CN109972115B - Hard alloy cutter with micro-nano diamond coating and preparation method thereof - Google Patents
Hard alloy cutter with micro-nano diamond coating and preparation method thereof Download PDFInfo
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- CN109972115B CN109972115B CN201711468369.5A CN201711468369A CN109972115B CN 109972115 B CN109972115 B CN 109972115B CN 201711468369 A CN201711468369 A CN 201711468369A CN 109972115 B CN109972115 B CN 109972115B
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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
- C23C16/0227—Pretreatment of the material to be coated by cleaning or etching
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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
- C23C16/22—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
- C23C16/271—Diamond only using hot filaments
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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
- C23C16/56—After-treatment
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Abstract
The invention provides a hard alloy cutter with a micro-nano diamond coating and a preparation method thereof, which relate to the field of processing and manufacturing of hard alloy cutters, and the preparation method of the hard alloy cutter with the micro-nano diamond coating comprises the following steps: the method comprises the steps of preparing a micron diamond coating on the surface of a hard alloy cutter, and then preparing a nano diamond coating on the surface layer of the micron diamond coating through etching to obtain the hard alloy cutter with the micron diamond coating, so that the technical problem that the hard alloy cutter is short in service life due to the fact that the bonding strength of the micron diamond coating and the hard alloy cutter obtained through a processing method in the prior art is low is solved, meanwhile, the problems that the surface precision of the nano diamond coating obtained through the processing method in the prior art is low and the hardness and the wear resistance are weakened can be solved, and the effect of delaying the service life of the hard alloy cutter is achieved.
Description
Technical Field
The invention relates to the technical field of machining and manufacturing of hard alloy cutters, in particular to a hard alloy cutter with a micro-nano diamond coating and a preparation method thereof.
Background
The diamond coating has good mechanical properties, such as high hardness, high elastic modulus, good wear resistance, excellent corrosion resistance, thermal conductivity and the like, and is widely applied to the superhard protective coating of hard alloy cutters (such as turning tools, milling cutters and the like) to prolong the overall processing life of the cutters.
At present, a micron diamond coating with a certain thickness is mainly deposited and grown on the surface of the hard alloy in industrial application, and the service life of the hard alloy cutter is prolonged. Due to the high surface roughness of the micron diamond coating, the surface of a processed workpiece needs to be polished subsequently. The existing improvement measures are basically improved by adopting the nano diamond coating, but the bonding strength between the nano diamond coating and the hard alloy cutter substrate is weak due to the limit of the performance of the nano diamond coating, and the service life is shortened. Currently, reducing the surface roughness of diamond coatings and improving the surface precision of machined workpieces are mainly achieved by means of single-layer nano-diamond coatings, composite diamond coatings (micro-nano composite coatings).
The single-layer nano diamond coating is formed by directly depositing and growing a layer of nano diamond with certain thickness on the surface of the hard alloy cutter. Due to the limitation of the existing preparation process and production equipment, the prepared nano coating has weaker bonding strength of the coating and the hard alloy cutter, and the hardness and the wear resistance of the nano coating are lower than those of the micron diamond. In a patent named nano diamond layer preparation method and a nano diamond blade (CN 105483643A), a chemical vapor deposition method is adopted to deposit and grow a nano diamond coating on a hard alloy cutter substrate, although the surface precision of the coating is improved, the service life of the hard alloy cutter is reduced because the bonding strength of the nano diamond coating and the hard alloy cutter substrate is lower.
The micron-nanometer composite diamond coating adopted at present is formed by growing a high-quality micron diamond coating on the surface of a hard alloy cutter and then growing a nanometer coating on the micron diamond coating in situ. Although the method improves the bonding strength of the integral coating and the hard alloy cutter to a certain extent, the problem of the interface bonding strength of the micro-diamond coating and the nano-diamond coating is also introduced, and the problem of the reduction of the hardness and the wear resistance of the nano-diamond coating caused by deposition growth is not relieved.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The first purpose of the invention is to provide a preparation method of a hard alloy cutter with a micro-nano diamond coating, so as to relieve the technical problem that the hard alloy cutter has a short service life due to the low bonding strength between the micro-nano diamond coating obtained by the processing method in the prior art and the hard alloy cutter, and simultaneously relieve the problems of low surface precision and reduced hardness and wear resistance of the nano diamond coating obtained by the processing method in the prior art.
