the surface of a workpiece by using a spin coating instrument, so that the surface of the workpiece is simultaneously provided with a compound of a boronizing layer, a two-dimensional material, a liquid lubricant and water;
opening the RTEC multifunctional friction wear testing machine, placing the composite side of the workpiece on the testing machine for running-in treatment, applying a load of 5N and a running-in speed of 18mm/s, wiping off liquid remained on the surface by using absolute ethyl alcohol after running-in for 20min, and constructing a layer of nanoscale borate film in a friction area.
The nano borate film prepared by the method is obtained, and the surface of the friction film contains an obvious borate peak through X-ray photoelectron spectroscopy (XPS) analysis and test; the XPS spectrum of the constructed borate ester nano film is shown in figure 3.
And (3) testing: a glycerol liquid lubricant is added on the surface of a borate film, an RTEC multifunctional friction and wear testing machine is adopted, a heating program is started, the temperature is increased to 100 ℃, the load is 30N, the linear velocity is 20mm/s, the friction coefficient in a stable stage is 0.004, and an ultra-low friction state is achieved at high temperature.
Example 3: the construction method of the high-temperature liquid super-smooth borate nano film comprises the following steps:
s1: preparing a boron-based coating, namely putting a bearing steel disc workpiece with the diameter of 30mm and the thickness of 5mm into a salt bath boronizing in an electrolytic molten salt furnace, and treating for 30min at the temperature of 900 ℃ under the current of 10A to obtain a workpiece coated with the boron-based coating; and after the workpiece is cooled, putting the workpiece into boiling hot water, heating for 1h, removing residual substances on the surface, and then putting the workpiece into an oven at 80 ℃ for drying to obtain the boron-based coating workpiece with a clean surface.
The boronizing method can also be solid boronizing or gas boronizing, the specific boronizing operation is not limited to the method mentioned in the embodiment, and after boronizing, the hardness of the boronized layer can reach HV1800.
S2: preparing a two-dimensional material solution, namely adding 0.1g of a two-dimensional material into 10g of deionized water, starting an ultrasonic cleaner, deagglomerating the two-dimensional material with the working frequency of 50kHz, the ultrasonic power of 200W and the oscillation time of 30min, and uniformly dispersing the two-dimensional material in the deionized water to obtain the 1wt% two-dimensional material solution.
The two-dimensional material is one or more of graphene oxide, graphene, molybdenum disulfide, tungsten disulfide and hexagonal boron nitride, wherein molybdenum disulfide is selected.
S3: liquid lubricant solution preparation-0.4 g of liquid lubricant is dissolved in deionized water, an ultrasonic cleaner is started, the working frequency is 50kHz, the ultrasonic power is 100W, the oscillation time is 20min, and the liquid temperature is 50 ℃, so that a uniformly dispersed 40wt% liquid lubricant solution is obtained.
The liquid lubricant R-OH is preferably one or more of hydroxyl-containing substances such as methanol, ethylene glycol, glycerol, glucose, sucrose, and polyethylene glycol, wherein polyethylene glycol is selected.
S4: and (3) suspension preparation, namely adding the liquid lubricant solution obtained in 5g of S3 into the two-dimensional material solution prepared in 5g of S2, and performing ultrasonic treatment to obtain a suspension containing 0.5wt% of two-dimensional material and 20wt% of liquid lubricant.
S5: forming, namely coating the suspension obtained in the step S4 on the surface of a workpiece by using a spin coater, so that the surface of the workpiece is simultaneously provided with a compound of a boronizing layer, a two-dimensional material, a liquid lubricant and water;
and opening the RTEC multifunctional friction wear testing machine, placing the composite side of the workpiece on the testing machine for running-in treatment, applying 10N load and 20mm/s running-in speed, wiping off residual liquid on the surface by using absolute ethyl alcohol after running-in for 20min, and constructing a layer of nano borate film in a friction area.
And (3) testing: adding 70wt% of glycerol and 30wt% of erythritol liquid lubricant to the surface of the borate film, starting a heating program by adopting an RTEC multifunctional friction and wear testing machine, heating to 125 ℃, loading 10N, and linear velocity of 10mm/s, wherein the friction coefficient in a stable stage is 0.008, and the borate film reaches an ultra-smooth state at high temperature.
Example 4: the construction method of the high-temperature liquid super-smooth borate nano film comprises the following steps:
s1: preparing a boron-based coating, namely putting a bearing steel disc workpiece with the diameter of 24mm and the thickness of 7.9mm into an electrolytic molten salt furnace for salt bath boronization, and treating for 30min at the temperature of 900 ℃ under the current of 20A to obtain a workpiece coated by the boron-based coating; and after the workpiece is cooled, putting the workpiece into boiled hot water, heating for 2 hours to remove residual substances on the surface, and then putting the workpiece into a 100 ℃ drying oven for drying to obtain the boron-based coating workpiece with a clean surface.
