CN112812628A - LIS coating and preparation method and application thereof - Google Patents
LIS coating and preparation method and application thereof Download PDFInfo
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- CN112812628A CN112812628A CN202110183684.3A CN202110183684A CN112812628A CN 112812628 A CN112812628 A CN 112812628A CN 202110183684 A CN202110183684 A CN 202110183684A CN 112812628 A CN112812628 A CN 112812628A
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- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 32
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 32
- 239000002131 composite material Substances 0.000 claims abstract description 30
- 239000000203 mixture Substances 0.000 claims abstract description 18
- 239000010687 lubricating oil Substances 0.000 claims abstract description 16
- 239000003822 epoxy resin Substances 0.000 claims description 38
- 229920000647 polyepoxide Polymers 0.000 claims description 38
- 239000010410 layer Substances 0.000 claims description 28
- 239000003921 oil Substances 0.000 claims description 25
- 230000001050 lubricating effect Effects 0.000 claims description 24
- 238000002156 mixing Methods 0.000 claims description 15
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- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
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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
- C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/12—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C09D127/18—Homopolymers or copolymers of tetrafluoroethene
-
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/04—Mixtures of base-materials and additives
- C10M169/044—Mixtures of base-materials and additives the additives being a mixture of non-macromolecular and macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/04—Elements
- C10M2201/041—Carbon; Graphite; Carbon black
- C10M2201/042—Carbon; Graphite; Carbon black halogenated, i.e. graphite fluoride
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/085—Phosphorus oxides, acids or salts
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
- C10M2213/04—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions obtained from monomers containing carbon, hydrogen, halogen and oxygen
- C10M2213/043—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions obtained from monomers containing carbon, hydrogen, halogen and oxygen used as base material
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
- C10M2213/06—Perfluoro polymers
- C10M2213/062—Polytetrafluoroethylene [PTFE]
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2217/06—Macromolecular compounds obtained by functionalisation op polymers with a nitrogen containing compound
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- Chemical & Material Sciences (AREA)
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Laminated Bodies (AREA)
Abstract
The invention provides an LIS coating and a preparation method and application thereof, wherein the LIS coating comprises lubricating oil and a solid coating, the solid coating comprises a low surface energy layer and a composite bonding layer which are sequentially stacked, and the lubricating oil is soaked in the low surface energy layer; the composition of the low surface energy layer includes GrF and PTFE. The LIS coating provided by the invention has the advantages of low friction coefficient, good chemical robustness and high corrosion resistance, and shows great application potential in the fields of tribology and metal corrosion protection.
Description
Technical Field
The invention belongs to the field of lubricating materials, particularly relates to an LIS coating and a preparation method and application thereof, and particularly relates to an LIS coating with a low friction coefficient and a preparation method and application thereof.
Background
Reducing frictional wear is essential in production life, as they often lead to failure of parts, excessive energy consumption and greenhouse gas emissions, even serious disasters, etc. Therefore, reducing mechanical energy consumption and prolonging the service life of equipment are important strategies. Liquid and grease-based lubricants are commonly used to reduce friction and wear in moving mechanical systems by creating a thin liquid film to isolate the friction elements. Recent studies have found that some water and oil-based lubricating oils exhibit super-lubricity. However, such super-lubricated state generally involves frictional reactions and surface adsorption of particular materials. It therefore requires specific friction pairs and often involves corrosive additives, which lead to corrosion of the friction pairs, limiting the range of applications of these lubricants. In addition, lubricant leakage and failure under extreme conditions (e.g., vacuum, low temperature or high temperature) are also common problems with liquid and grease-based lubricants.
As another important lubrication strategy, solid lubricant-based materials (including graphite, Polytetrafluoroethylene (PTFE), molybdenum disulfide (MoS)2) Diamond Like Carbon (DLC) coatings, etc.) can overcome leakage problems and even operate under harsh operating conditions. Some solid lubricants with appropriate friction pairs also achieve good super-lubricity, particularly at the micro/nano scale. However, these solid lubricant-based materials/coatings are severely limited by surface structure, friction pair composition and test conditions. For example, MoS2Are easily oxidized to lose the lubricating ability. Furthermore, the inability to self-replenish and limited large area applications have limited the use of these solid lubricant-based materials.
