CN114196239B - Low-temperature-cured wear-resistant inorganic phosphate bonded solid lubricating coating material and preparation method thereof - Google Patents

Low-temperature-cured wear-resistant inorganic phosphate bonded solid lubricating coating material and preparation method thereof Download PDF

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CN114196239B
CN114196239B CN202111628185.7A CN202111628185A CN114196239B CN 114196239 B CN114196239 B CN 114196239B CN 202111628185 A CN202111628185 A CN 202111628185A CN 114196239 B CN114196239 B CN 114196239B
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fumed silica
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inorganic phosphate
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吴平
陈磊
崔海霞
张岳
周惠娣
陈建敏
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Lanzhou Institute of Chemical Physics LICP of CAS
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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
    • C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
    • 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
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • 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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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • 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
    • C09D7/63—Additives non-macromolecular organic

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Abstract

The invention provides a low-temperature cured wear-resistant inorganic phosphate bonded solid lubricating coating material and a preparation method thereof, belonging to the technical field of coating materials. The paint comprises the following components in percentage by mass: 5-15% of fumed silica modified phosphate, 0.5-5% of organic alkali, 30-60% of layered dichalcogenide, 2-10% of rare earth fluoride, 2-6% of antimony trioxide and the balance of water; the fumed silica modified phosphate is prepared by a process comprising the steps of: inorganic phosphate, fumed silica nanoparticles and water are mixed for modification. According to the invention, the organic base is selected as a low-temperature curing agent, the organic base can promote complete curing at low temperature, and meanwhile, the flexible chain segment in the organic base can improve the flexibility of the coating, so that the coating material shows excellent comprehensive mechanical property and frictional wear property.

Description

Low-temperature-cured wear-resistant inorganic phosphate bonded solid lubricating coating material and preparation method thereof
Technical Field
The invention relates to the technical field of coating materials, in particular to a low-temperature-cured wear-resistant inorganic phosphate bonded solid lubricating coating material and a preparation method thereof.
Background
The inorganic phosphate bonding resin is widely applied to the fields of high-temperature lubrication, oxidation resistance, corrosion protection, surface lubrication and protection of related equipment parts in extreme special service environments such as space and nuclear radiation and the like due to the advantages of good temperature resistance, oxidation resistance, irradiation resistance (space irradiation, nuclear radiation and the like), special medium resistance and the like. However, inorganic phosphates have high brittleness due to their amorphous structural characteristics, and require high-temperature curing. Particularly, the wide application of the surface coating material in some special fields is severely limited by the high brittleness and the characteristic that the surface coating material with the thickness of only tens of microns can be completely cured by heating to 310 ℃ and keeping the temperature for more than 1 hour.
The high-temperature curing mechanism of the inorganic phosphate coating is an intermolecular dehydration crosslinking process in a high-temperature heating process among phosphoric acid molecules, and only when the temperature exceeds 310 ℃, the intermolecular dehydration reaction is complete, and the coating is completely cured. Based on the principle that alkali metal ions, metal oxides and the like participate in acid-base neutralization reaction to effectively reduce the curing temperature of inorganic phosphate resin, various low-temperature or even room-temperature curing inorganic phosphate composite coating materials, such as magnesium oxide, copper oxide, chromium oxide, silicate, phosphate and the like, are prepared in the prior art. Although the curing temperature can be reduced by the various curing agents, the curing rate is uncontrollable, and loose and porous structures are often formed after curing, so that the compactness of the coating is poor and the bonding force with the matrix is weak, namely, the reduction of the curing temperature is at the expense of the comprehensive mechanical property of the coating material. Therefore, the application of the method of reducing the curing temperature of inorganic phosphate by adding metal oxide or alkali metal ions in the coating field is still greatly limited, and the method is particularly more remarkable for lubricating protective coating materials with higher requirements on mechanical properties.
Disclosure of Invention
In view of the above, the present invention aims to provide a low-temperature cured wear-resistant inorganic phosphate bonded solid lubricating coating material and a preparation method thereof. The low-temperature-cured wear-resistant inorganic phosphate bonded solid lubricating coating material provided by the invention not only has the characteristic of low-temperature curing, but also has excellent comprehensive mechanical properties.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a low-temperature-cured wear-resistant inorganic phosphate bonded solid lubricating coating material which comprises the following components in percentage by mass: 5-15% of fumed silica modified phosphate, 0.5-5% of organic alkali, 30-60% of layered dichalcogenide, 2-10% of rare earth fluoride, 2-6% of antimony trioxide and the balance of water;
the fumed silica modified phosphate is prepared by a process comprising the steps of: inorganic phosphate, fumed silica nanoparticles and water are mixed for modification.
Preferably, the organic base is ethanolamine or diethanolamine.
Preferably, the inorganic phosphate is aluminum chromium phosphate.