The boronizing method can also be solid boronizing or gas boronizing, the specific boronizing operation is not limited to the method mentioned in the embodiment, and after boronizing, the hardness of the boronized layer can reach HV1800.
S2: preparing a two-dimensional material solution, namely adding 0.05g of a two-dimensional material into 10g of deionized water, starting an ultrasonic cleaner, deagglomerating the two-dimensional material and uniformly dispersing the two-dimensional material in the deionized water to obtain a 0.5wt% two-dimensional material solution, wherein the working frequency is 50kHz, the ultrasonic power is 200W, and the oscillation time is 60min.
The two-dimensional material is one or more of graphene oxide, graphene, molybdenum disulfide, tungsten disulfide and hexagonal boron nitride, wherein the graphene oxide is selected.
S3: preparing a liquid lubricant solution, namely dissolving 0.2g of liquid lubricant in deionized water, starting an ultrasonic cleaner, wherein the working frequency is 50kHz, the ultrasonic power is 100W, the oscillation time is 20min, and the liquid temperature is 50 ℃, so that a uniformly dispersed 20wt% liquid lubricant solution is obtained.
The liquid lubricant R-OH is preferably one or more of hydroxyl-containing substances such as methanol, ethylene glycol, glycerol, glucose, sucrose, and polyethylene glycol, wherein 0.1g of glycerol and 0.1g of pentadiol are used.
S4: suspension preparation-the liquid lubricant solution obtained in 5g of S3 was added to the two-dimensional material solution prepared in 5g of S2, and after ultrasonic treatment, a suspension containing 0.25wt% of the two-dimensional material and 20wt% of the liquid lubricant was obtained.
S5: forming, namely coating the suspension obtained in the step S4 on the surface of a workpiece by using a spin coating instrument, so that the surface of the workpiece is simultaneously provided with a compound of a boronizing layer, a two-dimensional material, a liquid lubricant and water;
and opening the RTEC multifunctional friction wear testing machine, placing the composite side of the workpiece on the testing machine for running-in treatment, applying 5N load and 20mm/s running-in speed, wiping off residual liquid on the surface by using absolute ethyl alcohol after running-in for 60min, and constructing a layer of nano borate film in a friction area.
And (3) testing: as shown in figure 4, 70wt% of glycerol and 30wt% of butyl tetraol liquid lubricant are added on the surface of the borate film, an RTEC multifunctional friction and wear testing machine is adopted, a heating program is started, the temperature is raised to 175 ℃, the load is 5N, the linear velocity is 18mm/s, the friction coefficient in a stable stage is 0.0065-0.01, and the borate film reaches a super-smooth state at high temperature.
Example 5: the construction method of the high-temperature liquid super-smooth borate nano film comprises the following steps:
s1: preparing a boron-based coating, namely putting a bearing steel disc workpiece with the diameter of 24mm and the thickness of 7.9mm into a boronizing furnace, and heating and preserving heat for 60min at 900 ℃ to obtain a workpiece coated with the boron-based coating; and after the workpiece is cooled, putting the workpiece into boiling hot water, heating for 2 hours to remove residual substances on the surface, and then putting the workpiece into a 100 ℃ oven for drying to obtain the boron-based coating workpiece with a clean surface.
S2: preparing a two-dimensional material solution, namely adding 0.05g of a two-dimensional material into 10g of deionized water, starting an ultrasonic cleaner, deagglomerating the two-dimensional material and uniformly dispersing the two-dimensional material in the deionized water to obtain a 0.5wt% two-dimensional material solution, wherein the working frequency is 50kHz, the ultrasonic power is 150W, and the oscillation time is 60min.
The two-dimensional material is one or more of graphene oxide, graphene, molybdenum disulfide, tungsten disulfide and hexagonal boron nitride, and the two-dimensional material is boron nitride.
S3: liquid lubricant solution preparation-0.5 g of liquid lubricant is dissolved in deionized water, an ultrasonic cleaner is started, the working frequency is 50kHz, the ultrasonic power is 100W, the oscillation time is 20min, and the liquid temperature is 50 ℃, so that a uniformly dispersed 20wt% liquid lubricant solution is obtained.
The liquid lubricant R-OH is preferably one or more of hydroxyl-containing substances such as methanol, ethylene glycol, glycerol, glucose, sucrose, and polyethylene glycol, wherein 0.4g of ethylene glycol and 0.1g of sucrose are used.
S4: suspension preparation-the liquid lubricant solution obtained in 5g of S3 was added to the two-dimensional material solution prepared in 5g of S2, and after ultrasonic treatment, a suspension containing 0.25wt% of the two-dimensional material and 20wt% of the liquid lubricant was obtained.
