CN113005488A - Preparation method of tungsten disulfide-doped composite coating with high hardness and low friction coefficient - Google Patents

Preparation method of tungsten disulfide-doped composite coating with high hardness and low friction coefficient Download PDF

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CN113005488A
CN113005488A CN202011599046.1A CN202011599046A CN113005488A CN 113005488 A CN113005488 A CN 113005488A CN 202011599046 A CN202011599046 A CN 202011599046A CN 113005488 A CN113005488 A CN 113005488A
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ptfe
concentration
composite coating
base material
electroplating
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郁水峰
汪鸿涛
许新花
李明辉
张根吉
李伟
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Bill Anda Shanghai Lubricating Material Co ltd
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Bill Anda Shanghai Lubricating Material Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/04—Electroplating: Baths therefor from solutions of chromium
    • C25D3/06—Electroplating: Baths therefor from solutions of chromium from solutions of trivalent chromium
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/10—Other heavy metals
    • C23G1/103—Other heavy metals copper or alloys of copper
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
    • C23G1/20—Other heavy metals
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/04—Electroplating: Baths therefor from solutions of chromium
    • C25D3/10—Electroplating: Baths therefor from solutions of chromium characterised by the organic bath constituents used
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/34—Pretreatment of metallic surfaces to be electroplated

Abstract

The invention relates to the technical field of materials, in particular to a preparation method of a tungsten disulfide doped composite coating with high hardness and low friction coefficient, which comprises the following steps: step S01, putting the base material into a container containing 100mL of acetone, and cleaning for 10min by adopting ultrasonic waves, wherein the power is set to be 90W; step S02, degreasing the base material by a chemical method, wherein the degreasing temperature is 70-80 ℃, and the time is 10-15 min; step S03, on the basis of step S02, the base material is acid-washed and activated for 4min by using hydrochloric acid with the volume fraction of 40-60%; step S04, electroplatingPlating a layer of Cr-WS on a substrate2-PTFE; the invention has the advantages of simple process, high deposition speed, low cost, good bonding strength and the like.

Description

Preparation method of tungsten disulfide-doped composite coating with high hardness and low friction coefficient
Technical Field
The invention relates to the technical field of materials, in particular to a preparation method of a tungsten disulfide doped composite coating with high hardness and low friction coefficient.
Background
Electroplating is a surface treatment technique for surface modification, and different coatings are applied to the surface of materials to meet different performance requirements, so that electroplating has been widely used in various fields of industrial production and scientific research. The chromium coating obtained by electroplating has good wear resistance, hardness and corrosion resistance, and can be used for decorative coatings and also for functional coatings in a large quantity. The traditional chromium plating adopts hexavalent chromium plating solution for electroplating chromium, the toxicity is very high and is about 100 times of that of trivalent chromium, and if the content of hexavalent chromium in water exceeds 0.1mg/L, the chromium is poisoned. In order to replace hexavalent chromium plating, many studies have been made, among which trivalent chromium is mainly used to replace hexavalent chromium plating, and is most promising. The trivalent chromium sulfate plating solution coating has the advantages of low pollution, high current efficiency and the like, and great progress is made in recent years.
In the research field, a great deal of research has been done on the preparation process of trivalent chromium composite coatings, and a sulfate trivalent chromium double-tank electroplating process was developed in 1981 by Caning in UK. Ibrahim et al invented a process for electroplating thick chromium from trivalent chromium using urea as a complexing agent in 1998. The research on acetate systems, formate systems and the like is mainly represented by Harbin industrial university in China, and small-scale production and application are obtained. Studies on trivalent chromium sulfate electroplating and titanium-based anodes were conducted in the 90 s of the 20 th century, at the university of industry in south and central, and at the university of guangzhou, in the second light. In the 20 th century, the chemical technology center of Beijing Lanlijiamei invented a BSC12 type trivalent chromium hard chromium electroplating solution, which has good stability and solves the problems of poor bonding force between the coating and the substrate and the failure to obtain a thick coating in the existing trivalent chromium electroplating technology, but the uniform plating capability of the trivalent chromium prepared by the method is not very good, and the frictional wear performance is further improved.