The second purpose of the invention is to provide a hard alloy cutter with a micro-nano diamond coating, which has the advantages of high surface precision and long service life.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
a preparation method of a hard alloy cutter with a micro-nano diamond coating comprises the following steps:
preparing a micron diamond coating on the surface of the hard alloy cutter, and then preparing a nano diamond coating on the surface layer of the micron diamond coating by etching to obtain the hard alloy cutter with the micro nano diamond coating.
Further, the hard alloy cutter is pretreated, and then the micron diamond coating is prepared on the surface of the hard alloy cutter.
Further, the pretreatment comprises the step of carrying out chemical etching treatment on the surface of the hard alloy cutter.
Further, carrying out sand blasting treatment on the surface of the hard alloy cutter and then carrying out chemical etching treatment; optionally, after the sand blasting, the cemented carbide tool is cleaned and then subjected to chemical etching.
Further, the step of chemically etching includes: etching with an alkali solution and then with an acid solution.
Further, the alkali solution includes K3[Fe(CN)]6An alkali solution consisting of KOH and water; alternatively, the K3[Fe(CN)]6And the mass ratio of KOH to water is (1-2): (1-2): 10; optionally, the acid solution comprises H2SO4And H2O2A composed acid solution; alternatively, the H2SO4And H2O2The volume ratio of (1-2): 10.
further, the step of chemically etching includes: placing a hard alloy cutter at K3[Fe(CN)]6Etching in alkali solution composed of KOH and water, removing alkali solution on the surface of the hard alloy cutter, and placing in H2SO4And H2O2Etching in the acid solution.
Furthermore, the preparation method also comprises the step of pre-planting seed crystals on the surface of the hard alloy cutter after the chemical etching treatment.
Further, the pre-seeding step includes: and placing the hard alloy cutter subjected to chemical etching treatment in diamond powder suspension for ultrasonic treatment.
Further, the diamond powder suspension has the following concentration: 2 to 5 wt%.
Further, the thickness of the prepared micron diamond coating is 1.5-3 microns.
Further, the method for preparing the micron diamond coating comprises the following steps: the micron diamond coating is prepared by a chemical vapor deposition method.
Further, the technological parameters of the chemical vapor deposition method for preparing the micron diamond coating comprise: the volume fraction of the methane is 2-5 percent, the air pressure is 0.8-2.5kPa, the temperature range is 1800-2200 ℃, the temperature range of the hard alloy cutter during treatment is 600-650 ℃, and the treatment time is 1-2.5 h; the preferable technological parameters are as follows: the volume fraction of the methane is 3-4%, the air pressure is 1.2-2kPa, the temperature range is 1900-2100 ℃, the temperature range of the hard alloy cutter during treatment is 610-640 ℃, and the treatment time is 1.2-2.2 h.
Further, the etching includes plasma etching.
Further, the technological parameters for preparing the nano-diamond coating by adopting plasma etching comprise: the air pressure range of the vacuum chamber is 1.5-2kPa, the filament temperature is 2000-2200 ℃, the temperature range of the hard alloy cutter during treatment is 600-650 ℃, the treatment time is 10-30min, and the preferable technological parameters are as follows: the pressure range of the vacuum chamber is 1.6-1.9kPa, the filament temperature is 2000-2200 ℃, the temperature range of the hard alloy cutter during treatment is 610-640 ℃, the treatment time is 15-25min, and the reaction gas is hydrogen.
A hard alloy cutter with a micro-nano diamond coating is prepared according to the preparation method of the hard alloy cutter with the micro-nano diamond coating.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, a micron diamond coating with a certain thickness is prepared on the surface of the hard alloy cutter, and then the nano diamond coating is prepared in the surface layer of the micron diamond coating through etching, so that the micro-nano diamond coating is obtained. Therefore, the strong bonding strength between the micro-nano diamond coating and the matrix of the hard alloy cutter is ensured, and the low surface roughness and high surface precision of the micro-nano diamond coating are also ensured. The preparation method can be used for precisely machining hard alloy cutters made of various high-hardness materials and composite materials, and can simultaneously achieve the purposes of prolonging the service life of the hard alloy cutters and improving the machining precision, thereby effectively reducing the machining cost.
