CN117403302B - High-strength high-toughness steel for bearings and preparation method thereof - Google Patents

High-strength high-toughness steel for bearings and preparation method thereof Download PDF

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CN117403302B
CN117403302B CN202311730050.0A CN202311730050A CN117403302B CN 117403302 B CN117403302 B CN 117403302B CN 202311730050 A CN202311730050 A CN 202311730050A CN 117403302 B CN117403302 B CN 117403302B
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molybdenum disulfide
treatment
steel
ultrasonic
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CN117403302A (en
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华晨轶
华志伟
钱若蓉
周一纯
钱若菁
过君
黄超
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Baolu Seiko Technology Wuxi Co ltd
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    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/40Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for rings; for bearing races
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21HMAKING PARTICULAR METAL OBJECTS BY ROLLING, e.g. SCREWS, WHEELS, RINGS, BARRELS, BALLS
    • B21H1/00Making articles shaped as bodies of revolution
    • B21H1/06Making articles shaped as bodies of revolution rings of restricted axial length
    • B21H1/12Making articles shaped as bodies of revolution rings of restricted axial length rings for ball or roller bearings
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21JFORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
    • B21J5/00Methods for forging, hammering, or pressing; Special equipment or accessories therefor
    • B21J5/002Hybrid process, e.g. forging following casting
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B1/00Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/06Surface hardening
    • C21D1/09Surface hardening by direct application of electrical or wave energy; by particle radiation
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D15/00Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00Electroplating: Baths therefor
    • C25D3/02Electroplating: Baths therefor from solutions
    • C25D3/56Electroplating: Baths therefor from solutions of alloys
    • C25D3/562Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of iron or nickel or cobalt

Abstract

The invention relates to the technical field of steel materials, in particular to a high-strength high-toughness bearing steel and a preparation method thereof, wherein the steel materials are sequentially subjected to primary homogenization treatment, upsetting, secondary homogenization treatment, pore-forming and ring rolling, machined into a blank, then subjected to laser fusion treatment, and treated by stearic acid to obtain a superhydrophobic surface, wherein a nickel-cobalt-nano tungsten carbide layer and a nickel-cobalt-modified molybdenum disulfide coating are sequentially formed on the surface of the steel by using a betaine hydrochloride-ethylene glycol eutectic ionic liquid as a solvent and an ultrasonic auxiliary plating process, so that gradient hardness is built and the wear resistance and corrosion resistance of the steel are greatly improved; firstly, stripping by liquid ultrasonic to obtain molybdenum disulfide nanosheets, then, carrying out microwave treatment, in-situ growing titanium dioxide on the molybdenum disulfide nanosheets, in-situ growing cobalt cerium organic bimetallic frameworks taking 2, 5-furandicarboxylic acid as an organic ligand on composite nano molybdenum disulfide, and providing a nano container for corrosion inhibitor 1-aminobenzotriazole.

Description

High-strength high-toughness steel for bearings and preparation method thereof
Technical Field
The invention relates to the technical field of steel materials, in particular to steel for a high-strength high-toughness bearing and a preparation method thereof.
Background
The bearing is an important component part of mechanical equipment parts, and has the main functions of supporting the mechanical rotating body and reducing the friction coefficient in the movement process of the mechanical rotating body. With the rapid development of fields such as automobiles, machine manufacturing and the like, the design stress and the light weight requirements of various bearings are continuously increased, and the high-strength high-toughness bearing has a huge application prospect.
The existing market multi-purpose steel materials are used for preparing various bearings, so that the performance of the bearings is determined by the performance of the steel materials, and the precision, performance and reliability of the bearings have decisive effects on the precision, performance and reliability of mechanical equipment. Meanwhile, before the bearing steel is put into use, plating treatment is usually carried out for enhancing the corrosion resistance and wear resistance of the bearing, but when the plating treatment is carried out, the problems of poor bonding force between a plating layer and a steel material, low yield and the like are easy to occur.
Disclosure of Invention
The invention aims to provide high-strength high-toughness steel for bearings and a preparation method thereof, so as to solve the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme:
the preparation method of the steel for the high-strength high-toughness bearing comprises the following steps:
s1: taking steel materials as raw materials, carrying out primary homogenization treatment, upsetting and drawing, secondary homogenization treatment, pore-forming, ring grinding, machining and forming, laser melting treatment and oil cooling;
s2: sequentially carrying out sanding, polishing, water washing, alkali washing, ultrasonic cleaning, acid washing and water washing on the fused steel material in the step S1 to obtain a pretreated substrate, and drying for later use;
s3: preparing a preplating solution containing nano tungsten carbide, putting the pretreated base material into the preplating solution, and carrying out ultrasonic auxiliary preplating treatment to obtain the preplating base material;
s4: preparing a composite plating solution containing modified nano molybdenum disulfide, and placing a pre-plated substrate into the composite plating solution for ultrasonic auxiliary plating treatment to obtain a substrate;
s5: and (3) immersing the base material in an ethanol solution of stearic acid, and drying to obtain the steel for the high-strength high-toughness bearing.