CN109385153A discloses an irradiation-resistant space solid lubricating coating and a preparation method thereof, wherein the solid lubricating coating comprises PTFE particles with the mass ratio of 80-90 parts and the size of 40-100 meshes, carbon fiber particles with the mass ratio of 10-20 parts and the size of 100-200 meshes, the solid lubricating coating has the advantages of low friction coefficient (0.132-0.192), less abrasion loss (1-15 mg), good irradiation resistance, uniform and continuous structure and the thickness of about 20 mu m, and the preparation method mainly comprises the steps of sample preparation, polishing treatment, PTFE particle screening, coating deposition, surface wiping, vacuum tribology performance testing and abrasive dust collection. The preparation method is scientific and reasonable, and has great achievement transformation potential and wide practical value. However, it only uses solid lubricant and cannot be self-replenished.
CN110453262A discloses a preparation method of an aluminum oxide/polytetrafluoroethylene composite self-lubricating film, which is characterized in that after the surface of an aluminum alloy is pretreated, the aluminum alloy is placed in electrolyte prepared from an oxide film to prepare an anodic oxide film; soaking aluminum alloy in PTFE solution, centrifuging at high speed, throwing particles into membrane pores and the surface of the membrane, and preparing a compact composite membrane; heat treating the aluminum alloy to obtain Al2O3The polytetrafluoroethylene composite self-lubricating film. The invention adopts a centrifugal method, and can solve the problems of large friction coefficient and poor self-lubricating property of the composite membrane caused by loose deposition of the lubricating particles in the anodic oxidation nano-pores, incompact lubrication particles and low filling rate. The invention can prepare the alumina composite membrane with high hardness, wear resistance and self-lubricating property at low cost, prolongs the service life of friction parts, reduces pollution caused by oil lubrication, and has wide application prospect in the fields of automobiles, machine manufacturing, light industry daily necessities manufacturing and the like.
The liquid lubricant in the prior production and life has the defects of matrix corrosion, high requirement on friction pair, easy leakage and the like, while the solid lubricant matrix has the problems of harsh tested test piece, difficult repair after damage, complex preparation, unsuitability for large-scale production and the like. Therefore, it is a problem to be solved how to provide a lubricating material which has good lubricity, works well in air, is not easy to leak, is easy to replenish, and can be mass-produced and applied.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide an LIS coating and a preparation method and application thereof, and particularly provides an LIS coating with a low friction coefficient and a preparation method and application thereof. The LIS coating provided by the invention has the advantages of low friction coefficient, good chemical robustness and high corrosion resistance, and shows great application potential in the fields of tribology and metal corrosion protection.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides an LIS (lubricant injected surface) coating, which includes a lubricant and a solid coating, wherein the solid coating includes a low surface energy layer and a composite adhesion layer, which are sequentially stacked, and the lubricant is infiltrated in the low surface energy layer.
The composition of the low surface energy layer comprises GrF (graphite fluoride) and PTFE (polytetrafluoroethylene), and preferably, the composition of the composite bonding layer comprises ZrP (alpha-zirconium phosphate) and epoxy resin.
The LIS coating with the specific structure combines the characteristics of a solid lubricating matrix and lubricating oil, realizes excellent liquid rejection and barrier properties, and has good self-cleaning, anti-corrosion, anti-icing and anti-pollution effects; and the inert solid coating is combined, so that the friction coefficient is low, the chemical robustness is good, and the corrosion resistance is high.