Preferably, the particle size of the fumed silica nanoparticles is 5-10 nm.
Preferably, the fumed silica-modified phosphate is prepared by a process comprising the steps of:
mixing phosphoric acid, chromium oxide, aluminum hydroxide and preparation water to perform acid-base neutralization and crosslinking reaction to obtain an aluminum-chromium phosphate dispersion;
and mixing the aluminum chromium phosphate dispersion liquid with the fumed silica nanoparticles for modification to obtain the fumed silica modified phosphate.
Preferably, the total mass of the phosphoric acid, the chromium oxide, the aluminum hydroxide, the fumed silica nanoparticles and the preparation water is 100%, the mass content of the phosphoric acid is 50-70%, the mass content of the chromium oxide is 3-10%, the mass content of the aluminum hydroxide is 10-20%, the mass content of the fumed silica nanoparticles is 0.5-5%, and the balance is the preparation water.
Preferably, the lamellar dichalcogenide is molybdenum disulfide or tungsten disulfide.
Preferably, the particle diameter of the lamellar dithio compound is 0.8-1.2 μm, and the thickness is 0.1-0.8 μm.
Preferably, the rare earth fluoride is lanthanum fluoride or cerium fluoride.
The invention also provides a preparation method of the low-temperature cured wear-resistant inorganic phosphate bonded solid lubricating coating material in the technical scheme, which comprises the following steps: and mixing the fumed silica modified phosphate, organic alkali, a layered disulfide, a rare earth fluoride, antimony trioxide and water to obtain the low-temperature cured wear-resistant inorganic phosphate bonded solid lubricating coating material.
The invention provides a low-temperature cured wear-resistant inorganic phosphate bonded solid lubricating coating material which comprises the following components in percentage by mass: 5-15% of fumed silica modified phosphate, 0.5-5% of organic alkali, 30-60% of layered dichalcogenide, 2-10% of rare earth fluoride, 2-6% of antimony trioxide and the balance of water; the fumed silica modified phosphate is prepared by a process comprising the steps of: inorganic phosphate, fumed silica nanoparticles and water are mixed for modification.
The low-temperature cured wear-resistant inorganic phosphate bonded solid lubricating coating material takes fumed silica modified inorganic phosphate as a bonding agent, organic alkali as a low-temperature curing agent and a surfactant, a lamellar dithio compound as a solid lubricating filler, rare earth fluoride and antimony trioxide as auxiliary functional fillers, and water as a diluent. According to the invention, the organic base is selected as the curing agent, and the organic base and the phosphoric acid are bridged to promote intramolecular dehydration to form a macromolecular network structure, so that the thorough dehydration condensation and complete curing at low temperature can be promoted, and the curing rate is slow and controllable; compared with the existing inorganic low-temperature curing agent, the organic base participates in the dehydration condensation process, the reaction rate is slow, the formed coating has good compactness, firm bonding force with a substrate and good wear resistance; the organic base also serves as a surfactant in the coating process, can promote self-leveling of the coating, and enables the surface roughness of the coating after curing to be lower.
The low-temperature-cured wear-resistant inorganic phosphate bonded solid lubricating coating material provided by the invention not only has the characteristic of low-temperature curing, but also has excellent comprehensive mechanical properties and frictional wear properties.
The invention also provides a preparation method of the low-temperature cured wear-resistant inorganic phosphate bonded solid lubricating coating material in the technical scheme, and the preparation method is simple in preparation process, short in production period, strong in operability and very suitable for scale production and popularization in the later period.
Drawings
FIG. 1 is a cross-sectional micro-topography of a composite coating prepared in example 1;
FIG. 2 is a graph of adhesion, flexibility and impact resistance tests for the composite coating prepared in example 1;
FIG. 3 is a plot of the coefficient of friction of a large spherical disc of the low temperature cured wear-resistant inorganic phosphate bonded solid lubricant coating material prepared in examples 1-4;
FIG. 4 is a graph showing the wear rate of the large spherical discs of the low temperature cured wear-resistant inorganic phosphate bonded solid lubricating coating materials prepared in examples 1-4.
Detailed Description
The invention provides a low-temperature-cured wear-resistant inorganic phosphate bonded solid lubricating coating material which comprises the following components in percentage by mass: 5-15% of fumed silica modified phosphate, 0.5-5% of organic alkali, 30-60% of layered dichalcogenide, 2-10% of rare earth fluoride, 2-6% of antimony trioxide and the balance of water;
The fumed silica modified phosphate is prepared by a process comprising the steps of: inorganic phosphate, fumed silica nanoparticles and water are mixed for modification.
In the present invention, unless otherwise specified, all the raw materials used are commercially available in the art.
The mass percentage of the organic base in the low-temperature cured wear-resistant inorganic phosphate bonded solid lubricating coating material provided by the invention is preferably 2-3%.
