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CN-121249190-B - MoS-based2Antifriction wear-resistant composite metal coating material and preparation method thereof

CN121249190BCN 121249190 BCN121249190 BCN 121249190BCN-121249190-B

Abstract

The invention discloses an antifriction and wear-resistant composite metal coating material based on MoS 2 and a preparation method thereof in the field of metal coatings, which can realize low friction coefficient stability far superior to that of the traditional metal coating by forming double low friction components through MoS 2 and nitrogen doped carbon graphite materials, and meanwhile, the metal-metal sulfide composite support phase endows the coating with high hardness and high toughness, the wear rate can be controlled at a lower level, and the core contradiction of poor wear resistance and poor antifriction caused by wear resistance of the traditional coating is solved. In the invention, moS 2 is wrapped by metal phase and nitrogen doped carbon graphite carbon, which can reduce contact with water molecules in air, avoid antifriction failure caused by MoO 3 generation, have excellent corrosion resistance with metal simple substance, can prevent corrosive medium from penetrating into the coating, and prolong the service life of the coating compared with the traditional coating under the corrosion-abrasion coupling working condition (such as ocean equipment and chemical pipelines).

Inventors

  • LIU EN
  • Ye Hezhou
  • Julio Villarfort
  • ZHU WENBIN
  • FAN HONGXIAN
  • ZHANG YIZHOU

Assignees

  • 毅骋智造新材料科技(太仓)有限公司

Dates

Publication Date
20260512
Application Date
20251203

Claims (10)