Therefore, the trivalent chromium coating still has certain limitations in the use process, and under the working condition that the trivalent chromium coating is seriously worn or even worn after parts (such as bearings, pipelines, axes and the like) under heavy-load and high-wear-resistance environments are used for a period of time, the microhardness of the trivalent chromium composite coating needs to be further improved, and the friction coefficient of the coating needs to be reduced.
Disclosure of Invention
The invention provides a preparation method of a tungsten disulfide doped composite coating with high hardness and low friction coefficient, which is used for solving the technical problem of poor friction and wear resistance of a trivalent chromium coating in the prior art.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the invention provides a preparation method of a tungsten disulfide doped composite coating with high hardness and low friction coefficient, which comprises the following steps:
step S01, putting the base material into a container containing 100mL of acetone, and cleaning for 10min by adopting ultrasonic waves, wherein the power is set to be 90W;
step S02, degreasing the base material by a chemical method, wherein the degreasing temperature is 70-80 ℃, and the time is 10-15 min;
step S03, on the basis of step S02, the base material is acid-washed and activated for 4min by using hydrochloric acid with the volume fraction of 40-60%;
step S04, plating a Cr-WS layer on the substrate by electroplating2-PTFE。
Preferably, in the electroplating process of the step S04, the doping amount of WS2 in the trivalent chromium electroplating solution is 0-3.5g/L, the concentration of PTFE is 12.5ml/L, the temperature of the electroplating solution is 45 ℃, the pH value is 1.5-2.5, and the current density is 35A/dm2The deposition time was 20 min.
Preferably, in step S02, the degreasing solution includes NaOH and Na2CO3、Na3PO4Wherein the concentration of NaOH is 20g/L, Na2CO3Has a concentration of 30g/L, Na3PO4The concentration of the base material is 30g/L, the solution is heated to 70-80 ℃, then the base material is added into the oil removing solution, and the oil removing time is 10-15min, so that the oil stains on the surface of the base material are completely removed.
Preferably, the doping amount of the WS2 is 0g/L, the concentration of the PTFE is 12.5ml/L, the temperature of the plating solution is 45 ℃, the pH value is 2, and the current density is 35A/dm2。
Preferably, the doping amount of WS2 is 1.75g/L, the concentration of PTFE is 12.5ml/L, the temperature of the plating solution is 45 ℃, the pH value is 2, and the current density is 35A/dm2。
Preferably, the doping amount of WS2 is 3.5g/L, the concentration of PTFE is 12.5ml/L, the temperature of the plating solution is 45 ℃, the pH value is 2, and the current density is 35A/dm2。
Preferably, the base material is an H70 brass sample with a length of 40mm, a width of 40mm and a thickness of 0.3 mm.
The technical scheme of the invention has the following beneficial technical effects:
the invention adopts electroplating to prepare Cr-WS2The wear-resistant self-lubricating treatment technology for the surface of the base material with the PTFE coating prepares the Cr-WS with excellent frictional wear performance and uniform surface by optimizing preparation process parameters2-PTFE abrasion resistant coating. Compared with the traditional process, the process complexity is reduced, the production cost is reduced, the frictional wear performance of the coating is improved, the coating can be used as a protective coating of a frictional wear resistant workpiece, and the preparation method has the advantages of simple process, high deposition speed, low cost, good bonding strength and the like.
