CN114539884A - Composite super-lubricating coating material, preparation method thereof, composite super-lubricating coating and application - Google Patents
Composite super-lubricating coating material, preparation method thereof, composite super-lubricating coating and application Download PDFInfo
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- CN114539884A CN114539884A CN202210369110.XA CN202210369110A CN114539884A CN 114539884 A CN114539884 A CN 114539884A CN 202210369110 A CN202210369110 A CN 202210369110A CN 114539884 A CN114539884 A CN 114539884A
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- polysiloxane
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- lubricating coating
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16C—SHAFTS; FLEXIBLE SHAFTS; ELEMENTS OR CRANKSHAFT MECHANISMS; ROTARY BODIES OTHER THAN GEARING ELEMENTS; BEARINGS
- F16C33/00—Parts of bearings; Special methods for making bearings or parts thereof
- F16C33/02—Parts of sliding-contact bearings
- F16C33/04—Brasses; Bushes; Linings
- F16C33/20—Sliding surface consisting mainly of plastics
- F16C33/201—Composition of the plastic
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16C—SHAFTS; FLEXIBLE SHAFTS; ELEMENTS OR CRANKSHAFT MECHANISMS; ROTARY BODIES OTHER THAN GEARING ELEMENTS; BEARINGS
- F16C2202/00—Solid materials defined by their properties
- F16C2202/50—Lubricating properties
Abstract
The invention relates to the technical field of high polymer materials, in particular to a composite super-lubricating coating material, a preparation method thereof, a composite super-lubricating coating and application thereof. The composite coating material contains epoxy resin monomer, curing agent and polysiloxane; the polysiloxane is selected from at least one of amino terminated polysiloxane, vinyl terminated polysiloxane, methyl terminated polysiloxane and hydroxyl terminated polysiloxane. The composite super-lubricating coating material provided by the invention can be used for preparing a composite super-lubricating coating which has an ultralow friction coefficient and extremely high wear resistance in various environments such as vacuum, dry nitrogen, dry air and high-humidity air, and the coating is compact and uniform and has good adhesiveness.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a composite super-lubricating coating material, a preparation method thereof, a composite super-lubricating coating and application thereof.
Background
In recent years, due to demands for high precision, high reliability and high transmission efficiency of mechanical equipment, demands for self-lubricating bearings and transmission parts having ultra-low friction/wear properties have been increasing. Therefore, the development of novel high-performance self-lubricating coating materials and technologies has great significance for the development of future important equipment and high-technology fields in China.
Ultra-lubricity can be divided into solid ultra-lubricity (including structural ultra-lubricity) and liquid ultra-lubricity. At present, a material system capable of realizing solid ultra-smoothness mainly comprises amorphous carbon, graphene, molybdenum disulfide and the like. However, the tribological properties of these materials are very significantly affected by the ambient atmosphere and humidity. For example, carbon-based super-lubricity materials such as amorphous carbon and graphene generally have super-lubricity only in a dry atmosphere and in vacuum, and the friction coefficient is difficult to reach a super-lubricity level in a high-humidity environment.
Epoxy resin is a very important coating material, and has wide application in the field of material surface protection due to good adhesion and corrosion resistance. But the overall coefficient of friction is high (>0.6) and the wear resistance is poor. At present, the antifriction and antiwear performance of epoxy resin is greatly modified by a nano composite technology. However, up to now, epoxy resin coating materials having stable super-lubricating properties have been rarely reported and disclosed.
Disclosure of Invention
The invention aims to solve the problems of high friction coefficient, poor abrasion resistance and the like of a propylene oxide coating material in the prior art, and provides a composite super-lubricating coating material, a preparation method thereof, a composite super-lubricating coating and application thereof.
In order to achieve the above object, the present invention provides, in one aspect, a composite super-lubricating coating material comprising an epoxy resin monomer, a curing agent, and a polysiloxane;
the polysiloxane is selected from at least one of amino terminated polysiloxane, vinyl terminated polysiloxane, methyl terminated polysiloxane and hydroxyl terminated polysiloxane.
The second aspect of the invention provides a preparation method of the composite super-lubricating coating material, which comprises the following steps:
the method comprises the following steps: adding the epoxy resin monomer and the curing agent according to the proportion, carrying out first ball milling, and uniformly mixing; adding the polysiloxane according to the proportion and carrying out second ball milling to obtain the composite super-lubricating coating material; or
The second method comprises the following steps: and dissolving the polysiloxane in an organic solvent, adding an epoxy resin monomer and a curing agent according to a proportion, stirring and mixing uniformly, and heating to remove the organic solvent to obtain the composite super-lubricating coating material.