In the present invention, the organic base is preferably ethanolamine or diethanolamine. In the present invention, the organic base serves as a low-temperature curing agent and a surfactant.
The mass percentage content of the lamellar dichalcogenide in the low-temperature-cured wear-resistant inorganic phosphate bonded solid lubricating coating material is preferably 40-50%.
In the present invention, the lamellar dichalcogenide is preferably molybdenum disulfide or tungsten disulfide. In the present invention, the lamellar dichalcogenide acts as a solid lubricating filler.
In the present invention, the particle diameter of the lamellar dithio compound is preferably 0.8 to 1.2 μm, and the thickness is preferably 0.1 to 0.8. mu.m.
The mass percentage content of the rare earth fluoride in the low-temperature cured wear-resistant inorganic phosphate bonded solid lubricating coating material provided by the invention is preferably 6-8%.
In the present invention, the rare earth fluoride is preferably lanthanum fluoride or cerium fluoride.
The mass percentage content of the antimony trioxide in the low-temperature cured wear-resistant inorganic phosphate bonded solid lubricating coating material provided by the invention is preferably 3-4%.
In the invention, the rare earth fluoride and the antimony trioxide are used as auxiliary functional fillers.
In the present invention, the water is preferably deionized water. In the present invention, the deionized water serves as a diluent.
The mass percentage content of fumed silica modified phosphate in the low-temperature cured wear-resistant inorganic phosphate bonded solid lubricating coating material is preferably 5-8%.
In the present invention, the inorganic phosphate is preferably aluminum chromium phosphate.
In the present invention, the fumed silica-modified phosphate is preferably prepared by a process comprising the steps of:
mixing phosphoric acid, chromium oxide, aluminum hydroxide and preparation water to perform acid-base neutralization and crosslinking reaction to obtain an aluminum-chromium phosphate dispersion;
and mixing the aluminum chromium phosphate dispersion liquid with the fumed silica nanoparticles for modification to obtain the fumed silica modified phosphate.
In the invention, the total mass of the phosphoric acid, the chromium oxide, the aluminum hydroxide, the fumed silica nanoparticles and the preparation water is 100%, the mass content of the phosphoric acid is preferably 50-70%, the mass content of the chromium oxide is preferably 3-10%, the mass content of the aluminum hydroxide is preferably 10-20%, the mass content of the fumed silica nanoparticles is preferably 0.5-5%, and the balance is the preparation water.
In the invention, the mass content of the fumed silica nanoparticles is preferably 1-2%.
Phosphoric acid, chromic oxide, aluminum hydroxide and preparation water are mixed to carry out acid-base neutralization crosslinking reaction, so as to obtain the aluminum-chromium phosphate dispersion liquid.
In the invention, the acid-base neutralization crosslinking reaction is preferably carried out at the temperature of 110-120 ℃ for 10-12 h, and preferably under the condition of mechanical stirring.
After the acid-base neutralization crosslinking reaction is finished, the obtained product is preferably naturally cooled to 50 ℃ to obtain the aluminum chromium phosphate dispersion liquid.
After the aluminum chromium phosphate dispersion liquid is obtained, the aluminum chromium phosphate dispersion liquid and the fumed silica nano particles are mixed and modified to obtain the fumed silica modified phosphate.
In the invention, the particle size of the fumed silica nanoparticles is preferably 5-10 nm.
In the present invention, the temperature of the modification is preferably 50 ℃.
After the modification is finished, the natural cooling is preferably carried out to the room temperature, so as to obtain the fumed silica modified phosphate.
The invention also provides a preparation method of the low-temperature cured wear-resistant inorganic phosphate bonded solid lubricating coating material in the technical scheme, which comprises the following steps: and mixing the fumed silica modified phosphate, organic alkali, a layered disulfide, a rare earth fluoride, antimony trioxide and water to obtain the low-temperature cured wear-resistant inorganic phosphate bonded solid lubricating coating material.
In the present invention, the mixing is preferably ball milling dispersion, and the specific parameters of the ball milling dispersion are not particularly limited in the present invention, and can be performed by using the methods well known to those skilled in the art.
The application mode of the low-temperature-cured wear-resistant inorganic phosphate bonded solid lubricating coating material is not particularly limited, and the method known by the technical personnel in the field can be adopted, specifically, the prepared low-temperature-cured wear-resistant inorganic phosphate bonded solid lubricating coating material is uniformly sprayed on the surface of a tinplate test piece or part by using a compressed air spray gun with the pressure of 0.4 MPa.
In the invention, before the spraying, the surface of the tinplate test piece is preferably subjected to 800-mesh sand paper grinding treatment or sand blasting treatment on the surface of the part, and the tinplate test piece and the part after grinding or sand blasting are subjected to ultrasonic treatment in an acetone solution for 30min to remove surface oil stains and rust stains.
