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CN119506823A - Porous diamond coating and preparation method and application thereof - Google Patents

Porous diamond coating and preparation method and application thereof Download PDF

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Publication number
CN119506823A
CN119506823A CN202311068812.5A CN202311068812A CN119506823A CN 119506823 A CN119506823 A CN 119506823A CN 202311068812 A CN202311068812 A CN 202311068812A CN 119506823 A CN119506823 A CN 119506823A
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China
Prior art keywords
diamond
silicon carbide
coating
intermediate layer
porous
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CN202311068812.5A
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Chinese (zh)
Inventor
王陶
周双庆
唐永炳
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Shenzhen Institute of Advanced Technology of CAS
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Shenzhen Institute of Advanced Technology of CAS
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Priority to CN202311068812.5A priority Critical patent/CN119506823A/en
Priority to PCT/CN2023/137580 priority patent/WO2025039418A1/en
Publication of CN119506823A publication Critical patent/CN119506823A/en
Pending legal-status Critical Current

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    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/02—Pretreatment of the material to be coated
    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26—Deposition of carbon only
    • C23C16/27—Diamond only
    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/32—Carbides
    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/52—Controlling or regulating the coating process

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Polishing Bodies And Polishing Tools (AREA)

Abstract

The invention provides a porous diamond coating, a preparation method and application thereof. The porous diamond coating comprises a metal matrix, wherein a silicon carbide composite intermediate layer is arranged on the surface of the metal matrix, mutually dispersed diamond grains are inlaid in the silicon carbide composite intermediate layer, gaps and a porous structure are formed among the dispersed diamond grains, and the porous diamond coating has the effect of preventing abrasive dust from being blocked. The porous diamond coating provided by the invention is good in processing quality, high in processing precision, low in wear rate and long in service life when being used for a cutter. In addition, the porous diamond coating is not limited by the shape of the tool, can realize rapid and controllable deposition on a miniature precision tool with any complex shape, and has the advantages of wide application range, high precision, low cost and the like. The invention also provides a preparation method and application of the porous diamond coating.

Description

Porous diamond coating and preparation method and application thereof
Technical Field
The invention belongs to the technical field of precision machining, and particularly relates to a porous diamond coating, a preparation method and application thereof.
Background
With the development of aerospace, microelectromechanical systems, microelectronics, medical devices, automobiles, and communications industries, there is an increasing demand for miniaturized high-precision parts, such as micro channels on microfluidic chips, micro heat converters, micro sensors, micro gyroscopes in navigation systems for aircraft and guided weapons, and the like. Most of the key core components of miniature are semiconductors, ceramic materials such as single crystal silicon for microprocessors and electrodes, quartz for susceptors and wafer carriers, silicon carbide for 5G rf chips, gallium nitride, silicon carbide, etc. These materials are typically difficult to process because of their high hardness, high brittleness, and very easy cleavage, and therefore, they have unstable processing accuracy and surface quality, and extremely high chip rate.
In the related art, for microminiature high-precision parts, ultra-fine machining is adopted, and ultra-precise turning, ultra-precise milling and ultra-precise grinding are performed by using a diamond cutter. Besides the characteristic that the semiconductor core component is difficult to process, the machined part is often complex and tiny in shape, the diameter of a micropore required to be drilled is between 1 mu m and 1mm, and the machining precision (0.1-1 mu m) and the surface roughness (Ra0.02-0.1 mu m) are required to be high. Traditional single crystal diamond and polycrystalline diamond (PCD) superhard cutter materials are required to be applied through processes such as embedding, sintering and the like, are prepared on the surface of a miniature precision tool with a complex shape, and have the defects of low density, poor uniformity, poor wear resistance and high workpiece surface roughness, so that the traditional single crystal diamond and polycrystalline diamond (PCD) superhard cutter materials are difficult to apply.
Disclosure of Invention
The present invention aims to solve at least one of the above technical problems in the prior art. Therefore, the invention provides a porous diamond coating, which is suitable for preparing a cutter coating with high processing precision, low wear rate and long service life through an intermediate layer and an anti-wear chip blocking porous structure formed among dispersed diamond grains.
The invention also provides a method for preparing the porous diamond coating.
The invention also provides application of the porous diamond coating.
The first aspect of the invention provides a porous diamond coating, which comprises a metal matrix, wherein a silicon carbide composite intermediate layer is arranged on the surface of the metal matrix, and dispersed diamond grains are inlaid in the silicon carbide composite intermediate layer.
Micro tools typically use cemented carbide or high speed steel as a substrate and diamond as a coating. In the ultra-fine machining process, a small cutting depth is required, and the adopted cutter needs to have a very sharp cutting edge and high stability. The tool base material is typically cemented carbide or high speed steel and is hard coated on its surface. Diamond is an ideal tool material for ultra-fine machining because of its excellent physicochemical properties such as extremely high hardness, extremely high wear resistance, extremely high elastic modulus, chemical affinity, etc.
