CN108149219B - Diamond composite coating cutter and preparation method thereof - Google Patents
Diamond composite coating cutter and preparation method thereof Download PDFInfo
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- CN108149219B CN108149219B CN201711339858.0A CN201711339858A CN108149219B CN 108149219 B CN108149219 B CN 108149219B CN 201711339858 A CN201711339858 A CN 201711339858A CN 108149219 B CN108149219 B CN 108149219B
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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
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
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Abstract
The invention provides a diamond composite coating cutter and a preparation method thereof, wherein the preparation method comprises the following steps: placing a hard alloy substrate in a seed crystal solution and carrying out ultrasonic treatment, and forming diamond mixed seed crystals on the surface of the hard alloy substrate, wherein the seed crystal solution consists of diamond particles, silicon carbide powder and water; and then, taking a mixed gas of hydrogen, methane and tetramethylsilane as a reaction gas source, and depositing a diamond composite coating on the surface of the hard alloy substrate on which the diamond mixed seed crystal is formed by adopting a chemical vapor deposition method to obtain the diamond composite coating cutter. The invention also provides a diamond composite coating cutter prepared by the method, and the method can effectively improve the binding force between the coating and the hard alloy substrate and prolong the service life of the cutter.
Description
Technical Field
The invention belongs to the field of coated cutters, and particularly relates to a diamond composite coated cutter and a preparation method thereof.
Background
With the development of technology, the demand for industrial tools, such as carbon fiber and high silicon aluminum materials, is higher and higher, and the tools have extremely high wear resistance, and diamond coated tools are gradually paid attention to due to good hardness and wear resistance. However, the bonding force between the diamond coating and the hard alloy in the existing diamond coated cutter is weak, and the diamond coating is easy to fall off in the using process, thereby seriously influencing the service life of the diamond coated cutter.
At present, researchers have proposed various methods for enhancing the bonding force between the diamond coating and the substrate, but the method has strict requirements on the substrate in the process of preparing the diamond coating or has too complex pretreatment process, and meanwhile, the operation flow is very complicated in the production process, so that the quality of the diamond coating cutter is difficult to ensure. Therefore, the method for improving the bonding strength of the hard alloy and the diamond coating has low requirement on the substrate, and the pretreatment operation is simple and easy to implement, and has important practical significance.
Disclosure of Invention
In view of the above, the present invention provides a diamond composite coating cutting tool and a method for manufacturing the same, so as to solve the above problems.
Specifically, the invention adopts the following technical scheme:
a preparation method of a diamond composite coating cutter comprises the following steps:
placing a hard alloy substrate in a seed crystal solution for ultrasonic treatment, and forming diamond mixed seed crystals on the surface of the hard alloy substrate to obtain the seeded hard alloy substrate; wherein the seed crystal solution consists of diamond particles, silicon carbide powder and water;
and (3) depositing the diamond composite coating by using hydrogen, methane and tetramethylsilane mixed gas as a reaction gas source and depositing the diamond composite coating on the seeded hard alloy substrate by adopting a chemical vapor deposition method to obtain the diamond composite coating cutter.
Based on the above, the mass ratio of the diamond particles, the silicon carbide powder and water is 1: (25-35): 1000.
based on the above, the seed crystal solution is formed by mixing diamond particle suspension with the particle size of 5-10 nm and silicon carbide powder with the particle size of 0.2-0.6 mu m.
Based on the above, in the diamond particle suspension, the number concentration of the diamond particles is 1016~1019/g。
The preparation method of the diamond particle suspension comprises the following steps: and mixing diamond particles with the particle size of 5-10 nm and water, and performing ultrasonic treatment to obtain the diamond particle suspension.
