CN111962112B - High-wear-resistance and corrosion-resistance Ni-Mo/diamond composite coating based on phase change and preparation method thereof - Google Patents
High-wear-resistance and corrosion-resistance Ni-Mo/diamond composite coating based on phase change and preparation method thereof Download PDFInfo
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- C25D3/00—Electroplating: Baths therefor
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- C25D3/56—Electroplating: Baths therefor from solutions of alloys
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- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
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- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
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- 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
- C25D5/10—Electroplating with more than one layer of the same or of different metals
- C25D5/12—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium
- C25D5/14—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium two or more layers being of nickel or chromium, e.g. duplex or triplex layers
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- C—CHEMISTRY; METALLURGY
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- 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
- C25D5/48—After-treatment of electroplated surfaces
- C25D5/50—After-treatment of electroplated surfaces by heat-treatment
Abstract
The invention discloses a high-wear-resistance and corrosion-resistance Ni-Mo/diamond composite coating based on phase change and a preparation method thereof, belonging to the technical field of metal material surface protective coatings. The composite electro-deposition technology is adopted to electroplate a Ni-Mo/diamond composite coating on the surface of the stainless steel. The coating has the advantages of low hardness, high film-based bonding strength, wear resistance and sea salt corrosion resistance. The composite coating prepared by the invention can be used for mechanical parts which are used in chemical industry, metallurgy industry, electric power industry, petroleum industry and the like and bear the friction and wear effects under corrosive environments and the like.
Description
The technical field is as follows:
the invention relates to the technical field of protective coatings on the surfaces of metal materials, in particular to a phase-change-based high-wear-resistance and corrosion-resistance Ni-Mo/diamond composite coating and a preparation method thereof.
The background art comprises the following steps:
a major problem with metal workpieces operating in high stress corrosive environments is degradation of the material surface. Surface degradation leads to a reduction in the wear and corrosion resistance of the material, ultimately resulting in a reduction in the useful life of the workpiece. The surface protection is an effective way for inhibiting the surface degradation of the material and improving the performance of the material on the premise of not changing the base material. Electroplating of pure metals, alloyed metals and composite coatings is a common surface protection technique.
The electroplated pure metal Cr layer has high hardness and excellent wear resistance and corrosion resistance, so that the electroplated pure metal Cr layer is widely applied to the fields of chemical industry, metallurgy, electric power, petroleum, aerospace and the like. Since the addition of chromic acid compounds to the plating bath is required for the plating of hard Cr layers, such compounds have proven to be toxic and carcinogenic, causing serious environmental and human hazards. Meanwhile, the electroplated hard Cr layer cannot meet the increasingly stringent performance requirements in the industry. Decades of researches show that the composite coating of the alloy matrix and the second phase hardening particles has excellent mechanical, mechanical and chemical properties and becomes a coating capable of replacing a hard Cr layer.
Recent research shows that the Ni-Mo/diamond composite coating has high microhardness and excellent corrosion resistance and wear resistance. Meanwhile, researchers also regulate and control the content of diamond and Mo elements and the final performance of the coating by changing the type and size of hard particles, experimental methods, electroplating parameters and the like. These methods have proven effective, but the effect is not ideal, mainly in that the addition of diamond reduces the sea salt corrosion resistance of the coating.
Diamond is an unstable form of carbon element at normal temperature, and diamond particles are gradually graphitized after the temperature reaches 1200-1500 ℃. The process is accelerated in metals such as Ni, fe, mo and the like, and the graphitization temperature is reduced. On the other hand, due to the existence of the alloy element Mo in the coating, the heat treatment becomes another way for realizing the performance optimization of the Ni-Mo/diamond composite coating by regulating and controlling the microstructure and phase change.