Further, the working conditions of the primary homogenization treatment are as follows: heating from 25 ℃ to 450 ℃ at a speed of 5 ℃/min, and preserving heat for 10-12h; the working conditions of upsetting and pulling are as follows: the upsetting and pulling are performed by two piers and one pier, and the pier pulling ratio is 1.8; the working conditions of the secondary homogenization treatment are as follows: heating from 25 ℃ to 450 ℃ at a speed of 5 ℃/min, and preserving heat for 5-6h; the working conditions of the grinding ring are as follows: rolling with a ring rolling machine, wherein the radial feeding speed of the ring rolling is 0.7mm/s, and preheating to 355 ℃ before ring rolling.
Further, the working conditions of the laser fusing treatment are as follows: under the argon environment, the diameter of a laser spot is 2mm, the laser power is 1.4kW, and the scanning speed is 5-7mm/s.
Further, the composition of the preplating solution is as follows: the method is characterized in that betaine hydrochloride-glycol ionic liquid is used as a solvent, and 72g/L of nickel chloride, 13g/L of nickel sulfamate, 45g/L of cobalt chloride and 5g/L of nano tungsten carbide are used.
Further, the working conditions of the ultrasonic-assisted pre-plating treatment are as follows: the preplating time is 1h, the preplating temperature is 65-70 ℃, and the ultrasonic power is 300W.
Further, the composition of the composite plating solution is as follows: the method is characterized in that betaine hydrochloride-glycol ionic liquid is used as a solvent, and 72g/L of nickel chloride, 13g/L of nickel sulfamate, 45g/L of cobalt chloride and 13g/L of modified nano molybdenum disulfide are used.
Further, the working conditions of the ultrasonic-assisted plating treatment are as follows: the plating time is 2h, the temperature is 65-70 ℃, and the ultrasonic power is 320W.
Further, the betaine hydrochloride-glycol ionic liquid is prepared from betaine hydrochloride and glycol according to the molar weight of 1:6, configuring.
Further, the preparation of the modified nano molybdenum disulfide comprises the following steps:
1) Dispersing molybdenum disulfide in deionized water by ultrasonic, adding N-methylpyrrolidone, performing ultrasonic treatment by an ultrasonic cell disruption instrument, centrifuging at 60% amplitude for 50-60min at 5000r/min for 1-2h, collecting precipitate by using an N-methylpyrrolidone solution, continuing ultrasonic treatment at 60% amplitude for 5h, and drying to obtain molybdenum disulfide nanosheets;
2) Adding a mixed solution of molybdenum disulfide nanosheets, isopropanol and tetrabutyl titanate into a nitric acid aqueous solution under the ice water bath condition, heating to 70-80 ℃, preserving heat for 3-4h, carrying out microwave for 10-15min at 80-100W, and drying to obtain composite nano molybdenum disulfide;
3) Mixing the composite nano molybdenum disulfide, polyvinylpyrrolidone, cerium nitrate, cobalt nitrate, N-dimethylacetamide, ethanol and deionized water, stirring for 12-14h, adding the mixed solution of 2, 5-furandicarboxylic acid, N-dimethylacetamide, ethanol and deionized water, carrying out ultrasonic treatment for 10-15min, preserving heat at 90-95 ℃ for 44-48h, and drying to obtain an intermediate preparation; dispersing the intermediate preparation in an acetone solution containing 1-aminobenzotriazole, transferring to a vacuum environment, reducing the air pressure to 0.08-0.09MPa, standing for 20-30min, taking out, centrifuging, continuously dispersing in the acetone solution of 1-aminobenzotriazole, repeating the operation for 3-5 times, and drying to obtain the modified nano molybdenum disulfide.
Further, the working conditions of the dipping treatment are as follows: the composition of the stearic acid ethanol solution is as follows: ethanol is used as a solvent, wherein the content of stearic acid is 0.1-0.2mol/L; the soaking time is 30-50min.
The invention has the beneficial effects that:
the invention provides a high-strength high-toughness bearing steel and a preparation method thereof.
The method selects steel materials as raw materials for the bearing, sequentially carries out primary homogenization treatment, upsetting and pulling, secondary homogenization treatment, pore forming and ring grinding, and is mechanically processed into a blank body, and the homogenization treatment is carried out before and after upsetting and pulling, so that the homogenization temperature of the two times is consistent by controlling the technological parameters, the time is kept to be half, the size and the number of steel precipitated phases are reduced, and the corrosion performance of the steel precipitated phases is improved; aiming at the problems of uneven distribution of a surface hardening layer and the like of the steel material treated by the traditional strengthening process, the invention improves the uniformity of the phase change hardening layer on the steel surface by controlling the power and scanning speed of laser, and achieves the purposes of high hardness of the hardening layer and easy realization of automation;
in order to improve the wear resistance and corrosion resistance of the steel, a gradient hardness layer is constructed on the surface of the fused steel through plating treatment twice; in order to solve the problems that a metal coating is easy to generate hydrogen embrittlement, a metal anode is easy to passivate, plating waste liquid is difficult to treat and the like in the existing aqueous solution plating process, the invention selects the betaine hydrochloride-ethylene glycol eutectic ionic liquid which has the advantages of good chemical heat stability, wide electrochemical window, low vapor pressure, good conductivity and low cost and low toxicity as a solvent.