GrF has excellent lubricating ability, extremely low surface energy, chemical inertness and a unique band gap structure, and can improve the lubricating ability and the corrosion resistance of the LIS coating; PTFE with small particle size and micron-level GrF are matched with each other, so that on one hand, the PTFE and the micron-level GrF are promoted to be uniformly dispersed, and on the other hand, a micro-nano structure is also constructed, so that the hydrophobicity of the coating is endowed.
ZrP is a synthetic two-dimensional inorganic material, is also an excellent solid lubricant, has excellent mechanical property and corrosion resistance, has good compatibility through the interaction of hydroxyl functional groups and polymers, and can effectively improve the mechanical property, the tribological property and the barrier property of polymer materials. The composite bonding layer is formed by interaction of ZrP and epoxy resin, so that the lubricity and corrosion resistance of the LIS coating can be improved, and GrF and PTFE can be bonded on the composite bonding layer to form the solid coating.
Preferably, the lubricating oil comprises any one of, or a combination of at least two of, PFPE (perfluoropolyether), 15# white oil, or 32# white oil, such as a combination of PFPE and 15# white oil, a combination of 15# white oil and 32# white oil, or a combination of PFPE and 32# white oil, but not limited to the combinations enumerated above, and other combinations not enumerated within the scope of the combinations enumerated above are equally applicable.
The selection of the specific lubricating oil can fully permeate into the low surface energy layer, so that the lubricating capability of the LIS coating is improved, and the friction coefficient is reduced.
Preferably, the oil content of the LIS coating is 0.08-0.1. mu.g/cm2。
Preferably, the mass ratio of the GrF to the PTFE is 1:0.8-1: 1.2.
Wherein the oil content may be 0.08 μ g/cm2、0.085μg/cm2、0.09μg/cm2、0.095μg/cm2Or 0.1. mu.g/cm2The mass ratio of GrF to PTFE may be, for example, 1:0.8, 1:0.9, 1:1, 1:1.1 or 1:1.2, but is not limited to the above-mentioned values or ratios, and other values or ratios not specified in the above-mentioned values or ratios are also applicable.
Preferably, the mass ratio of the ZrP to the epoxy resin is 1:3-1: 4.
Preferably, the epoxy resin includes any one or a combination of at least two of epoxy resin E44, epoxy resin E51, waterborne epoxy resin F0716 or epoxy resin 128, such as a combination of epoxy resin E44 and epoxy resin E51, a combination of epoxy resin E51 and waterborne epoxy resin F0716 or a combination of waterborne epoxy resin F0716 and epoxy resin 128, but not limited to the above-listed combinations, and other combinations not listed in the above-mentioned combination range are also applicable.
Preferably, the mass ratio of ZrP to GrF is 1:0.8-1: 1.2.
Preferably, the thickness of the composite adhesive layer is 13-17 μm.
Preferably, the thickness of the solid coating is 23-27 μm.
Wherein the mass ratio of ZrP and the epoxy resin may be 1:3, 1:3.1, 1:3.2, 1:3.3, 1:3.4, 1:3.5, 1:3.6, 1:3.7, 1:3.8, 1:3.9, or 1:4, etc., the mass ratio of ZrP and GrF may be 1:0.8, 1:0.9, 1:1, 1:1.1, or 1:1.2, etc., the thickness of the composite adhesion layer may be 13 μm, 14 μm, 15 μm, 16 μm, or 17 μm, etc., the thickness of the solid coating layer may be 23 μm, 24 μm, 25 μm, 26 μm, or 27 μm, etc., but not limited to the above-listed values or ratios, and other values or ratios within the above-listed values or ratios are also applicable.
The addition of the specific ZrP can ensure the adhesion and film forming property of the composite adhesive layer and ensure the stability of the LIS coating.
In a second aspect, the present invention provides a method for preparing the LIS coating as described above, the method comprising the steps of:
(1) dissolving and mixing epoxy resin and a curing agent by using a solvent, then mixing with ZrP, coating the obtained mixture on a substrate, and heating for precuring to obtain a composite bonding layer;
(2) mixing GrF and PTFE with a solvent, coating the mixture on the surface of the composite bonding layer obtained in the step (1), and curing to obtain a solid coating;
(3) and (3) adding lubricating oil to the surface of the solid coating obtained in the step (2) to cover the solid coating, and then placing for degreasing to obtain the LIS coating.