In a third aspect, the invention provides a composite super-lubricating coating prepared from the composite super-lubricating coating material.
In a fourth aspect, the invention provides a composite super-lubricating coating material and application of the composite super-lubricating coating in a transmission bearing.
The composite super-lubricating coating material provided by the invention can be used for preparing a composite super-lubricating coating which has an ultralow friction coefficient and extremely high wear resistance in various environments (such as vacuum, dry nitrogen, dry air and high-humidity air), and the coating is compact and uniform and has good adhesiveness.
Drawings
FIG. 1 is an SEM image of a cross section of a composite super-lubricating coating provided in example 1 of the present invention;
FIG. 2 is a friction curve diagram of the composite super-lubricating coating provided by the embodiment 1 of the invention in an atmospheric environment;
FIG. 3 is a friction curve of the composite super-lubricating coating provided in example 1 of the present invention in dry nitrogen;
FIG. 4 is a graph of the friction profile in air for a coating without polysiloxane provided in comparative example 1.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
According to a first aspect of the present invention, there is provided a composite super-lubricating coating material comprising an epoxy resin monomer, a curing agent and a polysiloxane;
the polysiloxane is selected from at least one of amino terminated polysiloxane, vinyl terminated polysiloxane, methyl terminated polysiloxane and hydroxyl terminated polysiloxane. The composite super-lubricating coating material provided by the invention can be used for preparing a composite super-lubricating coating which has an ultralow friction coefficient and extremely high wear resistance in various environments (such as vacuum, dry nitrogen, dry air and high-humidity air), and the coating is compact and uniform, good in adhesion and high in light transmittance.
In the present invention, the polysiloxane is polydimethylsiloxane as in the art.
According to a preferred embodiment of the present invention, the mass ratio of the epoxy resin monomer to the curing agent is 1-3:3-1 in terms of mass ratio.
According to a preferred embodiment of the invention, the polysiloxane constitutes from 1% to 30% by weight, preferably from 2 to 8% by weight, of the total mass of the coating material.
According to a preferred embodiment of the present invention, the methyl-terminated polysiloxane is a dimethyl-terminated polysiloxane and/or a trimethyl-terminated polysiloxane.
According to a preferred embodiment of the invention, the polysiloxane is an amino-terminated polysiloxane and/or a hydroxyl-terminated polysiloxane, preferably an amino-terminated polydimethylsiloxane and a hydroxyl-terminated polydimethylsiloxane.
According to a preferred embodiment of the present invention, the mass ratio of the amino-terminated polydimethylsiloxane to the hydroxyl-terminated polydimethylsiloxane is 1:0.6 to 1.5.
In the present invention, the epoxy resin monomer is not particularly limited, and epoxy resin monomers in the art can be used as the epoxy resin monomer of the present invention, and preferably, the epoxy resin monomer is at least one selected from the group consisting of bisphenol a type, bisphenol F type, aliphatic glycidyl ether and glycidyl ester type epoxy resin monomers. Preferably, the epoxy resin monomer is at least one of diglycidyl ether of bisphenol a, 3, 4-epoxycyclohexylmethyl-3, 4-epoxycyclohexylformate, and diglycidyl ester of 4, 5-epoxytetrahydrophthalic acid.
According to a preferred embodiment of the present invention, the epoxy resin monomer is a mixture of 3, 4-epoxycyclohexylmethyl-3, 4-epoxycyclohexylformate and bisphenol a diglycidyl ether, preferably, the mass ratio of 3, 4-epoxycyclohexylmethyl-3, 4-epoxycyclohexylformate to bisphenol a diglycidyl ether is 1: 2-4.
According to a preferred embodiment of the present invention, the curing agent is selected from at least one of amine or pyridine curing agents, preferably at least one of ethylenediamine, diphenylamine, aminodiphenylsulfone, polyamide, polyimide, polyetheramine, aminopyridine, vinylpyridine, and polyvinylpyridine.
The second aspect of the invention provides a preparation method of the composite super-lubricating coating material, which comprises the following steps:
the method comprises the following steps: adding the epoxy resin monomer and the curing agent according to the proportion, carrying out first ball milling, and uniformly mixing; adding the polysiloxane according to the proportion and carrying out second ball milling to obtain the composite super-lubricating coating material; or
The second method comprises the following steps: and dissolving the polysiloxane in an organic solvent, adding an epoxy resin monomer and a curing agent according to a proportion, stirring and mixing uniformly, and heating to remove the organic solvent to obtain the composite super-lubricating coating material.
