CN115652379A - Composite MoS with self-textured hard coating on surface 2 Film, preparation method and application thereof - Google Patents
Composite MoS with self-textured hard coating on surface 2 Film, preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a composite MoS with a self-textured hard coating on the surface 2 A film and a preparation method and application thereof relate to the technical field of surface treatment and frictional wear protection. The method comprises the steps of sequentially carrying out nickel electroplating and chemical nickel plating on the surface of a substrate to form a surface self-texturing nickel-based hard coating on the surface of the substrate; the electroplating solution adopted by the nickel electroplating comprises hard nanoparticles; performing electrophoretic deposition on MoS on the surface of the self-textured nickel-based hard coating 2 Film to obtain the surface self-textured hard coating composite MoS 2 A film. The invention can ensure the integrity of the friction surface while forming the surface microtexture, and greatly improve the coating composite MoS 2 The antifriction and wear-resistant effects of the solid lubricating film; moreover, the nickel-based hard coating prepared by the electroplating and chemical plating methods has good bonding force, good corrosion resistance and strong wear resistance, and is more beneficial to improving the antifriction and wear-resistant effects of the material; in addition, the invention can realize controllable preparation of the surface self-texturing degree.
Description
Technical Field
The invention relates to the technical field of surface treatment and frictional wear protection, in particular to a composite MoS with a self-textured hard coating on the surface 2 A film and a preparation method and application thereof.
Background
The moving system is always accompanied by frictional wear, and according to relevant statistics, about 1/3 of the disposable energy in the world is consumed by friction, and the generated wear also causes about 60% of equipment damage or failure. The lubrication and surface strengthening technology is one of the effective means for reducing friction and wear. Common application cases are as follows: coating compound lubricating oil, coating compound solid lubricating film (typically as coating compound MoS) 2 Solid lubricating film), nitriding/carbon layer composite lubrication, and the like. In the application of the coating composite solid lubricating film, the strength of the binding force between the lubricating phase and the coating surface directly determines the length of the acting time of the solid lubricating film on the coating surface, namely the difference of the lubricating life.
The surface texture technology can effectively improve the surface tribological performance by processing a lattice of pits or micro grooves with a certain size and arrangement on a friction surface by a material reducing manufacturing process such as mechanical external force or laser etching. The non-smooth surface composite MoS obtained by the technology 2 The solid lubricating film can improve MoS 2 The bonding strength with the coating collects and captures abrasive dust particles generated in the friction process, prevents the abrasive dust particles from scraping and damaging the surface of a friction pair in the sliding process, blocks the removal process of a lubricating phase, and realizes the aim of removing the lubricating phaseMoS 2 The slow release of the friction material prolongs the service life of friction, reduces abrasion and prolongs the service time of moving parts. Although the surface texture technology can improve the surface friction performance, the processing of the friction surface is essentially damaged, and microcracks can be generated in the processing process to influence the integrity of the friction surface, so that the coating fails prematurely.
Disclosure of Invention
In view of the above, the present invention aims to provide a composite MoS with a self-textured hard coating on the surface 2 A film and a preparation method and application thereof. The preparation method provided by the invention can ensure the integrity of the friction surface while forming the surface microtexture, and greatly improve the coating composite MoS 2 The antifriction and wear-resistant effects of the solid lubricating film.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a composite MoS with a self-textured hard coating on the surface 2 The preparation method of the film comprises the following steps:
sequentially carrying out nickel electroplating and chemical nickel plating on the surface of a substrate to form a surface self-textured nickel-based hard coating on the surface of the substrate; the electroplating solution adopted by the nickel electroplating comprises hard nanoparticles;
performing electrophoretic deposition on MoS on the surface of the self-textured nickel-based hard coating 2 Film to obtain the surface self-textured hard coating composite MoS 2 A film.
Preferably, the electroplating solution comprises the following components in percentage by weight: 40-50 g/L of nickel chloride, 250-300 g/L of nickel sulfate, 30-40 g/L of boric acid, 1.5-3.5 g/L of hard nanoparticles, 0.3-1 g/L of surfactant and water as solvent; the pH value of the electroplating solution is 4.0-6.0.
Preferably, the hard nanoparticles comprise SiC, si 3 N 4 And ZrO 2 One or more of the above; the particle size of the hard nano-particles is 10-100 nm.
