CN115521708A - Super-lubricating coating based on polydimethylsiloxane polymer molecular brush and preparation method thereof - Google Patents
Super-lubricating coating based on polydimethylsiloxane polymer molecular brush and preparation method thereof Download PDFInfo
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- CN115521708A CN115521708A CN202211283011.6A CN202211283011A CN115521708A CN 115521708 A CN115521708 A CN 115521708A CN 202211283011 A CN202211283011 A CN 202211283011A CN 115521708 A CN115521708 A CN 115521708A
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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
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/10—Block or graft copolymers containing polysiloxane sequences
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
- B05D5/08—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/50—Multilayers
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- B05D7/54—No clear coat specified
- B05D7/548—No curing step for the last layer
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
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Abstract
The invention relates to the technical field of preparation of super-lubricating coating materials, and particularly discloses a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush and a preparation method thereof, wherein the preparation method comprises the following steps: adding an organic solvent into the epoxy resin, stirring and adding a curing agent and polydimethylsiloxane, and dispersing the component 1; adding an organic solvent into the epoxy resin, stirring, adding polydimethylsiloxane, and dispersing to obtain a component 2; mixing the component 1 and the component 2, and stirring to obtain a mixture; and spraying the mixture on the surface of a substrate, solidifying, dripping non-polar liquid C on the surface of the coating, and standing to obtain the super-lubricating coating based on the polydimethylsiloxane polymer molecular brush. The lubricating coating obtained by the preparation method of the polydimethylsiloxane polymer molecular brush-based super-lubricating coating has the advantages of high wear resistance and low friction coefficient.
Description
Technical Field
The invention relates to the technical field of preparation of super-lubricating coating materials, in particular to a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush and a preparation method thereof.
Background
The friction and the abrasion cause the damage and the failure of the device, the service life is shortened, the fuel resource is used more rapidly, and the resource and the energy are wasted seriously. While a lubricious coating is critical to minimize damage to the underlying material and ensure low energy dissipation in the mechanical system. Polymer molecular brushes (such as polydimethylsiloxane molecular brushes) are bionic in the microstructure and the lubricating mechanism of natural synovial joints, and polymer chains form brush-type structures on the surfaces with high grafting density in a good solvent due to the exclusion of volume-dominant inter-chain interactions. Polymer molecular brushes as a lubricious coating can reduce the coefficient of dynamic friction of the modified surface by several orders of magnitude compared to bare or oil lubricated surfaces, thus drawing considerable attention from researchers.
The preparation method of the polymer molecular brush super-lubricating coating comprises a surface grafting method and a coating method, wherein a PDMS brush is introduced into thermosetting resin such as epoxy resin, polyurethane resin and the like. During curing, PDMS is grafted in an epoxy resin system through a ring-opening polymerization reaction, and tends to gather towards the surface of a coating due to the low surface energy and high flow characteristic of PDMS, so that a dense polymer molecular brush layer is formed on the surface of the coating.
However, the inventors found that the wear resistance of the polymer molecular brush super-lubricating coating in the related art needs to be improved, and a super-lubricating coating with high wear resistance and low friction coefficient is needed.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush and a preparation method thereof, so that the epoxy super-lubricating coating has high wear resistance and low friction coefficient.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a method for preparing a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush.
A preparation method of a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush comprises the following steps:
step one, preparing a component 1:
adding an organic solvent into the epoxy resin, stirring, adding a curing agent and polydimethylsiloxane, and performing ultrasonic dispersion to obtain a component 1; taking the total mass of the epoxy resin, the polydimethylsiloxane and the curing agent as a reference, the mass percent of the epoxy resin is 50-56%, the mass percent of the polydimethylsiloxane is 4-8%, and the balance is the curing agent;
step two, preparing a component 2:
adding an organic solvent into the epoxy resin, stirring, adding polydimethylsiloxane, and performing ultrasonic dispersion to obtain a component 2; based on the total mass of the epoxy resin and the polydimethylsiloxane, the mass percent of the epoxy resin is 80-90%, and the mass percent of the polydimethylsiloxane mixture is 10-20%;
step three, preparing a super-lubricating coating based on the polydimethylsiloxane polymer molecular brush:
mixing the component 1 and the component 2, and stirring to obtain a mixture; and spraying the mixture on the surface of a substrate, solidifying, dropwise adding a non-polar liquid C on the surface of the coating, and standing to obtain the super-lubricating coating based on the polydimethylsiloxane polymer molecular brush.
