Industrially applied materials are often selected based on strength requirements, but surface properties such as abrasion resistance, corrosion resistance, scratch resistance, and electrical conductivity are not necessarily satisfactory. Therefore, different coatings need to be selected to meet the surface performance requirements. The preparation of the coating can be achieved by mechanical plating, triboelectric plating, flow plating, laser plating, immersion plating, electrophoretic coating, composite plating and the like. In recent years, the high-speed development of composite coatings has become a newcomer of composite materials with its unique physical, chemical and mechanical properties, and has received extensive attention and has been recognized as a production technology. The composite plating is a special plating formed by uniformly intercalating one or several insoluble solid particles and fibers into a metal plating layer by metal electrodeposition or co-deposition. A super-hard material is used as a dispersed particle, and a composite plating layer formed of a metal is called a super-hard material composite plating layer. The diamond composite coating described in this paper belongs to this category. The preparation methods of the diamond composite coating mainly include chemical composite plating and composite electrodeposition.
Co-deposition mechanism of diamond particles and metal ions
The diamond particles added in the composite plating bath have strong chemical stability, and it does not participate in any chemical reaction during the plating process, but only the metal ions generated by the chemical (electrochemical) reaction are co-deposited on the surface of the substrate. Therefore, both electroless plating and electrodeposited composite coatings can be explained by the same mechanism. In the study of composite electroplating co-deposition, three co-deposition mechanisms have been proposed, namely mechanical co-deposition, electrophoretic co-deposition and adsorption co-deposition. Currently recognized as the two-stage adsorption theory proposed by N. Guglielmi in 1972. The model proposed by Gugliemi believes that the surface of the particles in the plating solution is surrounded by ions. After reaching the surface of the cathode, it is first loosely adsorbed (weakly adsorbed) on the surface of the cathode. This is a physical adsorption and is a reversible process. Secondly, as the electrode reaction proceeds, a part of the ions weakly adsorbed on the surface of the particles are reduced, and the particles are strongly adsorbed with the cathode. This is an irreversible process, and the particles gradually enter the surface of the cathode, and then the deposited metal is buried.
The mathematical treatment of the weak adsorption step of the model is in the form of Langmuir adsorption isotherm. For the strong adsorption step, it is considered that the strong adsorption rate of the particles is related to the coverage of the weak adsorption and the electric field at the interface of the electrode and the solution. Wang Lin et al. studied the co-deposition process of wear-resistant nickel-diamond composite coating. The surface: nickel-nickel co-deposition mechanism accords with Guglielmi's two-step adsorption model, and the speed control step is a strong adsorption step. So far, composite electrodeposition is the same as other new technologies and processes, and practice is far ahead of the theory. The research of its mechanism is constantly developing.
Preparation and application of diamond composite coating
2.1 Chemical composite diamond plating
Electroless plating is a metal deposition process by controlled chemical reduction under the catalysis of a metal surface without applying an electric current. A composite coating is obtained by adding insoluble particles to the plating solution to co-deposit with the metal. Chemical composite plating requires no power supply and auxiliary anode. It is not affected by the shape of the base material. It can be uniformly deposited in various parts of the material. The coating has high density and hardness, as well as self-lubricity, heat resistance, corrosion resistance and special decoration. It has a wide range of applications in aviation, machinery, chemical, metallurgical and nuclear industries. The properties of the composite electroless nickel plating vary with the type of particles selected. There are many types of diamonds, which can be roughly divided into two categories: single crystal and polycrystalline. The type of diamond selected for the preparation of the composite depends on the end use of the composite. Single crystal diamond is suitable for grinding and grinding because of its surface features with sharp corners.
Diamond crucibles and grinding wheels are used as composite surfaces, and natural single crystal diamonds are easy to use. The wear-resistant composite material cannot contain single crystal diamond, and the rough surface is easy to wear the mating surface, and the artificial polycrystalline diamond is generally used in the explosion method. Electroless nickel-polycrystalline diamond composites have good surface protection and scratch resistance. The thin layer of electroless nickel-diamond as the intermediate layer can improve the corrosion resistance of nickel-chromium plating deposits. It is one of the earliest electroless plating composite materials, and this coating is now mainly used for anti-wear. Table 1 shows the results of the wear resistance of the diamond coating by the Taber test machine [6], which is four times higher than that of the comparative sample, and is also superior to tool steel and cemented carbide.