The invention relates to one of the technical schemes of a porous diamond coating, which has at least the following beneficial effects:
In the processing of hard and brittle materials, on one hand, the hard coating of a processing tool, such as a diamond coating, has poor bonding force with a substrate, and the insufficient bonding of the diamond coating and a cutter substrate can directly lead to the failure of the coating and the low service life of the cutter, which is a key technical problem of the diamond coating technology. According to the invention, aiming at the reason of poor binding force, the silicon carbide composite intermediate layer is arranged on the surface of the metal substrate as a transition intermediate layer structure, so that the cobalt diffusion is restrained, the internal stress is reduced, and the binding force between the hard coating and the substrate is improved. On the other hand, the hard coating of the processing tool is easy to block the grinding wheel by abrasive dust generated in the grinding process, the processing quality is poor, the porous diamond coating of the invention is characterized in that the silicon carbide composite intermediate layer is inlaid with dispersed diamond grains, gaps and porous structures are formed among the dispersed diamond grains, and the effect of preventing the abrasive dust from blocking is achieved.
According to the porous diamond coating, the silicon carbide composite intermediate layer is arranged on the surface of the metal substrate, and the silicon carbide composite intermediate layer is inlaid with dispersed diamond grains. The bond strength of the metal matrix and the coating is related to thermal stress. In the preparation process, the growth temperature of the coating can reach more than eight hundred degrees centigrade, and when the temperature is reduced to room temperature, the thermal expansion coefficients of the substrate and the coating are different, so that thermal stress exists. The expansion coefficients of the hard alloy and the silicon carbide are different, and the expansion coefficient can be adjusted after the diamond is added. Specifically, the silicon carbide is more in the initial growth stage of the coating, the diamond is less, the thermal expansion coefficient is biased to silicon carbide, as the growth of the coating is reduced, the more the number of the diamond is, the larger the volume is, the thermal expansion coefficient is biased to diamond, and finally, the expansion coefficient is reduced, and the binding force between the porous diamond coating and the metal matrix is better.
The porous diamond coating of the present invention exhibits a tendency of a coefficient of thermal expansion from the metal substrate to the surface to become gradually smaller.
The porous diamond coating is not limited by the shape of the tool, can realize rapid and controllable deposition on a miniature precision tool with any complex shape, and has the advantages of wide application range, high precision, low cost and the like.
According to some embodiments of the invention, each diamond grain is partially embedded in the silicon carbide composite intermediate layer, and the other part is exposed outside the silicon carbide composite intermediate layer to form a protrusion.
The silicon carbide composite intermediate layer has the function similar to that of a binder, part of diamond grains can be buried in the silicon carbide composite intermediate layer, the bonding strength of a coating and a matrix is improved through the silicon carbide composite intermediate layer, the hole structure formed between the diamond grains can prevent the grinding wheel from being blocked by abrasive dust, and finally the service life of the grinding tool is prolonged. It will be appreciated that for a grinder to facilitate grinding, a large roughness is required, the grinder requires large particles on the surface, unlike a drill bit on which threads are provided to remove chips, but the grinder does not remove chips, and if the abrasive dust generated during the operation of the grinder is not removed in time, the grinder can easily scratch the surface of the workpiece being processed. The porous diamond coating of the invention has the advantages that the porous structures formed among the diamond grains provide accommodation places for abrasive dust generated in the working process of the grinding tool, and the abrasive dust generated in the working process of the grinding tool can flow into the holes, so that the surface of a processed workpiece is protected from being scratched.
For a typical coating, the diamond grains are entirely embedded in the coating or binder. In the porous diamond coating, one part of each diamond grain is buried in the silicon carbide composite intermediate layer, and the other part is exposed outside the silicon carbide composite intermediate layer to form a bulge.
According to some embodiments of the invention, the diamond grains have a height greater than a thickness of the silicon carbide composite intermediate layer.
The height and width of the diamond grain tip are equivalent to the height and width of the abrasive grain protrusion, respectively, and the abrasive grain size and density directly affect the grinding processability. The height of the diamond crystal grains is larger than the thickness of the silicon carbide composite intermediate layer, so that the surface of the silicon carbide composite intermediate layer is ensured to have enough abrasive particle bulges, and a better grinding effect is achieved.
According to some embodiments of the invention, the diamond grains are oriented perpendicular to the metal matrix surface.
According to some embodiments of the invention, the diamond grains comprise at least one of micron-sized diamond grains and submicron-sized diamond grains.
According to some embodiments of the invention, the metal matrix comprises cemented carbide or high speed steel.
According to some embodiments of the invention, the cemented carbide comprises YG6, YG8, YG6X and YG6M.
According to some embodiments of the invention, cemented carbides include YG6 4130511, YG6X 4130511, YG84130511, and YG6M 4160511.
In a second aspect, the invention provides a method for preparing the porous diamond coating, which comprises the following steps of sequentially pretreating the surface of the metal matrix with an alkaline solution and an acidic solution, and depositing the silicon carbide composite intermediate layer and the diamond grains on the surface of the metal matrix through hot wire chemical vapor deposition.
Common coating preparation processes include polycrystalline diamond (Polycrystalline Diamond, PCD for short), electroplating, electroless plating, chemical vapor deposition (Chemical Vapor Deposition, CVD for short), and the like. Diamond abrasive tools are typically made by electroplating or brazing. Among these, plating tools have poor die/matrix adhesion due to lack of chemical bonds. Brazed diamond can cause thermal damage due to high temperature brazing.