Further, the epoxy resin is one or more of bisphenol a type epoxy resin, bisphenol F type epoxy resin, aliphatic glycidyl ether type epoxy resin, glycidyl ester type epoxy resin, or glycidyl amine type epoxy resin.
Further, the polydimethylsiloxane is one or more of monoglycidyl ether end-capped polydimethylsiloxane, diglycidyl ether end-capped polydimethylsiloxane and trimethyl siloxane end-capped polydimethylsiloxane; the concentration of the polydimethylsiloxane molecular brush solution is 0.8-1 mol/L.
Further, the curing agent in the first step is one of polyamide, ethylenediamine, polyetheramine and diethylenetriamine.
Further, the nonpolar liquid C in the third step is one of methyl silicone oil, ethyl silicone oil, phenyl silicone oil, methyl hydroxy silicone oil, hydroxy hydrogen-containing silicone oil, dodecane, hexadecane, poly-alpha-olefin, toluene, isopropanol, and dimethylformamide.
Further, the organic solvent in the first step is one or more of ethyl acetate and ethanol; and in the second step, the organic solvent is one or more of acetone, toluene and xylene.
Furthermore, the curing temperature in the third step is 120-130 ℃, and the curing time is 2-3 h.
Further, the spraying pressure in the third step is 1500-1900 Psi.
Further, the standing environment after the nonpolar liquid C is dripped in the third step is a ventilated dust-free environment.
In a second aspect, the present invention provides a super-lubricious coating based on a polydimethylsiloxane polymer molecular brush.
A super-lubricating coating based on a polydimethylsiloxane polymer molecular brush is prepared by the method.
Compared with the prior art, the invention has the following technical effects:
the fluidity and extensibility of the polymer molecular brush influence the surface friction performance, while the nonpolar liquid (such as methyl silicone oil, phenyl silicone oil, hexadecane, poly-alpha-olefin, toluene, isopropanol and the like) has good miscibility with the polymer chain, which can cause the expansion of the polymer chain to increase the liquid fluidity of the polymer chain, thus being beneficial to remarkably improving the bearing capacity and lubricity of the friction surface of the coating by reducing the shear strength and improving the friction performance of the coating.
In the super-lubricating coating based on the polydimethylsiloxane polymer molecular brush, PDMS and epoxy resin are subjected to ring-opening polymerization reaction at high temperature and are connected together orderly and compactly, and a compact polydimethylsiloxane chain brush is formed on the surface of the coating. Non-polar liquids such as silicone oil have low surface tension. Has good compatibility with PDMS chains. When they come into contact, the surface of the coating is dissolved by a non-polar liquid such as silicone oil, which causes the polymer chains to move and rotate, just like a brush. Meanwhile, the PDMS chain is connected with the coating through a covalent bond, so that the compact polydimethylsiloxane chain brush layer has good mechanical strength and stability.
In addition, the good miscibility of the polymer chain and nonpolar liquids such as silicone oil can cause the expansion of the polymer chain, increase the liquid fluidity of the polymer chain, and be beneficial to the coating to remarkably improve the bearing capacity and lubricity of the friction surface by reducing the shear strength, thereby improving the friction performance of the coating. Finally, a liquid lubricating layer generated by dripping non-polar liquid such as silicon oil on the surface of the coating plays a role in lubricating, and simultaneously can cover the defects existing on the surface of the coating and not covered by the PDMS chain brush, so that the stability and the wear resistance of the coating are enhanced.
Therefore, the polydimethylsiloxane polymer molecular brush super-lubricating coating prepared by the method has good wear resistance, lubricating property and stability and better controllability.
Drawings
FIG. 1 is a pictorial representation of a coating in accordance with example 1 of the present invention;
FIG. 2 is a scanning electron microscope photograph of a polydimethylsiloxane polymer molecular brush super-lubricating coating prepared in example 1 of the present invention;
FIG. 3 is a graph of the wear scar and 3D topography of the PDMS polymer brush super-lubricating coating prepared in example 1 after friction test;
FIG. 4 is a plot of the friction coefficients of the lubricating coatings prepared in examples 1, 2, 3 of the present invention;
FIG. 5 is a plot of the friction coefficient of the lubricating coatings prepared in examples 4, 5 of the present invention;
FIG. 6 is a bar graph of the average coefficient of friction of the lubricating coatings prepared in examples 1, 2, 3 of the present invention;
FIG. 7 is a bar graph of wear rates of lubricating coatings prepared according to examples 1, 2, and 3 of the present invention;
FIG. 8 is a bar graph of the average coefficient of friction of the ultra-slip coatings prepared in inventive example 1 and comparative examples 1 and 2.