S5: forming, namely coating the suspension obtained in the step S4 on the surface of a workpiece by using a spin coating instrument, so that the surface of the workpiece is simultaneously provided with a compound of a boronizing layer, a two-dimensional material, a liquid lubricant and water;
opening the RTEC multifunctional friction wear testing machine, placing the composite side of the workpiece on the testing machine for running-in treatment, applying a load of 30N and a running-in speed of 20mm/s, wiping off liquid remained on the surface by using absolute ethyl alcohol after running-in for 60min, and constructing a layer of nanoscale borate film in a friction area.
And (3) testing: adding 50wt% of glycerol and 50wt% of erythritol liquid lubricant to the surface of the borate film, starting a heating program by adopting an RTEC multifunctional friction and wear testing machine, heating to 200 ℃, loading 10N, and linear velocity of 18mm/s, wherein the friction coefficient in a stable stage is 0.0095, and the borate film reaches an ultra-smooth state at high temperature.
Example 6: a borate nanofilm prepared as described in any of examples 1-5 above.
Example 7: a using method of the high-temperature liquid super-smooth borate nano film comprises the steps of adding a liquid lubricant to the surface of the borate nano film prepared in the embodiment 1-6, heating the borate nano film to 70-200 ℃, and applying a working load and speed to achieve a super-smooth state at a high temperature.
Comparative example 1: the behavior of testing the friction coefficient of the high-temperature liquid without the borate nano-film is carried out according to the following steps:
s1: preparing a boron-based high-hardness coating on the surface of a workpiece: specifically, a bearing steel disc workpiece with the diameter of 24mm and the thickness of 7.9mm is placed into a boronizing furnace and treated for 30min at 900 ℃ and the current of 20A, so as to obtain a workpiece coated with a boron-based coating.
S2: cleaning a boron-based coating workpiece: specifically, the boronized workpiece is taken out, cooled and then placed into boiling hot water, heated for 1 hour to remove residual substances on the surface, and placed into a 60 ℃ oven for drying treatment, so that the boron-based coating with a clean surface is obtained.
S3: and (3) testing: specifically, 50wt% of glycerol and 50wt% of erythritol liquid lubricant are added to the boronized surface, an RTEC multifunctional friction wear tester is adopted, a heating program is started, the temperature is raised to 70 ℃, the load is 5N, the speed is 10mm/s, the friction coefficient in a stable stage is 0.06, and the ultra-smooth state is not reached at high temperature.
Comparative example 2: the behavior of testing the friction coefficient of the high-temperature liquid without borate nano film is carried out according to the following steps:
s1: preparing a 1wt% graphene oxide two-dimensional material aqueous solution, specifically, adding 0.1g of graphene oxide into 10g of deionized water, starting an ultrasonic cleaner, wherein the working frequency of the ultrasonic cleaner is 50kHz, the ultrasonic power is 100W, and the ultrasonic time is 20min.
S2: preparing a 40wt% glycol aqueous solution, specifically, dissolving 0.4g glycol in deionized water, starting an ultrasonic cleaner, wherein the temperature of the ultrasonic cleaner is 50 ℃, the working frequency is 50kHz, the ultrasonic power is 100W, and the ultrasonic time is 10min, so as to obtain the 40wt% glycol aqueous solution.
S3: 5g of a 40wt% ethylene glycol aqueous solution was added to 5g of a 1wt% graphene oxide two-dimensional material aqueous solution, and subjected to ultrasonic treatment to obtain an aqueous solution containing 0.5wt% graphene oxide +20wt% ethylene glycol liquid lubricant.
S4: coating an aqueous solution containing 0.5wt% of graphene oxide and 20wt% of glycol liquid lubricant on the surface of a bearing steel workpiece (an original sample which is not subjected to boronizing treatment), and specifically, uniformly spreading the suspension by using a spin coater to ensure that the surface of the bearing steel simultaneously has a graphene oxide/glycol/water compound;
s5: running the compound on an RTEC multifunctional friction wear testing machine, applying 5N load, 10mm/s speed and room temperature, and wiping off residual liquid on the surface by using absolute ethyl alcohol after running-in for 20 min; since the original bearing steel surface does not contain B, no borate film is generated on the surface after running-in.
And (3) testing: adding 50wt% of glycerol and 50wt% of erythritol liquid lubricant, starting a heating program by adopting an RTEC multifunctional friction and wear testing machine, heating to 175 ℃, wherein the load is 5N, the speed is 18mm/s, the friction coefficient in a stable stage is 0.11, and the super-slip state is not reached at high temperature.
