CN114133769B - Lubricating protective coating for surface of sliding component in nuclear reactor system - Google Patents

Lubricating protective coating for surface of sliding component in nuclear reactor system Download PDF

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CN114133769B
CN114133769B CN202111517234.XA CN202111517234A CN114133769B CN 114133769 B CN114133769 B CN 114133769B CN 202111517234 A CN202111517234 A CN 202111517234A CN 114133769 B CN114133769 B CN 114133769B
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reactor system
nuclear reactor
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coating
protective coating
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CN114133769A (en
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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
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/18—Fireproof paints including high temperature resistant 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
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    • C09D7/61—Additives non-macromolecular inorganic

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Abstract

The invention provides a lubricating protective coating for the surface of a sliding part in a nuclear reactor system, which is prepared by taking inorganic silicon modified inorganic phosphate as a basic resin binder, taking a mixture of a flaky dithio compound and graphite as a solid lubricant, taking rare earth fluoride and a boron compound as neutron absorbers, taking antimony trioxide and titanium dioxide as auxiliary functional fillers, taking deionized water as a diluent, and performing ball milling and dispersion to obtain a uniform coating. After the paint is sprayed or brushed on a metal or alloy matrix, a uniform and compact high-temperature-resistant and radiation-resistant solid lubricating composite coating is formed after high-temperature curing. The performance test shows that the coating material has good comprehensive performances such as adhesive force, flexibility, impact resistance, water immersion resistance and the like on a metal or alloy matrix, has excellent high temperature resistance and irradiation resistance, and can be used for surface anti-sticking and lubrication protection of relevant sliding parts in a nuclear reactor system under special working conditions such as long-term high temperature, strong radiation and the like.