Many scholars in China have studied the electroless plating of diamond composite coatings. Wu Yucheng et al [7] showed that the addition of diamond particles (average size 14μm) in the nickel-phosphorus alloy deposition solution can significantly enhance the coating and improve the wear resistance. Wang Zheng et al [8] research shows that in addition to high hardness and good wear resistance, diamond composite coating also has excellent thermal conductivity and corrosion resistance, so it can greatly improve the service life of casting molds and cold working molds. Zhang Xinyi and other studies have shown that the effect of heat treatment on the structure and properties of Ni P diamond (<1μm) chemical composite coating shows that the composite coating has amorphous characteristics in the plated state, and the coating begins to crystallize at 300 ° C, at 200 ° C ~ 400 The °C coating has good wear resistance.
2.2 Composite electroplated diamond
The diamond is deposited in a metal plating layer by electroplating to obtain a diamond composite plating layer. In practical work, the metal coating acts as a binder and diamond plays a major role. China's diamond electroplated products were developed in the 1960s along with resin binders and bronze bond diamond abrasives. Later, various non-grinding tools were gradually developed. A relatively mature process has been formed. Diamond electroplating products are now widely used in the mechanical processing industry, electrical and electronic industry, optical glass industry, geological drilling industry, construction industry, arts and crafts and daily necessities. Play an irreplaceable role. The application of electroplated diamond composite coatings in new fields is also a hot topic.
Researches in Jinku and other studies have shown that the composite brush-plated diamond manufacturing process is simple, and the obtained coating has good hardness and wear resistance, and has broad industrial application prospects. Yu Hunkun et al. studied the properties of silver-based diamond composite coatings. The research shows that the higher the diamond content in the composite coating, the smaller the particle size, the smaller the wear rate, and the more obvious the contact current, thus improving the contact. The life of the head and its ability to withstand large contact currents. Li Yundong et al. proposed a new type of coated nickel-cobalt-manganese ternary alloy coating that can be well adapted to the requirements of electroplated diamond tools. The results show that the nickel-cobalt-manganese ternary alloy coating has higher comprehensive mechanical properties and much lower cobalt content than nickel-cobalt or nickel-manganese coating, and is more suitable for manufacturing electroplated diamond tools. It is a promising replacement replacement. Plating. Wang Wei et al. proposed a new method for forcibly honing the hard tooth surface with a diamond-coated worm wheel on the hobbing machine for the problems in the machining methods such as scraping and grinding in the hard tooth surface gear processing. The results show that the tool surface quality is good and the processing efficiency is high. Zhou Zhenjun and Others applied diamond composite plating to flexible abrasive tools. The results show that the composite coating improves the life and grinding efficiency of the abrasive. In addition, high-hardness gradient functional materials such as Ni diamond and Co diamond manufactured by composite plating have been successfully applied in the aerospace industry.
2.3 composite plating nano diamond
Most of the diamonds added in the early stage of composite plating are micron-sized. With the deepening of research on nanomaterials and nanotechnology, the introduction of nanoscale diamond particles into composite coatings has become a new trend in the development of composite plating. Nanodiamonds have the general properties of ultrafine particles such as volumetric effects, surface effects, and small-scale quantum effects. At the same time, it also has the general properties of diamond, such as high hardness, high thermal conductivity, high modulus of elasticity, high wear resistance, low specific heat capacity and excellent chemical stability. In recent years, Russia and Western countries have been competing to research and develop nano-diamond industrial products, and have been widely used in the fields of composite plating, grinding, polishing, lubrication, high-strength resin and rubber. There are also many units in China that are engaged in this research. Nano-diamond combines the dual properties of superhard materials and nanoparticles. With anti-wear and self-lubricating properties, it has a wide range of applications in tooling, grinding, composite plating, lubrication, and friction. Especially for precision instruments, high-gloss surface precision machining tools, nano-diamonds have properties unmatched by other materials.