In the prior art, molybdenum disulfide is generally directly used as a coating raw material, but the problems of poor process, low molybdenum disulfide content, no effect, excessive lubricating phase easy falling off, easy oxidation in the high-temperature preparation process and the like exist; according to the invention, firstly, the molybdenum disulfide nanosheets are obtained by liquid ultrasonic stripping, and then titanium dioxide is grown on the molybdenum disulfide nanosheets in situ by microwave treatment, so that the self-lubricating composite nano molybdenum disulfide with compact structure, uniform thickness, easy operation and high repetition rate and with a core-shell structure is obtained, and the high-temperature lubrication resistance of steel is improved; cobalt-cerium organic bimetallic frameworks taking 2, 5-furandicarboxylic acid as an organic ligand grow on the composite nano molybdenum disulfide in situ, a nano container is provided for a corrosion inhibitor 1-aminobenzotriazole, wherein cerium ions and the 1-aminobenzotriazole cooperate to play a role in corrosion inhibition, and the composite nano molybdenum disulfide is introduced into the composite plating solution, so that the wear resistance and corrosion resistance of a plating layer are effectively improved; and then, carrying out hydrophobic treatment on the steel surface by using stearic acid, combining two plating treatments, and endowing the steel material with a super-hydrophobic surface to improve the self-cleaning property of the steel material surface, wherein the introduction of the composite nano molybdenum disulfide in the plating layer can effectively enhance the binding force of the stearic acid and the steel material surface.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely in connection with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be noted that, if directional indications such as up, down, left, right, front, and rear are involved in the embodiment of the present invention, the directional indication is merely used to explain a relative positional relationship between a specific posture such as each component, a movement condition, and the like, and if the specific posture is changed, the directional indication is changed accordingly. In addition, the technical solutions of the embodiments may be combined with each other, but it is necessary to base that the technical solutions can be realized by those skilled in the art, and when the technical solutions are contradictory or cannot be realized, the combination of the technical solutions should be considered to be absent and not within the scope of protection claimed in the present invention.
The following description of the embodiments of the present invention will be presented in further detail with reference to the examples, which should be understood as being merely illustrative of the present invention and not limiting.
Example 1: the preparation method of the steel for the high-strength high-toughness bearing comprises the following steps:
s1: taking steel materials as raw materials, carrying out primary homogenization treatment, upsetting and drawing, secondary homogenization treatment, pore-forming, ring grinding, machining and forming, laser melting treatment and oil cooling;
the working conditions of the primary homogenization treatment are as follows: heating from 25 ℃ to 450 ℃ at a speed of 5 ℃/min, and preserving heat for 10 hours; the working conditions of upsetting and pulling are as follows: the upsetting and pulling are performed by two piers and one pier, and the pier pulling ratio is 1.8; the working conditions of the secondary homogenization treatment are as follows: heating from 25 ℃ to 450 ℃ at a speed of 5 ℃/min, and preserving heat for 5 hours; the working conditions of the grinding ring are as follows: rolling by a ring rolling machine, wherein the radial feeding speed of the ring rolling is 0.7mm/s, and the ring rolling is preheated to 355 ℃;
the working conditions of the laser fusing treatment are as follows: under the argon environment, the diameter of a laser spot is 2mm, the laser power is 1.4kW, and the scanning speed is 5mm/s;
s2: sequentially carrying out sanding, polishing, water washing, alkali washing, ultrasonic cleaning, acid washing and water washing on the fused steel material in the step S1 to obtain a pretreated substrate, and drying for later use;
s3: preparing a preplating solution containing nano tungsten carbide, putting the pretreated base material into the preplating solution, and carrying out ultrasonic auxiliary preplating treatment to obtain the preplating base material;
the composition of the preplating solution is as follows: taking betaine hydrochloride-glycol ionic liquid as a solvent, and 72g/L nickel chloride, 13g/L nickel sulfamate, 45g/L cobalt chloride and 5g/L nano tungsten carbide;
the betaine hydrochloride-glycol ionic liquid is prepared from betaine hydrochloride and glycol according to the molar weight of 1:6, configuring;