Description

Lubricating protective coating for surface of sliding component in nuclear reactor system
Technical Field
The invention relates to a lubricating and protecting coating for the surface of a sliding part in a nuclear reactor system, in particular to an inorganic phosphate coating for the long-term high-temperature lubricating and protecting of the surface of the sliding part under the special working conditions of high-low temperature alternation, strong radiation, helium medium and the like in the nuclear reactor system.
Background
Under the large background of carbon peaking and carbon neutralization, the transformation of an energy structure is accelerated, clean, low-carbon, safe and efficient green nuclear energy is developed, the natural trend of the world energy development is realized, and the natural selection of implementing ecological civilization construction strategy and energy revolution in China in a new era is realized. Nuclear reactors, which are the key core systems of nuclear power, contain a large number of moving parts, such as rolling and sliding bearings, gears, turbines, sprockets, and connecting sleeves, collars, etc. in control rod systems. The moving parts are subjected to coupling action in complex environments such as high-low temperature alternation, strong radiation, special media, dynamic friction and abrasion for a long time, and the surfaces of the parts are easy to lose efficacy due to abrasion, so that the operation stability and safety of the reactor are seriously influenced. Therefore, the surfaces of the relevant sliding parts must be subjected to surface lubrication protection treatment to ensure the safe and stable operation of the reactor.
The current lubricating material for the sliding parts of the nuclear reactor system is mainly ion-plated MoS 2 、MoS 2 -Ti、Au/MoS 2 And TiN/MoS 2 Thin film-like coating of equal multilayer structure, and plasma-sprayed Cr 3 C 2 The coatings have good high temperature resistance and radiation resistance, but the coating is limited to be used in a large amount in the nuclear field due to the limitations of complex process, high requirement on part precision, high price cost and the like. In contrast, organic bonded solid lubricating coatings represented by polyimide and polyetheretherketone are widely used, but due to degradation at high temperature and strong radiation, the organic bonded solid lubricating coatings have short life and are not suitable for long-term lubrication protection in nuclear radiation environments. The inorganic phosphoric acid bonding solid lubricating coating has good temperature resistance and irradiation resistance, is an ideal lubricating coating material applied to the field of nuclear radiation, but has the defects of brittleness, no bearing resistance and the like, and needs to be solved urgently. Therefore, the invention aims to solve the problem of the flexibility of the inorganic phosphate resin and develop a long-term lubricating and anti-sticking coating material which has excellent comprehensive mechanical properties and is suitable for the surface of a sliding part in a nuclear reactor system.
Disclosure of Invention
The invention aims to provide an inorganic phosphate coating suitable for lubricating and preventing adhesion of the surface of a sliding part in a nuclear reaction system and a preparation method thereof, and mainly aims to solve the problems of adhesion prevention and lubrication protection of a related sliding part in the nuclear reactor system under complex working conditions of long-term high-low temperature alternation, strong radiation and the like. The coating preparation and construction process is simple and the production cost is low.
The invention relates to a lubricating protective coating for the surface of a sliding part in a nuclear reactor system, which is prepared by grinding and dispersing inorganic silicon modified inorganic phosphate with good high temperature resistance and irradiation resistance in a ball mill tank for 48 hours to obtain a uniform coating by using inorganic silicon modified inorganic phosphate as a basic resin binder, a mixture of a flaky dithio compound and graphite as a solid lubricating filler, rare earth fluoride and a boron compound as neutron absorbers, antimony trioxide and titanium dioxide as auxiliary functional fillers and deionized water as diluents.
The invention relates to a lubricating protective coating for the surface of a sliding part in a nuclear reactor system, which comprises the following components in percentage by weight: 10-30% of inorganic silicon modified phosphate, 10-50% of layered dichalcogenide compound, 10-50% of graphite powder, 1-10% of rare earth fluoride, 0.5-2% of boron compound, 0.5-3% of antimony trioxide, 0.2-1.5% of titanium dioxide and the balance of deionized water.
The lamellar dithio compound is flaky molybdenum disulfide or flaky tungsten disulfide, the particle size is 0.8-1.2 mu m, the thickness is 0.1-0.8 mu m, and the purity is more than or equal to 98%.
The graphite powder has the particle size of 0.2 to 2 mu m, the thickness of 0.1 to 1.2 mu m and the purity of more than or equal to 98 percent.
The rare earth fluoride is lanthanum fluoride or cerium fluoride, the particle size is 200 to 500 nm, and the purity is more than or equal to 99%.
The boron compound is boron oxide, is an amorphous nano-particle with the particle size of 0.1 to 0.8.
The titanium dioxide is nanoparticles with the particle size of 10 to 100 nm.
The preparation method of the inorganic silicon modified inorganic phosphate comprises the steps of dispersing phosphoric acid, chromium trioxide and aluminum hydroxide powder in deionized water, heating to 105-115 ℃, refluxing for 1-2 hours, adding inorganic silicon, stirring for 1-2 hours to be homogeneous, and naturally cooling to room temperature to obtain the inorganic phosphate. Wherein the inorganic silicon is fumed silica or alkaline silica sol; the mass ratio of phosphoric acid to chromium trioxide is 12 to 1; the mass ratio of phosphoric acid to aluminum hydroxide powder is (1) - (4); the mass ratio of the phosphoric acid to the inorganic silicon is 28 to 1.