The hardness of the hard alloy cutter with the micron diamond coating obtained by the preparation method provided by the invention is 95 +/-3 GPa, the Young modulus is 1139.05 +/-362, and the friction coefficient under the load of 10N is about 0.08 +/-0.005.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
Fig. 1 is a surface topography of a micro-nano diamond coating on the surface of a cemented carbide tool provided in example 1;
fig. 2 is a friction coefficient diagram of the hard alloy tool provided in embodiment 1 for testing the micro-nano diamond coating under a load of 10N.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
One aspect of the invention provides a preparation method of a hard alloy cutter with a micro-nano diamond coating, which comprises the following steps:
preparing a micron diamond coating on the surface of the hard alloy cutter, and then preparing a nano diamond coating on the surface layer of the micron diamond coating by etching to obtain the hard alloy cutter with the micro nano diamond coating.
According to the invention, a micron diamond coating with a certain thickness is prepared on the surface of the hard alloy cutter, and then the nano diamond coating is prepared in the surface layer of the micron diamond coating through etching, so that the micro-nano diamond coating is obtained. Therefore, the strong bonding strength between the micro-nano diamond coating and the matrix of the hard alloy cutter is ensured, and the low surface roughness and high surface precision of the micro-nano diamond coating are also ensured. The preparation method can be used for precisely machining hard alloy cutters made of various high-hardness materials and composite materials, and can simultaneously achieve the purposes of prolonging the service life of the hard alloy cutters and improving the machining precision, thereby effectively reducing the machining cost.
The micro-nano diamond coating is a composite coating consisting of the micro-diamond coating and the nano-diamond coating.
The hard alloy cutter comprises a twist drill, a reamer, a boring cutter, a ball end milling cutter, a saw blade milling cutter, a taper milling cutter, a transposition end milling cutter, a transposition face milling cutter, a transposition dovetail milling cutter, a transposition three-side edge and the like.
As a preferred embodiment of the invention, the hard alloy cutter is pretreated, and then the micron diamond coating is prepared on the surface of the hard alloy cutter. The hard alloy cutter is pretreated, so that the bonding strength of the micro-nano diamond coating and the hard alloy cutter can be improved.
As a preferred embodiment of the present invention, the pretreatment comprises a step of subjecting the surface of the cemented carbide tool to a chemical etching treatment. Through chemical etching treatment, a defect part beneficial to generation of diamond is machined on the surface of the hard alloy cutter, and subsequent diamond nucleation is facilitated.
In a preferred embodiment of the present invention, the surface of the cemented carbide tool is subjected to a chemical etching process after being subjected to a sand blasting process. The surface of the hard alloy cutter can be roughly polished by adopting sand blasting treatment, grease and the like on the surface of the cutter are removed, and subsequent chemical etching treatment is facilitated.
In a preferred embodiment of the present invention, after the sand blasting, the cemented carbide tool is cleaned with acetone and/or alcohol and then subjected to a chemical etching process. The cleaning with acetone and/or alcohol can remove the dirt on the surface of the hard alloy cutter.
As a preferred embodiment of the present invention, the step of chemically etching includes: etching with an alkali solution and then with an acid solution. Etching the surface of the hard alloy cutter by using an alkali solution to coarsen the surface of the hard alloy cutter; and then etching by using acid to remove the cobalt Co on the surface of the hard alloy cutter so as to prevent the Co from damaging the surface bonding strength of the diamond coating and the hard alloy cutter.
As a preferred embodiment of the present invention, the alkali solution comprises K3[Fe(CN)]6An alkali solution consisting of KOH and water; alternatively, the K3[Fe(CN)]6And the mass ratio of KOH to water is (1-2): (1-2): 10; optionally, the acid solution comprises H2SO4And H2O2A composed acid solution; alternatively, the H2SO4And H2O2In a volume ratio of (1 to c)2): 10. optionally, the step of chemically etching includes: placing a hard alloy cutter at K3[Fe(CN)]6Etching in alkali solution composed of KOH and water, removing alkali solution on the surface of the hard alloy cutter, and placing in H2SO4And H2O2Etching in the acid solution. By optimizing the alkali solution and the acid solution and the concentration of the alkali solution and the concentration of the acid solution, the appearance of the surface of the hard alloy cutter can be easily combined with the diamond coating.