In addition, nanocomposite plating is also promising in electrical contact materials. Wu Yuankang and others use nano-diamond particles to enhance the silver-based coating, reduce the electric wear rate, and improve the service life of the electrical contacts and the ability to withstand high current strength. Domestic research in this field is still in its infancy. Accelerate research in this area and put it into use as soon as possible, both for national defense and civilian use. The main problems in the current research are:
(1) Dispersion of nanodiamond in the plating solution. Nanoscale diamond powder is now mainly produced by an explosion method. The average particle diameter is 4 to 10 nm. Composite plating requires that the diamond powder be uniformly dispersed in the plating solution. According to the definition of the colloidal dispersion system (radius is 10 9 to 10-7 m), the plating solution should be a colloidal dispersion system. The structure of the micelle in the sol is complicated, from the true solution to the sol, which is an ultra-fine heterogeneous phase with a phase interface from the homogeneous phase, and because the particles of the dispersed phase are small, the surface area is large, and the surface energy is also high, which makes The colloidal particles are in an unstable state, and they have a tendency to agglomerate and become larger particles to coagulate. Experiments show that the agglomeration of the plating solution doped with diamond micropowder is serious, and the agglomeration of nano-scale diamond powder is also serious in the obtained coating, which greatly affects the application of nano-diamond powder in practice.
(2) Selection of dispersant and dispersion method. Because nano-diamond powder is prone to particle agglomeration in the plating solution, it affects its practical application effect. Therefore, it is particularly important to disperse the powder in a medium (plating solution) to obtain a high stability, and a low viscosity suspension. Some agglomeration of diamond in the plating solution is caused by physical bonding (such as van der Waals force), called soft agglomeration; some are agglomeration caused by chemical bonding (such as hydrogen bonding), called hard agglomeration. There are various ways to open soft agglomeration, such as mechanical stirring, magnetic stirring, gas agitation, and ultrasonic dispersion. For hard agglomeration, in addition to the above methods, special treatment must be performed for their bonding type. To solve the problem of dispersion of nano-diamond powder in the plating solution, the most effective method is to surface-modify the surface of the powder. The selection of surfactants and the design of the dispersion method are particularly important. The available data indicate that anionic surfactants (such as sodium lauryl sulfate) can better increase the content of nanodiamond powder in the coating. But the effect is not satisfactory. In order to improve the content of nano-diamond in the composite coating, it is still necessary to further study different plating processes and explore effective surfactants.
Plated composite nano-diamond technology
1. Plating composite nano-diamond technology
The plated composite nano-diamond technology is the latest process for strengthening the surface of metal workpieces under normal temperature conditions, which can significantly improve the microhardness of the coating, improve the permeability and compactness of the nano-diamond in the coating, and enhance the wear resistance of the workpiece, and the method There is no special requirement for the workpiece to be machined, no adverse effect on the workpiece, and a wide application range. The plated composite nano-diamond technology can be widely used in machined cutting tool measuring tools, molds, bearings, cylinder liners, as well as magnetic disks and electronic connectors. It is suitable for strengthening metals in various industries such as machinery, electronics, automobile, petroleum, exploration and medical, military and so on. The requirements of the surface of the workpiece.
2, technical indicators
1. Appearance dark gray water suspension 2, carbon content ≥ 86.2% 3. Suspension pH value 5 4, ash content ≤ 2.5% 5. Average size 4-6 nm 6. Specific surface area 300±30 m2/g
3, adding methods
The plated composite nano-diamond technology can be realized on the standard chrome-plating process equipment according to the common process parameters: the nano-diamond aqueous suspension is added to the electrolyte in a certain proportion, and in order to ensure uniform dispersion, the entire electroless plating process needs to be ultrasonicated. Disperse, simultaneously magnetic or mechanical agitation, so that the diamond powder is uniformly suspended in the plating solution, and then added to the production plating tank and stirred uniformly, then the composite electroplating production can be performed. The nano-diamonds carried out with the workpiece during the electroplating production process can be precipitated in the recovery tank for recycling.
4, product performance
- high microhardness up to Hv 1000-1400;
- 3-5 times increase in wear resistance - 1.5-4 times increase in service life;
- the adhesion of the coating to the substrate is increased by 30-40%;
- strong coverage, uniform, smooth and detailed coating;
5. Economic benefits
1), reduce the thickness of chrome plating, save chromic anhydride 2), reduce power consumption 3), high current efficiency, fast deposition rate 4), improve yield
6, the proportion of use
The concentration of nanodiamond in the electrolyte is 5-20 kg/m3
1 m2 of coating with a thickness of 1 μm consumes 0.1 g of diamond. 1 kg of diamond can produce a coating area of ​​5-10 μm thickness of 1000-2000 m2.