the working conditions of the ultrasonic auxiliary pre-plating treatment are as follows: the preplating time is 1h, the preplating temperature is 70 ℃, and the current density is 10mA/cm 2 The ultrasonic power is 300W;
s4: preparing a composite plating solution containing modified nano molybdenum disulfide, and placing a pre-plated substrate into the composite plating solution for ultrasonic auxiliary plating treatment to obtain a substrate;
the composition of the composite plating solution is as follows: taking betaine hydrochloride-glycol ionic liquid as a solvent, and 72g/L nickel chloride, 13g/L nickel sulfamate, 45g/L cobalt chloride and 13g/L modified nano molybdenum disulfide;
the working conditions of the ultrasonic auxiliary plating treatment are as follows: the plating time is 2h, the temperature is 65 ℃, and the current density is 12mA/cm 2 The ultrasonic power is 320W;
the preparation method of the modified nano molybdenum disulfide comprises the following steps:
1) Dispersing 0.8g of molybdenum disulfide in 40mL of deionized water by ultrasonic, adding 0.24g of N-methylpyrrolidone, carrying out ultrasonic treatment by an ultrasonic cell disruption instrument, carrying out ultrasonic treatment for 50min at 60% of amplitude, centrifuging at 5000r/min for 1h, collecting precipitate by using 0mL of 6g/L of N-methylpyrrolidone solution, continuing ultrasonic treatment for 5h at 60% of amplitude, and drying to obtain molybdenum disulfide nanosheets;
2) Adding a mixed solution of 0.1g of molybdenum disulfide nanosheets, 20mL of isopropanol and 80mL of tetrabutyl titanate into 500mL of 0.2% nitric acid aqueous solution under the ice water bath condition, heating to 70 ℃, preserving heat for 4 hours, carrying out 80W microwave for 15 minutes, and drying to obtain composite nano molybdenum disulfide;
3) Mixing 240mg of composite nano molybdenum disulfide, 165mg of polyvinylpyrrolidone, 0.8mmol of cerium nitrate, 0.2mmol of cobalt nitrate, 9mLN, N-dimethylacetamide, 9mL of ethanol and 9mL of deionized water, stirring for 12h, adding a mixed solution of 1mmol of 2, 5-furandicarboxylic acid, 9mLN, N-dimethylacetamide, 9mL of ethanol and 9mL of deionized water, carrying out ultrasonic treatment for 10min, preserving heat at 90 ℃ for 48h, and drying to obtain an intermediate preparation; dispersing 100mg of intermediate preparation in 250mL of acetone solution containing 500mg of 1-aminobenzotriazole, transferring to a vacuum environment, reducing the air pressure to 0.08MPa, standing for 20min, taking out, centrifuging, continuously dispersing into 250mL of acetone solution containing 500mg of 1-aminobenzotriazole, repeating the operation for 3 times, and drying to obtain modified nano molybdenum disulfide;
s5: soaking the base material in ethanol solution of stearic acid, and drying to obtain high-strength high-toughness bearing steel; the working conditions of the dipping treatment are as follows: the composition of the stearic acid ethanol solution is as follows: ethanol is taken as a solvent, wherein the content of stearic acid is 0.1mol/L; the soaking time was 50min.
Example 2: the preparation method of the steel for the high-strength high-toughness bearing comprises the following steps:
s1: taking steel materials as raw materials, carrying out primary homogenization treatment, upsetting and drawing, secondary homogenization treatment, pore-forming, ring grinding, machining and forming, laser melting treatment and oil cooling;
the working conditions of the primary homogenization treatment are as follows: heating from 25 ℃ to 450 ℃ at a speed of 5 ℃/min, and preserving heat for 11h; the working conditions of upsetting and pulling are as follows: the upsetting and pulling are performed by two piers and one pier, and the pier pulling ratio is 1.8; the working conditions of the secondary homogenization treatment are as follows: heating from 25 ℃ to 450 ℃ at a speed of 5 ℃/min, and preserving heat for 5.5 hours; the working conditions of the grinding ring are as follows: rolling by a ring rolling machine, wherein the radial feeding speed of the ring rolling is 0.7mm/s, and the ring rolling is preheated to 355 ℃;
the working conditions of the laser fusing treatment are as follows: under the argon environment, the diameter of a laser spot is 2mm, the laser power is 1.4kW, and the scanning speed is 6mm/s;
s2: sequentially carrying out sanding, polishing, water washing, alkali washing, ultrasonic cleaning, acid washing and water washing on the fused steel material in the step S1 to obtain a pretreated substrate, and drying for later use;
s3: preparing a preplating solution containing nano tungsten carbide, putting the pretreated base material into the preplating solution, and carrying out ultrasonic auxiliary preplating treatment to obtain the preplating base material;
the composition of the preplating solution is as follows: taking betaine hydrochloride-glycol ionic liquid as a solvent, and 72g/L nickel chloride, 13g/L nickel sulfamate, 45g/L cobalt chloride and 5g/L nano tungsten carbide;