Preferably, the electroplating temperature of the electroplated nickel is 50-60 ℃, the electroplating time is less than 10min, and the current density is 2-8A/dm 2 。
Preferably, the electroless plating solution adopted by the electroless nickel plating comprises the following components in percentage by weight: 30-40 g/L of nickel sulfate, 25-30 g/L of sodium hypophosphite, 30-40 g/L of sodium acetate, 11-13 mL/L of lactic acid, 3-5 mg/L of thiourea and water as a solvent; the pH value of the chemical plating solution is 4.0-6.0.
Preferably, the plating temperature of the chemical nickel plating is 85-90 ℃, and the plating time is below 90 min.
Preferably, the electrophoretic deposition solution used for electrophoretic deposition comprises the following components in percentage by weight: moS 2 1-2 g/L, 0.3-1 g/L of surfactant and water as solvent.
Preferably, the voltage of the electrophoretic deposition is 10-36V, and the deposition time is less than or equal to 5min.
The invention provides the surface self-textured hard coating composite MoS prepared by the preparation method of the technical scheme 2 A film.
The invention also provides the surface self-texturing hard coating composite MoS adopting the technical scheme 2 Use of a film for protection against frictional wear.
The invention provides a composite MoS with a self-textured hard coating on the surface 2 The preparation method of the film comprises the following steps: sequentially carrying out nickel electroplating and chemical nickel plating on the surface of a substrate to form a surface self-textured nickel-based hard coating on the surface of the substrate; the electroplating solution adopted by the nickel electroplating comprises hard nanoparticles; performing electrophoretic deposition MoS on the surface of the self-texturing nickel-based hard coating 2 Film to obtain the composite MoS with the hard coating with self-textured surface 2 A film. According to the invention, the substrate is electroplated by using the electroplating solution containing the hard nanoparticles to manufacture the roughness on the surface of the substrate, and due to the good adaptability of chemical plating, the surface condition of the electroplated layer can be perfectly reproduced to the chemical plating layer, namely, the roughness is reflected on the friction surface through the chemical plating, so that the surface self-texturing is realized without influencing the integrity of the friction surface; obtaining a high-hardness coating through chemical plating; deposition of MoS by electrophoretic methods 2 The film realizes friction reduction and MoS is realized by a textured surface 2 The long-acting lubrication effect is achieved. The invention will electroplate and convert intoThe composite film with good texture is prepared by combining chemical plating and electrophoretic deposition, the integrity of a friction surface can be ensured while surface microtexturing is formed, and the coating and MoS (Mos surface modification) are improved 2 The bonding strength of the film is improved, and the coating composite MoS is greatly improved 2 The antifriction and wear-resistant effects of the solid lubricating film; and the nickel-based hard coating prepared by the electroplating and chemical plating methods has good bonding force, good corrosion resistance and strong wear resistance, and is more favorable for improving the antifriction and wear-resistant effects of the material. In addition, the method can regulate and control the surface roughness by regulating and controlling the addition amount of the hard nano particles and the electroplating time, realize the controllable preparation of the surface self-texturing degree and further realize the MoS 2 The service life of the lubricating phase is controllable.
Drawings
FIG. 1 shows a composite MoS with a self-textured hard coating on the surface prepared by the embodiment of the invention 2 The action mechanism of the film in the friction process is shown schematically;
FIG. 2 is an optical microscope image of the surface and measured values of roughness of the nickel electroplated layer (Ni-SiC coating) formed by electroplating in examples 1 to 4, wherein (a), (b), (c) and (d) in FIG. 2 correspond to example 1, example 2, example 3 and example 4, respectively;
FIG. 3 is a scanning electron microscope image and roughness measurement of the surface of a multi-layered nickel-based hard coating formed by electroplating and electroless plating in examples 1 to 4, wherein (a), (b), (c) and (d) in FIG. 3 correspond to example 1, example 2, example 3 and example 4, respectively;
FIG. 4 shows MoS in example 1 2 A three-dimensional image of the thickness of the film and a profile curve, wherein (a) in fig. 4 is the three-dimensional image of the thickness and (b) is the profile curve;
FIG. 5 shows the composite MoS with self-textured hard coating on the surface prepared in examples 1 to 4 2 The friction life curves of the films, M1, M2, M3 and M4 in fig. 5 correspond to example 1, example 2, example 3 and example 4, respectively.