Conclusion
Diamond composite coatings have been developed to date and have made great progress and have been widely used in many fields. As the research deepens, it is believed that more progress will be made to meet the needs of industrial development.
Co-deposition mechanism of diamond particles and metal ions
The diamond particles added in the composite plating bath have strong chemical stability, and it does not participate in any chemical reaction during the plating process, but only the metal ions generated by the chemical (electrochemical) reaction are co-deposited on the surface of the substrate. Therefore, both electroless plating and electrodeposited composite coatings can be explained by the same mechanism. In the study of composite electroplating co-deposition, three co-deposition mechanisms have been proposed, namely mechanical co-deposition, electrophoretic co-deposition and adsorption co-deposition. Currently recognized as the two-stage adsorption theory proposed by N. Guglielmi in 1972. The model proposed by Gugliemi believes that the surface of the particles in the plating solution is surrounded by ions. After reaching the surface of the cathode, it is first loosely adsorbed (weakly adsorbed) on the surface of the cathode. This is a physical adsorption and is a reversible process. Secondly, as the electrode reaction proceeds, a part of the ions weakly adsorbed on the surface of the particles are reduced, and the particles are strongly adsorbed with the cathode. This is an irreversible process, and the particles gradually enter the surface of the cathode, and then the deposited metal is buried.
The mathematical treatment of the weak adsorption step of the model is in the form of Langmuir adsorption isotherm. For the strong adsorption step, it is considered that the strong adsorption rate of the particles is related to the coverage of the weak adsorption and the electric field at the interface of the electrode and the solution. Wang Lin et al. studied the co-deposition process of wear-resistant nickel-diamond composite coating. The surface: nickel-nickel co-deposition mechanism accords with Guglielmi's two-step adsorption model, and the speed control step is a strong adsorption step. So far, composite electrodeposition is the same as other new technologies and processes, and practice is far ahead of the theory. The research of its mechanism is constantly developing.
Preparation and application of diamond composite coating
2.1 Chemical composite diamond plating
Electroless plating is a metal deposition process by controlled chemical reduction under the catalysis of a metal surface without applying an electric current. A composite coating is obtained by adding insoluble particles to the plating solution to co-deposit with the metal. Chemical composite plating requires no power supply and auxiliary anode. It is not affected by the shape of the base material. It can be uniformly deposited in various parts of the material. The coating has high density and hardness, as well as self-lubricity, heat resistance, corrosion resistance and special decoration. It has a wide range of applications in aviation, machinery, chemical, metallurgical and nuclear industries. The properties of the composite electroless nickel plating vary with the type of particles selected. There are many types of diamonds, which can be roughly divided into two categories: single crystal and polycrystalline. The type of diamond selected for the preparation of the composite depends on the end use of the composite. Single crystal diamond is suitable for grinding and grinding because of its surface features with sharp corners.
Diamond crucibles and grinding wheels are used as composite surfaces, and natural single crystal diamonds are easy to use. The wear-resistant composite material cannot contain single crystal diamond, and the rough surface is easy to wear the mating surface, and the artificial polycrystalline diamond is generally used in the explosion method. Electroless nickel-polycrystalline diamond composites have good surface protection and scratch resistance. The thin layer of electroless nickel-diamond as the intermediate layer can improve the corrosion resistance of nickel-chromium plating deposits. It is one of the earliest electroless plating composite materials, and this coating is now mainly used for anti-wear. Table 1 shows the results of the wear resistance of the diamond coating by the Taber test machine [6], which is four times higher than that of the comparative sample, and is also superior to tool steel and cemented carbide.
