CN107740067B - Chemical vapor deposition device and method for micro-cutter diamond coating - Google Patents
Chemical vapor deposition device and method for micro-cutter diamond coating Download PDFInfo
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- CN107740067B CN107740067B CN201710900693.3A CN201710900693A CN107740067B CN 107740067 B CN107740067 B CN 107740067B CN 201710900693 A CN201710900693 A CN 201710900693A CN 107740067 B CN107740067 B CN 107740067B
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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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Abstract
A chemical vapor deposition device and a chemical vapor deposition method for a micro-cutter diamond coating belong to the technical field of chemical vapor deposition preparation of diamond films. The vacuum pump is communicated with the vacuum reaction chamber through a vacuum needle valve, the hydrogen cylinder, the argon cylinder and the methane cylinder are communicated with the mixing box, the air inlet needle valve is fixed on a furnace cover of the vacuum reaction chamber, the pressure control device is communicated with the vacuum reaction chamber, the electrode assembly is fixed in the vacuum reaction chamber, the workbench is arranged in the vacuum reaction chamber, the micro-cutter is fixed on the workbench, two cables are led out from a heating power supply and are connected with the electrode assembly, the end part of a probe of the thermocouple is pasted with a hard alloy sheet, the infrared thermometer is arranged outside the vacuum reaction chamber through a support arranged on the infrared thermometer, four cold water pipes are externally connected with the cold water machine, two of the cold water pipes are communicated with the furnace cover of the vacuum reaction chamber, the other two cold water pipes are communicated with a furnace. The method is used for chemical vapor deposition of the diamond coating of the micro-cutter.
Description
Technical Field
The invention belongs to the technical field of diamond film chemical vapor deposition preparation, and particularly relates to a chemical vapor deposition device and a chemical vapor deposition method for a micro-cutter diamond coating.
Background
In recent years, micro products and related components are applied more and more widely in aerospace, medical treatment, machinery and biochemical equipment, so that micro-manufacturing technology is rapidly developed in the world, and higher requirements on the quality of micro-machining are provided. Research shows that improving the comprehensive cutting capacity of the micro-cutter material is an effective way to improve the machining precision and the cutting efficiency.
Diamond is the hardest substance in nature, and is an ideal material for abrasives and cutting tools because of its special properties such as high wear resistance, good thermal conductivity, and excellent chemical stability. However, single crystal diamond is extremely brittle and cannot be adapted to a processing environment with high strength or high impact load. Therefore, the single crystal diamond tool has a limited application field due to its disadvantages of high cost and poor impact resistance. However, there is a wide development space for a diamond film having good economical efficiency. In selecting a tool for machining, it is generally desirable that the tool have both a high hardness to ensure good wear resistance and good toughness to prevent chipping of the tool. The combination of the hard alloy substrate and the Chemical Vapor Deposition (CVD) diamond film just meets the requirement, because the combination of the hard alloy substrate and the CVD diamond film enables the cutter to show the high hardness and the good wear resistance of diamond, the toughness and the good impact resistance of the hard alloy, and in addition, the lower manufacturing cost enables the cutter to have wide application prospect in the field of micro-machining.
Chemical Vapor Deposition (CVD) diamond has excellent mechanical properties, extremely high hardness, low coefficient of friction, strong wear resistance, and stable surface chemical properties. Compared with single crystal diamond and polycrystalline diamond (PCD) compacts, the CVD diamond coating has low preparation cost, is suitable for substrates with complex shapes, and is easy to realize large-scale industrial production, so the CVD diamond coating is an ideal material for manufacturing micro cutters. The CVD diamond coating cutter has obvious advantages when processing non-ferrous metals and alloys thereof, composite materials, high polymer materials, inorganic non-metallic materials and other materials which are difficult to process.
At present, the chemical vapor deposition device aiming at the diamond coating of the micro-cutter in China is lack of a high-efficiency and economical commercialized product. And foreign related products have the defects of high price, low growth rate of the diamond film and the like, are usually only suitable for preparing large-area diamond coatings, and are difficult to ensure the coating quality in a small size range and complex morphology for micro-cutters. In the field of micro-machining, the demand of CVD diamond micro-cutters is huge, so that the development of a diamond coating micro-cutter chemical vapor deposition device and the verification of an effective deposition process thereof have very important significance.