CVD is a technique of forming a solid thin film by decomposition and chemical reaction between atoms in an activated environment (heat, light, plasma) by means of a precursor reactant. The method mainly comprises the steps of decomposing methane and hydrogen into active methyl free radicals and atomic hydrogen through hot wire heating, and forming a diamond coating on the surface of a sample through the chemical reaction of active particles by combining carbon-carbon with sp 3 bonds, wherein the total chemical reaction is CH 4 (air) — (heat activated) →C (diamond) +2H 2 (air). The diamond coating is deposited on the surface of the hard alloy cutter, so that the hardness and the wear resistance of the cutter surface can be greatly improved, and the service life of the cutter is prolonged. The preparation method of the CVD diamond coating can be classified into Hot filament CVD (Hot FILAMENT CVD, abbreviated as HFCVD), electron Assisted CVD (EACVD), microwave Plasma CVD (MPCVD) and the like according to the method of generating the activation environment, wherein the Hot filament HFCVD has the advantages of large deposition area and deposition uniformity, and is suitable for high loading and high uniformity coating of complex-shaped tools.
CVD coated diamond abrasive tools, because of the small grinding space between grains, the grinding created during the grinding process can clog the grinding space, resulting in a break in the grinding, limiting their practical application. Some new technologies or procedures are complex, have high cost, or are only suitable for continuous planar pure diamond coating, and cannot solve the problem that the grinding wheel is blocked by abrasive dust in the grinding process.
The invention relates to a technical scheme in a preparation method of a porous diamond coating, which has at least the following beneficial effects:
According to the preparation method, after the surface of the metal matrix is pretreated by using the alkaline solution and the acidic solution in sequence, diamond grains can be formed while the silicon carbide composite intermediate layer is formed on the surface of the metal matrix by deposition of hot filament chemical vapor deposition, and the diamond grains are mutually dispersed to form gaps and a porous structure, so that the effect of preventing abrasive dust from blocking is generated, and finally the problem of abrasive dust blocking is solved.
In the general diamond coating preparation process, nano diamond crystal seeds are required to be planted and adsorbed on the surface of a matrix in advance, and the preparation method does not need to be planted in advance, so that the cost is further reduced, and the operation is simplified.
According to the preparation method, the growth rates of the diamond grains and the silicon carbide layer are regulated, so that the heights of the diamond grains are higher than those of the silicon carbide layer, holes are formed among the diamond grains, the hole depth and the width are controllable, and the abrasive dust blockage is effectively prevented. Specifically, diamond and silicon carbide grow simultaneously, and the diamond grows faster, so that the diamond in the finally prepared coating is higher than the surface of the silicon carbide to form bulges.
Silicon carbide and diamond grow on the surface of the metal matrix at the same time, the interface of the matrix is gradually reduced to the surface of the top layer, the content of carbide gradually increases to the pure diamond of the top layer, so that the longitudinal thermal expansion coefficient of the coating gradually changes, the thermal stress concentrated on the interface is distributed on the transition layer containing silicon carbide, the internal stress of the coating can be obviously reduced, the binding force of the coating and the metal matrix is improved, and meanwhile, the fracture toughness of the diamond coating is improved.
The preparation method of the invention uses alkaline solution to pretreat the surface of the metal matrix, and aims to remove cobalt element on the surface and inhibit the generation of interface harmful graphite phase.
The preparation method of the invention uses acid solution to pretreat the surface of the metal matrix, and aims to further remove cobalt element on the surface and inhibit the generation of interface harmful graphite phase.
The preparation method of the invention can influence the growth of diamond grains, including grain orientation, grain size and coating thickness, by adjusting deposition parameters, and can control the height and width of the tips of the micron diamond grains, thereby adjusting the grinding performance of the cutter.
The preparation method can naturally form a porous structure after the coating is deposited, does not need subsequent treatment, and has simple operation and low cost.
The preparation method is not only suitable for plane-shaped tools, but also suitable for micro tools with complex shapes.
According to the preparation method, the uniform coating on the surface of the micro tool can be realized by depositing the composite diamond porous structure.
The preparation method of the invention does not need expensive equipment and complex process control, has low reaction conditions, easily obtained raw materials, low production cost and easy industrial production.
According to some embodiments of the invention, the alkaline solution comprises an inorganic base, ferricyanide, and water.
According to some embodiments of the invention, the mass of the inorganic base, the mass of ferricyanide and the volume ratio of water is 1:1:10-100.
According to some embodiments of the present invention, in the process of pretreating the surface of the metal substrate with the alkaline solution, ultrasound may be applied, where the time of ultrasonic etching is 5min to 50min, and the frequency of ultrasound is 80hz to 120hz.
According to some embodiments of the present invention, after the surface of the metal substrate is pretreated with the alkaline solution, the surface of the metal substrate may be cleaned with deionized water, where the number of times of cleaning may be multiple times, and the time of each cleaning may be 10min to 20min.
According to some embodiments of the invention, the acidic solution is a mixture of concentrated sulfuric acid and hydrogen peroxide.
According to some embodiments of the invention, the volume ratio of the concentrated sulfuric acid to the hydrogen peroxide is 10:10-100.
According to some embodiments of the invention, the surface of the metal substrate is pretreated with an acidic solution for 5s to 60s.
According to some embodiments of the present invention, after the surface of the metal substrate is pretreated with the acidic solution, the surface of the metal substrate may be cleaned with deionized water, where the number of times of cleaning may be multiple times, and the time of each cleaning may be 10min to 20min. After cleaning, the surface of the metal substrate can be blow-dried by nitrogen.