According to a preferred embodiment of the present invention, in the first method, the conditions of the first ball mill and the second ball mill independently comprise: the ball milling temperature is 20-60 ℃, the ball milling time is reasonably adjusted according to the ball milling temperature, and preferably, the ball milling time is 20-60 min.
According to a preferred embodiment of the present invention, in the second method, the mass ratio of the total mass of the polysiloxane, the epoxy resin monomer and the curing agent to the solvent is 1: 0.5-20.
According to a preferred embodiment of the present invention, in the second method, the heating temperature is not particularly limited as long as the organic solvent can be evaporated and removed, and preferably, the heating temperature is 40 to 200 ℃.
According to a preferred embodiment of the present invention, the organic solvent is at least one selected from the group consisting of methanol, ethanol, isopropanol and n-butanol.
According to a preferred embodiment of the present invention, in the second method, the mass ratio of the polysiloxane to the organic solvent is 0.001-0.4: 1.
According to a preferred embodiment of the invention, the prepared composite super-lubricating coating material can be pre-cured at 25-100 ℃, for example, epoxy resin monomer and amine curing agent are pre-cured at 25-45 ℃ and 2000 rpm, so as to adjust the viscosity of the composite super-lubricating coating material.
In a third aspect, the invention provides a composite super-lubricating coating prepared from the composite super-lubricating coating material.
The preparation method of the composite super-lubricating coating is not particularly limited, and for example, the composite super-lubricating coating material can be sprayed on the surface of a workpiece by a high-pressure spray gun; and curing at 40-200 ℃, preferably, curing for 12-24 hours to obtain the composite super-lubricating coating. The thickness of the coating is controlled to be 2-200 μm by adjusting the spraying time. The coating can be prepared by an injection method, for example, a workpiece is placed in a mould, then the composite super-lubricating coating material is injected into the mould and cured at the temperature of 40-200 ℃, and preferably, the composite super-lubricating coating is obtained after 12-24 hours of curing.
According to a preferred embodiment of the present invention, the coefficient of friction of the composite super-lubricating coating is 0.001 to 0.01.
According to a fourth aspect of the invention, the invention provides a composite super-lubricating coating material and application of the composite super-lubricating coating in a transmission bearing. The composite super-lubricating coating material has high bonding strength and is suitable for lubrication and wear-resistant protection of the surfaces of ceramics, plastics and various metal-based transmission bearings.
The present invention will be described in detail below by way of examples.
The transparency test method comprises the following steps:
the friction coefficient and wear resistance test method comprises the following steps: the friction wear tester with controllable environment is utilized, a ball-disc contact mode is adopted, the friction coefficient and the wear resistance of the composite super-lubricating coating are respectively tested in the environment of atmosphere (humidity is 10-90%) and dry nitrogen, and the test parameters are as follows: loading: 2-3N, speed: 0.1m/s, sliding mode: rotating, sliding for 60min, and pairing materials including 6mm bearing steel ball (CCr15), silicon nitride ball and alumina ball.
Example 1
(1) Respectively weighing 0.25g of bisphenol A diglycidyl ether epoxy monomer and curing agent (polyamide 650), adding the epoxy monomer and the curing agent into 6.0g of n-butyl alcohol solution dissolved with 0.015g of amino-terminated polydimethylsiloxane, carrying out ultrasonic treatment for 40min to completely dissolve the bisphenol A diglycidyl ether and the curing agent, stirring at the rotating speed of 600 revolutions per minute for 3h, and then placing in an oven at the temperature of 130 ℃ for baking for 10h to obtain the composite super-lubricating coating material;
(2) horizontally placing a stainless steel substrate in a polytetrafluoroethylene die, dripping the composite super-lubricating coating material prepared in the step (1) into the die, and curing at 50 ℃ for 18 hours to obtain the composite super-lubricating coating.
The initial coefficient of friction, the average coefficient of friction over 60min of slip test results are shown in table 1.
The Scanning Electron Microscope (SEM) image of the coating section is shown in figure 1, which shows that the coating prepared by the invention has the advantages of compactness, uniformity and good adhesiveness.
The friction curve of the composite super-lubricating coating provided by the embodiment 1 in the atmospheric environment is shown in FIG. 2; therefore, the coating prepared by the preparation method disclosed by the invention has a low friction coefficient in an atmospheric environment, and has a low average friction coefficient within 60min and a low average friction coefficient within 60min, which indicates that the coating has extremely high wear resistance.