the betaine hydrochloride-glycol ionic liquid is prepared from betaine hydrochloride and glycol according to the molar weight of 1:6, configuring;
the working conditions of the ultrasonic auxiliary pre-plating treatment are as follows: the preplating time is 1h, the preplating temperature is 68 ℃, and the current density is 10mA/cm 2 The ultrasonic power is 300W;
s4: preparing a composite plating solution containing modified nano molybdenum disulfide, and placing a pre-plated substrate into the composite plating solution for ultrasonic auxiliary plating treatment to obtain a substrate;
the composition of the composite plating solution is as follows: taking betaine hydrochloride-glycol ionic liquid as a solvent, and 72g/L nickel chloride, 13g/L nickel sulfamate, 45g/L cobalt chloride and 13g/L modified nano molybdenum disulfide;
the working conditions of the ultrasonic auxiliary plating treatment are as follows: the plating time is 2h, the temperature is 68 ℃, and the current density is 12mA/cm 2 The ultrasonic power is 320W;
the preparation method of the modified nano molybdenum disulfide comprises the following steps:
1) Dispersing 0.8g of molybdenum disulfide in 40mL of deionized water by ultrasonic, adding 0.24g of N-methylpyrrolidone, carrying out ultrasonic treatment by an ultrasonic cell disruption instrument, carrying out ultrasonic treatment at the amplitude of 60% for 55min, centrifuging at the speed of 5000r/min for 1.5h, collecting precipitate by using 0mL of 6g/L of N-methylpyrrolidone solution, continuing ultrasonic treatment at the amplitude of 60% for 5h, and drying to obtain molybdenum disulfide nanosheets;
2) Adding a mixed solution of 0.1g of molybdenum disulfide nanosheets, 20mL of isopropanol and 80mL of tetrabutyl titanate into 500mL of 0.2% nitric acid aqueous solution under the ice water bath condition, heating to 78 ℃, preserving heat for 3.5h, carrying out microwave for 12min at 90W, and drying to obtain composite nano molybdenum disulfide;
3) Mixing 240mg of composite nano molybdenum disulfide, 165mg of polyvinylpyrrolidone, 0.8mmol of cerium nitrate, 0.2mmol of cobalt nitrate, 9mLN, N-dimethylacetamide, 9mL of ethanol and 9mL of deionized water, stirring for 13h, adding a mixed solution of 1mmol of 2, 5-furandicarboxylic acid, 9mLN, N-dimethylacetamide, 9mL of ethanol and 9mL of deionized water, carrying out ultrasonic treatment for 13min, preserving heat at 92 ℃ for 46h, and drying to obtain an intermediate preparation; dispersing 100mg of intermediate preparation in 250mL of acetone solution containing 500mg of 1-aminobenzotriazole, transferring to a vacuum environment, reducing the air pressure to 0.08MPa, standing for 25min, taking out, centrifuging, continuously dispersing into 250mL of acetone solution containing 500mg of 1-aminobenzotriazole, repeating the operation for 4 times, and drying to obtain modified nano molybdenum disulfide;
s5: soaking the base material in ethanol solution of stearic acid, and drying to obtain high-strength high-toughness bearing steel; the working conditions of the dipping treatment are as follows: the composition of the stearic acid ethanol solution is as follows: ethanol is taken as a solvent, wherein the content of stearic acid is 0.15mol/L; the soaking time was 40min.
Example 3: the preparation method of the steel for the high-strength high-toughness bearing comprises the following steps:
s1: taking steel materials as raw materials, carrying out primary homogenization treatment, upsetting and drawing, secondary homogenization treatment, pore-forming, ring grinding, machining and forming, laser melting treatment and oil cooling;
the working conditions of the primary homogenization treatment are as follows: heating from 25 ℃ to 450 ℃ at a speed of 5 ℃/min, and preserving heat for 12 hours; the working conditions of upsetting and pulling are as follows: the upsetting and pulling are performed by two piers and one pier, and the pier pulling ratio is 1.8; the working conditions of the secondary homogenization treatment are as follows: heating from 25 ℃ to 450 ℃ at a speed of 5 ℃/min, and preserving heat for 6 hours; the working conditions of the grinding ring are as follows: rolling by a ring rolling machine, wherein the radial feeding speed of the ring rolling is 0.7mm/s, and the ring rolling is preheated to 355 ℃;
the working conditions of the laser fusing treatment are as follows: under the argon environment, the diameter of a laser spot is 2mm, the laser power is 1.4kW, and the scanning speed is 7mm/s;
s2: sequentially carrying out sanding, polishing, water washing, alkali washing, ultrasonic cleaning, acid washing and water washing on the fused steel material in the step S1 to obtain a pretreated substrate, and drying for later use;
s3: preparing a preplating solution containing nano tungsten carbide; placing the pretreated substrate into a preplating solution, and carrying out ultrasonic auxiliary preplating treatment to obtain a preplating substrate;