According to some embodiments of the invention, the hot wire chemical vapor deposition method comprises the steps of adjusting the distance between the surface of the metal matrix and the hot wire, vacuumizing, introducing mixed gas, heating the filament, and depositing a silicon carbide composite intermediate layer and diamond grains on the surface of the metal matrix.
According to some embodiments of the invention, the step of hot filament chemical vapor deposition comprises:
(1) Uniformly inserting a metal matrix into a copper plate with holes, placing under an air outlet of hot wire chemical vapor deposition, adjusting the distance from the top end of the metal matrix to the hot wire, and vacuumizing;
(2) Vacuumizing the step (1), and then introducing hydrogen, a carbon source and a silicon source, wherein the air pressure is kept at 1-10 kPa;
(3) Switching on a hot wire power supply, regulating the temperature of the hot wire, and continuously growing a silicon carbide composite interlayer and diamond grains;
(4) And after the growth is finished, closing gas, closing a power supply and vacuumizing.
According to some embodiments of the invention, the distance between the surface of the metal substrate and the hot wire is 15 mm-30 mm.
According to some embodiments of the invention, the mixed gas comprises hydrogen, a carbon source, and a silicon source.
According to some embodiments of the invention, the carbon source comprises methane.
According to some embodiments of the invention, the silicon source comprises an organosilane.
According to some embodiments of the invention, the organosilane comprises tetramethylsilane.
According to some embodiments of the invention, methane is present in the range of 1% -10% of the total gas volume.
According to some embodiments of the invention, the organosilane total gas volume ranges from 0.05% to 1%.
According to some embodiments of the invention, the filament is heated to a temperature of 1500 ℃ to 2800 ℃.
According to some embodiments of the invention, the silicon carbide composite intermediate layer and the diamond grains are deposited and grown for 1-15 hours.
A third aspect of the invention provides the use of a porous diamond coating as described or prepared by the method in a tool.
The invention relates to a technical scheme of application of a porous diamond coating in a cutter, which has at least the following beneficial effects:
the porous diamond coating provided by the invention is good in processing quality, high in processing precision, low in wear rate and long in service life when being used for a cutter.
According to the porous diamond coating, the silicon carbide composite intermediate layer is arranged on the surface of the metal substrate, and the silicon carbide composite intermediate layer is inlaid with dispersed diamond grains. The bond strength of the metal matrix and the coating is related to thermal stress. In the preparation process, the growth temperature of the coating can reach more than eight hundred degrees centigrade, and when the temperature is reduced to room temperature, the thermal expansion coefficients of the substrate and the coating are different, so that thermal stress exists. The expansion coefficients of the hard alloy and the silicon carbide are different, and the expansion coefficient can be adjusted after the diamond is added. Specifically, the silicon carbide is more in the initial growth stage of the coating, the diamond is less, the thermal expansion coefficient is biased to silicon carbide, as the growth of the coating is reduced, the more the number of the diamond is, the larger the volume is, the thermal expansion coefficient is biased to diamond, and finally, the expansion coefficient is reduced, and the binding force between the porous diamond coating and the metal matrix is better.
The porous diamond coating of the present invention exhibits a tendency of a coefficient of thermal expansion from the metal substrate to the surface to become gradually smaller.
The porous diamond coating is not limited by the shape of the tool, can realize rapid and controllable deposition on a miniature precision tool with any complex shape, and has wide application range, high precision and low cost.
According to some embodiments of the invention, the tool comprises a grinder, reamer, broach, riving knife or slotting knife.
Drawings
Fig. 1 is a schematic illustration of a process for preparing a porous diamond coating.
Fig. 2 is a graph of the silane coating versus the pot life of the substrate YG 6.
Fig. 3 is a coating surface micro-topography of example 22.
Fig. 4 is a coating surface micro-topography of example 23.
Detailed Description
The following are specific embodiments of the present invention, and the technical solutions of the present invention will be further described with reference to the embodiments, but the present invention is not limited to these embodiments.
In some embodiments of the invention, a porous diamond coating is provided, comprising a metal substrate having a silicon carbide composite intermediate layer on a surface thereof, the silicon carbide composite intermediate layer having dispersed diamond grains embedded therein.
Micro tools typically use cemented carbide or high speed steel as a substrate and diamond as a coating. In the ultra-fine machining process, a small cutting depth is required, and the adopted cutter needs to have a very sharp cutting edge and high stability. The tool base material is typically cemented carbide or high speed steel and is hard coated on its surface. Diamond is an ideal tool material for ultra-fine machining because of its excellent physicochemical properties such as extremely high hardness, extremely high wear resistance, extremely high elastic modulus, chemical affinity, etc.
It can be appreciated that in the processing of hard and brittle materials, on one hand, the poor bonding force between the hard coating, such as the diamond coating, and the substrate of the processing tool, and the insufficient bonding between the diamond coating and the substrate of the tool, can directly lead to the failure of the coating and the low service life of the tool, which is a key technical problem of the diamond coating technology. According to the invention, aiming at the reason of poor binding force, the silicon carbide composite intermediate layer is arranged on the surface of the metal substrate as a transition intermediate layer structure, so that the cobalt diffusion is restrained, the internal stress is reduced, and the binding force between the hard coating and the substrate is improved. On the other hand, the hard coating of the processing tool is easy to block the grinding wheel by abrasive dust generated in the grinding process, the processing quality is poor, the porous diamond coating of the invention is characterized in that the silicon carbide composite intermediate layer is inlaid with dispersed diamond grains, gaps and porous structures are formed among the mutually dispersed diamond grains, and the effect of preventing the abrasive dust from blocking is achieved.