Disclosure of Invention
The invention aims to solve the problem of preparing a diamond film of a micro-cutter, and discloses a chemical vapor deposition device and a chemical vapor deposition method for a diamond coating of the micro-cutter.
The purpose of the invention is realized by the following technical scheme:
the chemical vapor deposition device for the micro-cutter diamond coating comprises a gas supply system, a temperature control system and a vacuum reaction system, wherein the gas supply system comprises a hydrogen cylinder, an argon cylinder, a methane cylinder, a gas mixing box and a gas inlet needle valve, and the temperature control system comprises a heating power supply, a thermocouple display meter, an infrared thermometer, an electrode assembly, a workbench, a thermocouple and a compensation lead; the vacuum reaction system comprises a vacuum reaction chamber, a workbench base, a pressure control device, a water cooler, a vacuum pump, a vacuum meter and a vacuum needle valve;
the vacuum pump pass through vacuum needle valve and vacuum reaction chamber intercommunication, vacuum reaction chamber fix in workstation base top, the vacuum pump is fixed at workstation base bottom, hydrogen cylinder, argon gas cylinder and methane-generating cylinder pass through hose, air inlet needle valve and mixing box intercommunication, the air inlet needle valve fix on vacuum reaction chamber furnace lid, air inlet needle valve and vacuum reaction chamber intercommunication, pressure control device and vacuum reaction chamber intercommunication, electrode subassembly fix in vacuum reaction chamber, be fixed with three heater on the electrode subassembly, the workstation setting in vacuum reaction chamber, the microtool inserts in the graphite cover on the workstation to fix on the workstation through holding screw, heating power supply fix on the workstation base, heating power supply links to each other with two cable conductor one end, two cable conductor other ends be connected with electrode subassembly, the thermocouple is arranged on a thermocouple fixing table, the thermocouple fixing table is arranged in a vacuum reaction chamber, a hard alloy sheet is attached to the end portion of a probe of the thermocouple, one end of a compensation lead is connected to the thermocouple, the other end of the compensation lead is connected with a thermocouple display meter, the thermocouple display meter is arranged outside the vacuum reaction chamber, an infrared thermometer is arranged outside the vacuum reaction chamber through a support arranged on the infrared thermometer, four cold water pipes are externally connected with a water cooler, two of the cold water pipes are communicated with a water tank of a furnace cover of the vacuum reaction chamber, the other two cold water pipes are communicated with a water channel of a furnace body of the vacuum reaction chamber, and the vacuum meter is arranged on the furnace cover of the vacuum reaction chamber.
The chemical vapor deposition method for the diamond coating of the micro-cutter comprises the following steps:
the method comprises the following steps: fixing the micro-cutter on a workbench, firstly starting a water cooling machine to ensure that a chemical vapor deposition device of the diamond coating of the micro-cutter is in a cooling state, then working the device, pumping a vacuum reaction chamber into a vacuum state by a vacuum pump, and ensuring that the air pressure value is between 0.8 and 1.5 Pa.
Step two: after the vacuum reaction chamber is vacuumized, valves of a hydrogen bottle, an argon bottle and a methane bottle are opened, hydrogen, methane and argon are mixed according to the volume ratio of 93:4:3 and then are introduced into the vacuum reaction chamber, and the air pressure in the vacuum reaction chamber is kept within the range of 2-5 kPa;
step three: starting a heating power supply, heating the hot wire by an electrode assembly, measuring the temperature of the hot wire by an infrared thermometer, adjusting the heating power supply according to the measured temperature, and further controlling the temperature of the hot wire to be 2200-2500 ℃;
step four: hydrogen and methane in the vacuum reaction chamber generate chemical vapor deposition reaction under the action of a high-temperature hot wire, and the preparation of the diamond coating on the surface of the micro-cutter is finished after 5-7 hours of chemical deposition reaction;
step five: and after the reaction is finished, stopping the work of the heating power supply 5, gradually cooling the vacuum reaction chamber to room temperature under the action of circulating cooling water, closing valves of a hydrogen cylinder and a methane cylinder, introducing argon gas into the vacuum reaction chamber by a gas supply system to enable the vacuum reaction chamber to reach a normal pressure state, stopping the work of the gas supply system, opening the vacuum reaction chamber, checking the quality of the diamond coating on the surface of the micro-cutter, and finishing the deposition process.