Drawings
FIG. 1 is a graph showing WS in trivalent chromium plating solution in the course of electroplating in examples 1 to 72The concentrations of (a) are respectively 0g/L, 0.5g/L, 1.0g/L, 1.75g/L, 2.5g/L, 3.0g/L and 3.5g/L to obtain the corresponding Cr-WS2-XRD spectrum of PTFE composite coating;
FIG. 2a shows WS in a trivalent chromium plating bath during electroplating2At a concentration of 0g/L, the resulting electroplated Cr-WS2-SEM picture of surface topography of wear resistant coating of PTFE;
FIG. 2b shows WS in a trivalent chromium plating bath during electroplating2At a concentration of 0.5g/L, the resulting electroplated Cr-WS2-SEM picture of surface topography of wear resistant coating of PTFE;
FIG. 2c shows WS in a trivalent chromium plating bath during electroplating2At a concentration of 1.0g/L, the resulting electroplated Cr-WS2-SEM picture of surface topography of wear resistant coating of PTFE;
FIG. 2d shows WS in a trivalent chromium plating bath during electroplating2At a concentration of 1.75g/L, the resulting electroplated Cr-WS2-SEM picture of surface topography of wear resistant coating of PTFE;
FIG. 2e depicts WS in a trivalent chromium plating bath during electroplating2At a concentration of 2.5g/L, the resulting electroplated Cr-WS2-SEM picture of surface topography of wear resistant coating of PTFE;
FIG. 2f shows WS in a trivalent chromium plating bath during electroplating2At a concentration of 3.0g/L, the resulting electroplated Cr-WS2-SEM picture of surface topography of wear resistant coating of PTFE;
FIG. 2g shows WS in a trivalent chromium plating bath during electroplating2At a concentration of 3.5g/L, the resulting electroplated Cr-WS2-SEM picture of surface topography of wear resistant coating of PTFE;
FIG. 3 is a schematic view of WS in a trivalent chromium plating bath in the plating processes of examples 1-72The concentrations of (a) are respectively 0g/L, 0.5g/L, 1.0g/L, 1.75g/L, 2.5g/L, 3.0g/L and 3.5g/L to obtain the corresponding Cr-WS2-microhardness map of the PTFE composite coating;
FIG. 4 is a schematic view of WS in a trivalent chromium plating bath in the plating processes of examples 1-72The concentrations of (a) are respectively 0g/L, 0.5g/L, 1.0g/L, 1.75g/L, 2.5g/L, 3.0g/L and 3.5g/L to obtain the corresponding Cr-WS2-a plot of coefficient of friction for a PTFE composite coating;
FIG. 5 is a schematic view of WS in a trivalent chromium plating bath in the plating processes of examples 1-72The concentrations of (a) are respectively 0g/L, 0.5g/L, 1.0g/L, 1.75g/L, 2.5g/L, 3.0g/L and 3.5g/L to obtain the corresponding Cr-WS2-wear resistance profile of PTFE composite coating;
FIG. 6a is a schematic view of WS in a trivalent chromium plating bath in the electroplating processes of examples 1-72The surface energy spectrogram of the trivalent chromium composite coating when the concentration of (A) is 2.5 g/L;
FIG. 6b is a schematic view of WS in a trivalent chromium plating bath in the electroplating processes of examples 1-72SEM cross-sectional view of trivalent chromium composite coating at a concentration of 2.5 g/L.
Detailed Description
In order to make the technical means, the original characteristics, the achieved purposes and the effects of the invention easily understood, the invention is further described below with reference to specific embodiments and the attached drawings, but the following embodiments are only the preferred embodiments of the invention, and not all embodiments are provided. Based on the embodiments in the implementation, other embodiments obtained by those skilled in the art without any creative efforts belong to the protection scope of the present invention. Moreover, in the following description, descriptions of well-known structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present invention.
It should be noted that the preparation, characterization and measurement instruments used in the present invention:
Cr-WS obtained in various embodiments of the present invention2-the PTFE layer was analyzed for the crystallographic phase structure of the film using X-ray diffraction (XRD) instrument model D8 ADVANCE from Bruker;
Cr-WS analysis Using QuantaFEG450 field emission Environment Scanning Electron Microscope (SEM) with spectrometer (EDS) from FEI, USA2-composition, micro-topography and thickness of the PTFE layer;
measuring the microhardness of the composite coating by adopting a NANO Indenter G200 type NANO Indenter produced by Agilent company in the United states;
measuring the friction wear coefficient of the composite coating by using an HSR-2M reciprocating friction wear instrument of Kwakay science and technology Limited of Kwakawa;
a high-frequency rectifier of Fushuntai science and technology Limited in Shenzhen city is used for providing electroplating power supplies (50A and 24V);
the top and bottom mass values of each sample were weighed using an XP6 analytical balance (METTLER TOLEDO, Switzerland) and the abrasion resistance of the composite coating was evaluated by the loss-of-weight method.