The preparation method is simple to operate, and the LIS coating can be quickly and conveniently prepared.
Preferably, the mass ratio of the curing agent to the epoxy resin in the step (1) is 1:2.5-1: 3.5.
Preferably, the heating temperature of the step (1) is 75-85 ℃ and the time is 25-35 min.
Preferably, the curing temperature of the step (2) is 75-85 ℃ and the time is 2-4.5 h.
The mass ratio of the curing agent to the epoxy resin may be 1:2.5, 1:2.6, 1:2.7, 1:2.8, 1:2.9, 1:3, 1:3.1, 1:3.2, 1:3.3, 1:3.4 or 1:3.5, etc., the heating temperature may be 75 ℃, 76 ℃, 77 ℃, 78 ℃, 79 ℃, 80 ℃, 81 ℃, 82 ℃, 83 ℃, 84 ℃ or 85 ℃, the time may be 25min, 26min, 27min, 28min, 29min, 30min, 31min, 32min, 33min, 34min or 35min, etc., the curing temperature may be 75 ℃, 76 ℃, 77 ℃, 78 ℃, 79 ℃, 80 ℃, 81 ℃, 82 ℃, 83 ℃, 84 ℃ or 85 ℃, etc., the time may be 2h, 2.5h, 3h, 3.5h, 4h or 4.5h, etc., but is not limited to the values or the ratios listed above, and other values or ratios are not applicable.
Preferably, the placing in step (3) is vertical placing.
As a preferred technical scheme of the invention, the preparation method comprises the following steps:
(1) dissolving and mixing epoxy resin and a curing agent by using a solvent, then mixing with ZrP, coating the obtained mixture on a substrate, and heating at 75-85 ℃ for 25-35min for precuring to obtain a composite bonding layer;
(2) mixing GrF and PTFE with a solvent, coating the mixture on the surface of the composite bonding layer obtained in the step (1), and curing the mixture at 75-85 ℃ for 2-4.5h to obtain a solid coating;
(3) and (3) adding lubricating oil to the surface of the solid coating obtained in the step (2) to cover the solid coating, and then vertically placing for removing oil to obtain the LIS coating.
In a third aspect, the present invention also provides the use of a LIS coating as described above for the preparation of a lubricating material.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the invention, the LIS coating is prepared by selecting a specific material, and combines the characteristics of a solid lubricating matrix and lubricating oil, so that excellent liquid repellency and barrier property are realized, and the effects of self-cleaning, corrosion prevention, ice prevention and pollution prevention are good; the inert solid coating is combined, so that the friction coefficient is low, the chemical robustness is good, and the corrosion resistance is high;
(2) according to the invention, a low surface energy layer is prepared by selecting a specific material, wherein GrF has excellent lubricating ability, extremely low surface energy, chemical inertness and a unique band gap structure, so that the lubricating ability and corrosion resistance of the LIS coating can be improved; PTFE with small particle size and micron-level GrF are matched with each other, so that the PTFE and the micron-level GrF are promoted to be uniformly dispersed on one hand, and a micro-nano structure is also constructed on the other hand, so that the coating is endowed with hydrophobicity; meanwhile, specific lubricating oil is selected to be capable of fully permeating into the low surface energy layer, so that the lubricating capability of the LIS coating is improved, and the friction coefficient is reduced.