Compared with the prior art, the invention has the beneficial effects that:
the chemical vapor deposition device for the diamond coating of the micro-cutter has the characteristics of small space volume, high deposition quality of the diamond coating, suitability for coating of the micro-cutter and the like. The chemical vapor deposition device for the micro-cutter diamond coating utilizes the principle of chemical reaction of generating diamond by methane and hydrogen under specific conditions to form a film attached to the surface of the micro-cutter. The whole device consists of an air supply system, a temperature control system and a vacuum reaction system, and adopts new process steps, so that the aims of accelerating the growth rate of the diamond film on the substrate of the micro-cutter and improving the deposition quality of the diamond film on the surface of the micro-cutter can be fulfilled. The chemical vapor deposition device for the diamond coating of the micro-cutter has the characteristics of compact structure, low cost, high reliability and capability of producing the CVD coating diamond cutter in batch, and can realize the deposition of the diamond film with the micron-sized thickness.
The invention realizes the system integration of the chemical vapor deposition diamond coating and solves the problems of the overall design and the process flow of the hot wire method CVD coating of the diamond micro-cutter. The device and the method can accelerate the growth rate of the diamond on the substrate of the micro-cutter, improve the deposition quality of the diamond film on the surface of the micro-cutter, and reduce the volume of the device, thereby reducing the production cost.
Drawings
FIG. 1 is a front view of a chemical vapor deposition apparatus for micro-tool diamond coating of the present invention;
FIG. 2 is a front sectional view of a vacuum reaction chamber;
FIG. 3 is a left side view of the vacuum reaction chamber;
FIG. 4 is an enlarged view of a portion of FIG. 1 at A;
FIG. 5 is a partial enlarged view of FIG. 4 at B;
fig. 6 is a partially enlarged view of fig. 2 at C.
In the figure: the gas supply system comprises a hydrogen cylinder 1, an argon cylinder 2, a methane cylinder 3, a gas mixing box 4 and a gas inlet needle valve 14, and the temperature control system comprises a heating power supply 5, a thermocouple display meter 6, an infrared thermometer 7, an electrode assembly 16, a workbench 17, a thermocouple 20 and a compensation lead 21; the vacuum reaction system comprises a vacuum reaction chamber 8, a workbench base 10, a pressure control device 11, a water cooling machine 12, a vacuum pump 13, a vacuum gauge 15 and a vacuum needle valve 19.
Detailed Description
The technical solution of the present invention is further described below with reference to the accompanying drawings, but not limited thereto, and any modification or equivalent replacement of the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention shall be covered by the protection scope of the present invention.
The first embodiment is as follows: as shown in fig. 1 to 6, the present embodiment discloses a chemical vapor deposition apparatus for micro-cutter diamond coating, which comprises a gas supply system, a temperature control system and a vacuum reaction system, wherein the gas supply system comprises a hydrogen cylinder 1, an argon cylinder 2, a methane cylinder 3, a gas mixing box 4 and a gas inlet needle valve 14, and the temperature control system comprises a heating power supply 5, a thermocouple display meter 6, an infrared thermometer 7, an electrode assembly 16, a workbench 17, a thermocouple and a compensation lead 21; the vacuum reaction system comprises a vacuum reaction chamber 8, a workbench base 10, a pressure control device 11, a water cooler 12, a vacuum pump 13, a vacuum meter 15 and a vacuum needle valve 19;
vacuum pump 13 communicate with vacuum reaction chamber 8 through vacuum needle valve 19 (with vacuum pump 13 with reaction chamber 8 take out vacuum state, atmospheric pressure value control between 0.8 ~ 1.5 Pa), vacuum reaction chamber 8 fix in workstation base 10 top, vacuum pump 13 fixes bottom in workstation base 10, hydrogen cylinder 1, argon gas cylinder 2 and methane cylinder 3 communicate with mixing box 4 through hose, air inlet needle valve 14 (open the valve of hydrogen cylinder 1, argon gas cylinder 2 and methane cylinder 3, gas lets in gas mixing box 4 through hose, air inlet needle valve 14 in, hose and air inlet needle valve 14 pass through hose joint fixed connection), air inlet needle valve 14 fix on vacuum reaction chamber 8 furnace lid, air inlet needle valve 14 communicates with vacuum reaction chamber 8 (the open-close state of air inlet needle valve 14 is controlled by the solenoid valve), pressure control device 11 and vacuum reaction chamber 8 communicate (make vacuum reaction chamber 8 communicate under pressure control device 11's control