Based on the above, the step of depositing the diamond composite coating comprises: depositing a diamond composite coating on the seeded hard alloy substrate for 10-12 hours by adopting a hot wire chemical deposition method under the conditions that the power of a hot wire is 8-10 kW, the pressure is 800Pa and the temperature of the hot wire is 2000-2300 ℃ to obtain the diamond composite coating cutter; in the process of depositing the diamond composite coating, the flow of the tetramethylsilane mixed gas is reduced to zero from 2500-3500 sccm, the flow of the methane gas is 28-32 sccm, and the flow of the hydrogen gas is increased to 2800-3300 sccm from zero.
Based on the above, the step of depositing the diamond composite coating includes controlling the flow rates of the tetramethylsilane mixed gas, the methane gas and the hydrogen gas in a segmented manner in the process of depositing the diamond composite coating, and the specific control manner includes the following steps:
firstly, controlling the flow of the tetramethylsilane mixed gas to be 2500-3500 sccm and the flow of the methane gas to be 28-32 sccm for 30-50 min;
then controlling the flow of the tetramethylsilane mixed gas to be 1800-2200 sccm, the flow of the methane gas to be 28-32 sccm and the flow of the hydrogen gas to be 800-1200 sccm for 30-50 min;
then controlling the flow of the tetramethylsilane mixed gas to be 800-1200 sccm, the flow of the methane gas to be 28-32 sccm and the flow of the hydrogen gas to be 1800-2200 sccm for 30-50 min;
then controlling the flow of the tetramethylsilane mixed gas to be 400-600 sccm, the flow of the methane gas to be 28-32 sccm and the flow of the hydrogen gas to be 2300-2600 sccm for 30-50 min;
and finally stopping introducing the tetramethylsilane mixed gas, adjusting the flow of the methane gas to be 28-32 sccm and the flow of the hydrogen gas to be 2800-3300 sccm for 8-8.5 hours, and forming the diamond composite coating on the surface of the hard alloy substrate to obtain the diamond composite coating cutter.
Based on the above, the tetramethylsilane mixed gas is composed of 97-99% by volume of hydrogen and 1-3% by volume of tetramethylsilane.
Based on the above, the preparation method of the diamond composite coating cutter further comprises the steps of cleaning and sand blasting the hard alloy substrate in sequence before the step of seeding.
A diamond composite coating cutter is prepared by the preparation method of the diamond composite coating cutter.
Compared with the prior art, the invention has outstanding substantive characteristics and remarkable progress. Specifically, the preparation method of the diamond composite coating cutter provided by the invention comprises the steps of seeding and depositing the diamond composite coating, wherein diamond particles and silicon carbide powder are attached to the surface of the hard alloy in the seeding step, so that seeding is provided for the growth of later-stage silicon carbide and diamond, the nucleation amount of the diamond and the silicon carbide is increased, and the deposition of the diamond and the silicon carbide is facilitated; in the process of depositing the composite coating, mainly depositing silicon carbide and a small amount of diamond on the surface of the hard alloy in the initial stage, then gradually reducing the flow of the tetramethylsilane mixed gas, reducing the silicon carbide deposited on the surface of the hard alloy, and finally, reducing the flow of the tetramethylsilane mixed gas to zero, wherein only the diamond is deposited on the surface of the hard alloy. Meanwhile, the invention also provides a cutter prepared by the preparation method of the diamond composite coating cutter, and the cutter has the advantages of good impact resistance and long service life and has wide application prospect.
Drawings
Fig. 1 is a schematic view of the construction of a diamond composite coated cutting tool according to the present invention.
In the figure: 1. a substrate; 2. silicon carbide; 3. diamond.
Detailed Description
The technical solution of the present invention is further described in detail by the following embodiments.