Detailed Description
The invention provides a composite MoS with a self-textured hard coating on the surface 2 The preparation method of the film comprises the following steps:
sequentially carrying out electronickelling and chemical nickeling on the surface of a substrate to form a surface self-texturing nickel-based hard coating on the surface of the substrate; the electroplating solution adopted by the nickel electroplating comprises hard nanoparticles;
performing electrophoretic deposition on MoS on the surface of the self-textured nickel-based hard coating 2 Film to obtain the composite MoS with the hard coating with self-textured surface 2 A film.
The method comprises the steps of sequentially carrying out nickel electroplating and chemical nickel plating on the surface of a substrate, and forming a surface self-texturing nickel-based hard coating on the surface of the substrate. The substrate is not particularly required in the present invention, and a substrate material well known to those skilled in the art, such as carbon steel, aluminum alloy, etc., may be used. Prior to electroplating nickel, the present invention preferably pre-treats the substrate; the pretreatment preferably comprises grinding coarsening and ultrasonic cleaning which are sequentially carried out. In the invention, the grinding and roughening are preferably carried out by using 800-mesh abrasive paper, and the metal surface oxide is removed through the grinding and roughening, and surface textures are formed, so that the bonding force between the surface of the substrate and the coating is favorably improved; the ultrasonic cleaning preferably comprises ultrasonic cleaning in an organic solvent, preferably petroleum ether, and ultrasonic cleaning in an acidic solution, preferably 0.1mol/L dilute hydrochloric acid, in sequence, and impurities and oxides on the metal surface are further removed and sufficiently activated by the ultrasonic cleaning.
In the present invention, the plating solution preferably includes the following components in the amounts: 40-50 g/L of nickel chloride, preferably 45g/L; 250-300 g/L of nickel sulfate, preferably 280g/L; 30-40 g/L of boric acid, preferably 35g/L; 1.5-3.5 g/L of hard nano particles, preferably 1.8g/L; 0.3-1 g/L of surfactant, preferably 0.5g/L; the solvent is water; the pH value of the electroplating solution is 4.0-6.0. In the invention, the nickel chloride and the nickel sulfate are main salts and provide nickel ions required by the coating; the boric acid is used for maintaining the pH environment of the electroplating solution stable; the hard nanoparticles preferably comprise SiC, si 3 N 4 And ZrO 2 The particle size of the hard nanoparticles is preferably 10-100 nm; the invention adds hard nano particles into the electroplating solutionThe grains realize controllable preparation of the roughness of the texture of the surface of the coating, and do not influence the integrity of the friction surface. In the present invention, the surfactant preferably includes one or more of cetyltrimethylammonium bromide (CTAB), sodium Dodecylbenzenesulfonate (SDBS) and Sodium Dodecyl Sulfate (SDS); the surfactant can effectively disperse hard nanoparticles and prevent the particles from agglomerating. In the present invention, the method for preparing the plating solution preferably includes the steps of: mixing nickel chloride, nickel sulfate, boric acid and water, and separating a small amount of part from the obtained first mixed system; adding a surfactant and hard nanoparticles into the small amount of the mixture, and sequentially performing ultrasonic vibration dispersion and magnetic stirring dispersion on the obtained second mixed system to obtain a hard nanoparticle pre-dispersion system; and adding the hard nanoparticle pre-dispersion system into the rest part of the first mixed system, mixing, and adjusting the pH value to 4.0-6.0 to obtain the electroplating solution. In the invention, the time of ultrasonic vibration dispersion is preferably 60-90 min, the rotating speed of magnetic stirring dispersion is preferably 400-600 rpm, and the time is preferably 60-90 min; according to the invention, through the ultrasonic vibration dispersion and the magnetic stirring dispersion, the hard nanoparticles are pre-dispersed under the action of the surfactant, so that the uniform dispersion of the hard nanoparticles in the whole chemical plating solution is facilitated; the pH is preferably adjusted by means of the addition of an acid-base reagent, such as sulfuric acid or ammonia.