effect) The pressure in the chamber 8 is kept between 2 kPa and 5kPa to ensure the smooth proceeding of the chemical vapor deposition. Opening the argon bottle 2 while introducing hydrogen and methane, namely three-channel gas supply is adopted, the flow of three channels of gas is controlled by a mass flow meter, the deposition time is 6 hours, the standard reaction flow is 300 ml/min, the hydrogen in the mixed gas accounts for 93%, the capacity of the hydrogen bottle 1 is determined to be 10L, the capacities of the methane bottle 3 and the argon bottle 2 are 4L, and the volume ratio of the hydrogen, the methane and the argon is 93:4:3, the electrode assembly 16 is fixed in the vacuum reaction chamber 8, three hot wires are fixed on the electrode assembly 16 (the electrode assembly heats the hot wires to 2200-2500 ℃, the diameter of the hot wires is 1mm), the workbench 17 is arranged in the vacuum reaction chamber 8, a micro-cutter is inserted into a graphite sleeve on the workbench 17 and is fixed on the workbench 17 through a set screw (the workbench 17 and publication No. CN107058972A, publication No. 2017, 18 h 08-18 h), The invention discloses a three-dimensional precise displacement workbench for a micro-cutter coating applied in a thermal vacuum environment, which has the same structure and can realize lifting and plane displacement, wherein a heating power supply 5 is fixed on a workbench base 10, the heating power supply 5 is connected with two cable wires, the two cable wires are connected with an electrode assembly 16 (power is supplied to a hot wire through the electrode assembly 16) through a crimping terminal and a nut, a thermocouple 20 is arranged on a thermocouple fixing table, the thermocouple fixing table is arranged in a vacuum reaction chamber 8, a hard alloy sheet is adhered to the probe end part of the thermocouple 20, one end of a compensation lead 21 is connected to the thermocouple 20, the other end of the compensation lead 21 is connected with a thermocouple display table 6, the thermocouple display table 6 is arranged outside the vacuum reaction chamber 8 (because the thermocouple 20 cannot directly measure the surface temperature of the micro-cutter blade, the temperature of the hard alloy sheet is close to that of the cutting edge by sticking the hard alloy sheet on the probe end of the thermocouple 20, the surface temperature of the cutting edge is approximately measured by measuring the temperature of the hard alloy sheet, the infrared thermometer 7 is arranged outside the vacuum reaction chamber 8 through a self-provided bracket (the temperature of a hot wire is measured through a vacuum observation window on the vacuum reaction chamber 8, the bracket on the infrared thermometer 7 can realize the left-right and up-down movement of the infrared thermometer 9, so that a better measurement view field is obtained, and a more accurate measurement result is obtained), the water cooler 12 is externally connected with four cold water pipes, wherein two cold water pipes (respectively through cold water joints) are communicated with a water tank of a furnace cover of the vacuum reaction chamber 8, and the other two cold water pipes (respectively through cold water joints) are communicated with a water channel of a furnace body of the vacuum reaction chamber 8 (the vacuum reaction chamber 8 is communicated with the application publication No. CN106498367A, The structure of the invention patent application, which is entitled "compact vacuum reaction device for chemical vapor deposition of diamond film" and published on 2017, 03 and 15, is the same), and the vacuum gauge 15 is mounted on a furnace cover of the vacuum reaction chamber 8 (used for obtaining the air pressure information in the vacuum reaction chamber 8 and detecting the reaction process in a vacuum observation window of the vacuum reaction chamber 8 so as to ensure the deposition quality of the diamond film on the surface of the micro-cutter) (through a ball valve and a pressure gauge pipe joint).
The second embodiment is as follows: as shown in fig. 1 and 4, the embodiment is further explained for the first embodiment, and the chemical vapor deposition device for micro-cutter diamond coating further comprises a dust cover 9; the dust cover 9 is buckled on the vacuum reaction chamber 8 (for convenient observation and adjustment, the dust cover 9 is not fixedly connected with the workbench base 10).
The third concrete implementation mode: as shown in fig. 1-3, this embodiment is a further explanation of the first embodiment, vacuum needle valve 19 connect with vacuum reaction chamber 8 through clamp 18, KF external thread adapter and KF (namely vacuum needle valve 19 is connected with KF external thread adapter through the screw thread, KF connects with vacuum reaction chamber 8 cooperation and is connected, KF external thread adapter and KF connect through the clamp connection, can guarantee the gas tightness).