the composition of the preplating solution is as follows: taking betaine hydrochloride-glycol ionic liquid as a solvent, and 72g/L nickel chloride, 13g/L nickel sulfamate, 45g/L cobalt chloride and 5g/L nano tungsten carbide;
the betaine hydrochloride-glycol ionic liquid is prepared from betaine hydrochloride and glycol according to the molar weight of 1:6, configuring;
the working conditions of the ultrasonic auxiliary pre-plating treatment are as follows: the preplating time is 1h, the preplating temperature is 70 ℃, and the current density is 10mA/cm 2 The ultrasonic power is 300W;
s4: preparing a composite plating solution containing modified nano molybdenum disulfide, and placing a pre-plated substrate into the composite plating solution for ultrasonic auxiliary plating treatment to obtain a substrate;
the composition of the composite plating solution is as follows: taking betaine hydrochloride-glycol ionic liquid as a solvent, and 72g/L nickel chloride, 13g/L nickel sulfamate, 45g/L cobalt chloride and 13g/L modified nano molybdenum disulfide;
the working conditions of the ultrasonic auxiliary plating treatment are as follows: the plating time is 2h, the temperature is 70 ℃, and the current density is 12mA/cm 2 The ultrasonic power is 320W;
the preparation method of the modified nano molybdenum disulfide comprises the following steps:
1) Dispersing 0.8g of molybdenum disulfide in 40mL of deionized water by ultrasonic, adding 0.24g of N-methylpyrrolidone, carrying out ultrasonic treatment by an ultrasonic cell disruption instrument, carrying out ultrasonic treatment at 60% amplitude for 60min, centrifuging at 5000r/min for 2h, collecting precipitate by using 0mL of 6g/L of N-methylpyrrolidone solution, continuing ultrasonic treatment at 60% amplitude for 5h, and drying to obtain molybdenum disulfide nanosheets;
2) Adding a mixed solution of 0.1g of molybdenum disulfide nanosheets, 20mL of isopropanol and 80mL of tetrabutyl titanate into 500mL of 0.2% nitric acid aqueous solution under the ice water bath condition, heating to 80 ℃, preserving heat for 3h, carrying out 100W microwave for 10min, and drying to obtain composite nano molybdenum disulfide;
3) Mixing 240mg of composite nano molybdenum disulfide, 165mg of polyvinylpyrrolidone, 0.8mmol of cerium nitrate, 0.2mmol of cobalt nitrate, 9mLN, N-dimethylacetamide, 9mL of ethanol and 9mL of deionized water, stirring for 14h, adding a mixed solution of 1mmol of 2, 5-furandicarboxylic acid, 9mLN, N-dimethylacetamide, 9mL of ethanol and 9mL of deionized water, carrying out ultrasonic treatment for 15min, preserving heat at 95 ℃ for 44h, and drying to obtain an intermediate preparation; dispersing 100mg of intermediate preparation in 250mL of acetone solution containing 500mg of 1-aminobenzotriazole, transferring to a vacuum environment, reducing the air pressure to 0.09MPa, standing for 30min, taking out, centrifuging, continuously dispersing into 250mL of acetone solution containing 500mg of 1-aminobenzotriazole, repeating the operation for 5 times, and drying to obtain modified nano molybdenum disulfide;
s5: soaking the base material in ethanol solution of stearic acid, and drying to obtain high-strength high-toughness bearing steel; the working conditions of the dipping treatment are as follows: the composition of the stearic acid ethanol solution is as follows: ethanol is taken as a solvent, wherein the content of stearic acid is 0.2mol/L; the soaking time was 30min.
Comparative example 1: with example 3 as a control group, no laser fusing treatment was performed and the other steps were normal.
Comparative example 2: with example 3 as a control group, no pre-plating treatment was performed, and the other steps were normal.
Comparative example 3: with example 3 as a control group, the modified molybdenum disulfide was replaced with molybdenum disulfide nanosheets, and the other procedures were normal.
In the examples and comparative examples, the thickness of the pretreated substrate was 8mm, the thickness of the preplating layer was 80 μm, the thickness of the composite plating layer was 100 μm, and the thickness of the stearic acid treatment layer was 10nm.
The sources of the raw materials are as follows:
the steel material is 42CrMo steel, and comprises the following chemical components in percentage by mass: 0.4% of carbon, 0.3% of silicon, 0.6% of manganese, 1.2% of chromium, 0.27% of molybdenum and the balance of iron; nickel sulfamate N102822, nickel chloride N112126, cobalt chloride C116457, betaine hydrochloride B113358, ethylene glycol E103319, molybdenum disulfide M104968, N-methylpyrrolidone M119668, tetrabutyl titanate T104104, polyvinylpyrrolidone P110611, cerium nitrate C431279, cobalt nitrate C112729, N-dimethylacetamide D108096, 2, 5-furandicarboxylic acid F119129, 1-aminobenzotriazole A151238, nano tungsten carbide T431585, stearic acid S108289: ala Ding Shiji; nitric acid, isopropanol, ethanol, analytically pure: national drug group reagent.