Detailed Description
The present invention will be explained in further detail with reference to examples.
The base material used in the embodiment of the invention is 1060 aluminum plate, and the base material is provided with a pretreatment step before spraying, and the pretreatment step of the base material is specifically wiping with absolute ethyl alcohol before spraying.
Examples
Example 1
A preparation method of a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush comprises the following steps:
step one, preparing a component 1:
adding 2.6g of tetraglycidyl amine type epoxy resin, 25ml of absolute ethyl alcohol and 25ml of ethyl acetate into a 100ml beaker, stirring and dispersing for 40min on a magnetic stirrer at the rotating speed of 2000r/min, then adding 2.2g of polyamide and 0.2g of mono-glycidyl ether terminated polydimethylsiloxane, and performing ultrasonic dispersion for 20min to obtain a coating component 1;
step two, preparing a component 2:
adding 0.9g of tetraglycidyl amine type epoxy resin, 25ml of acetone and 25ml of xylene into a 100ml beaker, stirring and dispersing for 35min on a magnetic stirrer at the rotating speed of 1500r/min, then adding 0.05g of mono-glycidyl ether terminated polydimethylsiloxane and 0.05g of diglycidyl ether terminated polydimethylsiloxane, and ultrasonically dispersing for 15min to obtain a coating component 2;
step three, preparing a super-lubricating coating based on the polydimethylsiloxane polymer molecular brush:
firstly, mixing the component 1 and the component 2 in a 200ml beaker, and dispersing for 45min at the rotating speed of 2000r/min on magnetic stirring to obtain a mixture; then, the mixture was added to a spray equipment, sprayed onto the substrate surface at a pressure of 1500Psi, and the coating was cured at 120 ℃ for two hours; and finally, dripping 5ml of methyl silicone oil on the surface of the cured coating by using a dropper, and standing for 2 hours in a ventilated dust-free environment to obtain the super-lubricating coating based on the polydimethylsiloxane polymer molecular brush.
From FIG. 1, it can be seen that the polydimethylsiloxane polymer molecular brush super-lubricating coating prepared by the invention is flat and smooth; from FIG. 2, it can be seen that the surface of the coating is distributed with silicon oil pools with diameters varying from 8 to 77 μm.
Example 2
A preparation method of a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush comprises the following steps:
step one, preparing a component 1:
adding 2.55g of bisphenol A epoxy resin and 50ml of absolute ethyl alcohol into a 100ml beaker, stirring and dispersing for 45min on a magnetic stirrer at the rotating speed of 1800r/min, adding 2.15g of polyetheramine and 0.3g of mono-glycidyl ether terminated polydimethylsiloxane, and performing ultrasonic dispersion for 20min to obtain a coating component 1;
step two, preparing a component 2:
adding 0.85g of bisphenol A epoxy resin and 50ml of acetone into a 100ml beaker, stirring and dispersing for 30min on a magnetic stirrer at a rotating speed of 1600r/min, adding 0.15g of monoglycidyl ether terminated polydimethylsiloxane, and performing ultrasonic dispersion for 15min to obtain a coating component 2;
step three, preparing a super-lubricating coating based on the polydimethylsiloxane polymer molecular brush:
firstly, mixing the component 1 and the component 2 in a 200ml beaker, and dispersing for 50min at the rotating speed of 1800r/min on magnetic stirring to obtain a mixture; then, the mixture is added into a spraying device, sprayed on the surface of the base material under the pressure of 1700Psi,and curing the coating at 120 ℃ for two hours; finally, 5ml of poly alpha olefin is dripped on the surface of the solidified coating by using a dropper and stands for 2 hours in a ventilated dust-free environment, and the polydimethylsiloxane polymer molecular brush super-lubricating coating can be obtained 。
Example 3
A preparation method of a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush comprises the following steps:
step one, preparing a component 1:
adding 2.5g of bisphenol F type epoxy resin and 50ml of absolute ethyl alcohol into a 100ml beaker, stirring and dispersing for 50min on a magnetic stirrer at the rotating speed of 1600r/min, then adding 2.1g of ethylenediamine and 0.4g of trimethylsiloxane end-capped polydimethylsiloxane, and performing ultrasonic dispersion for 20min to obtain a coating component 1;
step two, preparing a component 2:
adding 0.8g of bisphenol F type epoxy resin and 50ml of xylene into a 100ml beaker, stirring and dispersing for 25min on a magnetic stirrer at the rotating speed of 1700r/min, then adding 0.2g of monoglycidyl ether terminated polydimethylsiloxane, and performing ultrasonic dispersion for 15min to obtain a coating component 2;
step three, preparing a super-lubricating coating based on the polydimethylsiloxane polymer molecular brush:
firstly, mixing a component 1 and a component 2 in a 200ml beaker, and dispersing for 45min at a rotating speed of 1600r/min on magnetic stirring to obtain a mixture; then, the mixture was added to a spray equipment, sprayed on the substrate surface at a pressure of 1900Psi, and the coating was cured at 120 ℃ for two hours; and finally, dripping 5ml of phenyl silicone oil on the surface of the cured coating by using a dropper, and standing for 2 hours in a ventilated dust-free environment to obtain the polydimethylsiloxane polymer molecular brush super-lubricating coating.