Drawings
FIG. 1 is a graph showing the results of a comparative test of coefficient of friction, wherein 1-LIS coating, 2-solid lubricant coating, 3-PFPE, 4-pure Q235 steel plate provided in example 1;
FIG. 2 is a plot of the impedance modulus, IZI, of samples versus frequency in a corrosion protection test, wherein 1 is the LIS coating provided in example 1, 2 is the solid lubricant coating, 3 is the coating provided in comparative example 4, 4 is a pure Q235 steel plate;
fig. 3 is a plot of the phase angle of samples in the corrosion test, where 1-LIS coating provided in example 1, 2-solid lubricant coating, 3-coating provided in comparative example 4, 4-pure Q235 steel plate.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
In the following examples, PTFE was obtained from Asahi glass Ltd, Japan, and had a particle size of 500 nm;
GrF is available from Shenyang Schiff science and technology, Inc. of China, with a 1:1 ratio of fluorine to carbon and a 5 μm particle size;
PFPE is available from DuPont, USA under the Krytox GPL105 model;
epoxy resin E44, epoxy resin E51 and epoxy resin 128 are purchased from Shenzhen Jitian chemical industry Co., Ltd, China;
curing agent polyetheramine D230 was purchased from Aladdin Chemicals, Inc., China;
ZrP is purchased from Sun, Inc. of China, and has a particle size of 1.64 μm;
graphite oxide is purchased from a novel Kenner carbon material;
graphene is available from yue chuang technologies ltd;
the carbon black is purchased from Luzhe chemical industry Co., Ltd, and the model is N330;
the remaining starting materials are commercially available.
Example 1
This example provides an LIS coating, which is prepared as follows:
(1) 1g of epoxy resin E44 and 0.33g of polyetheramine D230 were dissolved and mixed with 4g of acetone, and then mixed with 0.3g of ZrP, and the resulting mixture was coated on glass and heated at 80 ℃ for 30min to obtain a composite adhesive layer (thickness 15 μm);
(2) mixing 0.3g GrF and 0.3g PTFE with 4.4g ethanol, coating on the surface of the composite bonding layer obtained in the step (1), and curing at 80 ℃ for 4h to obtain a solid coating;
(3) PFPE is added on the surface of the solid coating obtained in the step (2) to cover the solid coating, and then the solid coating is vertically placed for 1 hour to remove oil, and the final oil content is 0.09 mu g/cm2The LIS coating (thickness 25 μm) was obtained.
Example 2
This example provides an LIS coating, which is prepared as follows:
(1) 1g of epoxy resin E51 and 0.29g of polyetheramine D230 were dissolved and mixed with 4g of acetone, and then mixed with 0.25g of ZrP, and the resulting mixture was coated on glass and heated at 75 ℃ for 35min to obtain a composite adhesive layer (thickness 13 μm);
(2) mixing 0.2g GrF and 0.24g PTFE with 4.4g ethanol, coating on the surface of the composite bonding layer obtained in the step (1), and curing at 75 ℃ for 4.5h to obtain a solid coating;
(3) adding 15# white oil on the surface of the solid coating obtained in the step (2) to cover the solid coating, and then vertically placing for 1h to remove the oil, wherein the final oil content is 0.08 mu g/cm2The LIS coating (thickness 23 μm) was obtained.
Example 3
This example provides an LIS coating, which is prepared as follows:
(1) 1g of epoxy resin 128 and 0.4g of polyetheramine D230 were dissolved and mixed with 4g of acetone, and then mixed with 0.33g of ZrP, and the resulting mixture was coated on glass and heated at 85 ℃ for 25min to obtain a composite adhesive layer (thickness 17 μm);
(2) mixing 0.4g GrF and 0.32g PTFE with 4.4g ethanol, coating on the surface of the composite bonding layer obtained in the step (1), and curing at 85 ℃ for 3.5h to obtain a solid coating;
(3) adding 32# white oil on the surface of the solid coating obtained in the step (2) to cover the solid coating, then vertically placing for 1h to remove the oil, and finally obtaining the oil content of 0.1 mu g/cm2The LIS coating (thickness 27 μm) was obtained.
Example 4
This example provides a LIS coating prepared in a manner consistent with example 1 except that PFPE was replaced with an equal amount of # 15 white oil in step (3).