The fourth concrete implementation mode: as shown in fig. 1, the first embodiment is further described, and the hydrogen cylinder 1, the argon cylinder 2, and the methane cylinder 3 are all provided with pressure reducing valves (capable of ensuring the output of the gas pressure within a certain range and protecting the pipelines connected with the gas pressure).
The fifth concrete implementation mode: this embodiment is further described with respect to the first embodiment, wherein the three filaments are arranged in a spatially horizontal parallel arrangement (to form a uniform temperature field near the microtome substrate).
The sixth specific implementation mode: as shown in fig. 2, fig. 3 and fig. 6, this embodiment is a further description of the first embodiment, the electrode assembly 16 enters the vacuum reaction chamber 8 through the KF flange and the KF joint, the KF flange and the KF joint are connected through the clamp 18 and the O-ring (i.e., the lid of the vacuum reaction chamber 8 is connected with the KF joint in a matching manner, the O-ring is placed between the KF flange and the KF joint, and the KF flange and the KF joint are connected through the clamp 18 and press the O-ring tightly, so as to ensure the air tightness).
The seventh embodiment: in this embodiment, the first embodiment is further explained, and the thermocouple 20 is a K-type thermocouple (the K-type thermocouple is currently most widely used and has a lower price).
The specific implementation mode is eight: as shown in fig. 1, 3 and 4, the first embodiment is further described, and the infrared thermometer 7 is an MR1SCSF two-color infrared thermometer made of retamazon.
The specific implementation method nine: as shown in fig. 1-6, the present embodiment discloses a chemical vapor deposition method for micro-tool diamond coating using the apparatus according to any one of the first to eighth embodiments, comprising the following steps:
the method comprises the following steps: fixing the micro-cutter on a workbench 17, firstly starting a water cooling machine 12 to ensure that the chemical vapor deposition device of the diamond coating of the micro-cutter is in a cooling state, then working the device, and pumping a vacuum reaction chamber 8 into a vacuum state by a vacuum pump 13 to ensure that the air pressure value is between 0.8 and 1.5 Pa.
Step two: after the vacuum reaction chamber 8 is vacuumized, valves of a hydrogen cylinder 1, an argon cylinder 2 and a methane cylinder 3 are opened, hydrogen, methane and argon are mixed according to the volume ratio of 93:4:3 (the gas is introduced into a gas mixing box 4 through a hose to form mixed gas), the mixed gas is introduced into the vacuum reaction chamber 8, the air pressure in the vacuum reaction chamber 8 is kept within the range of 2-5kPa (in order to achieve the gas protection and the cleaning requirement of the vacuum reaction chamber 8, the argon cylinder 2 is opened while the hydrogen and the methane are introduced, three-channel gas supply is adopted, the flow of three channels of gas is controlled by a mass flow meter, and the precision can reach +/-1% full range);
step three: starting the heating power supply 5, heating the hot wire by the electrode assembly 16, measuring the temperature of the hot wire by the infrared thermometer 7, adjusting the heating power supply 5 according to the measured temperature, and further controlling the temperature of the hot wire to be 2200-2500 ℃ (in the chemical vapor deposition reaction process, heating the hot wire to 2200-2500 ℃ by the electrode assembly 16 to decompose gas);
step four: hydrogen and methane in the vacuum reaction chamber 8 generate chemical vapor deposition reaction under the action of a high-temperature hot wire, and the preparation of the diamond coating on the surface of the micro-cutter is completed after 5-7 hours of chemical deposition reaction;
step five: after the reaction is finished, the heating power supply 5 stops working, the vacuum reaction chamber 8 is gradually cooled to room temperature under the action of circulating cooling water, valves of the hydrogen cylinder 1 and the methane cylinder 3 are closed, an air supply system introduces argon into the vacuum reaction chamber 8 to enable the vacuum reaction chamber 8 to reach a normal pressure state, the air supply system stops working, the vacuum reaction chamber 8 is opened, the quality of the diamond coating on the surface of the micro-cutter is checked, and the deposition process is finished.
In the invention, a hydrogen cylinder 1, an argon cylinder 2, a methane cylinder 3, an air inlet needle valve 14, a thermocouple display table 6, an infrared thermometer 7, an electrode assembly 16, a water cooler 12, a vacuum pump 13, a vacuum gauge 15, a vacuum needle valve 19 and the like are all outsourced products.