According to the porous diamond coating, the silicon carbide composite intermediate layer is arranged on the surface of the metal substrate, and the silicon carbide composite intermediate layer is inlaid with dispersed diamond grains. The bond strength of the metal matrix and the coating is related to thermal stress. In the preparation process, the growth temperature of the coating can reach more than eight hundred degrees centigrade, and when the temperature is reduced to room temperature, the thermal expansion coefficients of the substrate and the coating are different, so that thermal stress exists. The expansion coefficients of the hard alloy and the silicon carbide are different, and the expansion coefficient can be adjusted after the diamond is added. Specifically, the silicon carbide is more in the initial growth stage of the coating, the diamond is less, the thermal expansion coefficient is biased to silicon carbide, as the growth of the coating is reduced, the more the number of the diamond is, the larger the volume is, the thermal expansion coefficient is biased to diamond, and finally, the expansion coefficient is reduced, and the binding force between the porous diamond coating and the metal matrix is better.
The porous diamond coating of the present invention exhibits a tendency of a coefficient of thermal expansion from the metal substrate to the surface to become gradually smaller.
It can be understood that the porous diamond coating is not limited by the shape of the tool, can realize rapid and controllable deposition on a miniature precision tool with any complex shape, and has the advantages of wide application range, high precision, low cost and the like.
In some embodiments of the invention, each diamond grain is partially embedded in the silicon carbide composite intermediate layer and partially exposed outside the silicon carbide composite intermediate layer to form a protrusion.
The silicon carbide composite intermediate layer has the function similar to that of a binder, part of diamond grains can be buried in the silicon carbide composite intermediate layer, the bonding strength of a coating and a matrix is improved through the silicon carbide composite intermediate layer, the hole structure formed between the diamond grains can prevent the grinding wheel from being blocked by abrasive dust, and finally the service life of the grinding tool is prolonged. It will be appreciated that for a grinder to facilitate grinding, a large roughness is required, the grinder requires large particles on the surface, unlike a drill bit on which threads are provided to remove chips, but the grinder does not remove chips, and if the abrasive dust generated during the operation of the grinder is not removed in time, the grinder can easily scratch the surface of the workpiece being processed. The porous diamond coating of the invention has the advantages that the porous structures formed among the diamond grains provide accommodation places for abrasive dust generated in the working process of the grinding tool, and the abrasive dust generated in the working process of the grinding tool can flow into the holes, so that the surface of a processed workpiece is protected from being scratched.
For a typical coating, the diamond grains are entirely embedded in the coating or binder. In the porous diamond coating, one part of each diamond grain is buried in the silicon carbide composite intermediate layer, and the other part is exposed outside the silicon carbide composite intermediate layer to form a bulge.
In some embodiments of the invention, the height of the diamond grains is greater than the thickness of the silicon carbide composite intermediate layer.
The height and width of the diamond grain tip are equivalent to the height and width of the abrasive grain protrusion, respectively, and the abrasive grain size and density directly affect the grinding processability. The height of the diamond crystal grains is larger than the thickness of the silicon carbide composite intermediate layer, so that the surface of the silicon carbide composite intermediate layer is ensured to have enough abrasive particle bulges, and a better grinding effect is achieved.
In some embodiments of the invention, the diamond grains are oriented perpendicular to the metal matrix surface.
In some embodiments of the invention, the diamond grains comprise at least one of micron-sized diamond grains and submicron-sized diamond grains.
In some embodiments of the invention, the metal matrix comprises cemented carbide or high speed steel.
In some embodiments of the present invention, cemented carbide includes YG6, YG8, YG6X, and YG6M.
In some embodiments of the invention, cemented carbides include YG6 4130511, YG6X 4130511, YG84130511, and YG6M 4160511.
In still other embodiments of the present invention, the present invention provides a method of preparing the porous diamond coating of the present invention comprising the steps of sequentially pre-treating the surface of a metal substrate with an alkaline solution and an acidic solution, and depositing a silicon carbide composite intermediate layer and diamond grains on the surface of the metal substrate by hot wire chemical vapor deposition.
Common coating preparation processes include polycrystalline diamond (Polycrystalline Diamond, PCD for short), electroplating, electroless plating, chemical vapor deposition (Chemical Vapor Deposition, CVD for short), and the like. Diamond abrasive tools are typically made by electroplating or brazing. Among these, plating tools have poor die/matrix adhesion due to lack of chemical bonds. Brazed diamond can cause thermal damage due to high temperature brazing.
CVD is a technique of forming a solid thin film by decomposition and chemical reaction between atoms in an activated environment (heat, light, plasma) by means of a precursor reactant. The method mainly comprises the steps of decomposing methane and hydrogen into active methyl free radicals and atomic hydrogen through hot wire heating, and forming a diamond coating on the surface of a sample through the chemical reaction of active particles by combining carbon-carbon with sp 3 bonds, wherein the total chemical reaction is CH 4 (air) — (heat activated) →C (diamond) +2H 2 (air). The diamond coating is deposited on the surface of the hard alloy cutter, so that the hardness and the wear resistance of the cutter surface can be greatly improved, and the service life of the cutter is prolonged. The preparation method of the CVD diamond coating can be classified into Hot filament CVD (Hot FILAMENT CVD, abbreviated as HFCVD), electron Assisted CVD (EACVD), microwave Plasma CVD (MPCVD) and the like according to the method of generating the activation environment, wherein the Hot filament HFCVD has the advantages of large deposition area and deposition uniformity, and is suitable for high loading and high uniformity coating of complex-shaped tools.