Wherein, the base material adopts an H70 brass sample, the length is 40mm, the width is 40mm, and the thickness is 0.3 mm.
Example 1.
A preparation method of a tungsten disulfide doped composite coating with high hardness and low friction coefficient comprises the following steps:
step S01, putting the base material into a container containing 100mL of acetone, and cleaning for 10min by adopting ultrasonic waves, wherein the power is set to be 90W;
step S02, degreasing the base material by a chemical method, wherein the degreasing temperature is 70-80 ℃, and the time is 10-15 min;
step S03, on the basis of step S02, the base material is acid-washed and activated for 4min by using hydrochloric acid with the volume fraction of 40-60%;
step S04, plating a Cr-WS layer on the substrate by electroplating2-PTFE。
In step S02, the degreasing solution comprises NaOH and Na2CO3、Na3PO4Wherein the concentration of NaOH is 20g/L, Na2CO3Has a concentration of 30g/L, Na3PO4The concentration of the base material is 30g/L, the solution is heated to 70-80 ℃, then the base material is added into the oil removing solution, and the oil removing time is 10-15min, so that the oil stains on the surface of the base material are completely removed.
In the electroplating process of step S04, the concentration of PTFE in the trivalent chromium electroplating solution is 12.5ml/L, the temperature of the electroplating solution is 45 ℃, the pH value is 2.0, and the current density is 35A/dm2. Stirring slowly by using a magnetic stirrer, and depositing for 20 minutes to obtain Cr-WS2-PTFE abrasion resistant coating.
Example 2
Different from the embodiment 1, the WS in trivalent chromium electroplating solution in the electroplating process in the step S04 is the preparation method of the tungsten disulfide doped composite coating with high hardness and low friction coefficient2The doping amount is 0.5g/L, the concentration of PTFE is 12.5ml/L, the temperature of the plating solution is 45 ℃, the pH value is 2.0, and the current density is 35A/dm2。
Example 3
Different from the embodiment 1, the preparation method of the tungsten disulfide doped composite coating with high hardness and low friction coefficient comprises the step S04 of electroplatingWS in chromium-valent electroplating baths2The doping amount is 1.0g/L, the concentration of PTFE is 12.5ml/L, the temperature of the plating solution is 45 ℃, the pH value is 2.0, and the current density is 35A/dm2。
Example 4
Different from the embodiment 1, the WS in trivalent chromium electroplating solution in the electroplating process in the step S04 is the preparation method of the tungsten disulfide doped composite coating with high hardness and low friction coefficient2The doping amount is 1.75g/L, the concentration of PTFE is 12.5ml/L, the temperature of the plating solution is 45 ℃, the pH value is 2.0, and the current density is 35A/dm2。
Example 5
Different from the embodiment 1, the WS in trivalent chromium electroplating solution in the electroplating process in the step S04 is the preparation method of the tungsten disulfide doped composite coating with high hardness and low friction coefficient2The doping amount is 2.5g/L, the concentration of PTFE is 12.5ml/L, the temperature of the plating solution is 45 ℃, the pH value is 2.0, and the current density is 35A/dm2。
Example 6
Different from the embodiment 1, the WS in trivalent chromium electroplating solution in the electroplating process in the step S04 is the preparation method of the tungsten disulfide doped composite coating with high hardness and low friction coefficient2The doping amount is 3.0g/L, the concentration of PTFE is 12.5ml/L, the temperature of the plating solution is 45 ℃, the pH value is 2.0, and the current density is 35A/dm2。
Example 7
Different from the embodiment 1, the WS in trivalent chromium electroplating solution in the electroplating process in the step S04 is the preparation method of the tungsten disulfide doped composite coating with high hardness and low friction coefficient2The doping amount is 3.5g/L, the concentration of PTFE is 12.5ml/L, the temperature of the plating solution is 45 ℃, the pH value is 2.0, and the current density is 35A/dm2。
In conclusion, the invention obtains the Cr-WS by the electroplating technology2Wear-resistant coating of PTFE and by controlling WS in the plating bath during electroplating2To a concentration of (a) to finally obtain a Cr-WS obtained by electroplating2Wear-resistant PTFE coating, resulting Cr-WS2The PTFE composite coating has compact structure, uniform size and high resistanceThe abrasion performance is excellent.