Example 1
A preparation method of a diamond composite coating cutter comprises the following steps:
preparing diamond particles with the grain diameter of 5-10 nm of a seed crystal solution, silicon carbide powder with the grain diameter of 0.2-0.6 mu m and water according to the mass ratio of 1: 30: 1000, weighing, and carrying out ultrasonic mixing on diamond particles to obtain a diamond particle suspension; uniformly mixing the silicon carbide powder and the diamond particle suspension to obtain a seed crystal solution; the diamond particles in the diamond particle suspension had a particle number concentration of 1016~1019/g;
The method comprises the following steps of (1) carrying out ultrasonic seeding on a hard alloy substrate in a seeding solution, forming diamond mixed seed crystals on the surface of the hard alloy substrate, and then drying to obtain the seeded hard alloy substrate;
the method comprises the following steps of depositing a diamond composite coating on the surface of a seeded hard alloy substrate by a hot wire chemical deposition method by taking hydrogen, methane and tetramethylsilane mixed gas as a reaction gas source under the conditions that the power of a hot wire is 10kW, the pressure is 800Pa and the temperature of the hot wire is 2100 ℃, and controlling the flow rates of the tetramethylsilane mixed gas, the methane gas and the hydrogen in a segmented manner in the process of depositing the diamond composite coating, wherein the specific control mode comprises the following steps: controlling the flow rate of the tetramethylsilane mixed gas to be 3000sccm and the flow rate of the methane gas to be 30sccm for 30 min; then controlling the flow of the tetramethylsilane mixed gas to be 2000sccm, the flow of the methane gas to be 30sccm and the flow of the hydrogen gas to be 1000sccm for 30 min; then controlling the flow of the tetramethylsilane mixed gas to be 1000sccm, the flow of the methane gas to be 30sccm and the flow of the hydrogen gas to be 2000sccm for 30 min; then controlling the flow of the tetramethylsilane mixed gas to be 500sccm, the flow of the methane gas to be 30sccm and the flow of the hydrogen gas to be 2500sccm for 30 min; finally stopping introducing the tetramethylsilane mixed gas, controlling the flow of the methane gas to be 30sccm and the flow of the hydrogen gas to be 3000sccm 8h, and forming the diamond composite coating on the surface of the seeded hard alloy substrate to obtain the diamond composite coating cutter with the structure shown in figure 1; wherein the tetramethylsilane mixed gas consists of 99% by volume of hydrogen and 1% by volume of tetramethylsilane.
Example 2
A preparation method of a diamond composite coating cutter comprises the following steps:
preparing diamond particles with the grain diameter of 5-10 nm of a seed crystal solution, 0.2-0.6 mu m of silicon carbide powder and water according to the mass ratio of 1: 30: 1000, weighing, and carrying out ultrasonic mixing on diamond particles to obtain a diamond particle suspension; uniformly mixing the silicon carbide powder and the diamond particle suspension to obtain a seed crystal solution; the diamond particles in the diamond particle suspension had a particle number concentration of 1016~1019/g;
The method comprises the following steps of (1) carrying out ultrasonic treatment on a hard alloy substrate in a seed crystal solution by using seed crystals, and forming diamond mixed seed crystals on the surface of the hard alloy substrate to obtain the seeded hard alloy substrate;
the method for depositing the diamond composite coating comprises the following steps of taking hydrogen, methane and tetramethylsilane mixed gas as a reaction gas source, adopting a hot wire chemical deposition method, depositing the diamond composite coating on the surface of the seeded hard alloy substrate under the conditions that the power of a hot wire is 8kW, the pressure is 800Pa and the temperature of the hot wire is 2000 ℃, and controlling the flow rates of the tetramethylsilane mixed gas, the methane gas and the hydrogen gas in a segmented mode in the process of depositing the diamond composite coating, wherein the specific control mode comprises the following steps: controlling the flow of the tetramethylsilane mixed gas to be 2500sccm and the flow of the methane gas to be 28sccm for 50 min; then controlling the flow rate of the tetramethylsilane mixed gas to be 1800sccm, the flow rate of the methane gas to be 32sccm and the flow rate of the hydrogen gas to be 800sccm for 50 min; then controlling the flow of the tetramethylsilane mixed gas to be 800sccm, the flow of the methane gas to be 28sccm and the flow of the hydrogen gas to be 1800sccm for 30 min; then controlling the flow rate of the tetramethylsilane mixed gas to be 400sccm, the flow rate of the methane gas to be 28sccm and the flow rate of the hydrogen gas to be 2300sccm for 50 min; and finally stopping introducing the tetramethylsilane mixed gas, controlling the flow of the methane gas to be 28sccm and the flow of the hydrogen gas to be 2800sccm 8.5h, and forming the diamond composite coating on the surface of the seeded hard alloy substrate to obtain the diamond composite coating cutter, wherein the tetramethylsilane mixed gas consists of the hydrogen gas with the volume fraction of 97% and the tetramethylsilane gas with the volume fraction of 3%.