CVD coated diamond abrasive tools, because of the small grinding space between grains, the grinding created during the grinding process can clog the grinding space, resulting in a break in the grinding, limiting their practical application. Some new technologies or procedures are complex, have high cost, or are only suitable for continuous planar pure diamond coating, and cannot solve the problem that the grinding wheel is blocked by abrasive dust in the grinding process.
It can be understood that the preparation method of the invention sequentially pretreats the surface of the metal matrix with the alkaline solution and the acidic solution, and then forms diamond grains while forming the silicon carbide composite intermediate layer on the surface of the metal matrix by hot filament chemical vapor deposition, and the diamond grains are mutually dispersed to form gaps and a porous structure, thereby producing the effect of preventing the abrasive dust from blocking and finally solving the problem of abrasive dust blocking.
In the general diamond coating preparation process, nano diamond crystal seeds are required to be planted and adsorbed on the surface of a matrix in advance, and the preparation method does not need to be planted in advance, so that the cost is further reduced, and the operation is simplified.
According to the preparation method, the growth rates of the diamond grains and the silicon carbide layer are regulated, so that the heights of the diamond grains are higher than those of the silicon carbide layer, holes are formed among the diamond grains, the hole depth and the width are controllable, and the abrasive dust blockage is effectively prevented. Specifically, diamond and silicon carbide grow simultaneously, and the diamond grows faster, so that the diamond in the finally prepared coating is higher than the surface of the silicon carbide to form bulges.
Silicon carbide and diamond grow on the surface of the metal matrix at the same time, the interface of the matrix is gradually reduced to the surface of the top layer, the content of carbide gradually increases to the pure diamond of the top layer, so that the longitudinal thermal expansion coefficient of the coating gradually changes, the thermal stress concentrated on the interface is distributed on the transition layer containing silicon carbide, the internal stress of the coating can be obviously reduced, the binding force of the coating and the metal matrix is improved, and meanwhile, the fracture toughness of the diamond coating is improved.
The method for coating the porous diamond comprises the following steps of sequentially pretreating the surface of a metal matrix by using an alkaline solution and an acidic solution, and depositing a silicon carbide composite intermediate layer and diamond grains on the surface of the metal matrix by hot filament chemical vapor deposition.
The preparation process of the porous diamond coating of the present invention can be better understood by referring to fig. 1, the surface of the metal matrix cemented carbide is provided with cobalt 1 and tungsten carbide 2, the surface of the metal matrix is pretreated by an alkaline solution and an acidic solution in sequence, and then a silicon carbide composite intermediate layer 3 and diamond grains 4 are formed on the surface of the metal matrix by simultaneous deposition of hot filament chemical vapor deposition.
By adjusting the deposition parameters, the growth of the diamond grains 4, including grain orientation, grain size, and coating thickness, can be affected, and the micrometer diamond grain tip height and width can be controlled, thereby adjusting the grinding performance of the tool. The mutually dispersed diamond grains 4 can naturally form a porous structure, no subsequent treatment is needed, the operation is simple, and the cost is low.
The preparation method is not only suitable for plane-shaped tools, but also suitable for micro tools with complex shapes.
According to the preparation method, the uniform coating on the surface of the micro tool can be realized by depositing the composite diamond porous structure.
The preparation method of the invention does not need expensive equipment and complex process control, has low reaction conditions, easily obtained raw materials, low production cost and easy industrial production.
In some embodiments of the invention, the alkaline solution comprises an inorganic base, ferricyanide, and water.
In some embodiments of the invention, the mass of the inorganic base, the mass of ferricyanide and the volume ratio of water is 1:1:10-100.
In some embodiments of the invention, ultrasound may be applied during the pretreatment of the surface of the metal substrate with the alkaline solution for 5min to 50min, with the frequency of the ultrasound being 80hz to 120hz.
In some embodiments of the present invention, after the surface of the metal substrate is pretreated with the alkaline solution, the surface of the metal substrate may be rinsed with deionized water, and the number of rinsing may be multiple times.
In some embodiments of the invention, the acidic solution is a mixture of concentrated sulfuric acid and hydrogen peroxide.
In some embodiments of the invention, the volume ratio of the concentrated sulfuric acid to the hydrogen peroxide is 10:10-100.
In some embodiments of the invention, the surface of the metal substrate is pretreated with an acidic solution for 5s to 60s.
In some embodiments of the present invention, after the surface of the metal substrate is pretreated with the acidic solution, the surface of the metal substrate may be rinsed with deionized water, and the number of rinsing may be multiple times. After cleaning, the surface of the metal substrate can be blow-dried by nitrogen.
In some embodiments of the invention, the hot wire chemical vapor deposition method comprises the steps of adjusting the distance between the surface of the metal matrix and the hot wire, vacuumizing, introducing mixed gas, heating the filament, and depositing a silicon carbide composite interlayer and diamond grains on the surface of the metal matrix.