As a preferred embodiment of the present invention, the preparation method further comprises the step of pre-seeding the surface of the cemented carbide tool after the chemical etching treatment. The nucleation points can be formed on the surface of the hard alloy cutter by pre-planting the seed crystals, which is beneficial to the nucleation growth of the diamond coating.
As a preferred embodiment of the present invention, the pre-seeding step includes: and placing the hard alloy cutter subjected to chemical etching treatment in diamond powder suspension for ultrasonic treatment. Optionally, the diamond powder suspension has a concentration of: 2 to 5 wt%.
In the ultrasonic treatment process, diamond particles collide with the surface of the cutter through ultrasound, so that some fine defects are generated on the surface of the cutter, and some diamond particles are embedded into the surface of the cutter. Typical but non-limiting concentrations of diamond powder suspension are for example: 2, 3, 4 or 5 wt%.
As a preferred embodiment of the present invention, the micro diamond coating is prepared to have a thickness of 1.5 to 3 microns. In the preferred embodiment described above, the typical but non-limiting thicknesses of the micro-diamond coating are for example: 1.5 microns, 2 microns, 2.5 microns, or 3 microns.
As a preferred embodiment of the present invention, a method of preparing a microdiamond coating includes: the micron diamond coating is prepared by a chemical vapor deposition method. The micron diamond coating is prepared by adopting a vapor deposition method, can be processed by utilizing traditional equipment, reduces the generation cost and is easy to realize.
As a preferred embodiment of the invention, the process parameters of the chemical vapor deposition method for preparing the micron diamond coating comprise: the volume fraction of the methane is 2-5 percent, the air pressure is 0.8-2.5kPa, the temperature range is 1800-2200 ℃, the temperature range of the hard alloy cutter during treatment is 600-650 ℃, and the treatment time is 1-2.5 h; the preferable technological parameters are as follows: the volume fraction of the methane is 3-4%, the air pressure is 1.2-2kPa, the temperature range is 1900-2100 ℃, the temperature range of the hard alloy cutter during treatment is 610-640 ℃, and the treatment time is 1.2-2.2 h.
As a preferred embodiment of the present invention, the etching includes plasma etching. The nano diamond coating obtained by plasma etching has more uniform structure and higher surface precision.
As a preferred embodiment of the invention, the process parameters for preparing the nano-diamond coating by adopting the plasma etching comprise the following steps: the air pressure range of the vacuum chamber is 1.5-2kPa, the filament temperature is 2000-2200 ℃, the temperature range of the hard alloy cutter during treatment is 600-650 ℃, the treatment time is 10-30min, and the preferable technological parameters are as follows: the pressure range of the vacuum chamber is 1.6-1.9kPa, the filament temperature is 2000-2200 ℃, the temperature range of the hard alloy cutter during treatment is 610-640 ℃, the treatment time is 15-25min, and the reaction gas is hydrogen.
In the micro-nano diamond coating prepared by the preferred embodiment, the diamond particles in the micro-nano diamond coating are 1-1.5 microns, and the diamond particles in the nano diamond coating are 10-100 nanometers.
The invention also provides a hard alloy cutter with the micro-nano diamond coating, which is prepared according to the preparation method of the hard alloy cutter with the micro-nano diamond coating.
The hardness of the hard alloy cutter with the micron diamond coating obtained by the preparation method provided by the invention is 95 +/-3 GPa, the Young modulus is 1139.05 +/-362, and the friction coefficient under the load of 10N is about 0.08 +/-0.005.
The present invention will be described in further detail with reference to examples and comparative examples.