In the invention, the electroplating temperature of the electroplated nickel is preferably 50-60 ℃, and more preferably 55 ℃; the plating time is preferably 10min or less, more preferably 1 to 5min; the current density is preferably 2 to 8A/dm 2 More preferably 5A/dm 2 (ii) a The specific operation of the nickel electroplating is as follows: connecting a substrate serving as a workpiece to be plated with a negative electrode of a power supply to serve as a cathode, connecting a pure nickel plate (namely pure nickel serving as an ion supplement source of electroplating solution) with a positive electrode of the power supply to serve as an anode, placing the assembled cathode and anode in the electroplating solution with the temperature of 50-60 ℃, and adjusting the current of the power supply to be 2-8A/dm 2 The surface of the substrate is subjected to nickel electroplating at a current density of (1). Through the electroplating nickel, a nickel-based coating containing hard nano-particles with a surface nodular structure is formed on the surface of a substrate (note thatIs a Ni-hard nanoparticle coating); moreover, the surface roughness can be regulated and controlled by regulating and controlling the addition amount of the hard nanoparticles and the electroplating time, so that the controllable preparation of the surface self-texturing degree is realized, specifically comprising the following steps: the electroplating time is prolonged, the roughness of the surface of the coating is increased, and the self-texturing degree is further enhanced; the addition amount of the hard nano particles is increased or reduced, the content of the hard particles deposited in the nickel-based coating is influenced, the surface roughness of the coating is further influenced, and the self-texturing degree is regulated and controlled.
In the invention, the electroless plating solution used for the electroless nickel plating preferably comprises the following components in percentage by weight: 30-40 g/L of nickel sulfate, preferably 36g/L; 25-30 g/L sodium hypophosphite, preferably 28g/L; 30-40 g/L of sodium acetate, preferably 34g/L; 11-13 mL/L lactic acid, preferably 12.4mL/L, and 3-5 mg/L thiourea, preferably 4mg/L; the solvent is water; the pH value of the electroless plating solution is preferably 4.0 to 6.0. In the invention, the nickel sulfate and the sodium hypophosphite are respectively a main salt and a reducing agent, wherein the main salt provides nickel ions, and the reducing agent can reduce the nickel ions into metallic nickel; the sodium acetate is used as a buffering agent, plays a role in acid-base stabilization, keeps the pH value of a system to fluctuate within a certain range, and effectively avoids H in the reaction process + Influence the pH value of the system; the lactic acid is used as a complexing agent and forms a relatively stable chelate with nickel ions in the chemical plating solution, so that the concentration of free nickel ions in the system is reduced, and the addition of the lactic acid can control the deposition speed so as to ensure the uniformity and fineness of a plating layer and the stability of the plating solution; the thiourea is used as a stabilizer to prevent spontaneous decomposition of the electroless plating solution. The preparation method of the chemical plating solution has no special requirements, and the components are uniformly mixed; the pH of the electroless plating solution is adjusted by adding an acid-base reagent, such as sulfuric acid or ammonia. In the invention, the plating temperature of the chemical nickel plating is preferably 85-90 ℃, and more preferably 89 ℃; the plating time is preferably 90min or less, and more preferably 15min; and immersing the substrate after nickel electroplating in the chemical plating solution to carry out chemical plating. In the chemical plating process, nickel ions in the chemical plating solution are reduced into nickel by sodium hypophosphite, and meanwhile, phosphorus and partial metallic nickel form a covalent state,thus forming a wear-resistant and corrosion-resistant nickel-phosphorus alloy coating (noted as NiP coating) on the surface of the coating after nickel electroplating, and further forming a surface self-textured nickel-based hard coating on the surface of the substrate.
After the surface self-texturing nickel-based hard coating is formed on the surface of the substrate, the surface self-texturing nickel-based hard coating is subjected to electrophoretic deposition MoS 2 Film to obtain the surface self-textured hard coating composite MoS 2 A film. In the invention, the electrophoretic deposition solution used for electrophoretic deposition preferably comprises the following components in percentage by weight: moS 2 1-2 g/L, preferably 1.5-2 g/L; 0.3-1 g/L of surfactant, preferably 0.5g/L, and water as solvent; the surfactant is preferably cetyltrimethylammonium bromide (CTAB), which is effective in dispersing MoS 2 And the agglomeration phenomenon is avoided. The preparation method of the electrophoretic deposition solution has no special requirements, and all the components are uniformly mixed 2 Dispersion, i.e. the electrophoretic deposition solution. In the present invention, the voltage of the electrophoretic deposition is preferably 10 to 36V, more preferably 25V; the deposition time is preferably less than or equal to 5min, more preferably 2min; the electrophoretic deposition is carried out at room temperature. In the process of electrophoretic deposition, the substrate after chemical nickel plating is connected with the negative electrode of a power supply, and the positive electrode of the power supply is connected with a graphite electrode. The invention deposits MoS on the surface of the self-textured nickel-based hard coating by an electrophoretic deposition method 2 The film has simple process and is beneficial to realizing industrial production; furthermore, the MoS can be improved by the method of electrophoretic deposition 2 The bonding strength and the surface hardness of the film are favorable for reducing the friction coefficient of the film layer.