Example 3
A preparation method of a diamond composite coating cutter comprises the following steps:
preparing diamond particles with the grain diameter of 5-10 nm of a seed crystal solution, 0.2-0.6 mu m of silicon carbide powder and water according to the mass ratio of 1: 30: 1000, weighing, and carrying out ultrasonic mixing on diamond particles to obtain a diamond particle suspension; uniformly mixing the silicon carbide powder and the diamond particle suspension to obtain a seed crystal solution; in the diamond particle suspensionThe diamond particles have a particle number concentration of 1016~1019/g;
The method comprises the following steps that (1) a hard alloy substrate is cleaned and subjected to sand blasting treatment in sequence through seed crystals, then the hard alloy substrate is placed in a seed crystal solution for ultrasonic treatment, and diamond mixed seed crystals are formed on the surface of the hard alloy substrate to obtain the seeded hard alloy substrate;
the method comprises the following steps of depositing a diamond composite coating on the surface of a seeded hard alloy substrate by a hot wire chemical deposition method under the conditions that the power of a hot wire is 9kW, the pressure is 800Pa and the temperature of the hot wire is 2300 ℃, and controlling the flow rates of tetramethylsilane mixed gas, methane gas and hydrogen gas in a segmented manner in the process of depositing the diamond composite coating, wherein the specific control mode comprises the following steps: firstly, controlling the flow of the tetramethylsilane mixed gas to be 3500sccm and the flow of the methane gas to be 32sccm for 40 min; then controlling the flow rate of the tetramethylsilane mixed gas to be 2200sccm, the flow rate of the methane gas to be 31sccm and the flow rate of the hydrogen gas to be 1200sccm for 45 min; then controlling the flow rate of the tetramethylsilane mixed gas to be 1200sccm, the flow rate of the methane gas to be 32sccm and the flow rate of the hydrogen gas to be 2200sccm 45 min; then controlling the flow rate of the tetramethylsilane mixed gas to be 600sccm, the flow rate of the methane gas to be 32sccm and the flow rate of the hydrogen gas to be 2600sccm for 35 min; and finally stopping introducing the tetramethylsilane mixed gas, controlling the flow of the methane gas to be 32sccm and the flow of the hydrogen gas to be 3300sccm for 8.5 hours, and forming the diamond composite coating on the surface of the seeded hard alloy substrate to obtain the diamond composite coating cutter.
Wherein the tetramethylsilane mixed gas consists of 98% by volume of hydrogen and 2% by volume of tetramethylsilane.
Comparative experiment 1
The comparative experiment differs from example 1 in that: and replacing the tetramethylsilane mixed gas with an equal amount of hydrogen.
The comparative experiment differs from example 1 in that: the flow of the tetramethylsilane mixed gas is unchanged in the deposition process.
Comparative experiment 3
The comparative experiment differs from example 1 in that: which does not include the step of seeding.
Performance characterization
The coating bonding force of the diamond composite coating cutters prepared in the examples 1 to 3 and the comparative experiment was tested by using a sand blasting method, and the sand blasting pressure was 4 × 105Pa, the aperture of the nozzle is 1mm, silicon carbide with the grain diameter of 0.5 μm is selected, the surface of the coating of the diamond composite coating cutter is vertically sprayed, the time required for spraying the coating is recorded, and the test results are shown in Table 1.