Example 1
The embodiment is a hard alloy cutter with a micro-nano diamond coating, and the preparation method comprises the following steps:
step a): sand blasting treatment: YG6 indexable face milling cutter sold in domestic market is used as a substrate, white corundum is firstly used for carrying out wet sand blasting treatment on the substrate, the pressure intensity during the sand blasting treatment is 200kPa, the granularity of sand grains is 800 meshes, and after the sand blasting treatment is finished, the hard alloy cutter, indexable face milling cutter is placed in mixed solution of acetone and alcohol for ultrasonic cleaning for 15 min;
step b): chemical etching treatment: the hard alloy cutter with the surface cleaned and dried is placed still at K3[Fe(CN)]6Murakami alkali solution composed of KOH and water is kept standing for 10min, wherein K3[Fe(CN)]6And the mass ratio of KOH to water is 1: 1: 10, respectively placing the mixture in deionized water and absolute ethyl alcohol solution for ultrasonic cleaning for 10min, and removing residual alkali liquor and surface adhesive substances; then the hard alloy cutter is placed in a static state in H2SO4And H2O2In acid solution of composition 10s, wherein H2SO4And H2O2Is 1: 10, washing with water, placing in absolute ethyl alcohol, ultrasonically cleaning for 20min, and drying with argon;
step c): preparing a micron diamond coating: depositing a micron diamond coating by adopting a hot wire chemical vapor deposition method and taking hydrogen and methane as reaction gases, wherein the process conditions during the hot wire chemical vapor deposition are as follows: the volume of methane accounts for 5% of the total gas volume, the air pressure of a vacuum chamber is 2kPa, the filament temperature is 2200 ℃, the temperature of a hard alloy cutter is 650 ℃, the processing time is 2.5h, and the thickness of the micron diamond coating prepared by the process is 3 microns;
step d): preparing a nano diamond coating: preparing the nano-diamond coating on the surface layer of the micron diamond coating by adopting an in-situ plasma etching method, wherein the plasma etching process conditions are as follows: the reaction gas is high-purity hydrogen with the purity of more than 99.999 percent, the air pressure of a vacuum chamber is 2kPa, the filament temperature is 2200 ℃, the temperature of the hard alloy cutter is 650 ℃ during treatment, the treatment time is 30min, and the size of nano particles in the nano diamond coating obtained after treatment is about 80 nm.
Example 2
The embodiment is a hard alloy cutter with a micro-nano diamond coating, and the preparation method comprises the following steps:
step a): chemical etching treatment: YG6 indexable face milling cutter sold in domestic market is used as a base body, and a hard alloy cutter with a cleaned and dried surface is placed at K3[Fe(CN)]6Standing in Murakami alkali solution composed of KOH and water for 8min, wherein K is3[Fe(CN)]6And the mass ratio of KOH to water is 2: 1: 10, respectively placing the mixture in deionized water and absolute ethyl alcohol solution for ultrasonic cleaning for 10min, and removing residual alkali liquor and surface adhesive substances; then the hard alloy cutter is placed in a static state in H2SO4And H2O2In acid solution of composition 10s, wherein H2SO4And H2O2Is 2: 10, washing with water, placing in absolute ethyl alcohol, ultrasonically cleaning for 20min, and drying with argon;
step b): preparing a micron diamond coating: depositing a micron diamond coating by adopting a hot wire chemical vapor deposition method and taking hydrogen and methane as reaction gases, wherein the process conditions during the hot wire chemical vapor deposition are as follows: the volume of methane accounts for 3% of the total gas volume, the air pressure of a vacuum chamber is 2kPa, the filament temperature is 2000 ℃, the temperature of a hard alloy cutter is 650 ℃, the processing time is 2.5h, and the thickness of the micron diamond coating prepared by the process is 3 microns;
step c): preparing a nano diamond coating: preparing the nano-diamond coating on the surface layer of the micron diamond coating by adopting an in-situ plasma etching method, wherein the plasma etching process conditions are as follows: the reaction gas is high-purity hydrogen with the purity of more than 99.999 percent, the air pressure of a vacuum chamber is 1.9kPa, the filament temperature is 2000 ℃, the temperature of the hard alloy cutter during processing is 640 ℃, the processing time is 20min, and the size of nano particles in the nano diamond coating obtained after processing is about 80 nm.