In the invention, the thickness of the coating after spraying is preferably 15-20 mu m.
After the spraying is finished, preferably, the paint is placed in the air for 5 to 6 hours to be dried, and then is cured in a forced air drying oven, wherein the curing conditions are preferably as follows: keeping the temperature at 80 plus or minus 5 ℃ for 3 hours, then heating to 190 plus or minus 10 ℃ and keeping the temperature for 3 hours, and naturally cooling to room temperature for use.
In order to further illustrate the present invention, the low temperature cured wear-resistant inorganic phosphate bonded solid lubricant coating material and the method for preparing the same provided by the present invention are described in detail below with reference to examples, which should not be construed as limiting the scope of the present invention.
Example 1
Preparing the low-temperature curing lubricating coating: accurately weighing 115g of phosphoric acid with the mass fraction of 85 percent, adding the phosphoric acid into a three-neck flask, adding 8g of chromium trioxide, mechanically stirring the mixture until the chromium trioxide is completely dissolved, continuously adding 36g of deionized water, slowly adding 20g of 97wt percent aluminum hydroxide powder into the three-neck flask, stirring the mixture until the aluminum hydroxide is completely dissolved, heating the mixture to 105 +/-5 ℃ for refluxing for 1 hour, adding 4g of fumed silica nanoparticles, continuously mechanically stirring the mixture for 2 hours, and cooling the mixture to room temperature. Respectively weighing 20g of the solution (containing 11.6g of fumed silica modified phosphate), adding 1.8g of ethanolamine, 80g of molybdenum disulfide, 5g of antimony trioxide, 5g of lanthanum fluoride and 60g of deionized water, uniformly mixing, transferring to a ball milling tank, carrying out ball milling and dispersing for 48h to obtain uniform coating slurry, marked as No. 1, wherein the mass content of the fumed silica modified phosphate in the low-temperature curing lubricating coating is 6.75%, the mass content of organic alkali ethanolamine is 1.05%, the mass content of layered molybdenum disulfide is 46.57%, the mass content of lanthanum fluoride is 2.91%, the mass content of antimony trioxide is 2.91%, and the balance is water.
Performance of the low temperature cured lubricating coating: and spraying the dispersed slurry on the surface of the part by using compressed air or compressed nitrogen (the surface of the part is pretreated by sand blasting and acetone ultrasound before spraying). The thickness of the coating was controlled to be 15 μm by controlling the number of spraying. And (3) placing the sprayed part in the air for 5 hours, and then curing in a forced air drying oven under the following curing conditions: keeping the temperature at 80 +/-5 ℃ for 3 hours, then heating to 190 ℃ and keeping the temperature for 3 hours, and naturally cooling to room temperature.
The cured coating is soaked in boiling water for 12 hours, and then has no phenomena of bubbling, peeling and the like, the adhesion is 0 grade, the flexibility is 1mm, the impact resistance is more than 50cm, the average friction coefficient of the coating in the atmosphere is 0.046, and the wear rate is 0.51 multiplied by 10 -6 mm 3 /(N·m)。
Example 2
Preparing the low-temperature curing lubricating coating: accurately weighing 115g of phosphoric acid with the mass fraction of 85 percent, adding the phosphoric acid into a three-neck flask, adding 8g of chromium trioxide, mechanically stirring the mixture until the chromium trioxide is completely dissolved, continuously adding 36g of deionized water, slowly adding 20g of 97wt percent aluminum hydroxide powder into the three-neck flask, stirring the mixture until the aluminum hydroxide is completely dissolved, heating the mixture to 105 +/-5 ℃ for refluxing for 1 hour, adding 4g of fumed silica nanoparticles, continuously mechanically stirring the mixture for 2 hours, and cooling the mixture to room temperature. Respectively weighing 20g of the solution (containing 11.6g of fumed silica modified phosphate), adding 3.5g of ethanolamine, 80g of molybdenum disulfide, 5g of antimony trioxide, 5g of cerium fluoride and 60g of deionized water, uniformly mixing, transferring the mixture into a ball milling tank, and carrying out ball milling and dispersion for 48 hours to obtain uniform coating slurry, marked as No. 2, wherein the mass content of the fumed silica modified phosphate in the low-temperature curing lubricating coating is 6.69%, the mass content of the ethanolamine is 2.02%, the mass content of the layered molybdenum disulfide is 46.11%, the mass content of the cerium fluoride is 2.88% and the mass content of the antimony trioxide is 2.88%.
Performance of low temperature cured lubricating coatings: and spraying the dispersed slurry on the surface of the part by using compressed air or compressed nitrogen (the surface of the part is pretreated by sand blasting and acetone ultrasound before spraying). The thickness of the coating was controlled to be 15 μm by controlling the number of spraying. And (3) placing the sprayed part in the air for 6 hours, and then curing in a forced air drying oven under the following curing conditions: keeping the temperature at 80 +/-5 ℃ for 3 hours, then heating to 190 ℃ and keeping the temperature for 3 hours, and naturally cooling to room temperature.