The invention combines the hard wear-resistant nickel-based coating and MoS 2 Compounding solid lubricating film, regulating surface shape, and utilizing microtexture to make abrasive dust and MoS 2 The storage effect of the lubricating phase achieves the slow release effect of the lubricating phase, and the controllable extension of the friction life is realized. The invention can greatly improve the coating composite MoS while ensuring the integrity of the friction surface 2 Antifriction of solid lubricating filmsWear-resistant effect; in addition, the electroplating and chemical plating technology adopted by the invention is mature, the electrophoretic deposition technology is simple, and the industrialization prospect is wide.
The invention provides the surface self-textured hard coating composite MoS prepared by the preparation method of the technical scheme 2 A film. The invention provides a composite MoS with a self-textured hard coating on the surface 2 The film has excellent antifriction and wear-resistant effects, and the surface self-texturing hard coating is compounded with MoS in the friction process 2 The film can collect and capture abrasive dust particles generated in the friction process, and the abrasive dust particles are prevented from scraping and damaging the surface of the friction pair in the sliding process; can also realize the MoS 2 The slow release of the lubricating phase prolongs the friction life, reduces the abrasion and prolongs the service time of the moving parts. In the invention, the surface self-texturing hard coating composite MoS 2 The film preferably comprises a nickel-based coating containing hard nano particles, a nickel-phosphorus alloy coating and MoS which are sequentially compounded on the surface of a substrate 2 Film, surface self-texturing hard coating composite MoS of said structure 2 The mechanism of action of the film during rubbing is shown in figure 1. The invention provides a composite MoS with a self-textured hard coating on the surface 2 The film can be effectively applied to the field of friction and wear protection.
The following examples are combined to prepare the composite MoS with the surface self-textured hard coating provided by the invention 2 The films and their preparation and use are described in detail but are not to be construed as limiting the scope of the invention.
Example 1
Surface self-texturing hard coating composite MoS 2 The film is prepared by the following steps:
(1) Pretreatment of the surface of a substrate: and (3) polishing the surface of the roughened substrate by using 800-mesh abrasive paper, cleaning the substrate by using deionized water, then placing the substrate in petroleum ether for ultrasonic cleaning for 5min, taking out the substrate for cleaning, and placing the substrate in 0.1mol/L diluted hydrochloric acid solution for ultrasonic cleaning for 5min.
(2) Electroplating a Ni-SiC coating: the electroplating solution is prepared from 45g/L of nickel chloride, 280g/L of nickel sulfate, 35g/L of boric acid, 1.8g/L of silicon carbide nanoparticles (with the particle size of 50 nm) and 05g/L Cetyl Trimethyl Ammonium Bromide (CTAB), deionized water as solvent, and pH 4.5; the preparation method of the electroplating solution comprises the following steps: the surfactant CTAB and the silicon carbide nanoparticles were added to a small amount of the plating solution, dispersed by ultrasonic vibration and magnetic stirring at a speed of about 500rpm for 90min each, and then the resulting predispersed silicon carbide nanoparticle system was added to the entire plating solution. Connecting the substrate as the workpiece to be plated with the negative pole of a power supply, connecting a pure nickel plate with the positive pole of the power supply, placing the substrate in an electroplating solution (at the temperature of 55 ℃), adjusting the current of the power supply, and maintaining the current density at 5A/dm 2 The electroplating time is 1min to form an electroplated nickel layer.
(3) Electroless plating (nickel-phosphorus alloy coating): the chemical plating solution consists of 36g/L nickel sulfate, 28g/L sodium hypophosphite, 34g/L sodium acetate, 12.4mL/L lactic acid and 4mg/L thiourea, the solvent is deionized water, and the pH value is 5.1; and completely immersing the electroplated sample in the chemical plating solution (the temperature is 89 ℃), and plating for 15min to form the chemical nickel plating layer. And electroplating and chemically plating to obtain the nickel-based hard coating with the self-textured surface.