Example 3
The embodiment is a hard alloy cutter with a micro-nano diamond coating, and the preparation method comprises the following steps:
step a): pretreatment: taking YG6 indexable face milling cutter sold in domestic market as a substrate, and placing the hard alloy cutter-indexable face milling cutter in a mixed solution of acetone and alcohol for ultrasonic cleaning for 15 min;
step b): chemical etching treatment: the hard alloy cutter with the surface cleaned and dried is placed still at K3[Fe(CN)]6Murakami alkali solution composed of KOH and water is kept standing for 10min, wherein K3[Fe(CN)]6And the mass ratio of KOH to water is 1: 2: 10, respectively placing the mixture in deionized water and absolute ethyl alcohol solution for ultrasonic cleaning for 10min, and removing residual alkali liquor and surface adhesive substances; then the hard alloy cutter is placed in a static state in H2SO4And H2O2In acid solution of composition 10s, wherein H2SO4And H2O2Is 1.5: 10, washing with water, placing in absolute ethyl alcohol, ultrasonically cleaning for 20min, and drying with argon;
step c): preparing a micron diamond coating: depositing a micron diamond coating by adopting a hot wire chemical vapor deposition method and taking hydrogen and methane as reaction gases, wherein the process conditions during the hot wire chemical vapor deposition are as follows: the volume of methane accounts for 4% of the total gas volume, the air pressure of a vacuum chamber is 0.8kPa, the filament temperature is 2200 ℃, the temperature of a hard alloy cutter is 600 ℃, the processing time is 2.5h, and the thickness of the micron diamond coating prepared by the process is 2 microns;
step d): preparing a nano diamond coating: preparing the nano-diamond coating on the surface layer of the micron diamond coating by adopting an in-situ plasma etching method, wherein the plasma etching process conditions are as follows: the reaction gas is high-purity hydrogen with the purity of more than 99.999 percent, the air pressure of a vacuum chamber is 1.6kPa, the filament temperature is 2100 ℃, the temperature of the hard alloy cutter during treatment is 600 ℃, the treatment time is 10min, and the size of nano particles in the nano diamond coating obtained after treatment is about 10 nm.
Example 4
The embodiment is a hard alloy cutter with a micro-nano diamond coating, and the preparation method comprises the following steps:
step a): sand blasting treatment: YG6 indexable face milling cutter sold in domestic market is used as a substrate, white corundum is firstly used for carrying out wet sand blasting treatment on the substrate, the pressure intensity during the sand blasting treatment is 180kPa, the sand grain size is 1000 meshes, and after the sand blasting treatment is finished, the hard alloy cutter, indexable face milling cutter is placed in mixed solution of acetone and alcohol for ultrasonic cleaning for 10 min;
step b): chemical etching treatment: the hard alloy cutter with the surface cleaned and dried is placed still at K3[Fe(CN)]6Murakami alkali solution composed of KOH and water is kept standing for 15min, wherein K3[Fe(CN)]6And the mass ratio of KOH to water is 2: 2: 10, respectively placing the mixture in deionized water and absolute ethyl alcohol solution for ultrasonic cleaning for 8min, and removing residual alkali liquor and surface adhesive substances; then the hard alloy cutter is placed in a static state in H2SO4And H2O2In acid solution of composition 20s, wherein H2SO4And H2O2Is 1: 10, washing with water, placing in absolute ethyl alcohol, ultrasonically cleaning for 15min, and drying with argon;
step c): pre-planting seed crystal treatment: placing the chemically etched hard alloy cutter in diamond powder suspension with the concentration of 2 wt% for ultrasonic treatment for 30 min;
step d): preparing a micron diamond coating: depositing a micron diamond coating by adopting a hot wire chemical vapor deposition method and taking hydrogen and methane as reaction gases, wherein the process conditions during the hot wire chemical vapor deposition are as follows: the volume of methane accounts for 2% of the total gas volume, the air pressure of a vacuum chamber is 1.5kPa, the filament temperature is 1800 ℃, the temperature of a hard alloy cutter is 620 ℃, the processing time is 1.5h, and the thickness of the micron diamond coating prepared by the process is 3 microns;
step e): preparing a nano diamond coating: preparing the nano-diamond coating on the surface layer of the micron diamond coating by adopting an in-situ plasma etching method, wherein the plasma etching process conditions are as follows: the reaction gas is high-purity hydrogen with the purity of more than 99.999 percent, the air pressure of a vacuum chamber is 1.5kPa, the filament temperature is 2100 ℃, the temperature of the hard alloy cutter during treatment is 640 ℃, the treatment time is 25min, and the size of nano particles in the nano diamond coating obtained after treatment is about 90 nm.