The invention discloses a using method of a lubricating protective coating for the surface of a sliding part in a nuclear reactor system. And (3) after coating, placing in the air for 5 to 6 hours, keeping the temperature at 120 +/-10 ℃ for 2 hours after the surface is dried, continuing to heat to 310 ℃, keeping the temperature for 1 hour, and naturally cooling to room temperature to obtain the completely cured lubricating protective coating. The thickness of the coating is controlled by the coating times, and the general thickness is 20 to 100 mu m. The lubricating protective coating is suitable for lubricating and preventing burning and sticking on the surface of metal or alloy in a nuclear radiation environment at the temperature of RT-800 ℃.
The invention has the following advantages and beneficial effects:
1. the lubricating protective coating for the surface of the sliding component in the nuclear reactor system, which is prepared by the invention, has the advantages of simple preparation process, convenient construction and low cost, and is beneficial to engineering application.
2. According to the invention, inorganic silicon modified phosphate with good temperature resistance and radiation resistance is used as continuous phase bonding resin, and the high-temperature oxidation and radiation damage of the filler can be effectively reduced through the coating effect of the resin on the lubricating filler and the functional filler; on the other hand, the rare earth fluoride can generate a synergistic lubrication effect with the lubricating filler, the bearing capacity of the coating is improved, the service life of the coating is prolonged, neutrons of an annihilation part can be absorbed, and the damage of strong irradiation to the lubricating and functional filler is further reduced. Finally, the coating is ensured to have a long-term lubricating and protecting function, and the designed operation cycle of the reactor for more than forty years is met.
3. The invention is suitable for long-term surface lubrication and anti-sticking protection of relevant metal sliding parts in a nuclear reactor system in severe environments of high and low temperature alternation, heavy load and strong radiation, adopts a spraying, brushing or dip-coating mode to prepare a coating on the surface of metal or alloy subjected to sand blasting treatment, and has excellent comprehensive properties such as coating adhesion, flexibility, impact resistance, high temperature resistance and the like after high-temperature curing. 1.34X 10 of 6 After Gy gamma ray irradiation, the coating surface is intact (figure 1), the average friction coefficient is less than 0.06, the abrasion life is more than 150 ten thousand turns in helium medium, and the abrasion rate is less than 9.0 multiplied by 10 -8 mm/Nm (figures 2 and 3) is basically consistent with the tribology performance before irradiation, and still shows good antifriction and wear-resistant performances.
Drawings
FIG. 1 is a microstructure of the coating after irradiation with gamma rays.
FIG. 2 is a graph of the coefficient of friction of the coating in different media before and after gamma irradiation.
FIG. 3 is a comparison of the average coefficient of friction and wear rate of the coating in different media before and after gamma irradiation.
Detailed Description
The present invention will be described in further detail below by way of examples with reference to the accompanying drawings, but the present invention is not limited to the following embodiments.
Example 1
Preparation of a lubricating protective coating for the surfaces of sliding parts in a nuclear reactor system: accurately weighing 340g of 85% phosphoric acid, adding into a three-neck flask, adding 25g of chromium trioxide, mechanically stirring until the phosphoric acid is completely dissolved, continuously adding 110 g of deionized water, slowly adding 60g of 97% aluminum hydroxide powder into the three-neck flask, stirring until the aluminum hydroxide is completely dissolved, heating to 110 +/-5 ℃, refluxing for 1 hour, adding 12g of fumed silica nanoparticles for improving the flexibility of the inorganic chromium phosphate aluminum binder, continuously mechanically stirring for 2 hours, and cooling to room temperature to obtain the inorganic silicon modified chromium phosphate aluminum binder. Weighing 40g of the modified chromium phosphate aluminum binder, adding 25g of molybdenum disulfide, 25g of graphite powder, 2g of antimony trioxide, 5g of lanthanum fluoride, 2g of boron oxide, 1 g of titanium dioxide nanoparticles and 150 g of deionized water, uniformly mixing, transferring to a ball milling tank (grinding beads are agate beads or ceramic beads with the particle size of 0.5-3 mm), and carrying out ball milling dispersion at the speed of 72 rpm for 48 hours to obtain the uniform coating.
And (3) coating the uniformly dispersed paint on the metal matrix subjected to sand blasting in a spraying mode, standing in the air for 5-6 hours, keeping the temperature in a high-temperature muffle furnace at 120 ℃ for 2 hours, continuously heating to 310 ℃ and keeping the temperature for 1 hour, and naturally cooling to room temperature to obtain the lubricating protective coating.
In this embodiment, the performance parameters of the lubricating protective coating for the surface of the sliding component in the nuclear reactor system are as follows:
the adhesion force of the lubricating protective coating coated with the thickness of 20 mu m is grade 1 (GB/T9286), the flexibility reaches 1mm (GB/T1731), the impact resistance is more than 50cm (GB/T1732), and the coating is 1.34 x 10 6 The surface was intact after Gy gamma irradiation. The average coefficient of friction of the coating after irradiation in the atmosphere was 0.068 and in the helium medium was 0.048The wear life exceeds 150 ten thousand revolutions.
Example 2