In some embodiments of the invention, the step of hot filament chemical vapor deposition comprises:
(1) Uniformly inserting a metal matrix into a copper plate with holes, placing under an air outlet of hot wire chemical vapor deposition, adjusting the distance from the top end of the metal matrix to the hot wire, and vacuumizing;
(2) Vacuumizing the step (1), and then introducing hydrogen, methane and organosilane (tetramethylsilane or silane), wherein the air pressure is kept at 1-10 kPa;
(3) Switching on a hot wire power supply, regulating the temperature of the hot wire, and continuously growing a silicon carbide composite interlayer and diamond grains;
(4) And after the growth is finished, closing gas, closing a power supply and vacuumizing.
In some embodiments of the invention, the distance between the surface of the metal substrate and the hot wire is 15 mm-30 mm.
In some embodiments of the invention, the co-gas includes hydrogen, methane, and an organosilane.
In some embodiments of the invention, methane is present in the range of 1% -10% of the total gas volume.
In some embodiments of the invention, the organosilane total gas volume ranges from 0.05% to 1%.
In some embodiments of the invention, the filament is heated to a temperature of 1500 ℃ to 2800 ℃.
In some embodiments of the invention, the silicon carbide composite intermediate layer and the diamond grains are deposited and grown for 1 to 15 hours.
In still other embodiments of the present invention, the present invention provides the use of a porous diamond coating of the present invention or a porous diamond coating prepared by the method in a tool.
It can be appreciated that the porous diamond coating of the invention has good processing quality, high processing precision, low wear rate and long service life when being used for cutters.
The porous diamond coating is not limited by the shape of the tool, can realize rapid and controllable deposition on a miniature precision tool with any complex shape, and has wide application range, high precision and low cost.
In some embodiments of the invention, the tool comprises a grinder, reamer, broach, riving knife, or slotting tool.
The technical solution of the present invention will be better understood by combining the following specific embodiments.
According to the invention, the silicon carbide composite intermediate layer is added between the substrate and the diamond coating, and the silicon carbide is similar to a binder, so that part of diamond grains are buried in the silicon carbide layer, and the bonding strength of the coating and the substrate is improved. Specifically, diamond and silicon carbide grow simultaneously at the beginning of the preparation, however, since the growth rate of diamond is faster, diamond is higher than the silicon carbide surface in the finally prepared coating, forming protrusions. And holes are formed among the diamond grains, the hole depth and the width are controllable, and the abrasive dust blockage is effectively prevented.
Examples 1-20 in Table 1 below are comparative in terms of the duration of their operation for coating preparation on several different substrate surfaces, divided between the addition of an intermediate layer and the absence of an intermediate layer, and different silane contents.
The preparation method comprises the following specific steps:
1. firstly, carrying out chemical pretreatment on the hard alloy precision grinding tool, immersing the working area of the hard alloy precision grinding tool into a mixed alkali solution (K 3Fe(CN)6∶KOH∶H2 O=1:1:10), and carrying out ultrasonic (100 Hz) corrosion in an ultrasonic pool for 15min. And then taking out the hard alloy precision grinding tool, and ultrasonically cleaning the hard alloy precision grinding tool with deionized water for 3 times, wherein each time is 10 minutes. After the washing, a mixed acid solution (a mixture of concentrated sulfuric acid and hydrogen peroxide) was prepared, 10mL of the concentrated sulfuric acid solution and 100mL of the hydrogen peroxide solution were weighed, and the two were sufficiently mixed. And (3) placing the cleaned hard alloy precision grinding tool into a mixed acid solution to be corroded for 30 seconds, taking out, placing into deionized water, and ultrasonically cleaning for 3 times, wherein each time is 10 minutes. After the cleaning is finished, the material is dried by nitrogen.
2. Evenly inserting the hard alloy micro grinding tool into a copper plate with holes, placing under an air outlet of hot wire chemical vapor deposition, adjusting the distance from the top end of the hard alloy micro grinding tool to the hot wire to be 15mm, and vacuumizing. Hydrogen, methane and tetramethylsilane (1% tetramethylsilane, 99% hydrogen) were introduced at gas flows of 800sccm and 16sccm, respectively, and the gas pressure was maintained at 3kPa. And (3) turning on a hot wire power supply, wherein the temperature of the hot wire is 2200 ℃, firstly growing for 2 hours, and then turning off the tetramethylsilane to continue growing for 5 hours.
TABLE 1 comparison of the presence or absence of an intermediate layer and the variation in silane content
From the above table, it can be seen that the working time of the coating prepared from the four base materials all shows the same law: the working time of the grinding tool added with the silicon carbide composite intermediate layer is obviously prolonged compared with that of the grinding tool without the silicon carbide composite intermediate layer, the working time of the grinding tool is prolonged along with the increase of the content of tetramethylsilane by the same base material, and the graph of the coating silane prepared by the base material YG6 and the working time is shown in the graph of fig. 2. This shows that the silicon carbide composite intermediate layer adopted by the invention can effectively increase the binding force of the diamond coating and increase the working time of the grinding tool.
The "operating time period" refers to the time from the start of the machining of the grinding tool to the occurrence of cracks on the surface of the machined position, when the machining quality is deteriorated.