The friction curve of the composite super-lubricating coating provided by the example 1 in dry nitrogen is shown in FIG. 3; therefore, the coating prepared by the preparation method disclosed by the invention has a low friction coefficient in a dry atmospheric environment, the average friction coefficient within 60min is low, and the average friction coefficient within 60min is low, so that the coating has extremely high wear resistance.
Example 2
(1) Weighing 0.75g of bisphenol A diglycidyl ether epoxy monomer and 0.25g of curing agent (polyamide 650), placing the monomers and the curing agent in a ball milling tank, ball milling for 60 minutes at the rotating speed of 400 revolutions per minute in the environment of room temperature (25 ℃), uniformly mixing the resin monomers and the curing agent, adding 0.015g of hydroxyl-terminated polydimethylsiloxane, and stirring for 3 hours at the rotating speed of 600 revolutions per minute under the condition of room temperature to obtain the composite super-lubricating coating material;
(2) spraying the composite super-lubricating coating material on the surface of a workpiece (stainless steel sheet) by using a high-pressure spray gun, and standing the sprayed workpiece in a 120 ℃ oven for 12 hours to cure the coating.
The initial coefficient of friction, the average coefficient of friction over 60min of slip test results are shown in table 1.
Example 3
(1) Weighing 0.25g of 3, 4-epoxy cyclohexyl methyl-3, 4-epoxy cyclohexyl formic ether epoxy monomer and 0.25g of curing agent (ethylene diamine) and placing the monomers and the curing agent in a ball milling tank, ball milling for 60min at the rotating speed of 400 r/min in the environment of room temperature (25 ℃), uniformly mixing the resin monomers and the curing agent, adding 0.015g of amino-terminated polydimethylsiloxane, and stirring for 3h at the rotating speed of 600 r/min at the room temperature to obtain the composite super-lubricating coating material;
(2) horizontally placing the stainless steel wafer in a polytetrafluoroethylene die, dripping the super-lubricating coating material prepared in the step (1) into the die, and curing at 180 ℃ for 12 hours to obtain the composite super-lubricating coating.
The initial coefficient of friction, the average coefficient of friction over 60min of slip test results are shown in table 1.
Example 4
Compared with the embodiment 1, the difference is that the epoxy resin monomer is a mixture of 3, 4-epoxy cyclohexyl methyl-3, 4-epoxy cyclohexyl formate and bisphenol A diglycidyl ether epoxy resin monomer, and the mass ratio is 1: 3; the other conditions were the same as in example 1.
The initial coefficient of friction, the average coefficient of friction over 60min of slip test results are shown in table 1.
Example 5
The procedure is as in example 1 except that the polysiloxane is a hydroxy terminated polydimethylsiloxane.
The initial coefficient of friction, the average coefficient of friction over 60min of slip test results are shown in table 1.
Example 6
The difference from example 5 was that the amount of the hydroxyl terminated polydimethylsiloxane was 0.032g, and the other conditions were the same as example 5.
The initial coefficient of friction, the average coefficient of friction over 60min of slip test results are shown in table 1.
Example 7
The same procedure as in example 5 was repeated, except that the amount of the hydroxyl-terminated polydimethylsiloxane used was 0.1.25g, as compared with example 5.
The initial coefficient of friction, the average coefficient of friction over 60min of slip test results are shown in table 1.
Example 8
The difference from example 6 is that the polysiloxane is a mixture of hydroxy terminated polydimethylsiloxane and amino terminated polydimethylsiloxane in a 1:1 ratio by mass, the other conditions being the same as example 6.
The initial coefficient of friction, the average coefficient of friction over 60min of slip test results are shown in table 1.
Comparative example 1
(1) Weighing 0.25g of bisphenol F resin monomer and 0.25g of curing agent (polyamide 650), placing the mixture in a ball milling tank, ball milling the mixture for 60 minutes at the rotating speed of 400 revolutions per minute in the environment of room temperature (25 ℃), uniformly mixing the resin monomer and the curing agent, and ball milling the mixture for 60 minutes at the room temperature to obtain a coating material;
(2) and (3) spraying the coating material on the surface of a workpiece (a stainless steel wafer) by using a high-pressure spray gun, and standing the sprayed workpiece in a drying oven at 100 ℃ for 12 hours to cure the coating.
The initial coefficient of friction, the average coefficient of friction over 60min of slip test results are shown in table 1.
The friction curve of the coating prepared in comparative example 1 in air is shown in fig. 4, and it can be seen that the coefficient of friction value of the coating exceeds 0.6.