Chinese patent (grant No. CN 108796564A) proposes to improve the hardness, wear resistance and corrosion resistance in sulfuric acid solution of Ni-Mo/diamond composite coating by means of heat treatment. The heat treatment temperature reported in the patent is lower, being 450 ℃. The research shows that the composite coating only has the segregation and aggregation processes of the Mo element to the grain boundary at the temperature, and does not have phase transformation. Therefore, the method of improving the hardness and wear resistance of the coating in this patent is achieved by changing the distribution of the solid solution elements. On the other hand, documents and patents that graphitize diamond in the composite coating by raising the heat treatment temperature have not been reported so far.
The invention content is as follows:
the invention aims to provide a high-wear-resistant and corrosion-resistant Ni-Mo/diamond composite coating based on phase change and a preparation method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a high wear-resisting corrosion-resistant Ni-Mo/diamond composite coating based on phase change is formed by uniformly doping diamond particles in Ni-Mo alloy; the content of Mo in the Ni-Mo alloy is 17-19 at.%, and the balance is Ni; the doping amount of the diamond particles in the composite coating is 18-21 vol.%.
The Ni-Mo alloy comprises Ni (Mo) solid solution, a precipitation phase MoNi and a strengthening phase Mo 2 C。
The Ni (Mo) solid solution is nanocrystalline, and the grain size of the Ni (Mo) solid solution is 17-64 nm.
The precipitation phase MoNi and the strengthening phase Mo 2 The grain size of C is 63-245 nm.
The diamond particles have a particle size of about 0.7 to 1 μm.
The composite coating is prepared on a stainless steel substrate, the microhardness of the composite coating is 6.2GPa, the coating/substrate binding force reaches more than 55MPa, and the wear rate is as low as 3.37 multiplied by 10 -6 mm 3 mN, much lower than 6.98X 10 without heat treatment -5 mm 3 /mN。
The corrosion current density of the composite coating in 3.5wt.% NaCl solution is 1.85 muA cm –2 Is better than 9.82 mu A cm when not heat treated –2 。
The preparation method of the Ni-Mo/diamond composite coating based on the phase change, high wear resistance and corrosion resistance comprises the steps of firstly preparing the Ni-Mo/diamond composite coating on a stainless steel substrate by adopting a composite electroplating technology, and then carrying out high-temperature heat treatment at 730-765 ℃ on the coating to obtain the Ni-Mo/diamond composite coating based on the phase change, high wear resistance and corrosion resistance. The method specifically comprises the following steps:
(1) Pre-plating a Ni layer on a stainless steel substrate: the preplating Ni layer adopts watt plating solution, and the preplating technological parameters are as follows: the current density is 2 to 4A/dm 2 The electroplating time is 5-10 min, and the pH value of the watt plating solution is 4.4-4.6; the watt liquid comprises the following components: 240-250 g/L of nickel sulfate, 35-50 g/L of nickel chloride, 35-40 g/L of boric acid and sugar0.4-0.6 g/L of refined sodium, 0.1-0.2 g/L of lauryl sodium sulfate and the balance of water.
(2) Preparing the Ni-Mo/diamond composite coating by adopting a direct-current electroplating method: the electroplating solution used comprises the following components: 60-80 g/L of nickel sulfate, 60-80 g/L of sodium citrate, 4g/L of sodium molybdate, 0.4-0.6 g/L of saccharin sodium, 0.1-0.2 g/L of sodium dodecyl sulfate, 120g/L of diamond particles and the balance of water; the parameters of the electroplating process are as follows: the pH value of the electroplating solution is 8.5-9.5, the temperature of the solution during electroplating is 30-35 ℃, the stirring speed is 70-90 rpm, and the current density is 3A/dm 2 The electroplating time is 2h;
(3) And (3) heat treatment: after the electroplating is finished, the coating is cleaned by alcohol and dried, and then is annealed in vacuum for 1-2 h at the high temperature of 730-765 ℃. After the composite coating is subjected to high-temperature heat treatment for 1-2 h at 730-765 ℃ which exceeds the graphitization temperature of the diamond, incomplete graphitization is performed on the diamond particles.