(4) Electrophoretic deposition of MoS 2 Film formation: moS 2 The dispersion consisted of 2g/L of MoS 2 And 0.5g/L CTAB, the solvent is deionized water, and MoS is dispersed and stirred by ultrasonic 2 The dispersion is uniform. During electrophoretic deposition, a sample with a self-textured nickel-based hard coating formed on the surface is connected with a negative electrode of a power supply, a graphite electrode is selected as a positive electrode, the voltage is set to be 25V, the electrophoretic time is 2min, and MoS is compounded on the surface of the self-textured nickel-based hard coating 2 A film.
Example 2
Surface self-texturing hard coating composite MoS 2 The film is prepared by the following steps:
(1) Pretreatment of the surface of a substrate: and (3) polishing the roughened substrate surface by using 800-mesh sand paper, cleaning the substrate by using deionized water, then placing the substrate in petroleum ether for ultrasonic cleaning for 5min, taking out the substrate for cleaning, and placing the substrate in 0.1mol/L dilute hydrochloric acid solution for ultrasonic cleaning for 5min.
(2) Electroplating a Ni-SiC coating: the electroplating solution consists of 45g/L of nickel chloride, 280g/L of nickel sulfate, 35g/L of boric acid, 1.8g/L of silicon carbide nanoparticles (with the particle size of 30 nm) and 0.5g/L of CTAB, and the solvent isDeionized water, pH 4.6; the preparation method of the electroplating solution comprises the following steps: the surfactant CTAB and the silicon carbide nanoparticles were added to a small amount of the plating solution, dispersed by ultrasonic vibration and magnetic stirring at a speed of about 500rpm for 90min each, and then the resulting predispersed silicon carbide nanoparticle system was added to the entire plating solution. Connecting the substrate as the workpiece to be plated with the negative pole of a power supply, connecting a pure nickel plate with the positive pole of the power supply, placing the substrate in an electroplating solution (at the temperature of 55 ℃), adjusting the current of the power supply, and maintaining the current density at 5A/dm 2 The electroplating time is 2min to form an electroplated nickel layer.
(3) Electroless nickel coating (nickel-phosphorous alloy coating): the chemical plating solution consists of 36g/L nickel sulfate, 28g/L sodium hypophosphite, 34g/L sodium acetate, 12.4mL/L lactic acid and 4mg/L thiourea, the solvent is deionized water, and the pH value is 5.0; and completely immersing the electroplated sample in an electroless plating solution (at the temperature of 89 ℃) and plating for 15min to form an electroless plating layer. And obtaining the nickel-based hard coating with the self-textured surface through the electroplating and the chemical plating.
(4) Electrophoretic deposition of MoS 2 Film formation: moS 2 The dispersion consisted of 2g/L of MoS 2 And 0.5g/L CTAB, the solvent is deionized water, and MoS is dispersed and stirred by ultrasonic 2 The dispersion is uniform. During electrophoretic deposition, a sample with a self-textured nickel-based hard coating formed on the surface is connected with a negative electrode of a power supply, a graphite electrode is selected as a positive electrode, the voltage is set to be 25V, the electrophoretic time is 2min, and MoS is compounded on the surface of the self-textured nickel-based hard coating 2 A film.
Example 3
Surface self-texturing hard coating composite MoS 2 The film is prepared by the following steps:
(1) Pretreatment of the surface of a substrate: and (3) polishing the surface of the coarsened substrate by using 800-mesh sand paper, cleaning the substrate by using deionized water, placing the substrate in petroleum ether for ultrasonic cleaning for 5min, taking out the substrate for cleaning, and placing the substrate in 0.1mol/L dilute hydrochloric acid solution for ultrasonic cleaning for 5min.
(2) Electroplating a Ni-SiC coating: the electroplating solution consists of 45g/L nickel chloride, 280g/L nickel sulfate, 35g/L boric acid, 1.8g/L silicon carbide nanoparticles (with the particle size of 60 nm) and 0.5g/L CTAB, the solvent is deionized water, and the pH value is 4.3; the preparation method of the electroplating solution comprises the following steps: activating the surfaceThe sex agent CTAB and the silicon carbide nano-particles are added into a small amount of electroplating solution, dispersed by ultrasonic vibration and magnetic stirring at the speed of about 500rpm for 90min respectively, and then the obtained pre-dispersed silicon carbide nano-particle system is added into the whole electroplating solution. Connecting the substrate as the workpiece to be plated with the negative pole of a power supply, connecting a pure nickel plate with the positive pole of the power supply, placing the substrate in an electroplating solution (at the temperature of 55 ℃), adjusting the current of the power supply, and maintaining the current density at 5A/dm 2 And forming an electroplated nickel layer within 3min of electroplating time.