Comparative example 2
Compared with the coating of the embodiment 1, the difference is that the polysiloxane is benzyl end-capped polydimethylsiloxane, the percentage of the total mass of the coating is 12 percent, and the other conditions are the same as the embodiment 1.
The initial coefficient of friction, the average coefficient of friction over 60min of slip test results are shown in table 1.
TABLE 1
The results in table 1 show that the composite super-lubricating coating material provided by the invention has an ultra-low friction coefficient, and the average friction coefficient within 60min is low, which indicates that the composite super-lubricating coating material has extremely high wear resistance.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. The composite super-lubricating coating material is characterized by comprising an epoxy resin monomer, a curing agent and polysiloxane;
the polysiloxane is selected from at least one of amino terminated polysiloxane, vinyl terminated polysiloxane, methyl terminated polysiloxane and hydroxyl terminated polysiloxane.
2. The composite super-lubricious coating material of claim 1,
the polysiloxane accounts for 1 to 30 weight percent of the total mass of the coating material, and preferably 2 to 8 weight percent; and/or
The mass ratio of the epoxy resin monomer to the curing agent is 1-3: 3-1.
3. The composite super lubricant coating material according to claim 1 or 2,
the methyl terminated polysiloxane is dimethyl terminated polysiloxane and/or trimethyl terminated polysiloxane; and/or
The epoxy resin monomer is selected from at least one of bisphenol A type, bisphenol F type, polyphenol type glycidyl ether, aliphatic glycidyl ether and glycidyl ester type epoxy resin monomer; and/or
The curing agent is selected from at least one of amine and/or pyridine curing agents, preferably at least one of ethylenediamine, diphenylamine, aminodiphenylsulfone, polyamide, polyimide, polyether amine, aminopyridine, vinylpyridine and polyvinylpyridine.
4. The composite super lubricant coating material according to any one of claims 1 to 3,
the epoxy resin monomer is a mixture of aliphatic glycidyl ether and bisphenol A type glycidyl ether, and preferably, the mass ratio of the aliphatic glycidyl ether to the bisphenol A type glycidyl ether is 1: 2-4; and/or
The polysiloxane is amino-terminated polysiloxane and/or hydroxyl-terminated polysiloxane, preferably amino-terminated polydimethylsiloxane and hydroxyl-terminated polydimethylsiloxane.
5. The method for preparing the composite super-lubricating coating material as claimed in any one of claims 1 to 4, wherein the method comprises the following steps:
the method comprises the following steps: adding the epoxy resin monomer and the curing agent according to the proportion, carrying out first ball milling, and uniformly mixing; adding the polysiloxane according to the proportion and carrying out second ball milling to obtain the composite super-lubricating coating material; or
The second method comprises the following steps: and dissolving the polysiloxane in an organic solvent, adding an epoxy resin monomer and a curing agent according to a proportion, stirring and mixing uniformly, and heating to remove the organic solvent to obtain the composite super-lubricating coating material.
6. The production method according to claim 5,
in the first method, the conditions of the first ball milling and the second ball milling independently comprise: the ball milling temperature is 25-100 ℃, and the ball milling time is 30-360 min; and/or
In the second method, the mass ratio of the total mass of the polysiloxane, the epoxy resin monomer and the curing agent to the solvent is 1: 0.5-20; the heating temperature is 40-200 ℃.
7. The production method according to claim 5 or 6,
in the second method, the mass ratio of the polysiloxane to the organic solvent is 0.001-0.4: 1; the organic solvent is selected from at least one of methanol, ethanol, isopropanol and n-butanol.
8. A composite super-lubricating coating prepared from the composite super-lubricating coating material as claimed in any one of claims 1 to 4.
9. The composite super-lubricious coating of claim 8,
the friction coefficient of the composite super-lubricating coating is 0.001-0.01.
10. Use of the composite super-lubricating coating material of any one of claims 1 to 4 and the composite super-lubricating coating of claim 8 or 9 in a drive bearing.
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| CN115521708A (en) * | 2022-10-20 | 2022-12-27 | 陕西科技大学 | Super-lubricating coating based on polydimethylsiloxane polymer molecular brush and preparation method thereof |
| CN116285659A (en) * | 2023-02-17 | 2023-06-23 | 长沙理工大学 | Method for preventing bone fragments on surface of medical miniature abrasive drill from adhering |
| CN116790304A (en) * | 2023-06-28 | 2023-09-22 | 江西理工大学 | Solid-oil composite super-lubrication system and application thereof |
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