The design mechanism of the invention is as follows:
the invention adopts the electroplating process to prepare the composite coating on the stainless steel substrate, then carries out heat treatment on the coating, raises the heat treatment temperature to 730-765 ℃ above the graphitization temperature of the diamond, and controls the time of the heat treatment to lead the diamond to have incomplete graphitization. Experimental results show that Mo with lubricating effect is prepared by graphitizing diamond 2 The C phase greatly improves the wear resistance and sea salt corrosion resistance of the Ni-Mo/diamond composite coating.
The invention has the following advantages and beneficial effects:
1. the Ni-Mo/diamond composite coating based on phase change prepared by the invention has high hardness and shows excellent wear resistance under the dry friction condition. The micro Vickers hardness of the coating after vacuum annealing is 6.2-9.7 GPa, and the wear rate of the coating is as low as 3.37 multiplied by 10 - 6 mm 3 mN; much lower than 6.98X 10 without heat treatment -5 mm 3 /mN。
2. The Ni-Mo/diamond composite coating based on phase change prepared by the invention has good corrosion resistance in a sea salt corrosion environment; the corrosion current density of the coating after heat treatment in a 3.5wt.% NaCl solution was1.85μA cm –2 Is better than that of 9.82 mu A cm without heat treatment –2 。
3. The Ni-Mo/diamond composite coating based on phase change prepared by the invention has high binding force with a substrate, and the binding force between the coating and the substrate is 56-65 MPa.
4. The Ni-Mo/diamond composite coating based on phase change prepared by the invention can be applied to mechanical parts bearing the friction and wear effects in corrosive environments and the like in the industries of chemical industry, metallurgy, electric power, petroleum and the like.
Description of the drawings:
FIG. 1 shows the surface morphology of a Ni-Mo/diamond composite coating; wherein: in the as-deposited state, (b) 600 ℃ and (c) 750 ℃.
FIG. 2 is an XRD pattern of the Ni-Mo/diamond composite coating.
FIG. 3 is a diffraction pattern of diamond particles of the Ni-Mo/diamond composite coating after heat treatment at 750 ℃.
FIG. 4 is the microhardness of the Ni-Mo/diamond composite coating.
FIG. 5 shows the average friction coefficient and wear rate of the Ni-Mo/diamond composite coating.
Fig. 6 is a polarization curve of the Ni-Mo/diamond composite coating in a 3.5wt.% NaCl solution.
The specific implementation mode is as follows:
the invention is explained in detail below with reference to the figures and the specific embodiments. And the characterization means of the microstructure and the micro-morphology of the coating comprise a Scanning Electron Microscope (SEM), an energy spectrum analysis (EDS), an X-ray diffractometer (XRD) and a Transmission Electron Microscope (TEM).
The process for preparing the Ni-Mo/diamond composite coating which has low hardness and high wear resistance and corrosion resistance comprises the following steps:
(1) Firstly, sand paper is sequentially carried out on the surface of a sample to be ground into 800 meshes and 200 meshes of glass shots for shot blasting, acetone is used for removing oil, alcohol is used for removing impurities, diluted hydrochloric acid is used for activating, and a Ni layer is preplated. The composition of the pre-plating solution (watt solution) is as follows: 240-250 g/L of nickel sulfate, 35-50 g/L of nickel chloride, 35-40 g/L of boric acid, 0.4-0.6 g/L of saccharin sodium, 0.1-0.2 g/L of sodium dodecyl sulfate and the balance of water. The technological parameters of preplating are as follows: sample as cathode, pure Ni plate as anode with 3cm of pole distance and 2-4A/dm of current density 2 pH 4.4-4.8 (diluted H with 20 vol.%) 2 SO 4 Solution conditioning), the temperature is room temperature, and the electroplating time is 5-10 min. And after preplating, washing with deionized water and drying.