  1. 1. A preparation method of an antifriction and wear-resistant composite metal coating material based on MoS 2 is characterized by comprising the following steps: A1, dissolving 3-aminopyrazole in a mixed solution of anhydrous DMF and N, N-dimethyl ethylenediamine, introducing flowing nitrogen, adding anhydrous potassium carbonate and cuprous chloride, uniformly mixing, adding 2-bromopyridine, continuously stirring until a reaction system is uniform, raising the reaction temperature to perform reflux reaction, adding deionized water to quench after the reaction is finished, adding ethyl acetate to extract, collecting an organic phase, washing the organic phase with a saturated NaCl aqueous solution, drying the organic phase to remove water, and concentrating by rotary evaporation to obtain an intermediate 1; A2, dissolving the intermediate 1 prepared in the step A1 in anhydrous dichloromethane, transferring to an ice water bath condition, stirring for full cooling, slowly adding triethylamine, uniformly mixing, dropwise adding acryloyl chloride, stirring in the ice water bath after the dropwise adding, transferring to a room temperature condition for continuous reaction for 2-3 hours, adding a saturated sodium bicarbonate aqueous solution for quenching reaction, collecting an organic phase, sequentially washing the organic phase with deionized water, a hydrochloric acid aqueous solution and a saturated NaCl aqueous solution, drying, removing water, and concentrating under reduced pressure to obtain an intermediate 2; A3, dissolving ammonium heptamolybdate in deionized water, adding nitric acid, uniformly mixing, transferring into a high-pressure reaction kettle, heating to perform heat treatment, cooling to room temperature after the reaction is finished, centrifuging, collecting precipitate, washing with deionized water, and freeze-drying to obtain MoO 3 nano material; A4, dispersing the MoO 3 nano material prepared in the step A3 in deionized water, adding sodium dodecyl benzene sulfonate, mixing uniformly, placing in an ice water bath condition, dropwise adding the intermediate 2 reaction solution into the reaction system, continuously stirring until the reaction system is in a uniform state, adding a potassium persulfate aqueous solution, keeping stirring and reacting for 6-8 hours under the ice water bath condition, centrifuging, discarding the supernatant, repeatedly washing with deionized water and absolute ethyl alcohol in sequence, and freeze-drying to obtain the MoO 3 /polymer composite material; A5, dispersing the MoO 3 /polymer composite material prepared in the step A4 in deionized water, adding metal salt aqueous solution, carrying out complexation reaction under the condition of room temperature, centrifuging after the reaction is finished, discarding the supernatant, repeatedly washing with deionized water, and freeze-drying to obtain the metal complex MoO 3 /polymer composite material; And A6, respectively placing the metal complex MoO 3 /polymer composite material and thiourea prepared in the step A5 in two quartz boats, placing the quartz boat containing thiourea in the upstream of a tube furnace, placing the quartz boat containing the metal complex MoO 3 /polymer composite material in the downstream of the tube furnace, introducing mixed gas of H 2 /Ar into the tube furnace, raising the temperature for vulcanization reaction, stopping heating after the reaction is finished, naturally cooling to room temperature, repeatedly washing with deionized water and absolute ethyl alcohol, performing vacuum drying, and performing ball milling treatment to obtain the metal coating material.
  2. 2. The preparation method of the friction-reducing wear-resistant composite metal coating material based on MoS 2 , which is disclosed in claim 1, is characterized in that in step A1, the mass ratio of 3-aminopyrazole to 2-bromopyridine is 1:2.3-2.8, the mass concentration of 3-aminopyrazole in anhydrous DMF is 0.02-0.03g/mL, and the mass ratio of 3-aminopyrazole, anhydrous potassium carbonate and cuprous chloride is 1:3.5-4.5:0.012-0.018.
  3. 3. The preparation method of the MoS 2 -based antifriction and wear-resistant composite metal coating material is characterized in that in the step A1, the addition volume of N, N-dimethyl ethylenediamine is 0.5-0.6% of the volume of anhydrous DMF, and in the step A1, the reaction temperature of the reflux reaction is 100-120 ℃ and the reaction time of the reflux reaction is 12-18h.
  4. 4. The method for preparing the MoS 2 -based antifriction and wear-resistant composite metal coating material is characterized in that in the step A2, the mass-volume ratio between the intermediate 1 and the acrylic chloride is 1.25-1.875g/mL, and the mass-volume ratio between the intermediate 1 and the triethylamine is 0.6-1.0g/mL.
  5. 5. The method for preparing the MoS 2 -based antifriction and wear-resistant composite metal coating material, which is characterized in that in the step A3, the mass concentration of the ammonium heptamolybdate in deionized water is 0.016-0.025g/mL, the mass-volume ratio between the ammonium heptamolybdate and nitric acid is 1-1.33g/mL, the heat treatment temperature is 180-200 ℃, and the heat treatment time is 18-24h.
  6. 6. The preparation method of the friction-reducing wear-resistant composite metal coating material based on MoS 2 is characterized in that in the step A4, the mass concentration of the MoO 3 nano material in deionized water is 2-2.5mg/mL, the addition mass of sodium dodecyl benzene sulfonate is 5-10% of the mass of the MoO 3 nano material, the mass concentration of potassium persulfate in a potassium persulfate aqueous solution is 6-14mg/mL, and the addition mass of the potassium persulfate is 28-30% of the mass of an intermediate 2.
  7. 7. The preparation method of the friction-reducing wear-resistant composite metal coating material based on MoS 2 , which is characterized in that in the step A4, the preparation method of the intermediate 2 reaction solution specifically comprises the steps of placing the intermediate 2 in a flask, adding 1M hydrochloric acid aqueous solution and absolute ethyl alcohol, uniformly stirring, and then performing ultrasonic treatment to obtain the intermediate 2 reaction solution, wherein the mass volume ratio of the intermediate 2 to the 1M hydrochloric acid aqueous solution in the intermediate 2 reaction solution is 0.01-0.025g/mL, and the mass volume ratio of the intermediate 2 to the absolute ethyl alcohol in the intermediate 2 reaction solution is 0.1-0.25g/mL.
  8. 8. The method for preparing the friction-reducing wear-resistant composite metal coating material based on MoS 2 , which is characterized in that in the step A5, the mass ratio of MoO 3 /polymer composite material to metal salt is 3.3-5:1, the mass concentration of the metal salt in the metal salt aqueous solution is 4-6mg/mL, the metal salt comprises at least one of copper nitrate, copper sulfate, zinc nitrate and cobalt nitrate, the stirring speed of the complexing reaction is 500-700rpm, and the reaction time of the complexing reaction is 3-5h.
  9. 9. The preparation method of the friction-reducing wear-resistant composite metal coating material based on MoS 2 , which is disclosed in claim 8, is characterized in that in step A6, the mass ratio of the metal complex MoO 3 /polymer composite material to thiourea is 1:1.2-1.5, the reaction temperature of the vulcanization reaction is 300-330 ℃, the heating rate of the vulcanization reaction is 8-10 ℃ per minute, and the reaction time of the vulcanization reaction is 2-3h.
  10. 10. A friction-reducing wear-resistant composite metal coating material based on MoS 2 , which is characterized by being prepared by the preparation method according to any one of claims 1-9.