Example 4
A preparation method of a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush is carried out according to the method in the embodiment 1, and is characterized in that epoxy resin in raw materials is aliphatic glycidyl ether type epoxy resin, a curing agent is polyether amine, an organic solution B is toluene, and a non-polar liquid C is hexadecane; and the addition amount of the aliphatic glycidyl ether type epoxy resin is 2.8g, the addition amount of the polyether amine is 2g, the addition amount of the mono-glycidyl ether end-capped polydimethylsiloxane is 0.2g, the curing temperature in the third step is 130 ℃, and the curing time is 3h.
Example 5
A preparation method of a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush is carried out according to the method in the embodiment 1, and the difference is that epoxy resin in raw materials is glycidyl ester type epoxy resin, a curing agent is diethylenetriamine, and nonpolar liquid C is isopropanol.
Example 6
A preparation method of a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush is carried out according to the method in the embodiment 1, and the difference is that epoxy resin in raw materials is glycidyl amine type epoxy resin, and nonpolar liquid C is dimethylformamide.
Comparative example
Comparative example 1
A method for preparing a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush is carried out according to the method in the example 1, and the difference is that dimethyl silicone oil is not dripped on the surface of the solidified coating in the third step.
Comparative example 2
A method of preparing a super-lubricious coating based on a polydimethylsiloxane polymer molecular brush was performed as in example 1, except that no polydimethylsiloxane was added in both step one and step two.
Performance detection
The lubricating coatings of examples 1 to 5 and comparative examples 1 to 2 were subjected to a friction test under the following test conditions: and (3) oppositely grinding the super-lubricating coating and the steel ball, wherein the friction test conditions are as follows: the load is 3N, the rotating speed is 5cm/s, the running time is 1.0h, and the friction coefficient and the wear rate are average values of 3-5 times of tests.
Referring to fig. 3 to 8, fig. 3 is a wear scar and 3D topography map of the polydimethylsiloxane polymer molecular brush super-lubricating coating prepared in example 1 of the invention after a friction test; FIG. 4 is a graph of the friction coefficient of the lubricating coatings prepared in examples 1, 2, 3 of the present invention, and FIG. 5 is a graph of the friction coefficient of the lubricating coatings prepared in examples 4, 5; FIG. 6 is a bar graph of the average coefficient of friction of the lubricating coatings prepared in examples 1, 2, 3, 4, 5 of the present invention; FIG. 7 is a bar graph of wear rates of lubricating coatings prepared according to examples 1, 2, 3, 4, 5 of the present invention; FIG. 8 is a bar graph of the average coefficient of friction of ultra-slip coatings prepared in inventive example 1 and comparative examples 1 and 2.