The cured coating is soaked in boiling water for 12 hours without bubbling, peeling and the like, the adhesion is 0 grade through a circling method test, the flexibility is 1mm, the impact resistance is more than 50cm, the average friction coefficient of the coating in the atmosphere is 0.053, and the wear rate is 0.58 multiplied by 10 -6 mm 3 /(N·m)。
Example 3
Preparing the low-temperature curing lubricating coating: accurately weighing 115g of phosphoric acid with the mass fraction of 85 percent, adding the phosphoric acid into a three-neck flask, adding 8g of chromium trioxide, mechanically stirring the mixture until the chromium trioxide is completely dissolved, continuously adding 36g of deionized water, slowly adding 20g of 97wt percent aluminum hydroxide powder into the three-neck flask, stirring the mixture until the aluminum hydroxide is completely dissolved, heating the mixture to 105 +/-5 ℃ for refluxing for 1 hour, adding 4g of fumed silica nanoparticles, continuously mechanically stirring the mixture for 2 hours, and cooling the mixture to room temperature. Respectively weighing 50g of the solution, adding 13g of diethanolamine, 150g of molybdenum disulfide, 10g of antimony trioxide, 15g of lanthanum fluoride and 200g of deionized water, uniformly mixing, transferring the mixture into a ball milling tank, carrying out ball milling and dispersing for 48 hours to obtain uniform coating slurry, marked as No. 3, wherein the mass content of gas phase silicon dioxide modified phosphate in the low-temperature curing lubricating coating is 7.68%, the mass content of diethanolamine is 2.97%, the mass content of layered molybdenum disulfide is 34.25%, the mass content of lanthanum fluoride is 3.42%, and the mass content of antimony trioxide is 2.28%.
Performance of the low temperature cured lubricating coating: and spraying the dispersed slurry on the surface of the part by using compressed air or compressed nitrogen (the surface of the part is pretreated by sand blasting and acetone ultrasound before spraying). The thickness of the coating was controlled to be 15 μm by controlling the number of spraying. And (3) placing the sprayed part in the air for 6 hours, and then curing in a forced air drying oven under the following curing conditions: keeping the temperature at 80 +/-5 ℃ for 3 hours, then heating to 190 ℃ and keeping the temperature for 3 hours, and naturally cooling to room temperature.
The cured coating is soaked in boiling water for 12 hours without bubbling, peeling and the like, the adhesion is 0 grade through a circling method test, the flexibility is 1mm, the impact resistance is more than 50cm, the average friction coefficient of the coating in the atmosphere is 0.046, and the wear rate is 0.39 multiplied by 10 -6 mm 3 /(N·m)。
Example 4
Preparing the low-temperature curing lubricating coating: accurately weighing 115g of phosphoric acid with the mass fraction of 85 percent, adding the phosphoric acid into a three-neck flask, adding 8g of chromium trioxide, mechanically stirring the mixture until the chromium trioxide is completely dissolved, continuously adding 36g of deionized water, slowly adding 20g of 97wt percent aluminum hydroxide powder into the three-neck flask, stirring the mixture until the aluminum hydroxide is completely dissolved, heating the mixture to 105 +/-5 ℃ for refluxing for 1 hour, adding 4g of fumed silica nanoparticles, continuously mechanically stirring the mixture for 2 hours, and cooling the mixture to room temperature. Respectively weighing 40g of the solution, adding 16g of diethanolamine, 120g of tungsten disulfide, 10g of antimony trioxide, 10g of cerium fluoride and 200g of deionized water, uniformly mixing, transferring to a ball milling tank, carrying out ball milling and dispersing for 48 hours to obtain uniform coating slurry, marked as No. 4, wherein the mass content of fumed silica modified phosphate in the low-temperature curing lubricating coating is 5.86%, the mass content of diethanolamine is 4.04%, the mass content of layered tungsten disulfide is 30.30%, the mass content of cerium fluoride is 2.53%, and the mass content of antimony trioxide is 2.53%.
Performance of low temperature cured lubricating coatings: and spraying the dispersed slurry on the surface of the part by using compressed air or compressed nitrogen (the surface of the part is pretreated by sand blasting and acetone ultrasound before spraying). The thickness of the coating was controlled to be 15 μm by controlling the number of spraying. And (3) placing the sprayed part in the air for 6 hours, and then curing in a forced air drying oven under the following curing conditions: keeping the temperature at 80 +/-5 ℃ for 3 hours, then heating to 190 ℃ and keeping the temperature for 3 hours, and naturally cooling to room temperature.