(3) Electroless nickel coating (nickel-phosphorous alloy coating): the chemical plating solution consists of 36g/L nickel sulfate, 28g/L sodium hypophosphite, 34g/L sodium acetate, 12.4mL/L lactic acid and 4mg/L thiourea, the solvent is deionized water, and the pH value is 4.8; and completely immersing the electroplated sample in an electroless plating solution (at the temperature of 89 ℃) and plating for 15min to form an electroless plating layer. And obtaining the nickel-based hard coating with the self-textured surface through the electroplating and the chemical plating.
(4) Electrophoretic deposition of MoS 2 Film formation: moS 2 The dispersion consisted of 2g/L of MoS 2 And 0.5g/L CTAB, the solvent is deionized water, and MoS is dispersed and stirred by ultrasonic 2 The dispersion is uniform. Connecting a sample with the self-texturing nickel-based hard coating on the surface with a negative electrode of a power supply during electrophoretic deposition, selecting a graphite electrode as a positive electrode, setting the voltage to be 25V, performing electrophoresis for 2min, and compositing MoS on the surface of the self-texturing nickel-based hard coating 2 A film.
Example 4
Surface self-texturing hard coating composite MoS 2 The film is prepared by the following steps:
(1) Pretreatment of the surface of a substrate: and (3) polishing the roughened substrate surface by using 800-mesh sand paper, cleaning the substrate by using deionized water, then placing the substrate in petroleum ether for ultrasonic cleaning for 5min, taking out the substrate for cleaning, and placing the substrate in 0.1mol/L dilute hydrochloric acid solution for ultrasonic cleaning for 5min.
(2) Electroplating a Ni-SiC coating: the electroplating solution consists of 45g/L nickel chloride, 280g/L nickel sulfate, 35g/L boric acid, 1.8g/L silicon carbide nanoparticles (with the particle size of 60 nm) and 0.5g/L CTAB, the solvent is deionized water, and the pH value is 4.2; the preparation method of the electroplating solution comprises the following steps: adding a surfactant CTAB and silicon carbide nanoparticles into a small amount of electroplatingIn liquid, the dispersion was carried out by ultrasonic vibration and magnetic stirring at a speed of about 500rpm for 90 minutes each, and then the resulting predispersed silicon carbide nanoparticle system was added to the entire plating solution. Connecting the substrate as the workpiece to be plated with the negative pole of a power supply, connecting a pure nickel plate with the positive pole of the power supply, placing the substrate in an electroplating solution (at the temperature of 55 ℃), adjusting the current of the power supply, and maintaining the current density at 5A/dm 2 The electroplating time is 4min to form an electroplated nickel layer.
(3) Electroless nickel coating (nickel-phosphorous alloy coating): the chemical plating solution consists of 36g/L nickel sulfate, 28g/L sodium hypophosphite, 34g/L sodium acetate, 12.4mL/L lactic acid and 4mg/L thiourea, the solvent is deionized water, and the pH value is 4.6; and completely immersing the electroplated sample in an electroless plating solution (at the temperature of 89 ℃) and plating for 15min to form an electroless plating layer. And obtaining the nickel-based hard coating with the self-textured surface through the electroplating and the chemical plating.
(4) Electrophoretic deposition of MoS 2 Film formation: moS 2 The dispersion consisted of 2g/L of MoS 2 And 0.5g/L CTAB, the solvent is deionized water, and MoS is dispersed and stirred by ultrasonic 2 The dispersion is uniform. During electrophoretic deposition, a sample with a self-textured nickel-based hard coating formed on the surface is connected with a negative electrode of a power supply, a graphite electrode is selected as a positive electrode, the voltage is set to be 25V, the electrophoretic time is 2min, and MoS is compounded on the surface of the self-textured nickel-based hard coating 2 A film.
FIG. 2 is an optical microscope image of the surface and measured values of roughness of the nickel electroplated layer (Ni-SiC coating) formed by electroplating in examples 1 to 4, wherein (a), (b), (c) and (d) in FIG. 2 correspond to example 1, example 2, example 3 and example 4, respectively. The results in fig. 2 show that the surface roughness of the coating shows a positive correlation increasing trend with the increase of the plating time.