(2) And depositing the Ni-Mo/diamond composite coating by adopting a composite electroplating technology. The electroplating solution comprises the following components: 60-80 g/L of nickel sulfate, 60-80 g/L of sodium citrate, 4g/L of sodium molybdate, 0.4-0.6 g/L of saccharin sodium, 0.1-0.2 g/L of sodium dodecyl sulfate, 120g/L of diamond particles and the balance of water; the parameters of the electroplating process are as follows: the pH value of the electroplating solution is 8.5-9.5, the temperature of the solution during electroplating is 30-35 ℃, the stirring speed is 70-90 rpm, and the current density is 3A/dm 2 The electroplating time is 2h.
(3) After the electrodeposition is finished, cleaning and drying by ultrasonic alcohol, and then carrying out high-temperature vacuum annealing treatment at 730-765 ℃ for 1-2 h.
Example 1:
(1) Sample surface pretreatment: polishing a stainless steel sample piece to 800-mesh SiC sand paper, performing shot blasting treatment by 200-mesh glass shots, performing ultrasonic cleaning and impurity removal by using alcohol and ultrasonic cleaning and oil removal by using acetone for 5min respectively, and finally soaking in 20vol.% HCl solution for 45s for surface activation.
(2) Pre-plating a Ni layer: directly putting the pretreated sample into watt liquid for Ni electroplating treatment, wherein the adopted process parameters are as follows: current density 3A/dm 2 The pH value is 4.4-4.8, the temperature is room temperature, and the electroplating time is 5min. And after preplating, washing with deionized water and drying.
(3) Composite electrodeposition Ni-Mo/diamond composite coating: the preplated sample is washed by deionized water and then is put into a composite electroplating solution, and the components of the electroplating solution are as follows: 60g/L of nickel sulfate, 80g/L of sodium citrate, 4g/L of sodium molybdate, 0.6g/L of saccharin sodium, 0.2g/L of sodium dodecyl sulfate, 120g/L of diamond particles and the balance of water; the selected electroplating process comprises the following steps: the pH value of the electroplating solution is 9, the temperature of the solution during electroplating is 35 ℃, and the current density is 3A/dm 2 The stirring speed was 80rpm and the plating time was 2 hours. The preparation process of the composite electroplating solution comprises the following steps: adding deionized water into a beaker, and respectively adding nickel sulfate, sodium citrate and molybdic acidSodium, sodium dodecyl sulfate and saccharin sodium, and adjusting the pH value by using an ammonia water solution after the medicine in the solution is completely dissolved. And then adding the micron diamond particles into the solution after the pH value is adjusted, firstly magnetically stirring for 30min, and then ultrasonically dispersing for 30min. And immediately carrying out the composite electrodeposition experiment after the ultrasonic dispersion is finished.
(4) After the electroplating experiment is finished, part of the sample is sealed in a vacuum quartz tube for annealing treatment, and the vacuum degree is 10 2 Pa, temperature of 600 ℃ and 750 ℃, heat preservation time of 1h, heating rate of 10 ℃/min, and furnace cooling after the heat preservation stage is finished.
In the prepared composite coating, the content of Mo in the Ni-Mo alloy matrix is 18at.%, and the balance is Ni; the volume fraction of diamond particles in the composite coating is about 21vol.%.
The microscopic scanning topography of the composite coating is shown in fig. 1. As can be seen from the figure, the surface of the composite coating presents obvious cauliflower-like appearance, and the diamond particles are uniformly and densely distributed in the matrix metal. The heat treatment temperature has little influence on the appearance of the coating.