The cured coating is soaked in boiling water for 12 hours without the phenomena of bubbling, peeling and the like, the adhesion is 0 grade, the flexibility is 1mm, the impact resistance is more than 50cm, and the average friction of the coating in the atmosphere is tested by a circling methodCoefficient of 0.058 and wear rate of 0.54X 10 -6 mm 3 /(N·m)。
Example 5
Preparing the low-temperature curing lubricating coating: accurately weighing 115g of phosphoric acid with the mass fraction of 85 percent, adding the phosphoric acid into a three-neck flask, adding 8g of chromium trioxide, mechanically stirring the mixture until the chromium trioxide is completely dissolved, continuously adding 36g of deionized water, slowly adding 20g of 97wt percent aluminum hydroxide powder into the three-neck flask, stirring the mixture until the aluminum hydroxide is completely dissolved, heating the mixture to 105 +/-5 ℃ for refluxing for 1 hour, adding 4g of fumed silica nanoparticles, continuously mechanically stirring the mixture for 2 hours, and cooling the mixture to room temperature. 60g of the solution is weighed respectively, 8g of diethanolamine, 200g of molybdenum disulfide, 15g of antimony trioxide, 15g of lanthanum fluoride and 300g of deionized water are added, the mixture is uniformly mixed and then transferred to a ball milling tank for ball milling and dispersion for 48 hours to obtain uniform coating slurry, wherein the mass content of fumed silica modified phosphate in the low-temperature curing lubricating coating is 5.82%, the mass content of diethanolamine is 1.34%, the mass content of layered molybdenum disulfide is 33.44%, the mass content of lanthanum fluoride is 2.51% and the mass content of antimony trioxide is 2.51%.
Performance of the low temperature cured lubricating coating: and spraying the dispersed slurry on the surface of the part by using compressed air or compressed nitrogen (the surface of the part is pretreated by sand blasting and acetone ultrasound before spraying). The thickness of the coating was controlled to be 15 μm by controlling the number of spraying. And (3) placing the sprayed part in the air for 6 hours, and then curing in a forced air drying oven under the following curing conditions: keeping the temperature at 80 +/-5 ℃ for 3 hours, then heating to 190 ℃ and keeping the temperature for 3 hours, and naturally cooling to room temperature.
The cured coating is soaked in boiling water for 12 hours, and then has no phenomena of bubbling, peeling and the like, the adhesion is 0 grade through a circling method test, the flexibility is 1mm, the impact resistance is more than 50cm, the average friction coefficient of the coating in the atmosphere is 0.040, and the wear rate is 0.46 multiplied by 10 -6 mm 3 /(N·m)。
Example 6
Preparing the low-temperature curing lubricating coating: accurately weighing 115g of phosphoric acid with the mass fraction of 85 percent, adding the phosphoric acid into a three-neck flask, adding 8g of chromium trioxide, mechanically stirring the mixture until the chromium trioxide is completely dissolved, continuously adding 36g of deionized water, slowly adding 20g of 97wt percent aluminum hydroxide powder into the three-neck flask, stirring the mixture until the aluminum hydroxide is completely dissolved, heating the mixture to 105 +/-5 ℃ for refluxing for 1 hour, adding 4g of fumed silica nanoparticles, continuously mechanically stirring the mixture for 2 hours, and cooling the mixture to room temperature. Respectively weighing 50g of the solution, adding 6g of diethanolamine, 150g of molybdenum disulfide, 15g of antimony trioxide, 15g of lanthanum fluoride and 260g of deionized water, uniformly mixing, transferring to a ball milling tank, carrying out ball milling, dispersing for 48 hours, and obtaining uniform coating slurry, wherein the mass content of fumed silica modified phosphate in the low-temperature curing lubricating coating is 5.85%, the mass content of diethanolamine is 1.21%, the mass content of layered molybdenum disulfide is 30.24%, the mass content of lanthanum fluoride is 3.02%, and the mass content of antimony trioxide is 3.02%.
Performance of the low temperature cured lubricating coating: and spraying the dispersed slurry on the surface of the part by using compressed air or compressed nitrogen (the surface of the part is pretreated by sand blasting and acetone ultrasound before spraying). The thickness of the coating was controlled to 15 μm by controlling the number of spraying. And (3) placing the sprayed part in the air for 5 hours, and then curing in a forced air drying oven under the following curing conditions: keeping the temperature at 80 +/-5 ℃ for 3 hours, then heating to 190 ℃ and keeping the temperature for 3 hours, and naturally cooling to room temperature.