Preparation of a lubricating protective coating for the surfaces of sliding parts in a nuclear reactor system: accurately weighing 340g of 85% phosphoric acid, adding into a three-neck flask, adding 25g of chromium trioxide, mechanically stirring until the phosphoric acid is completely dissolved, continuously adding 110 g of deionized water, slowly adding 60g of 97% aluminum hydroxide powder into the three-neck flask, stirring until the phosphoric acid is completely dissolved, heating to 110 +/-5 ℃, refluxing for 1 hour, adding 12g of alkaline silica sol, continuously mechanically stirring for 2 hours, and cooling to room temperature to obtain the inorganic silicon modified chromium aluminum phosphate binder. Weighing 40g of the modified chromium phosphate aluminum binder, adding 30g of molybdenum disulfide, 20g of graphite powder, 3 g of antimony trioxide, 4g of lanthanum fluoride, 2g of boron oxide, 1 g of titanium dioxide nanoparticles and 150 g of deionized water, uniformly mixing, transferring to a ball milling tank, and carrying out ball milling dispersion at a speed of 72 rpm for 48 hours to obtain a uniform coating. And (3) coating the uniformly dispersed paint on the metal matrix subjected to sand blasting in a spraying mode, standing in the air for 5-6 hours, keeping the temperature in a high-temperature muffle furnace at 120 ℃ for 2 hours, continuously heating to 310 ℃ and keeping the temperature for 1 hour, and naturally cooling to room temperature to obtain the lubricating protective coating.
In this embodiment, the performance parameters of the lubricating protective coating for the surface of the sliding component in the nuclear reactor system are as follows:
the adhesion force of the lubricating protective coating coated with the thickness of 20 mu m is grade 1 (GB/T9286), the flexibility reaches 1mm (GB/T1731), the impact resistance is more than 50cm (GB/T1732), and the coating is 1.34 x 10 6 The surface was intact after Gy gamma irradiation. After irradiation, the average friction coefficient of the coating in the atmosphere is 0.065, the average friction coefficient in a helium medium is 0.042, and the wear life is over 150 ten thousand turns.
Example 3
Preparation of a lubricating protective coating for the surfaces of sliding parts in a nuclear reactor system: accurately weighing 340g of 85% phosphoric acid, adding the phosphoric acid into a three-neck flask, adding 25g of chromium trioxide, mechanically stirring until the phosphoric acid is completely dissolved, continuously adding 110 g of deionized water, slowly adding 60g of 97% aluminum hydroxide powder into the three-neck flask, stirring until the aluminum hydroxide is completely dissolved, heating to 110 +/-5 ℃, refluxing for 1 hour, adding 12g of fumed silica nanoparticles for improving the flexibility of the inorganic chromium phosphate aluminum binder, continuously mechanically stirring for 2 hours, and cooling to room temperature to obtain the inorganic silicon modified chromium phosphate aluminum binder. Weighing 40g of the modified chromium phosphate aluminum binder, adding 25g of tungsten disulfide, 25g of graphite powder, 2g of antimony trioxide, 5g of cerium fluoride, 2g of boron oxide, 1 g of titanium dioxide nanoparticles and 150 g of deionized water, uniformly mixing, transferring to a ball milling tank, and carrying out ball milling dispersion at a speed of 72 rpm for 48 hours to obtain a uniform coating.
And (3) coating the uniformly dispersed paint on a metal matrix subjected to sand blasting in a spraying manner, standing in the air for 5 to 6 hours, keeping the temperature in a high-temperature muffle furnace at 120 ℃ for 2 hours, continuously heating to 310 ℃, keeping the temperature for 1 hour, and naturally cooling to room temperature to obtain the lubricating protective coating.
In this embodiment, the performance parameters of the lubricating protective coating for the surface of the sliding component in the nuclear reactor system are as follows:
the adhesion force of the lubricating protective coating coated with the thickness of 20 mu m is grade 1 (GB/T9286), the flexibility reaches 1mm (GB/T1731), the impact resistance is more than 50cm (GB/T1732), and the coating is 1.34 x 10 6 The surface was intact after Gy gamma irradiation. After irradiation, the average friction coefficient of the coating in the atmosphere is 0.072, the average friction coefficient of the coating in a helium medium is 0.05, and the abrasion life is over 150 ten thousand revolutions.
Example 4
Preparation of a lubricating protective coating for the surfaces of sliding parts in a nuclear reactor system: accurately weighing 340g of 85% phosphoric acid, adding into a three-neck flask, adding 25g of chromium trioxide, mechanically stirring until the phosphoric acid is completely dissolved, continuously adding 110 g of deionized water, slowly adding 60g of 97% aluminum hydroxide powder into the three-neck flask, stirring until the aluminum hydroxide is completely dissolved, heating to 110 +/-5 ℃, refluxing for 1 hour, adding 12g of fumed silica nanoparticles for improving the flexibility of the inorganic chromium phosphate aluminum binder, continuously mechanically stirring for 2 hours, and cooling to room temperature to obtain the inorganic silicon modified chromium phosphate aluminum binder. Weighing 40g of the modified chromium phosphate aluminum binder, adding 20g of tungsten disulfide, 30g of graphite powder, 3 g of antimony trioxide, 4g of lanthanum fluoride, 2g of boron oxide, 1 g of titanium dioxide nanoparticles and 150 g of deionized water, uniformly mixing, transferring to a ball milling tank, and carrying out ball milling dispersion at a speed of 72 rpm for 48 hours to obtain a uniform coating.
And (3) coating the uniformly dispersed paint on the metal matrix subjected to sand blasting in a spraying mode, standing in the air for 5-6 hours, keeping the temperature in a high-temperature muffle furnace at 120 ℃ for 2 hours, continuously heating to 310 ℃ and keeping the temperature for 1 hour, and naturally cooling to room temperature to obtain the lubricating protective coating.
In this embodiment, the performance parameters of the lubricating protective coating for the surface of the sliding component in the nuclear reactor system are as follows:
the adhesion force of the lubricating protective coating coated with the thickness of 20 mu m is grade 1 (GB/T9286), the flexibility reaches 1mm (GB/T1731), the impact resistance is more than 50cm (GB/T1732), and the coating is 1.34 x 10 6 The surface was intact after Gy gamma irradiation. After irradiation, the average friction coefficient of the coating in the atmosphere is 0.075, the average friction coefficient in a helium medium is 0.054, and the wear life exceeds 150 ten thousand revolutions.