Many scholars in China have studied the electroless plating of diamond composite coatings. Wu Yucheng et al [7] showed that the addition of diamond particles (average size 14μm) in the nickel-phosphorus alloy deposition solution can significantly enhance the coating and improve the wear resistance. Wang Zheng et al [8] research shows that in addition to high hardness and good wear resistance, diamond composite coating also has excellent thermal conductivity and corrosion resistance, so it can greatly improve the service life of casting molds and cold working molds. Zhang Xinyi and other studies have shown that the effect of heat treatment on the structure and properties of Ni P diamond (<1μm) chemical composite coating shows that the composite coating has amorphous characteristics in the plated state, and the coating begins to crystallize at 300 ° C, at 200 ° C ~ 400 The °C coating has good wear resistance.
2.2 Composite electroplated diamond
The diamond is deposited in a metal plating layer by electroplating to obtain a diamond composite plating layer. In practical work, the metal coating acts as a binder and diamond plays a major role. China's diamond electroplated products were developed in the 1960s along with resin binders and bronze bond diamond abrasives. Later, various non-grinding tools were gradually developed. A relatively mature process has been formed. Diamond electroplating products are now widely used in the mechanical processing industry, electrical and electronic industry, optical glass industry, geological drilling industry, construction industry, arts and crafts and daily necessities. Play an irreplaceable role. The application of electroplated diamond composite coatings in new fields is also a hot topic.
Researches in Jinku and other studies have shown that the composite brush-plated diamond manufacturing process is simple, and the obtained coating has good hardness and wear resistance, and has broad industrial application prospects. Yu Hunkun et al. studied the properties of silver-based diamond composite coatings. The research shows that the higher the diamond content in the composite coating, the smaller the particle size, the smaller the wear rate, and the more obvious the contact current, thus improving the contact. The life of the head and its ability to withstand large contact currents. Li Yundong et al. proposed a new type of coated nickel-cobalt-manganese ternary alloy coating that can be well adapted to the requirements of electroplated diamond tools. The results show that the nickel-cobalt-manganese ternary alloy coating has higher comprehensive mechanical properties and much lower cobalt content than nickel-cobalt or nickel-manganese coating, and is more suitable for manufacturing electroplated diamond tools. It is a promising replacement replacement. Plating. Wang Wei et al. proposed a new method for forcibly honing the hard tooth surface with a diamond-coated worm wheel on the hobbing machine for the problems in the machining methods such as scraping and grinding in the hard tooth surface gear processing. The results show that the tool surface quality is good and the processing efficiency is high. Zhou Zhenjun and Others applied diamond composite plating to flexible abrasive tools. The results show that the composite coating improves the life and grinding efficiency of the abrasive. In addition, high-hardness gradient functional materials such as Ni diamond and Co diamond manufactured by composite plating have been successfully applied in the aerospace industry.
2.3 composite plating nano diamond
Most of the diamonds added in the early stage of composite plating are micron-sized. With the deepening of research on nanomaterials and nanotechnology, the introduction of nanoscale diamond particles into composite coatings has become a new trend in the development of composite plating. Nanodiamonds have the general properties of ultrafine particles such as volumetric effects, surface effects, and small-scale quantum effects. At the same time, it also has the general properties of diamond, such as high hardness, high thermal conductivity, high modulus of elasticity, high wear resistance, low specific heat capacity and excellent chemical stability. In recent years, Russia and Western countries have been competing to research and develop nano-diamond industrial products, and have been widely used in the fields of composite plating, grinding, polishing, lubrication, high-strength resin and rubber. There are also many units in China that are engaged in this research. Nano-diamond combines the dual properties of superhard materials and nanoparticles. With anti-wear and self-lubricating properties, it has a wide range of applications in tooling, grinding, composite plating, lubrication, and friction. Especially for precision instruments, high-gloss surface precision machining tools, nano-diamonds have properties unmatched by other materials.
In addition, nanocomposite plating is also promising in electrical contact materials. Wu Yuankang and others use nano-diamond particles to enhance the silver-based coating, reduce the electric wear rate, and improve the service life of the electrical contacts and the ability to withstand high current strength. Domestic research in this field is still in its infancy. Accelerate research in this area and put it into use as soon as possible, both for national defense and civilian use. The main problems in the current research are:
(1) Dispersion of nanodiamond in the plating solution. Nanoscale diamond powder is now mainly produced by an explosion method. The average particle diameter is 4 to 10 nm. Composite plating requires that the diamond powder be uniformly dispersed in the plating solution. According to the definition of the colloidal dispersion system (radius is 10 9 to 10-7 m), the plating solution should be a colloidal dispersion system. The structure of the micelle in the sol is complicated, from the true solution to the sol, which is an ultra-fine heterogeneous phase with a phase interface from the homogeneous phase, and because the particles of the dispersed phase are small, the surface area is large, and the surface energy is also high, which makes The colloidal particles are in an unstable state, and they have a tendency to agglomerate and become larger particles to coagulate. Experiments show that the agglomeration of the plating solution doped with diamond micropowder is serious, and the agglomeration of nano-scale diamond powder is also serious in the obtained coating, which greatly affects the application of nano-diamond powder in practice.