The XRD pattern of the composite coating is shown in fig. 2, and it can be seen from fig. 2 that the as-deposited coating shows a distinct preferential growth phenomenon, in which the diffraction peak at 43.9 ° in the XRD pattern corresponds to the Ni (111) and diamond (111) diffraction crystal planes, the diffraction peak at 50.7 ° corresponds to the Ni (200) diffraction crystal plane, and the diffraction peak at 75.5 ° corresponds to the Ni (220) and diamond (220) diffraction crystal planes. The grain size of the coating is calculated to be 7nm by the full width at half maximum of the (111) diffraction peak and the diffraction angle by utilizing the Sherrer formula. No diffraction peak related to Mo element was observed in the coating, indicating that the Ni — Mo matrix metal is a supersaturated Ni (Mo) solid solution. After the heat treatment at 600 ℃, the intensity of the diffraction peak of Ni (111) is increased, which shows that the crystal grains grow to a certain degree, and the size of the crystal grains is about 17.1nm through calculation. Meanwhile, a new diffraction peak appears on XRD and is positioned at 40.8 degrees, and the diffraction peak is found by comparing with a standard XRD diffraction pattern library to correspond to the (041) crystal face of the MoNi phase. This indicates that a MoNi precipitate phase precipitates in the Ni (Mo) solid solution. When the heat treatment temperature reaches 750 ℃, the alloy is mixed with Mo 2 The new diffraction peak corresponding to C is detectedAnd (4) obtaining. This indicates that at this temperature, the diamond particles in the coating graphitized and reacted with Mo to form Mo 2 C, precipitating phase. MoNi and Mo were counted by TEM observation 2 The size of the C precipitation phase is about 200 nm.
The TEM diffraction spectrum of the diamond particles of the composite coating after heat treatment at 750 ℃ is shown in FIG. 3. It can be seen from fig. 3 that the diamond particles maintained the structure of diamond, and this result indicates that the graphitization process of the diamond particles was not completely performed. Incomplete graphitization of the diamond occurs due to the large size of the co-deposited particles and the short heat treatment time.
After the composite coating is ground by using 2000-mesh sand paper and polished by using 1.5-micron diamond, the load of 0.49N is adopted, the pressure is maintained for 15s, the size of an indentation is measured, and the hardness of the coating is calculated to be 4. The micro Vickers hardness of the coating in a deposition state is 6.6GPa, and the micro Vickers hardness of the coating after heat treatment at 600 ℃ and 750 ℃ is 9.7GPa and 6.2GPa respectively. The hardness of the composite coating after 600 ℃ heat treatment is improved mainly due to the fact that Mo element diffuses to a grain boundary and stabilizes the grain boundary in the heat treatment process. When the temperature reaches 750 ℃, the main reasons for the hardness reduction of the coating are the growth of Ni-Mo matrix grains and MoNi phase grains and the graphitization of diamond.
Plating a single-sided Ni-Mo/diamond composite coating on stainless steel, and carrying out heat treatment on part of samples. The bonding force between the coating and the substrate in the deposition state is 65MPa measured by adopting a tensile test method, and the bonding force is 56MPa and 57MPa respectively after heat treatment at 600 ℃ and 750 ℃. This indicates that both the as-deposited composite coating and the heat treated composite coating have good adhesion, and the heat treatment temperature has less effect on the adhesion.
Grinding and polishing the composite coating, and determining the wear resistance of the coating by adopting a rotary ball disc type experimental method, wherein the determination parameters are as follows: opposite grinding pair
Al 2 O 3 The ball was subjected to an experiment in an atmospheric environment at a load of 1.96N, a rotation speed of 200rpm, a rotation radius of 3mm and a wear time of 2 hours. The sample after the experiment is subjected to wear surface through a step instrumentThe product was measured and the average friction coefficient and wear rate were finally calculated as shown in fig. 5. The as-deposited coatings had average coefficients of friction and wear rates of 0.77 and 6.98X 10, respectively -5 mm 3 and/mN. After heat treatment at 600 ℃, the average friction coefficient and the wear rate of the coating are slightly reduced to 0.72 and 4.5 multiplied by 10 respectively -5 mm 3 and/mN. Their reduction is mainly due to the increase in the hardness of the coating. After the heat treatment at 750 ℃, the average friction coefficient and the wear rate of the coating are greatly reduced and are respectively 0.65 and 3.37 multiplied by 10 -6 mm 3 mN, the wear rate is 1/20 of that of the sediment state. The abraded surface of the grinding mark is observed to have a large number of grooves which are formed by the diamond particles falling off from the coating, and the number of the grooves is larger than that of the coating under the other two conditions. This indicates that the diamond particles in the coating still act as a reinforcing phase after a heat treatment at 750 ℃. However, this decrease in wear resistance is mainly due to Mo in view of the large decrease in coating hardness 2 Lubrication of C.