Comparative example 1
The comparative example is a hard alloy cutter with a micro-nano diamond coating, and the preparation method comprises the following steps: directly depositing and growing a layer of nano diamond with certain thickness on the surface of a hard alloy cutter-an indexable face milling cutter.
Comparative example 2
The comparative example is a hard alloy cutter with a micro-nano diamond coating, and the preparation method comprises the following steps: firstly, a high-quality micron diamond coating is grown on the surface of a hard alloy cutter-an indexable face milling cutter, and then a nano coating is grown on the micron diamond coating in situ.
And (3) comparison test:
the hardness, young's modulus and friction coefficient of the coatings of the cemented carbide inserts of examples 1-4 and comparative examples 1-2 were subjected to performance tests, and the same materials were subjected to cutting and grinding tests using the cemented carbide inserts of each example and comparative example, and the service lives of the cemented carbide inserts at the time of damage were recorded, and the test results are shown in table 1. Wherein the coefficient of friction is the coefficient of friction tested under a force of 10N.
TABLE 1 results of Performance test of each example and comparative example
As can be seen from table 1, the hardness of the micro-nano diamond coating in examples 1 to 4 is much higher than that of comparative examples 1 and 2, and the service life index of the hard alloy tool in examples 1 to 4 is also much higher than that of comparative examples 1 and 2, which indicates that the bonding strength between the micro-nano diamond coating and the hard alloy tool is good for the hard alloy tool prepared by the preparation method provided by the present invention.
In addition, the service life index of the hard alloy cutter in the embodiments 1 and 4 is higher than that in the embodiments 2 and 3, which shows that the sand blasting in the pretreatment process can improve the bonding strength between the micro-nano diamond coating and the hard alloy cutter, so that the use frequency of the hard alloy cutter is improved.
Compared with example 4, the service life of example 4 is also longer than that of example 1, which shows that the pre-seeding treatment process can increase the bonding strength between the micro-nano diamond coating and the cemented carbide tool, thereby prolonging the service life.
In conclusion, the hard alloy cutter prepared by the preparation method provided by the invention has excellent bonding strength between the micro-nano diamond coating and the surface of the hard alloy cutter, and meanwhile, the micro-nano diamond coating has higher surface hardness and extremely low surface roughness, and the friction coefficient is lower than 0.1, so that the hard alloy cutter with the micro-nano diamond coating, which is prepared by the preparation method provided by the invention, integrates longer service life and higher precision, and has extremely strong market competitiveness.
The preparation method provided by the invention has simple process, can finish processing and manufacturing by adopting conventional equipment, and is beneficial to saving processing cost.
While particular embodiments of the present invention have been illustrated and described, it would be obvious that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention.
Claims (10)
1. A preparation method of a hard alloy cutter with a micro-nano diamond coating is characterized by comprising the following steps:
preparing a micron diamond coating on the surface of the hard alloy cutter, and then preparing a nano diamond coating on the surface layer of the micron diamond coating by etching to obtain the hard alloy cutter with the micro nano diamond coating.
2. The method for preparing a hard alloy cutter with a micro-nano diamond coating according to claim 1, wherein the hard alloy cutter is pretreated, and then the micro diamond coating is prepared on the surface of the hard alloy cutter.
3. The method for preparing the hard alloy cutter with the micro-nano diamond coating according to claim 2, wherein the pretreatment comprises a step of performing chemical etching treatment on the surface of the hard alloy cutter.
4. The method for preparing the hard alloy cutter with the micro-nano diamond coating according to claim 3, wherein the step of chemically etching comprises the following steps: etching with an alkali solution and then with an acid solution.
5. The method for preparing a cemented carbide tool with micro-nano diamond coating according to claim 4, wherein the alkali solution comprises K3[Fe(CN)]6An alkali solution consisting of KOH and water;
the acid solution comprises H2SO4And H2O2A composed acid solution;
the step of chemically etching comprises: placing a hard alloy cutter at K3[Fe(CN)]6Etching in alkali solution composed of KOH and water, removing alkali solution on the surface of the hard alloy cutter, and placing in H2SO4And H2O2Etching in the acid solution.