Example 5
This example provides a LIS coating prepared in a manner consistent with example 1 except that PFPE was replaced with an equal amount of 32# white oil in step (3).
Example 6
This example provides an LIS coating prepared in accordance with example 1 except that 0.3g of PTFE was replaced with 0.15g of PTFE in step (2).
Example 7
This example provides an LIS coating prepared in accordance with example 1 except that 0.45g of PTFE was replaced with 0.3g of PTFE in step (2).
Example 8
This example provides a LIS coating prepared in a manner consistent with example 1 except that 1g of epoxy E44 was replaced with 0.6g of epoxy E44 in step (1).
Example 9
This example provides a LIS coating prepared in a manner consistent with example 1 except that 1g of epoxy E44 was replaced with 1.5g of epoxy E44 in step (1).
Comparative example 1
This comparative example provides a LIS coating prepared in a manner consistent with example 1, except that the equivalent amount of carbon black was substituted for GrF in step (2).
Comparative example 2
This comparative example provides an LIS coating prepared in a manner consistent with example 1, except that in step (2) GrF was replaced with an equivalent amount of graphene.
Comparative example 3
This comparative example provides a LIS coating prepared in a manner consistent with example 1, except that in step (2) GrF was replaced with an equal amount of graphite oxide.
Comparative example 4
This comparative example provides a coating, the preparation method is as follows:
1g of epoxy resin E44 and 0.33g of polyetheramine D230 were mixed and dissolved in 4g of acetone, and the mixture obtained was coated on glass and heated at 80 ℃ for 30min to give the coating (thickness 15 μm).
And (3) hydrophobic effect test:
the LIS coatings provided in examples 1-9 and comparative examples 1-3 were measured for static water Contact Angle (CA) and Sliding Angle (SA) at 5. mu.L and 10. mu.L water drops using a contact angle meter (VCA optima, USA), respectively, and the results are as follows
The above data show that the LIS coating provided by the present invention has excellent hydrophobic effect, and comparative examples 1, 6 and 7 can find that the hydrophobic effect is further improved within the range of the preferred GrF and PTFE mass ratio of the present invention.
And (3) tribology test:
tribological tests were performed in ball-and-plate mode using a CETR reciprocating tribometer (RTEC MFT-5000). A stationary 440C bearing ball (diameter 6.35mm, surface roughness 50nm) was slid on the LIS coatings provided in examples 1-9 and comparative examples 1-3 with a reciprocating distance of 10 mm. Before the test, the steel ball is cleaned by ultrasonic wave with acetone. To investigate the effect of the applied load on the lubricating performance, the test loads were set at 10N (140MPa, Hertz contact), 30N (200MPa) and 50N (240MPa), with a fixed frequency of 5 Hz. To investigate the effect of frequency (speed), the test frequencies were set at 5Hz, 10Hz and 20Hz, with a fixed load of 10N. All tests were carried out at 25 ℃ with a relative humidity of 70%. Each sliding pair is repeated at least three times to ensure accuracy. The ratio of the tangential force (Fx) and the normal force (Fz) is used as the coefficient of friction (COF). The values of Fx and Fz were automatically recorded using force sensors and the wear rate of the steel balls was used to evaluate the lubricity of the coating. The specific wear rate of the steel ball is calculated according to the following formula:
wear rate (mm)3/Nm)＝ΔV/Ld×103
Wherein, Δ V is the abrasion loss of the steel ball, L is the normal load, and d is the total sliding distance. The volume loss (Δ V) of the spheres is given by the equation given in ASTM G99:
ΔV＝(πh/6)[3d2/4+h2]
wherein: h ═ r- [ r2-d2/4]1/2D is the diameter of the grinding crack, and r is the radius of the steel ball. The test conditions were 10N, 5Hz and a duration of 20 minutes. The test results were as follows:
the results show that the LIS coating provided by the invention has good lubricating effect and low steel ball wear rate, and the lubricating effect of the LIS coating is greatly improved by selecting GrF.