Performance test:
hardness: the test is carried out by using a Vickers microhardness tester, the load is 2N, and the loading time is 10s; abrasion resistance: testing by using a vertical universal friction and wear testing machine, namely testing the grinding material GCr15 with the load of 15N, the rotating speed of a rotating disc of 100r/min and the wear time of 40min by using an electronic balance to measure the mass (the precision is 0.1 mg) of the sample before and after the sample is worn, firstly keeping the temperature of the sample at 400 ℃ for 2 hours, and then cooling to 25 ℃ for testing; hydrophobicity: characterizing a water contact angle, and testing with 2 mu L deionized water drops; salt spray resistance: referring to GB/T1771-2007, the operating temperature is 37 ℃, the concentration of sodium chloride is 60g/L, and the pH is 6.9; the results obtained are shown in Table 1 below;
TABLE 1
Example 1 Example 2 Example 3 Comparative example 1 Comparative example 2 Comparative example 3
Hardness (HV) 817 818 821 641 683 730
Wearing capacity (mg) 0.24 0.24 0.23 0.25 0.58 0.92
Water contact angle (°) 157 158 159 156 155 148
Salt spray resistance (2400 h) Rust-free Rust-free Rust-free / / /
The invention provides a high-strength high-toughness bearing steel and a preparation method thereof, wherein a steel material is subjected to fusion treatment by laser, then the fused steel is subjected to plating treatment by a preplating solution containing nano tungsten carbide and a composite plating solution containing modified nano molybdenum disulfide in sequence, gradient hardness is built on the surface of the steel, the wear resistance and corrosion resistance of the steel material are greatly improved, and then the steel material is subjected to treatment by stearic acid, so that the high-strength high-toughness bearing steel with a hydrophobic surface is obtained, and the performance is not tested in table 1.
Comparing example 3 with comparative example 1, it is known that the steel is selected as the raw material for the bearing, and the invention aims at the problems of uneven distribution of the surface hardening layer and the like of the steel treated by the traditional fusing process, and improves the uniformity of the phase change hardening layer on the surface of the steel material by controlling the power and the scanning speed of laser, thereby achieving the purposes of high hardness of the hardening layer and easy realization of automation;
comparing example 3 with comparative example 2, it is known that in order to improve the wear resistance of steel, the invention introduces a nickel-cobalt-molybdenum disulfide coating on the surface of steel by utilizing an ultrasonic auxiliary plating process, and in order to improve the binding force between the wear-resistant coating of the nickel-cobalt-molybdenum disulfide coating and the surface of steel, a nickel-cobalt-nano tungsten carbide layer is pre-plated on the surface of fused steel, and meanwhile, the mechanical property of steel is greatly improved.
As can be seen by comparing the example 3 with the comparative example 3, the molybdenum disulfide is generally directly used as the coating raw material in the prior art, but the problems of insufficient molybdenum disulfide content, no effect, excessive lubricating phase easy falling off, easy oxidative decomposition in the high-temperature preparation process and the like are caused by the poor process; according to the invention, firstly, the molybdenum disulfide nanosheets are obtained by liquid ultrasonic stripping, and then titanium dioxide is grown on the molybdenum disulfide nanosheets in situ by microwave treatment, so that the self-lubricating composite nano molybdenum disulfide with compact structure, uniform thickness, easy operation and high repetition rate and with a core-shell structure is obtained, and the high-temperature lubrication resistance of steel is improved; cobalt-cerium organic bimetallic frameworks taking 2, 5-furandicarboxylic acid as an organic ligand grow on composite nano molybdenum disulfide in situ, a nano container is provided for a corrosion inhibitor 1-aminobenzotriazole, wherein cerium ions and the 1-aminobenzotriazole cooperatively play a role in the corrosion inhibitor, and composite nano molybdenum disulfide is introduced into a composite plating solution, so that the wear resistance and corrosion resistance of a plating layer are effectively improved; and then, carrying out hydrophobic treatment on the steel surface by using stearic acid, combining two plating treatments, and endowing the steel super-hydrophobic surface with the effect of improving the self-cleaning property of the steel surface, wherein the bonding force between the stearic acid and the steel surface can be effectively enhanced by introducing the composite nano molybdenum disulfide into the plating layer.
In conclusion, the high-strength high-toughness bearing steel prepared by the method has good application prospect.
The foregoing description is only exemplary embodiments of the present invention and is not intended to limit the scope of the invention, and all equivalent structural changes made by the present invention or direct/indirect application in other related technical fields are included in the scope of the present invention.