The cured coating is soaked in boiling water for 12 hours without bubbling, peeling and the like, the adhesion is 0 grade through a circling method test, the flexibility is 1mm, the impact resistance is more than 50cm, the average friction coefficient of the coating in the atmosphere is 0.05, and the wear rate is 0.55 multiplied by 10 -6 mm 3 /(N·m)。
Example 7
Preparing the low-temperature curing lubricating coating: accurately weighing 115g of phosphoric acid with the mass fraction of 85 percent, adding the phosphoric acid into a three-neck flask, adding 8g of chromium trioxide, mechanically stirring the mixture until the chromium trioxide is completely dissolved, continuously adding 36g of deionized water, slowly adding 20g of 97wt percent aluminum hydroxide powder into the three-neck flask, stirring the mixture until the aluminum hydroxide is completely dissolved, heating the mixture to 105 +/-5 ℃ for refluxing for 1 hour, adding 4g of fumed silica nanoparticles, continuously mechanically stirring the mixture for 2 hours, and cooling the mixture to room temperature. Respectively weighing 30g of the solution, adding 2g of diethanolamine, 110g of molybdenum disulfide, 10g of antimony trioxide, 6g of lanthanum fluoride and 100g of deionized water, uniformly mixing, transferring to a ball milling tank, carrying out ball milling, dispersing for 48 hours, and obtaining uniform coating slurry, wherein the mass content of fumed silica modified phosphate in the low-temperature curing lubricating coating is 6.74%, the mass content of diethanolamine is 0.78%, the mass content of layered molybdenum disulfide is 42.64%, the mass content of lanthanum fluoride is 2.33%, and the mass content of antimony trioxide is 3.88%.
Performance of low temperature cured lubricating coatings: and spraying the dispersed slurry on the surface of the part by using compressed air or compressed nitrogen (the surface of the part is pretreated by sand blasting and acetone ultrasound before spraying). The thickness of the coating was controlled to be 15 μm by controlling the number of spraying. And (3) placing the sprayed part in the air for 5 hours, and then curing in a forced air drying oven under the following curing conditions: keeping the temperature at 80 +/-5 ℃ for 3 hours, then heating to 190 ℃ and keeping the temperature for 3 hours, and naturally cooling to room temperature.
The cured coating is soaked in boiling water for 12 hours without bubbling, peeling and the like, the adhesion is 0 grade through a circling method test, the flexibility is 1mm, the impact resistance is more than 50cm, the average friction coefficient of the coating in the atmosphere is 0.054, and the wear rate is 0.42 multiplied by 10 -6 mm 3 /(N·m)。
Example 8
Preparing the low-temperature curing lubricating coating: accurately weighing 115g of 85% phosphoric acid, adding into a three-neck flask, adding 8g of chromium trioxide, mechanically stirring until the chromium trioxide is completely dissolved, continuously adding 36g of deionized water, slowly adding 20g of 97 wt% aluminum hydroxide powder into the three-neck flask, stirring until the aluminum hydroxide is completely dissolved, heating to 105 +/-5 ℃, refluxing for 1 hour, adding 4g of fumed silica nanoparticles, continuously mechanically stirring for 2 hours, and cooling to room temperature. Respectively weighing 30g of the solution, adding 4g of ethanolamine, 105g of tungsten disulfide, 8g of antimony trioxide, 10g of lanthanum fluoride and 110g of deionized water, uniformly mixing, transferring to a ball milling tank, carrying out ball milling, dispersing for 48 hours, and obtaining uniform coating slurry, wherein the mass content of fumed silica modified phosphate in the low-temperature curing lubricating coating is 6.52%, the mass content of ethanolamine is 1.50%, the mass content of layered tungsten disulfide is 39.33%, the mass content of lanthanum fluoride is 3.75%, and the mass content of antimony trioxide is 3.00%.
Performance of low temperature cured lubricating coatings: and spraying the dispersed slurry on the surface of the part by using compressed air or compressed nitrogen (the surface of the part is pretreated by sand blasting and acetone ultrasound before spraying). The thickness of the coating was controlled to be 15 μm by controlling the number of spraying. And (3) placing the sprayed part in the air for 5 hours, and then curing in a forced air drying oven under the following curing conditions: keeping the temperature at 80 +/-5 ℃ for 3 hours, then heating to 190 ℃ and keeping the temperature for 3 hours, and naturally cooling to room temperature.
The cured coating is soaked in boiling water for 12 hours without bubbling, peeling and the like, the adhesion is 0 grade through a circling method test, the flexibility is 1mm, the impact resistance is more than 50cm, the average friction coefficient of the coating in the atmosphere is 0.058, and the wear rate is 0.59 multiplied by 10 -6 mm 3 /(N·m)。
FIG. 1 shows the cross-sectional micro-morphology of the composite coating prepared in example 1 of the present invention, wherein the coating thickness is 15 μm and the coating bonds well with the metal substrate. After the coating is soaked in boiling water for 12 hours, the phenomena of bubbling, peeling and the like do not exist, and the adhesion is tested to be 0 grade by a circle drawing method, which shows that the coating realizes complete curing at 190 ℃, the coating is well combined with a matrix, and the coating has excellent hot water soaking resistance.