6. The method for preparing the hard alloy cutter with the micro-nano diamond coating according to claim 3, characterized by further comprising the step of pre-seeding the surface of the hard alloy cutter after chemical etching treatment;
the step of pre-seeding comprises: and placing the hard alloy cutter subjected to chemical etching treatment in diamond powder suspension for ultrasonic treatment.
7. The method for preparing a hard alloy cutter with a micro-nano diamond coating according to any one of claims 1 to 6, wherein the thickness of the prepared micro diamond coating is 1.5 to 3 microns.
8. The method for preparing a hard alloy cutter with a micro-nano diamond coating according to any one of claims 1 to 6, wherein the method for preparing the micro-nano diamond coating comprises the following steps: preparing a micron diamond coating by using a chemical vapor deposition method;
the technological parameters of the chemical vapor deposition method for preparing the micron diamond coating comprise: the volume fraction of the methane is 2-5 percent, the air pressure is 0.8-2.5kPa, the temperature range is 1800-2200 ℃, the temperature range of the hard alloy cutter during treatment is 600-650 ℃, and the treatment time is 1-2.5 h.
9. The method for preparing a hard alloy cutter with a micro-nano diamond coating according to any one of claims 1 to 6, wherein the etching comprises plasma etching;
the technological parameters for preparing the nano diamond coating by adopting plasma etching comprise: the air pressure range of the vacuum chamber is 1.5-2kPa, the filament temperature is 2000-2200 ℃, the temperature range of the hard alloy cutter during the treatment is 600-650 ℃, and the treatment time is 10-30 min.
10. A cemented carbide tool with a micro-nano diamond coating, characterized in that the cemented carbide tool with the micro-nano diamond coating is prepared according to the preparation method of any one of claims 1 to 9.
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| CN111286735A (en) * | 2020-03-25 | 2020-06-16 | 惠州市中德纳微科技有限公司 | Efficient composite liquid for pretreatment of diamond coating substrate of cutter and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0251264A1 (en) * | 1986-07-03 | 1988-01-07 | Mitsubishi Materials Corporation | Diamond-coated Tungsten carbide base sintered hard alloy material for insert of a cutting tool |
| CN1978310A (en) * | 2005-12-09 | 2007-06-13 | 中国科学院物理研究所 | Surface nano tip array and its preparing method |
| CN104233216A (en) * | 2014-10-09 | 2014-12-24 | 南京航空航天大学 | Preparation method of titanium-based boron-doped diamond electrode provided with nano-structure array on surface |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100480772B1 (en) * | 2000-01-05 | 2005-04-06 | 삼성에스디아이 주식회사 | Forming method of micro structure with surface roughness of nano scale |
-
2017
- 2017-12-28 CN CN201711468369.5A patent/CN109972115B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0251264A1 (en) * | 1986-07-03 | 1988-01-07 | Mitsubishi Materials Corporation | Diamond-coated Tungsten carbide base sintered hard alloy material for insert of a cutting tool |
| CN1978310A (en) * | 2005-12-09 | 2007-06-13 | 中国科学院物理研究所 | Surface nano tip array and its preparing method |
| CN104233216A (en) * | 2014-10-09 | 2014-12-24 | 南京航空航天大学 | Preparation method of titanium-based boron-doped diamond electrode provided with nano-structure array on surface |
Non-Patent Citations (4)
| Title |
|---|
| "‘Nano-rods" of single crystalline diamond";Y.Ando et al.;《Diamond and related materials》;20031031;第633-637页 * |
| "Design of nano/micro-structured diamond coating on cemented carbide";Zhang Lin et al.;《Key Engineering Materials》;20160520;第554-559页 * |
| "纳米金刚石膜-一种新的具有广阔应用前景的CVD金刚石";韩毅松等;《人工晶体学报》;20020430;第31卷(第2期);第158-163页 * |
| "酸浸+等离子体刻蚀YG6微米-纳米金刚石复合涂层工具研究";苗晋琦等;《金刚石与磨料磨具工程》;20051030;第18-23页 * |
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