The LIS coating, the solid lubricant coating (the solid coating obtained in step (2) of example 1), PFPE, and the pure Q235 steel plate (Ra 200nm) provided in example 1 were subjected to a friction coefficient comparison test, and the test procedure was as described above, and the results are shown in fig. 1, where 1 is the LIS coating provided in example 1, 2 is the solid lubricant coating, 3 is PFPE, and 4 is the pure Q235 steel plate. It can be seen from figure 1 that the invention provides a product with a lower coefficient of friction than the prior art.
And (3) corrosion prevention test:
the samples were tested for impedance modulus | Z | and phase angle using a CS electrochemical workstation (CorrTest CS310H) with a wt 3.5% aqueous sodium chloride solution as the corrosive medium. Three-electrode working mode of CS electrochemical workstation, wherein electrodes are Saturated Calomel Electrode (SCE) (reference electrode), platinum (Pt) (counter electrode) and sampleArticle (working electrode). Among these, the samples were the LIS coating provided in example 1, the solid lubricating coating (solid coating obtained in step (2) in example 1), the coating provided in comparative example 4, and the pure Q235 steel sheet. The contact area of the sample and the corrosive medium is 0.19cm during the test2The sinusoidal interference is 20mV measured using Electrochemical Impedance Spectroscopy (EIS) at a frequency range of 0.1Hz-10 kHz.
In order to quantitatively study the corrosion resistance of the coating, an electrochemical corrosion test was performed in a 3.5 wt% NaCl aqueous solution using a three-electrode system. The LIS coating provided in example 1, the solid lubricating coating (the solid coating obtained in step (2) in example 1), the coating provided in comparative example 4, and the pure Q235 steel sheet were evaluated for corrosion resistance by Electrochemical Impedance Spectroscopy (EIS). The impedance modulus | Z | as a function of frequency is plotted in fig. 2, where 1 is the LIS coating provided in example 1, 2 is the solid lubricant coating, 3 is the coating provided in comparative example 4, and 4 is pure Q235 steel plate. Where | Z | at 0.01Hz, can be used to evaluate the barrier properties of the coating, i.e. the greater the | Z | value the better the corrosion resistance of the sample. Compared with unprotected pure Q235 steel plate (| Z(f＝0.01Hz)＝8.89×102ohm·cm2) And the coating (pure epoxy coating) provided in comparative example 4 (| Z(f＝0.01Hz)＝5.61×103ohm·cm2) In contrast, solid lubricating coating (| Z(f＝0.01Hz)＝2.63×107ohm·cm2) And LIS coating (| Z(f＝0.01Hz)＝9.96×107ohm·cm2) Lambada Z-(f＝0.01Hz)The value is obviously improved, which shows that the waterproof coatings have good anticorrosion performance.
In addition, the phase angle plot shown in fig. 3 can also be used to characterize the corrosion resistance of the coating, where 1 is the LIS coating provided in example 1, 2 is the solid lubricant coating, 3 is the coating provided in comparative example 4, and 4 is pure Q235 steel plate. Wherein a high phase angle over a wide frequency range indicates a good corrosion resistance of the coating. The phase angle of the pure Q235 steel plate and the coating provided in comparative example 4 was small in almost the entire frequency range, whereas the phase angle of the solid lubricating coating and the LIS coating provided in example 1 was large, and showed good corrosion resistance particularly in the higher frequency range. In addition, electrochemical impedance spectroscopy analysis resultsIt is also shown that the LIS coating provided in example 1 has a higher | Z(f＝0.01Hz)And phase angle, and thus has better corrosion resistance than solid lubricant coatings.
The above data show that the LIS coating provided by the present invention has better corrosion resistance than the prior art.