Further, the preparation method of the tungsten disulfide doped composite coating with high hardness and low friction coefficient is easy for industrial production and reduces the production cost.
For a better understanding of the invention, examples 1-7, WS in electroplating, i.e., trivalent chromium plating baths, are each separately described2The concentrations of the Cr-WS are respectively 0g/L, 0.5g/L, 1.0g/L, 1.75g/L, 2.5g/L, 3.0g/L and 3.5g/L to obtain the corresponding Cr-WS2XRD spectra of the PTFE composite coatings were determined, and the results are shown in FIG. 1, and it can be seen from FIG. 1 that different WS are2Cr-WS at concentration2The pattern shapes of the PTFE composite coatings are similar, and different WS are prepared under the condition that the current density, the electroplating duration, the concentration of PTFE, the pH value and the temperature are kept unchanged in the electroplating process2Content of Cr-WS2The XRD line of the PTFE composite coating shows a Cr diffraction peak at 44.3 degrees 2 theta. According to XRD pattern, with WS2Increasing concentration of Cr-WS2The intensity of the diffraction peak of the PTFE composite coating increases and then decreases, that is to say, Cr-WS2The crystalline strength of the PTFE composite coating is first increased and then decreased. In WS2At a concentration of 2.5g/L, the diffraction peak of trivalent chromium is strongest, and other WS2The intensity of the diffraction peak of the trivalent chromium with concentration is relatively weaker, which shows that the crystallinity of the Cr phase formed in the electroplating coating is better; however, PTFE and WS were not observed in the XRD spectrum (FIG. 1)2Due to the diffraction peak of Cr-WS2PTFE and WS in PTFE composite coatings2The content of nano particles is small.
Examples 1 to 7, WS in electroplating Process, trivalent chromium plating bath2SEM pictures of (b) at concentrations of 0g/L, 0.5g/L, 1.0g/L, 1.75g/L, 2.5g/L, 3.0g/L and 3.5g/L, respectively. As can be seen from FIGS. 2a-2e, in WS2When the concentration of (b) is 0-2.5g/L, Cr-WS2-the PTFE composite coating wraps the nano-particle WS2And PTFE, with WS2Increase in the concentration of (A) WS in the coating2The amount of embedding is increased and the dispersion is more and more uniform, and the PTFE particles are embeddedThe amount gradually decreases. This is due to the fact that with WS2Increase of particles in the bath WS2The concentration of the particles is higher and higher, WS is formed during the electroplating process2The probability of particles becoming embedded in the coating increases and WS on the surface of the coating is thereby entered2The more particles, when WS2The rate of particles entering the surface of the coating is equal to WS2WS in composite coatings at the rate of particle insertion into the coating2Particle reaches a maximum value, WS2WS in the composite coating when the concentration of the particles is 2.5g/L2The particle compounding amount reaches the maximum. When the concentration is increased from 2.5g/L to 3.5g/L, WS in the composite coating is increased from 2e to 2g2The amount of particles compounded begins to decrease due to WS2The particles have physical properties of large density, large specific surface area, high specific surface energy and the like, and WS2PTFE particles are easy to generate polymerization and sedimentation and do not present a suspension uniform state, the adsorption quantity of the particles on the coating surface is reduced, the composite quantity is not increased or even reduced, and Cr-WS2The quality of the surface of the PTFE composite coating gradually deteriorates, cracks appear, and the appearance becomes poor.