The method can realize the growth of the diamond coating on the surfaces of different hard alloy matrix materials, and can realize the controllable growth of the diamond coating by adjusting the growth temperature (wire bottom distance), the methane content, the silane content, the air pressure, the growth time and other conditions, thereby obtaining the diamond coating with different thicknesses and different grain sizes.
Example variable parameters and coating growth conditions are shown in table 2, with other parameters remaining consistent. The method comprises the following specific steps:
1. Firstly, carrying out chemical pretreatment on the hard alloy precision grinding tool, immersing the working area of the hard alloy precision grinding tool into a mixed alkali solution (K 3Fe(CN)6∶KOH∶H2 O=1:1:20), and carrying out ultrasonic (100 Hz) corrosion in an ultrasonic pool for 15min. And then taking out the hard alloy precision grinding tool, and ultrasonically cleaning the hard alloy precision grinding tool with deionized water for 3 times, wherein each time is 10 minutes. After the washing, a mixed acid solution (a mixture of concentrated sulfuric acid and hydrogen peroxide) was prepared, 10mL of the concentrated sulfuric acid solution and 100mL of the hydrogen peroxide solution were weighed, and the two were sufficiently mixed. And (3) placing the cleaned hard alloy precision grinding tool into a mixed acid solution to be corroded for 30 seconds, taking out, placing into deionized water, and ultrasonically cleaning for 3 times, wherein each time is 10 minutes. After the cleaning is finished, the material is dried by nitrogen.
2. And uniformly inserting the hard alloy micro grinding tool into a copper plate with holes, placing the copper plate under an air outlet of hot wire chemical vapor deposition, and vacuumizing. Different growth temperatures and pressures were set. And (3) introducing hydrogen, methane and silane after vacuumizing, and controlling and adjusting the content percentages of the methane and the silane. And (3) turning on a hot wire power supply, turning on the hot wire power supply, firstly growing for 2 hours under the condition of introducing tetramethylsilane, and then turning off the tetramethylsilane to continue growing for different time. And after the growth is finished, closing the gas, closing the power supply and vacuumizing.
TABLE 2 different growth parameters and coating growth conditions
As can be seen from table 2, the inventive method allows for the growth of diamond coatings of different thickness and different grain size on the surface of different cemented carbide substrate materials. Fig. 3 and 4 show the surface topography of the coatings of examples 22 and 23, respectively, and it can be seen that the corresponding diamond coating was successfully deposited on the surface of the abrasive tool, and the coating was a porous composite structure, which can solve the problem of abrasive dust blockage.
The present invention has been described in detail with reference to the embodiments, but the present invention is not limited to the embodiments, and various changes can be made within the knowledge of those skilled in the art without departing from the spirit of the present invention.

Claims (18)

1. The porous diamond coating is characterized by comprising a metal matrix, wherein a silicon carbide composite intermediate layer is arranged on the surface of the metal matrix, and dispersed diamond grains are inlaid in the silicon carbide composite intermediate layer.
2. The porous diamond coating of claim 1, wherein each of the diamond grains is partially embedded in the silicon carbide composite intermediate layer and partially exposed outside the silicon carbide composite intermediate layer to form a protrusion.
3. The porous diamond coating of claim 1, wherein the diamond grains have a height greater than a thickness of the silicon carbide composite intermediate layer.
4. The porous diamond coating of claim 1, wherein the diamond grains are oriented perpendicular to the metal substrate surface.
5. The porous diamond coating of any one of claims 1 to 4, wherein the diamond grains comprise at least one of micron-sized diamond grains and submicron-sized diamond grains.
6. A porous diamond coating according to any one of claims 1 to 4, wherein the metal substrate comprises cemented carbide or high speed steel.
7. A method of preparing a porous diamond coating according to any one of claims 1 to 6, comprising the step of depositing the silicon carbide composite intermediate layer and the diamond grains on the surface of the metal substrate by hot wire chemical vapor deposition after sequentially pre-treating the surface of the metal substrate with an alkaline solution and an acidic solution.
8. The method of claim 7, wherein the alkaline solution comprises an inorganic base, ferricyanide, and water.
9. The method according to claim 8, wherein the mass of the inorganic base, the mass of ferricyanide and the volume ratio of water is 1:1:10-100.
10. The method of claim 7, wherein the acidic solution is a mixture of concentrated sulfuric acid and hydrogen peroxide.
11. The method of claim 10, wherein the volume ratio of concentrated sulfuric acid to hydrogen peroxide is 10:10-100.
12. The method of claim 7, wherein the hot wire chemical vapor deposition method comprises adjusting the distance between the surface of the metal substrate and the hot wire, vacuumizing, introducing mixed gas, heating the filament, and depositing a silicon carbide composite interlayer and diamond grains on the surface of the metal substrate.
13. The method of claim 12, wherein the surface of the metal substrate is 15mm to 30mm from the hot wire.
14. The method of claim 12, wherein the mixed gas comprises hydrogen, methane, and organosilane.
15. The method of claim 12, wherein the filament is heated to a temperature of 1500 ℃ to 2800 ℃.
16. The method of claim 12, wherein the silicon carbide composite intermediate layer and the diamond grains are deposited and grown for a period of 1h to 15h.
17. Use of a porous diamond coating according to any one of claims 1 to 6 or prepared according to the method of any one of claims 7 to 16 in a tool.
18. The use of claim 17, wherein the tool comprises a grinder, reamer, broach, riving knife or slotting knife.
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