FIG. 2 shows the adhesion, flexibility and impact resistance test results of the composite coating prepared in example 1 of the present invention, where the adhesion is 0 according to GB/T9286 standard, the flexibility is 1mm according to GB/T1731 standard, and the impact resistance of the coating is greater than 50cm according to GB/T1732 standard, which shows that the coating has good bonding with the substrate and also has good comprehensive mechanical properties such as flexibility and impact resistance.
FIG. 3 is a curve of the friction coefficient of an atmospheric balloon disk of the low-temperature cured composite lubricating coating prepared in embodiments 1 to 4 of the present invention, and the average friction coefficients of the composite coatings with different organic base contents are all between 0.03 and 0.06, which shows that the low-temperature cured coating has good antifriction performance.
FIG. 4 shows an atmospheric balloon disk with a low-temperature cured composite lubricating coating prepared in embodiments 1 to 4 of the present inventionThe wear rate of the composite coating corresponding to different contents of organic alkali is 0.4-0.6 multiplied by 10 -6 mm 3 Within the range of/(/ N · m), the coating is said to have good abrasion resistance.
Table 1 shows the main performance index test results of the products in the examples, and it can be known that the low-temperature cured wear-resistant inorganic phosphate bonded solid lubricating coating material provided by the present invention not only has the characteristic of low-temperature curing, but also has excellent comprehensive mechanical properties.
TABLE 1 Main Performance index of the products in the examples
Figure BDA0003440467660000121
Wherein, the flexibility is determined to be qualified after being folded on a direct 1MM test bar according to the standard without falling off; the coating is impact-resistant, namely the impact hammer impacts at the height of 50cm, and the coating does not fall off, namely the coating is qualified.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner. It should be noted that, for those skilled in the art, without departing from the principle of the present invention, several improvements and modifications can be made, and these improvements and modifications should also be construed as the protection scope of the present invention.

Claims (9)

1. The low-temperature-cured wear-resistant inorganic phosphate bonded solid lubricating coating material is characterized by comprising the following components in percentage by mass: 5-15% of fumed silica modified phosphate, 0.5-5% of organic alkali, 30-60% of layered dichalcogenide, 2-10% of rare earth fluoride, 2-6% of antimony trioxide and the balance of water; the organic alkali is ethanolamine or diethanolamine;
the fumed silica modified phosphate is prepared by a process comprising the steps of: inorganic phosphate, fumed silica nanoparticles and water are mixed for modification.
2. The low temperature cure wear-resistant inorganic phosphate bonded solid lubricant coating material of claim 1, wherein the inorganic phosphate is aluminum chromium phosphate.
3. The low-temperature-cured wear-resistant inorganic phosphate bonded solid lubricating coating material according to claim 1 or 2, wherein the fumed silica nanoparticles have a particle size of 5-10 nm.
4. The low temperature cure wear-resistant inorganic phosphate bonded solid lubricant coating material of claim 2, wherein the fumed silica-modified phosphate is prepared by a process comprising:
mixing phosphoric acid, chromium oxide, aluminum hydroxide and preparation water to perform acid-base neutralization and crosslinking reaction to obtain an aluminum-chromium phosphate dispersion;
and mixing the aluminum chromium phosphate dispersion liquid with the fumed silica nanoparticles for modification to obtain the fumed silica modified phosphate.
5. The low-temperature-curing wear-resistant inorganic phosphate bonded solid lubricating coating material as claimed in claim 4, wherein the mass content of phosphoric acid is 50-70%, the mass content of chromium oxide is 3-10%, the mass content of aluminum hydroxide is 10-20%, the mass content of fumed silica nanoparticles is 0.5-5%, and the balance is water for preparation, based on 100% of the total mass of the phosphoric acid, the chromium oxide, the aluminum hydroxide, the fumed silica nanoparticles and the water for preparation.
6. The low temperature cure wear-resistant inorganic phosphate bonded solid lubricant coating material of claim 1, wherein the layered dichalcogenide is molybdenum disulfide or tungsten disulfide.
7. The low-temperature-cured wear-resistant inorganic phosphate bonded solid lubricating coating material according to claim 1 or 6, wherein the lamellar dichalcogenide compound has a particle size of 0.8 to 1.2 μm and a thickness of 0.1 to 0.8 μm.
8. The low temperature cure wear-resistant inorganic phosphate bonded solid lubricant coating material of claim 1, wherein the rare earth fluoride is lanthanum fluoride or cerium fluoride.
9. The preparation method of the low-temperature-cured wear-resistant inorganic phosphate bonded solid lubricating coating material as claimed in any one of claims 1 to 8, characterized by comprising the following steps:
and mixing the fumed silica modified phosphate, organic alkali, a layered disulfide, a rare earth fluoride, antimony trioxide and water to obtain the low-temperature cured wear-resistant inorganic phosphate bonded solid lubricating coating material.
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