Description

MoS 2 -based antifriction and wear-resistant composite metal coating material and preparation method thereof Technical Field The invention belongs to the technical field of metal coating, and particularly relates to an antifriction and wear-resistant composite metal coating material based on MoS 2 and a preparation method thereof. Background In the fields of industrial manufacturing, aerospace, rail transit, energy equipment and the like, frictional wear of mechanical parts is a core problem that leads to equipment failure, shortened life and increased energy consumption. About 70% of component failures in mechanical systems result from surface wear, and 30% of the energy consumption is used to overcome frictional resistance. Particularly under the working conditions of heavy load, high speed, high temperature or severe media (such as humid and corrosive environments), the traditional metal base materials (such as steel, aluminum alloy, titanium alloy and the like) have low surface hardness and high friction coefficient (generally between 0.3 and 0.8), are easy to generate adhesive wear, abrasive particle wear or fatigue wear, and severely restrict the reliability and service life of equipment. Therefore, developing a surface modification technology with low friction coefficient, high wear resistance and strong matrix binding force becomes a key direction for solving the industrial friction and wear problems. The metal coating is used as one of core technologies for surface modification, and the surface performance of the material can be effectively improved by constructing a functional protective layer on the surface of the substrate. The traditional antifriction and wear-resistant metal coating mainly depends on a single metal (such as Cr, ni and W) or alloy (such as Ni-P, co-W, fe-Cr-B) system, and although the abrasion risk of abrasive particles can be reduced by improving the surface hardness, the traditional antifriction and wear-resistant metal coating has the defects of higher friction coefficient, poor high-temperature stability, weak environmental adaptability (such as microcrack corrosion of a hard chromium coating in a humid environment) and the like. For example, in the field of aeroengine bearings, the friction coefficient of a traditional Ni-based alloy coating can rise to more than 0.4 under the working condition of more than 350 ℃, the abrasion rate is improved by 3-5 times compared with that of the traditional Ni-based alloy coating at room temperature, long-term service requirements are difficult to meet, in a wind power equipment gearbox, the Fe-Cr-B coating on the surface of a steel substrate has higher hardness, but the coating is easily peeled off due to interface corrosion in an outdoor humid environment, the average replacement period is only 1-2 years, and the maintenance cost is high. Molybdenum disulfide (MoS 2) is used as a typical lamellar Transition Metal Sulfide (TMDs), and has excellent antifriction characteristics, namely extremely low interlayer shearing force, low friction coefficient of 0.02-0.05 in a dry environment and excellent chemical stability due to a unique hexagonal lamellar structure (atoms in layers are bonded through strong covalent bonds and are connected through weak van der waals force), so that the molybdenum disulfide is an ideal antifriction functional component. In the early 50 s of the last century, moS 2 was used in solid lubricants (e.g., grease additives, dry film lubricants), but the pure MoS 2 coating has two major core short plates, namely, weak bonding force with the metal substrate, easy peeling under load, strong environmental sensitivity, and in air with humidity >50%, moS 2 easily reacts with water molecules to generate MoO 3 (a brittle oxide), resulting in a sudden rise of friction coefficient to over 0.3, and a sharp drop of wear resistance. In the existing MoS 2 -based composite coating research, the reported metal matrix mainly comprises Ni, co, cr, al and an alloy thereof, and the preparation method comprises electroplating, chemical plating, thermal spraying (such as plasma spraying and supersonic flame spraying), physical vapor deposition (PVD (such as magnetron sputtering and arc ion plating), chemical Vapor Deposition (CVD) and the like. For example, the Ni-P-MoS 2 composite coating prepared by adopting the chemical plating method can reduce the friction coefficient to 0.15-0.2 by dispersing MoS 2 particles in the Ni-P coating, and the friction coefficient is reduced by 30-40% compared with that of a pure Ni-P coating, but the method has the problems of uneven MoS 2 dispersion, limited coating thickness and the like, and is difficult to meet the requirement of heavy-duty parts on thick coatings. In addition, the existing composite coating has the common problem of insufficient antifriction and abrasion resistance, namely when the addition amount of MoS 2 is too high, the friction coefficient can be obviously reduced, but the hardne