Claims (9)

1. The preparation method of the steel for the high-strength high-toughness bearing is characterized by comprising the following steps of:
s1: taking steel materials as raw materials, carrying out primary homogenization treatment, upsetting and drawing, secondary homogenization treatment, pore-forming, ring grinding, machining and forming, laser melting treatment and oil cooling;
s2: sequentially carrying out sanding, polishing, water washing, alkali washing, ultrasonic cleaning, acid washing and water washing on the fused steel material in the step S1 to obtain a pretreated substrate, and drying for later use;
s3: preparing a preplating solution containing nano tungsten carbide, putting the pretreated base material into the preplating solution, and carrying out ultrasonic auxiliary preplating treatment to obtain the preplating base material;
s4: preparing a composite plating solution containing modified nano molybdenum disulfide, putting a preplating substrate into the composite plating solution, and performing ultrasonic auxiliary plating treatment to obtain the substrate;
s5: soaking the base material in ethanol solution of stearic acid, and drying to obtain high-strength high-toughness bearing steel;
the preparation method of the modified nano molybdenum disulfide comprises the following steps:
1) Dispersing molybdenum disulfide in deionized water by ultrasonic, adding N-methylpyrrolidone, centrifuging at the speed of 50-60min and 5000r/min for 1-2h, collecting precipitate by using an N-methylpyrrolidone solution, continuing ultrasonic treatment for 5h, and drying to obtain molybdenum disulfide nanosheets;
2) Adding a mixed solution of molybdenum disulfide nanosheets, isopropanol and tetrabutyl titanate into a nitric acid aqueous solution under the ice water bath condition, heating to 70-80 ℃, preserving heat for 3-4h, carrying out microwave for 10-15min at 80-100W, and drying to obtain composite nano molybdenum disulfide;
3) Mixing the composite nano molybdenum disulfide, polyvinylpyrrolidone, cerium nitrate, cobalt nitrate, N-dimethylacetamide, ethanol and deionized water, stirring for 12-14h, adding the mixed solution of 2, 5-furandicarboxylic acid, N-dimethylacetamide, ethanol and deionized water, carrying out ultrasonic treatment for 10-15min, preserving heat at 90-95 ℃ for 44-48h, and drying to obtain an intermediate preparation; dispersing the intermediate preparation in an acetone solution containing 1-aminobenzotriazole, transferring to a vacuum environment, reducing the air pressure to 0.08-0.09MPa, standing for 20-30min, taking out, centrifuging, continuously dispersing in the acetone solution of 1-aminobenzotriazole, repeating the operation for 3-5 times, and drying to obtain the modified nano molybdenum disulfide.
2. The method for preparing high-strength high-toughness bearing steel according to claim 1, wherein the working conditions of the primary homogenization treatment are as follows: heating from 25 ℃ to 450 ℃ at a speed of 5 ℃/min, and preserving heat for 10-12h; the working conditions of upsetting and pulling are as follows: the upsetting and pulling are performed by two piers and one pier, and the pier pulling ratio is 1.8; the working conditions of the secondary homogenization treatment are as follows: heating from 25 ℃ to 450 ℃ at a speed of 5 ℃/min, and preserving heat for 5-6h; the working conditions of the grinding ring are as follows: rolling with a ring rolling machine, wherein the radial feeding speed of the ring rolling is 0.7mm/s, and preheating to 355 ℃ before ring rolling.
3. The method for preparing high-strength high-toughness bearing steel according to claim 1, wherein the working conditions of the laser fusing treatment are as follows: under the argon environment, the diameter of a laser spot is 2mm, the laser power is 1.4kW, and the scanning speed is 5-7mm/s.
4. The method for preparing high-strength high-toughness bearing steel according to claim 1, wherein the working conditions of the ultrasonic-assisted pre-plating treatment are as follows: the preplating time is 1h, the preplating temperature is 65-70 ℃, and the ultrasonic power is 300W; the working conditions of the ultrasonic auxiliary plating treatment are as follows: the plating time is 2h, the temperature is 65-70 ℃, and the ultrasonic power is 320W.
5. The method for producing a steel for high-strength and high-toughness bearings according to claim 1, wherein the working conditions of the dipping treatment are: the composition of the stearic acid ethanol solution is as follows: ethanol is used as a solvent, wherein the content of stearic acid is 0.1-0.2mol/L; the soaking time is 30-50min.
6. The method for producing a steel for high-strength and high-toughness bearings according to claim 1, wherein the composition of the pre-plating solution is: the method is characterized in that betaine hydrochloride-glycol ionic liquid is used as a solvent, and 72g/L of nickel chloride, 13g/L of nickel sulfamate, 45g/L of cobalt chloride and 5g/L of nano tungsten carbide are used.
7. The method for preparing high-strength high-toughness bearing steel according to claim 1, wherein the composition of the composite plating solution is as follows: the method is characterized in that betaine hydrochloride-glycol ionic liquid is used as a solvent, and 72g/L of nickel chloride, 13g/L of nickel sulfamate, 45g/L of cobalt chloride and 13g/L of modified nano molybdenum disulfide are used.
8. The method for preparing the high-strength and high-toughness bearing steel according to claim 6 or 7, wherein the betaine hydrochloride-ethylene glycol ionic liquid is betaine hydrochloride and ethylene glycol according to the molar weight of 1:6, configuring.
9. A steel for high strength and high toughness bearings, characterized by being prepared by the preparation method according to any one of claims 1 to 7.
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