The polarization curve of the composite coating in a 3.5wt.% NaCl solution is shown in fig. 6. It can be seen from the figure that as the heat treatment temperature increases, the corrosion potential of the coating moves toward the positive potential, and the corrosion current becomes smaller. This indicates that the corrosion resistance of the coating increases with increasing heat treatment temperature. The results show that MoNi and Mo 2 The presence of phase C is beneficial to improving the corrosion resistance of the coating.
The example results show that the method for inducing the phase change of the coating through heat treatment successfully improves the wear resistance and the corrosion resistance of the Ni-Mo/diamond composite coating, and meanwhile, the composite coating has excellent bonding strength. The result shows that the Ni-Mo/diamond composite coating can be applied to a large number of mechanical parts bearing the friction and wear effects in the corrosion and other environments in the industries of chemical engineering, metallurgy, electric power, petroleum and the like.
Claims (8)
1. A high wear-resistant and corrosion-resistant Ni-Mo/diamond composite coating based on phase change is characterized in that: the composite coating is formed by uniformly distributing diamond particles in Ni-Mo alloy; the content of Mo in the Ni-Mo alloy is 17-19 at.%, and the balance is Ni; the addition amount of the diamond particles in the composite coating is 18-21 vol%; the Ni-Mo alloy comprises Ni (Mo) solid solution, a precipitation phase MoNi and a strengthening phase Mo2C.
2. The phase-transition based high wear and corrosion resistant Ni-Mo/diamond composite coating according to claim 1, characterized in that: the Ni (Mo) solid solution is nanocrystalline, and the grain size of the Ni (Mo) solid solution is within the range of 17-64 nm.
3. The phase-transition based high wear and corrosion resistant Ni-Mo/diamond composite coating according to claim 1, characterized in that: the grain sizes of the precipitation phase MoNi and the strengthening phase Mo2C are 63-245 nm.
4. The high wear and corrosion resistant Ni-Mo/diamond composite coating based on phase change according to claim 1, characterized in that: the particle size of the diamond particles is 0.7-1 μm.
5. The phase-transition based high wear and corrosion resistant Ni-Mo/diamond composite coating according to claim 1, characterized in that: the composite coating is prepared on a stainless steel substrate, the microhardness of the composite coating is 6.2GPa, the coating/substrate binding force reaches more than 55MPa, and the wear rate is as low as 3.37 multiplied by 10 < -6 > mm < 3 >/mN.
6. The high wear and corrosion resistant Ni-Mo/diamond composite coating based on phase change according to claim 1, characterized in that: the corrosion current density of the composite coating in a 3.5wt.% NaCl solution is 1.85 muA cm-2.
7. The method for preparing the high wear and corrosion resistant Ni-Mo/diamond composite coating based on phase change according to claim 1, wherein: the method comprises the steps of firstly preparing a Ni-Mo/diamond composite coating on a stainless steel substrate by adopting a composite electroplating technology, carrying out high-temperature heat treatment on the coating, and carrying out vacuum annealing at the high temperature of 730-765 ℃ for 1-2 h to obtain the high-wear-resistance and corrosion-resistance Ni-Mo/diamond composite coating based on phase change.
8. The method for preparing the high wear and corrosion resistant Ni-Mo/diamond composite coating based on phase transition as claimed in claim 7, wherein: after the composite coating is subjected to high-temperature heat treatment for 1-2 h at 730-765 ℃ which exceeds the graphitization temperature of the diamond, incomplete graphitization is generated on the diamond particles.
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