(2) Selection of dispersant and dispersion method. Because nano-diamond powder is prone to particle agglomeration in the plating solution, it affects its practical application effect. Therefore, it is particularly important to disperse the powder in a medium (plating solution) to obtain a high stability, and a low viscosity suspension. Some agglomeration of diamond in the plating solution is caused by physical bonding (such as van der Waals force), called soft agglomeration; some are agglomeration caused by chemical bonding (such as hydrogen bonding), called hard agglomeration. There are various ways to open soft agglomeration, such as mechanical stirring, magnetic stirring, gas agitation, and ultrasonic dispersion. For hard agglomeration, in addition to the above methods, special treatment must be performed for their bonding type. To solve the problem of dispersion of nano-diamond powder in the plating solution, the most effective method is to surface-modify the surface of the powder. The selection of surfactants and the design of the dispersion method are particularly important. The available data indicate that anionic surfactants (such as sodium lauryl sulfate) can better increase the content of nanodiamond powder in the coating. But the effect is not satisfactory. In order to improve the content of nano-diamond in the composite coating, it is still necessary to further study different plating processes and explore effective surfactants.
Plated composite nano-diamond technology
1. Plating composite nano-diamond technology
The plated composite nano-diamond technology is the latest process for strengthening the surface of metal workpieces under normal temperature conditions, which can significantly improve the microhardness of the coating, improve the permeability and compactness of the nano-diamond in the coating, and enhance the wear resistance of the workpiece, and the method There is no special requirement for the workpiece to be machined, no adverse effect on the workpiece, and a wide application range. The plated composite nano-diamond technology can be widely used in machined cutting tool measuring tools, molds, bearings, cylinder liners, as well as magnetic disks and electronic connectors. It is suitable for strengthening metals in various industries such as machinery, electronics, automobile, petroleum, exploration and medical, military and so on. The requirements of the surface of the workpiece.
2, technical indicators
1. Appearance dark gray water suspension 2, carbon content ≥ 86.2% 3. Suspension pH value 5 4, ash content ≤ 2.5% 5. Average size 4-6 nm 6. Specific surface area 300±30 m2/g
3, adding methods
The plated composite nano-diamond technology can be realized on the standard chrome-plating process equipment according to the common process parameters: the nano-diamond aqueous suspension is added to the electrolyte in a certain proportion, and in order to ensure uniform dispersion, the entire electroless plating process needs to be ultrasonicated. Disperse, simultaneously magnetic or mechanical agitation, so that the diamond powder is uniformly suspended in the plating solution, and then added to the production plating tank and stirred uniformly, then the composite electroplating production can be performed. The nano-diamonds carried out with the workpiece during the electroplating production process can be precipitated in the recovery tank for recycling.
4, product performance
- high microhardness up to Hv 1000-1400;
- 3-5 times increase in wear resistance - 1.5-4 times increase in service life;
- the adhesion of the coating to the substrate is increased by 30-40%;
- strong coverage, uniform, smooth and detailed coating;
5. Economic benefits
1), reduce the thickness of chrome plating, save chromic anhydride 2), reduce power consumption 3), high current efficiency, fast deposition rate 4), improve yield
6, the proportion of use
The concentration of nanodiamond in the electrolyte is 5-20 kg/m3
1 m2 of coating with a thickness of 1 μm consumes 0.1 g of diamond. 1 kg of diamond can produce a coating area of ​​5-10 μm thickness of 1000-2000 m2.
Conclusion
Diamond composite coatings have been developed to date and have made great progress and have been widely used in many fields. As the research deepens, it is believed that more progress will be made to meet the needs of industrial development.
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