As can be seen from FIG. 3, the coating is still intact after 1h of friction under 3N load, only slight abrasion marks are left on the surface of the coating, and the wear resistance is higher than that of most super-lubricating coatings; as can be seen from FIGS. 3 to 7, the lubricating coatings prepared in examples 1 to 5 exhibited low friction coefficients and wear rates after rubbing for 1 hour under a load of 3N, the average friction coefficient was maintained between 0.01 and 0.035, and the wear rate was as low as 1.7X 10 -4 mm 3 ·N·m -1 And the lubricating coating prepared in the example 1 only leaves slight grinding marks on the surface, the average depth of the grinding marks is 1.59 mu m, and the average width of the grinding marks is 87.14 mu m, which shows that the polydimethylsiloxane polymer molecular brush super-lubricating coating prepared by the invention has excellent anti-wear and anti-wear properties; from fig. 8, it can be shown from example 1 and comparative examples 1-2 that the polydimethylsiloxane chain brush and the dimethylsilicone oil in the coating prepared by the invention have obvious improvement effect on the friction performance of the lubricating coating.
Claims (10)
1. A preparation method of a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush is characterized by comprising the following steps:
step one, preparing a component 1:
adding an organic solvent into the epoxy resin, stirring, adding a curing agent and polydimethylsiloxane, and performing ultrasonic dispersion to obtain a component 1; taking the total mass of the epoxy resin, the polydimethylsiloxane and the curing agent as a reference, the mass percent of the epoxy resin is 50-56%, the mass percent of the polydimethylsiloxane is 4-8%, and the balance is the curing agent;
step two, preparing a component 2:
adding an organic solvent into the epoxy resin, stirring, adding polydimethylsiloxane, and performing ultrasonic dispersion to obtain a component 2; based on the total mass of the epoxy resin and the polydimethylsiloxane, the mass percent of the epoxy resin is 80-90%, and the mass percent of the polydimethylsiloxane mixture is 10-20%;
step three, preparing a super-lubricating coating based on the polydimethylsiloxane polymer molecular brush:
mixing the component 1 and the component 2, and stirring to obtain a mixture; and spraying the mixture on the surface of a substrate, solidifying, dropwise adding a non-polar liquid C on the surface of the coating, and standing to obtain the super-lubricating coating based on the polydimethylsiloxane polymer molecular brush.
2. The method for preparing the super-lubricating coating based on the polydimethylsiloxane polymer molecular brush as claimed in claim 1, wherein the epoxy resin is one or more of bisphenol A epoxy resin, bisphenol F epoxy resin, aliphatic glycidyl ether epoxy resin, glycidyl ester epoxy resin or glycidyl amine epoxy resin.
3. The method for preparing the ultra-lubricating coating based on the polydimethylsiloxane polymer molecular brush as claimed in claim 1, wherein the polydimethylsiloxane is one or more of monoglycidyl ether terminated polydimethylsiloxane, diglycidyl ether terminated polydimethylsiloxane and trimethyl siloxane terminated polydimethylsiloxane.
4. The method for preparing the ultra-lubricating coating based on the polydimethylsiloxane polymer molecular brush as claimed in claim 1, wherein the curing agent in the first step is one of polyamide, ethylenediamine, polyetheramine and diethylenetriamine.
5. The method for preparing the ultra-lubricating coating based on the polydimethylsiloxane polymer molecular brush as claimed in claim 1, wherein the nonpolar liquid C in the step three is one of methyl silicone oil, ethyl silicone oil, phenyl silicone oil, methylphenyl silicone oil, methyl hydroxyl silicone oil, hydroxyl hydrogen-containing silicone oil, dodecane, hexadecane, poly-alpha-olefin, toluene, isopropanol and dimethylformamide.
6. The method for preparing the ultra-lubricating coating based on the polydimethylsiloxane polymer molecular brush as claimed in the claim 1, wherein the organic solvent in the step one is one or more of ethyl acetate and ethanol; and in the second step, the organic solvent is one or more of acetone, toluene and xylene.
7. The preparation method of the polydimethylsiloxane polymer molecular brush-based super-lubricating coating as claimed in claim 1, wherein the curing temperature in the third step is 120-130 ℃, and the curing time is 2-3 h.
8. The preparation method of the polydimethylsiloxane polymer molecular brush-based super-lubricating coating as claimed in claim 1, wherein the spraying pressure in the third step is 1500-1900 Psi.
9. The method for preparing the super-lubricating coating based on the polydimethylsiloxane polymer molecular brush as claimed in claim 1, wherein the standing environment after the nonpolar liquid C is dripped in the step three is a ventilated dust-free environment.
10. A super-lubricating coating based on molecular brushes of polydimethylsiloxane polymers, characterized in that it is obtained by the process according to claims 1 to 9.
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