TABLE 1 Diamond composite coated cutting tools prepared in examples 1-3 and comparative experiments 1-3
Coating bonding force of
As can be seen from Table 1, the preparation method of the diamond composite coating cutter provided by the invention can effectively improve the bonding force between the diamond coating and the hard alloy substrate.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention and not to limit it; although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art will understand that: modifications to the specific embodiments of the invention or equivalent substitutions for parts of the technical features may be made; without departing from the spirit of the present invention, it is intended to cover all aspects of the invention as defined by the appended claims.
Claims (3)
1. A preparation method of a diamond composite coating cutter comprises the following steps:
seed crystal, namely placing a hard alloy substrate in a seed crystal solution and carrying out ultrasonic treatment to form diamond mixture on the surface of the hard alloy substrateSeed crystals are combined to obtain a seeded hard alloy matrix; wherein the seed crystal solution is formed by mixing diamond particle suspension with the particle size of 5-10 nm and silicon carbide powder with the particle size of 0.2-0.6 mu m; the mass ratio of the diamond particles to the silicon carbide powder to water is 1: (25-35): 1000, parts by weight; in the diamond particle suspension, the diamond particles had a particle number concentration of 1016~1019/g;
Depositing a diamond composite coating, namely depositing the diamond composite coating on the seeded hard alloy substrate for 10-12 hours by using a hot wire chemical deposition method by taking a mixed gas of hydrogen, methane and tetramethylsilane as a reaction gas source under the conditions that the power of a hot wire is 8-10 kW, the pressure is 800Pa and the temperature of the hot wire is 2000-2300 ℃, so as to obtain a diamond composite coating cutter;
wherein, in the process of depositing the diamond composite coating, the flow rates of the tetramethylsilane mixed gas, the methane gas and the hydrogen gas are controlled in a segmented manner, and the specific control mode comprises the following steps:
firstly, controlling the flow of the tetramethylsilane mixed gas to be 2500-3500 sccm and the flow of the methane gas to be 28-32 sccm for 30-50 min;
then controlling the flow of the tetramethylsilane mixed gas to be 1800-2200 sccm, the flow of the methane gas to be 28-32 sccm and the flow of the hydrogen gas to be 800-1200 sccm for 30-50 min;
then controlling the flow of the tetramethylsilane mixed gas to be 800-1200 sccm, the flow of the methane gas to be 28-32 sccm and the flow of the hydrogen gas to be 1800-2200 sccm for 30-50 min;
then controlling the flow of the tetramethylsilane mixed gas to be 400-600 sccm, the flow of the methane gas to be 28-32 sccm and the flow of the hydrogen gas to be 2300-2600 sccm for 30-50 min;
finally stopping introducing the tetramethylsilane mixed gas, and adjusting the flow of the methane gas to be 28-32 sccm and the flow of the hydrogen gas to be 2800-3300 sccm for 8-8.5 hours;
the tetramethylsilane mixed gas consists of 97-99% of hydrogen by volume fraction and 1-3% of tetramethylsilane gas by volume fraction.
2. The method for preparing a diamond composite coated cutting tool according to claim 1, further comprising the step of cleaning and blasting the cemented carbide substrate in sequence before the step of seeding.
3. A diamond composite coated cutting tool, characterized in that it is manufactured by the method of manufacturing a diamond composite coated cutting tool according to claim 1 or 2.
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CN110983293A (en) * | 2019-12-26 | 2020-04-10 | 广东省新材料研究所 | Hard alloy part with diamond coating, preparation method and application thereof |
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CN113718226A (en) * | 2021-09-03 | 2021-11-30 | 科汇纳米技术(深圳)有限公司 | Preparation method of hard alloy material surface diamond layer, hard alloy material and application thereof |
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