Examples 1 to 7, WS in electroplating Process, trivalent chromium plating bath2The concentrations of (a) are respectively 0g/L, 0.5g/L, 1.0g/L, 1.75g/L, 2.5g/L, 3.0g/L and 3.5g/L to obtain the corresponding Cr-WS2The microhardness of the PTFE composite coating was determined and fitted to a curve as shown in FIG. 3, as can be seen from the curve of FIG. 3, as the WS changes2The particle concentration is increased, and the hardness of the plating layer is reduced, then increased, and then reduced. The analysis in the chapter shows that the microhardness of the composite coating is related to the content and distribution state of the second phase particles in the composite coating, namely WS in the coating2And PTFE particles. In WS2At a concentration of 0-1.0g/L, with WS2Added into trivalent chromium composite plating solution due to WS2And the PTFE particles themselves have a lower hardness, WS2And PTFE particles enter the surface of the coating and are embedded in the coating, but are also unevenly distributed, so that Cr-WS is formed2The hardness of the PTFE composite coating decreases. With WS in the plating solution2The concentration of particles is increased, at WS2At a concentration of 1.0-2.5g/L, Cr-WS2-PTFE compositeThe hardness of the coating increased correspondingly, probably due to WS2As the particles become increasingly uniformly distributed over the surface of the coating, WS2The particles have the function of catalyzing crystallization, so that the coating generates lattice distortion, and the crystallinity of the coating is improved, which is similar to that of an XRD pattern in WS2The maximum diffraction peak intensity was consistent at a concentration of 2.5 g/L. With WS2Further increase of particles from a concentration of 2.5g/L to 3.5g/L WS2Excessive particles, increased collision in the moving process of the particles and increased instability of the plating solution, resulting in Cr-WS2The surface quality of the PTFE composite coating is reduced, and the hardness is also reduced.
Examples 1 to 7, WS in electroplating Process, trivalent chromium plating bath2The concentrations of (a) are respectively 0g/L, 0.5g/L, 1.0g/L, 1.75g/L, 2.5g/L, 3.0g/L and 3.5g/L to obtain the corresponding Cr-WS2The coefficient of friction of the PTFE composite coating was determined and fitted to a curve of the coefficient of friction as shown in FIG. 4, as WS2The increase in concentration increases the coefficient of friction of the coating first to decrease and then to increase. Because with WS2Increase in concentration, WS2And PTFE particles enter the surface of the coating in a compounding way, and WS is in trivalent chromium compound plating solution2The amount of suspended nanoparticles is correspondingly increased, WS during electroplating2The probability of particles becoming embedded in the coating increases and WS on the surface of the coating is thereby entered2The amount of particles also increases when WS2The rate of particle entry into the coating surface is equal to WS2WS in coating at rate of particle insertion into coating2The particles reaching the highest value, i.e. WS2At a concentration of 2.5g/L, Cr-WS2WS in PTFE composite coatings2The compounding amount of (A) is optimal. When the composite coating is rubbed on the surface of an object, WS in the coating2And PTFE particles have a very low friction coefficient, and the lubricating particles in the composite coating are easily extruded into the surface layer to form a uniform lubricating film, so that Cr-WS2The PTFE composite coating exhibits excellent lubricating properties. When WS is present in trivalent chromium baths2When the concentration is further increased, WS in the plating solution at this time2Too high a concentration of particles, WS2And PTFE particles are polymerized to settle, WS2And PTFE nanoparticles in the plating solutionIn the suspension is difficult to maintain uniformly and stably, thereby reducing WS2And the effective concentration of PTFE particles, the lubricating properties decrease, and the coefficient of friction increases.
Examples 1 to 7, WS in electroplating Process, trivalent chromium plating bath2The concentrations of (a) are respectively 0g/L, 0.5g/L, 1.0g/L, 1.75g/L, 2.5g/L, 3.0g/L and 3.5g/L to obtain the corresponding Cr-WS2The wear resistance of the PTFE composite coating was determined and fitted to a wear characteristic curve as shown in FIG. 5, as WS in trivalent chromium bath2Increased content of Cr-WS2The wear resistance of the PTFE composite coating decreases and increases, and the wear resistance increases and decreases. This is because the wear resistance of the material is mainly closely related to the hardness and the coefficient of friction of the coating, in WS2At a concentration of 0-2.5g/L, Cr-WS2The hardness of the PTFE composite coating increases and the coefficient of friction decreases, with an increase in the shear strength and an increase in the abrasion resistance of the coating, in WS2Has a concentration of 2.5g/L to an optimum value, and during the wear process, Cr-WS2The lubricating particles of the PTFE composite coating can be subjected to mechanical and chemical changes with objects on the mating surface to form a transfer film, so that direct frictional contact between metals is reduced, and abrasion is reduced. With WS2The concentration of (A) continues to increase, at WS2WS in the plating solution at a concentration of 2.5-3.5g/L2The concentration of (A) is too high, the stability of the composite plating solution is obviously reduced, and Cr-WS2The hardness of the PTFE composite coating is reduced, the friction coefficient is obviously increased, and therefore, the Cr-WS2The wear amount of the PTFE composite plating layer is increased, and the wear resistance is reduced.