In conclusion, the prepared high-temperature liquid ultra-smooth borate nano film can realize a friction coefficient lower than 0.01 in a high-temperature liquid environment at 70-200 ℃, the temperature is obviously higher than the currently mainstream reported ultra-smooth room temperature environment, the constructed borate nano film has the characteristic of wide applicable temperature range, the temperature range comprises the temperature of common gear oil, the service temperature of an automobile engine and the temperature limit close to that of a liquid lubricant, and the borate nano film has good industrial application value, and can realize ultra-smooth behavior in an atmospheric environment without special inert atmosphere; the construction method of the high-temperature liquid ultra-smooth borate nano film can endow the critical metal-based moving parts such as bearings, gears and hydraulic pumps of the aircraft engine with low friction coefficients in a high-temperature service state, and realizes high-reliability long-life lubrication of the critical parts.

Claims (10)

1. A construction method of a high-temperature liquid super-smooth borate nano-film is characterized by comprising the following steps:
preparing a boronizing layer on the surface of a workpiece, cleaning the boronized workpiece in boiling water, and drying to remove residual substances on the surface of the workpiece;
adding a two-dimensional material into deionized water; dissolving a liquid lubricant in deionized water; adding a liquid lubricant solution into a two-dimensional material solution, and carrying out ultrasonic treatment to obtain a uniformly dispersed two-dimensional material suspension, wherein the two-dimensional material accounts for 0.01-1 wt%, and the liquid lubricant accounts for 5-50 wt%;
coating the two-dimensional material suspension on the surface of a workpiece containing a boron-based coating to form a compound, mounting the workpiece on an abrasion tester to grind the compound, applying a load not greater than 30N, wherein the grinding speed is not less than 10mm/s, and after grinding for 5-60 min, cleaning the residual two-dimensional material suspension to obtain the borate nano film.
2. The method for constructing a high-temperature liquid ultra-smooth borate nano-film according to claim 1, wherein the two-dimensional material is one or more of graphene oxide, graphene, molybdenum disulfide, tungsten disulfide, and hexagonal boron nitride.
3. The method for constructing the high-temperature liquid super-smooth borate nano-film according to claim 1 or 2, wherein the liquid lubricant is one or more of R-OH.
4. The method for constructing the high-temperature liquid ultra-smooth borate nano-film according to claim 1, wherein the borate nano-film has a thickness of 3 to 100nm.
5. The method for constructing the high-temperature liquid super-smooth borate nano-film as claimed in claim 1, wherein the two-dimensional material solution is ultrasonically treated at a frequency of 40-60 kHz with a power of 100-200W for 15-60 min.
6. The method for constructing the high-temperature liquid super-smooth borate nano-film according to claim 1, wherein the liquid lubricant solution is subjected to ultrasonic treatment at a temperature of 40-60 ℃, a frequency of 40-60 kHz, a power of 100-150W and a treatment time of 10-20 min during preparation of the liquid lubricant solution.
7. The method for constructing the high-temperature liquid super-smooth borate nano-film as claimed in claim 1, wherein the ultrasonic treatment frequency is 40-60 kHz, the power is 30-500W, and the treatment time is 10-120 min when preparing the two-dimensional material suspension.
8. The method for constructing a high-temperature liquid super-smooth borate nano-film according to claim 1, wherein the residual liquid is washed with absolute ethyl alcohol.
9. A high temperature liquid ultra-smooth borate nanofilm prepared by the method of any one of claims 1-8.
10. The use method of the high-temperature liquid super-smooth borate nano-film is characterized in that a liquid lubricant is added to the surface of the borate nano-film prepared by the method in any one of claims 1 to 8, the temperature is raised to 70-200 ℃ after heating, and the working load and speed are applied.
CN202210469388.4A 2022-04-28 2022-04-28 High-temperature liquid super-smooth borate nano-film and construction method and use method thereof Pending CN115558926A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08103724A (en) * 1994-10-04 1996-04-23 Nippon Steel Corp Surface treatment method for steel pipe joint of excellent resistance to galling
US20210094067A1 (en) * 2019-09-30 2021-04-01 Uchicago Argonne, Llc Low friction coatings
CN113512459A (en) * 2021-07-13 2021-10-19 西北工业大学 Ultra-low friction solid-liquid composition containing boronizing layer and method for reducing friction of workpiece by using ultra-low friction solid-liquid composition

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08103724A (en) * 1994-10-04 1996-04-23 Nippon Steel Corp Surface treatment method for steel pipe joint of excellent resistance to galling
US20210094067A1 (en) * 2019-09-30 2021-04-01 Uchicago Argonne, Llc Low friction coatings
CN113512459A (en) * 2021-07-13 2021-10-19 西北工业大学 Ultra-low friction solid-liquid composition containing boronizing layer and method for reducing friction of workpiece by using ultra-low friction solid-liquid composition

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