Testing the adhesion of the bottom layer:
the coated surface was scribed with a cutter to make 100 equal area square grids, and then the grid areas were taped with high tack tape (3M610 scotch tape) and the tape was peeled off. And according to the residual grid area after the test, the adhesion of the coating is classified into 0-5 grades, wherein the 0 grade is the best adhesion, and the 5 grade is the worst adhesion. The tests performed on the LIS coatings provided in examples 1, 8 and 9 show that the adhesion of the LIS coating provided in example 1 is rated at the optimal 0 level, and the adhesion of the LIS coatings provided in examples 8 and 9 are rated at 2 and 1 levels, respectively, indicating that too little epoxy resin or too much epoxy resin affects the adhesion.
The applicant states that the present invention is illustrated by the above examples to the LIS coating of the present invention and the method of preparation and application thereof, but the present invention is not limited to the above examples, i.e. it does not mean that the present invention must be implemented by means of the above examples. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
Claims (10)
1. An LIS coating is characterized by comprising lubricating oil and a solid coating, wherein the solid coating comprises a low surface energy layer and a composite bonding layer which are sequentially stacked, and the lubricating oil is soaked in the low surface energy layer;
the low surface energy layer comprises GrF and PTFE, and the composite bonding layer comprises ZrP and epoxy resin.
2. The LIS coating of claim 1, wherein the lubricating oil comprises any one of PFPE, 15# white oil, or 32# white oil, or a combination of at least two thereof.
3. The LIS coating according to claim 1 or 2, wherein the LIS coating has an oil content of 0.08-0.1 μ g/cm2。
4. The LIS coating according to any one of claims 1-3, wherein the mass ratio of GrF to PTFE is 1:0.8-1: 1.2.
5. The LIS coating according to any one of claims 1-4, wherein the ZrP and the epoxy resin are present in a mass ratio of 1:3 to 1: 4;
preferably, the epoxy resin comprises any one of or a combination of at least two of epoxy resin E44, epoxy resin E51, waterborne epoxy resin F0716 or epoxy resin 128;
preferably, the mass ratio of ZrP to GrF is 1:0.8-1: 1.2.
6. The LIS coating of any one of claims 1-5, wherein the composite adhesive layer has a thickness of 13-17 μm;
preferably, the thickness of the solid coating is 23-27 μm.
7. A method of preparing the LIS coating according to any one of claims 1-6, comprising the steps of:
(1) dissolving and mixing epoxy resin and a curing agent by using a solvent, then mixing with ZrP, coating the obtained mixture on a substrate, and heating for precuring to obtain a composite bonding layer;
(2) mixing GrF and PTFE with a solvent, coating the mixture on the surface of the composite bonding layer obtained in the step (1), and curing to obtain a solid coating;
(3) and (3) adding lubricating oil to the surface of the solid coating obtained in the step (2) to cover the solid coating, and then placing for degreasing to obtain the LIS coating.
8. The method for preparing the LIS coating as claimed in claim 7, wherein the mass ratio of the curing agent and the epoxy resin in the step (1) is 1:2.5-1: 3.5;
preferably, the heating temperature in the step (1) is 75-85 ℃ and the time is 25-35 min;
preferably, the curing temperature of the step (2) is 75-85 ℃, and the time is 2-4.5 h;
preferably, the placing in step (3) is vertical placing.
9. The method for preparing a LIS coating according to claim 8 or 9, wherein the method for preparing comprises the following steps:
(1) dissolving and mixing epoxy resin and a curing agent by using a solvent, then mixing with ZrP, coating the obtained mixture on a substrate, and heating at 75-85 ℃ for 25-35min for precuring to obtain a composite bonding layer;
(2) mixing GrF and PTFE with a solvent, coating the mixture on the surface of the composite bonding layer obtained in the step (1), and curing the mixture at 75-85 ℃ for 2-4.5h to obtain a solid coating;
(3) and (3) adding lubricating oil to the surface of the solid coating obtained in the step (2) to cover the solid coating, and then vertically placing for removing oil to obtain the LIS coating.
10. Use of a LIS coating according to any of claims 1-6 in the preparation of a lubricating material.
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