FIG. 3 is a scanning electron microscope image and roughness measurement of the surface of a multi-layered nickel-based hard coating layer formed by electroplating and electroless plating in examples 1 to 4, wherein (a), (b), (c) and (d) in FIG. 3 correspond to example 1, example 2, example 3 and example 4, respectively. The results of fig. 3 show that the surface topography of the multilayer coating better reflects the topography characteristics of the bottom coating, and the surface roughness of the multilayer coating shows a positive correlation growth trend along with the prolonging of the electroplating time.
FIG. 4 shows MoS in example 1 2 The thickness three-dimensional image and the profile curve of the film are shown in fig. 4, in which (a) is the thickness three-dimensional image and (b) is the profile curve. FIG. 4 results show that MoS was prepared 2 The thickness of the film is uniform.
FIG. 5 shows the composite MoS with self-textured hard coating on the surface prepared in examples 1 to 4 2 The friction life curves of the films, M1, M2, M3 and M4 in fig. 5 correspond to example 1, example 2, example 3 and example 4, respectively, and the friction test conditions are as follows: the rotating radius is 5mm, the load is 5N, the diameter of the grinding ball (material 440C) is 8mm, and the rotating speed is 500r/min. FIG. 5 shows that the present invention can implement the MoS 2 Maintenance of the lubricating phase, thereby achieving long-lasting lubrication.
According to the comparative results of the above examples, the introduction of the hard nanoparticles into the nickel-based coating can form a textured surface on the surface, the roughness of the coating surface layer is provided by the Ni-hard nanoparticle layer of the bottom layer, no mechanical processing process exists, and the integrity is necessarily superior to that of a subtractive material manufacturing process; the roughness of the Ni-hard nanoparticle layer increases with the production time and this trend is still true after the surface production of nickel-phosphorous alloy coatings. And MoS 2 After the solid lubricating film is compounded, the textured surface can effectively prolong MoS 2 The friction life of (c).
The embodiment shows that the composite film with good texture is prepared by combining electroplating, chemical plating and electrophoretic deposition, the integrity of the friction surface can be ensured while the surface microtexture is formed, and the coating composite MoS is greatly improved 2 The antifriction and wear-resistant effects of the solid lubricating film.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. Composite MoS with self-textured hard coating on surface 2 A method for producing a film, characterized in thatThe method comprises the following steps:
sequentially carrying out nickel electroplating and chemical nickel plating on the surface of a substrate to form a surface self-textured nickel-based hard coating on the surface of the substrate; the electroplating solution adopted by the nickel electroplating comprises hard nanoparticles;
performing electrophoretic deposition on MoS on the surface of the self-textured nickel-based hard coating 2 Film to obtain the surface self-textured hard coating composite MoS 2 A film.
2. The production method according to claim 1, wherein the plating solution comprises the following components in amounts: 40-50 g/L of nickel chloride, 250-300 g/L of nickel sulfate, 30-40 g/L of boric acid, 1.5-3.5 g/L of hard nanoparticles, 0.3-1 g/L of surfactant and water as a solvent; the pH value of the electroplating solution is 4.0-6.0.
3. The production method according to claim 1 or 2, wherein the hard nanoparticles comprise SiC, si 3 N 4 And ZrO 2 One or more of the above; the particle size of the hard nano-particles is 10-100 nm.
4. The production method according to claim 1 or 2, wherein the plating temperature of the nickel plating is 50 to 60 ℃, the plating time is 10min or less, and the current density is 2 to 8A/dm 2 。
5. The preparation method of claim 1, wherein the electroless nickel plating solution comprises the following components in percentage by weight: 30-40 g/L of nickel sulfate, 25-30 g/L of sodium hypophosphite, 30-40 g/L of sodium acetate, 11-13 mL/L of lactic acid, 3-5 mg/L of thiourea and water as a solvent; the pH value of the chemical plating solution is 4.0-6.0.
6. The method according to claim 1 or 5, wherein the electroless nickel plating is performed at a plating temperature of 85 to 90 ℃ for a plating time of 90min or less.
7. The preparation method of claim 1, wherein the electrophoretic deposition solution used for electrophoretic deposition comprises the following components in percentage by weight: moS 2 1-2 g/L, 0.3-1 g/L of surfactant and water as solvent.
8. The method according to claim 1 or 7, wherein the voltage of the electrophoretic deposition is 10-36V, and the deposition time is 5min or less.
9. Surface self-texturing hard coating composite MoS prepared by the preparation method of any one of claims 1 to 8 2 A film.
10. The surface self-textured hard coat composite MoS of claim 9 2 Use of a film for protection against frictional wear.
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