Claims (6)

1. A lubrication protective coating for the surface of a sliding part in a nuclear reactor system is prepared by taking inorganic phosphate modified by inorganic silicon as a basic resin binder, taking a mixture of a flaky dithio compound and graphite as a solid lubricant, taking a rare earth fluoride and a boron compound as neutron absorbers, taking antimony trioxide and titanium dioxide as auxiliary functional fillers, taking deionized water as a diluent, and performing ball milling dispersion to obtain a uniform coating; the weight percentage of each raw material component is as follows: 10-30% of inorganic silicon modified phosphate, 10-50% of flaky dichalcogenide, 10-50% of graphite powder, 1-10% of rare earth fluoride, 0.5-2% of boron compound, 0.5-3% of antimony trioxide, 0.2-1.5% of titanium dioxide and the balance of deionized water; the inorganic silicon modified inorganic phosphate is prepared from the following raw materials by the following process: dispersing phosphoric acid, chromium oxide and aluminum hydroxide powder in deionized water, heating to 105-115 ℃, refluxing for 1-2 hours, adding inorganic silicon, stirring for 1-2 hours to obtain a homogeneous phase, and naturally cooling to room temperature to obtain the product; the inorganic silicon is fumed silica or alkaline silica sol.
2. The lubricating protective coating for a surface of a sliding member in a nuclear reactor system as set forth in claim 1, wherein: the flaky dithio compound is flaky molybdenum disulfide or flaky tungsten disulfide.
3. A lubricant protective coating for the surfaces of sliding parts in a nuclear reactor system as claimed in claim 1, wherein: the rare earth fluoride is lanthanum fluoride or cerium fluoride.
4. A lubricant protective coating for the surfaces of sliding parts in a nuclear reactor system as claimed in claim 1, wherein: the boron compound is boron oxide nanoparticles.
5. A lubricant protective coating for the surfaces of sliding parts in a nuclear reactor system as claimed in claim 1, wherein: the titanium dioxide is nano particles with the particle size of less than 200 nm.
6. A lubricant protective coating for the surfaces of sliding parts in a nuclear reactor system as claimed in claim 1, wherein: the mass ratio of the phosphoric acid to the chromium trioxide is 12 to 1; the mass ratio of the phosphoric acid to the aluminum hydroxide powder is 2 to 1; the mass ratio of the phosphoric acid to the inorganic silicon is 28 to 1.
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CN114672366B (en) * 2022-03-30 2023-07-18 西安建筑科技大学 High-temperature antioxidant self-lubricating composite coating and preparation and use methods thereof
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CN115491247B (en) * 2022-09-29 2023-06-02 中国科学院兰州化学物理研究所 High-temperature-resistant solid lubricating coating and preparation and application thereof
CN116554950B (en) * 2023-05-19 2024-04-26 中国科学院兰州化学物理研究所 Friction matching pair method for wide-temperature-range lubrication and application

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