From the above examples, it was realized that WS can be controlled in trivalent chromium plating baths2To obtain WS2Cr-WS of different contents2PTFE composite coatings by comparison of different WS2Doped pair electroplating of Cr-WS2The influence of the microstructure and the mechanical properties of the PTFE composite coating, which defines that the concentration of PTFE is 12.5ml/L and the current density is 35A/dm2The pH value is about 2.0, the temperature of the plating solution is 45 ℃, the deposition time is 20min, and the Cr-WS is2Optimum WS for PTFE composite coating2The doping amount is 2.5 g/L. At the doping amountCr-WS prepared under2The PTFE composite coating has compact structure, uniform grain size, tight combination between the coating and the matrix and optimal surface wear resistance.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and the above embodiments and descriptions are only preferred embodiments of the present invention and are not intended to limit the present invention, and that various changes and modifications may be made without departing from the spirit and scope of the present invention, which fall within the scope of the claimed invention. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (7)

1. A preparation method of a tungsten disulfide doped composite coating with high hardness and low friction coefficient is characterized by comprising the following steps:
step S01, putting the base material into a container containing 100mL of acetone, and cleaning for 10min by adopting ultrasonic waves, wherein the power is set to be 90W;
step S02, degreasing the base material by a chemical method, wherein the degreasing temperature is 70-80 ℃, and the time is 10-15 min;
step S03, on the basis of step S02, the base material is acid-washed and activated for 4min by using hydrochloric acid with the volume fraction of 40-60%;
step S04, plating a Cr-WS layer on the substrate by electroplating2-PTFE。
2. The method as claimed in claim 1, wherein in the electroplating process of step S04, the amount of WS2 in the trivalent chromium electroplating solution is 0-3.5g/L, the concentration of PTFE is 12.5ml/L, the temperature of the electroplating solution is 45 ℃, the pH is 1.5-2.5, and the current density is 35A/dm2The deposition time was 20 min.
3. The tungsten disulfide blend of claim 1 having high hardness and low coefficient of frictionThe preparation method of the composite coating is characterized in that in the step S02, the oil removing solution comprises NaOH and Na2CO3、Na3PO4Wherein the concentration of NaOH is 20g/L, Na2CO3Has a concentration of 30g/L, Na3PO4The concentration of the base material is 30g/L, the solution is heated to 70-80 ℃, then the base material is added into the oil removing solution, and the oil removing time is 10-15min, so that the oil stains on the surface of the base material are completely removed.
4. The method for preparing the tungsten disulfide doped composite coating with high hardness and low friction coefficient according to claim 2, wherein the WS2 doping amount is 0g/L, the PTFE concentration is 12.5ml/L, the plating solution temperature is 45 ℃, the pH value is 2, and the current density is 35A/dm2。
5. The method for preparing the tungsten disulfide doped composite coating with high hardness and low friction coefficient according to claim 2, wherein the WS2 doping amount is 1.75g/L, the PTFE concentration is 12.5ml/L, the plating solution temperature is 45 ℃, the pH value is 2, and the current density is 35A/dm2。
6. The method for preparing the tungsten disulfide doped composite coating with high hardness and low friction coefficient according to claim 2, wherein the WS2 doping amount is 3.5g/L, the PTFE concentration is 12.5ml/L, the plating solution temperature is 45 ℃, the pH value is 2, and the current density is 35A/dm2。
7. The method for preparing the tungsten disulfide doped composite coating with high hardness and low friction coefficient according to claim 1, wherein the base material is H70 brass sample with length of 40mm, width of 40mm and thickness of 0.3 mm.
CN202011599046.1A 2020-12-30 2020-12-30 Preparation method of tungsten disulfide-doped composite coating with high hardness and low friction coefficient Pending CN113005488A (en)

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