Claims (8)
1. A chemical vapor deposition device for micro-cutter diamond coating is characterized in that: the device comprises a gas supply system, a temperature control system and a vacuum reaction system, wherein the gas supply system comprises a hydrogen cylinder (1), an argon cylinder (2), a methane cylinder (3), a gas mixing box (4) and a gas inlet needle valve (14), and the temperature control system comprises a heating power supply (5), a thermocouple display meter (6), an infrared thermometer (7), an electrode assembly (16), a workbench (17), a thermocouple (20) and a compensation lead (21); the vacuum reaction system comprises a vacuum reaction chamber (8), a workbench base (10), a pressure control device (11), a water cooling machine (12), a vacuum pump (13), a vacuum meter (15) and a vacuum needle valve (19);
vacuum pump (13) communicate with vacuum reaction chamber (8) through vacuum needle valve (19), vacuum reaction chamber (8) fix in workstation base (10) top, bottom in vacuum pump (13) are fixed in workstation base (10), hydrogen cylinder (1), argon gas bottle (2) and methane-generating cylinder (3) communicate with mixing box (4) through hose, air inlet needle valve (14) fix on vacuum reaction chamber (8) furnace lid, air inlet needle valve (14) communicate with vacuum reaction chamber (8), pressure control device (11) communicate with vacuum reaction chamber (8), electrode subassembly (16) fix in vacuum reaction chamber (8), be fixed with three heater on electrode subassembly (16), workstation (17) set up in vacuum reaction chamber (8), the microtooler inserts in the graphite cover on workstation (17), the heating power supply (5) is fixed on a workbench (17) through a set screw, the heating power supply (5) is connected with one end of two cables, the other end of the two cables is connected with an electrode assembly (16), a thermocouple (20) is arranged on a thermocouple fixing table, the thermocouple fixing table is arranged in a vacuum reaction chamber (8), a hard alloy sheet is pasted on the probe end part of the thermocouple (20), one end of a compensation lead (21) is connected on the thermocouple (20), the other end of the compensation lead (21) is connected with a thermocouple display meter (6), the thermocouple display meter (6) is arranged outside the vacuum reaction chamber (8), the infrared thermometer (7) is arranged outside the vacuum reaction chamber (8) through a self-contained bracket, and the water cooler (12) is externally connected with four cold water pipes, two of the cold water pipes are communicated with a water tank of a furnace cover of the vacuum reaction chamber (8), the other two cold water pipes are communicated with a water channel of a furnace body of the vacuum reaction chamber (8), and the vacuum meter (15) is arranged on the furnace cover of the vacuum reaction chamber (8); and the vacuum needle valve (19) is connected with the vacuum reaction chamber (8) through a hoop (18), a KF external thread adapter and a KF connector.
2. The micro-tool diamond coated chemical vapor deposition apparatus of claim 1, wherein: the chemical vapor deposition device for the micro-cutter diamond coating further comprises a dust cover (9); the dust cover (9) is buckled on the vacuum reaction chamber (8).
3. The micro-tool diamond coated chemical vapor deposition apparatus of claim 1, wherein: and the hydrogen cylinder (1), the argon cylinder (2) and the methane cylinder (3) are all provided with pressure reducing valves.
4. The micro-tool diamond coated chemical vapor deposition apparatus of claim 1, wherein: the three hot wires are arranged in a spatial horizontal parallel mode.
5. The micro-tool diamond coated chemical vapor deposition apparatus of claim 1, wherein: electrode subassembly (16) get into vacuum reaction chamber (8) through KF flange and KF joint, KF flange and KF joint pass through clamp (18) and O type sealing washer and connect.
6. The micro-tool diamond coated chemical vapor deposition apparatus of claim 1, wherein: the thermocouple (20) is a K-type thermocouple.
7. The micro-tool diamond coated chemical vapor deposition apparatus of claim 1, wherein: the infrared thermometer (7) adopts an MR1SCSF two-color infrared thermometer of Rathamaran.
8. A chemical vapor deposition method for realizing micro-cutter diamond coating by using the device of any one of claims 1 to 7, which is characterized in that: the method comprises the following steps:
the method comprises the following steps: fixing the micro cutter on a workbench (17), firstly starting a water cooling machine (12) to ensure that a chemical vapor deposition device of the diamond coating of the micro cutter is in a cooling state, then working the device, and pumping a vacuum reaction chamber (8) into a vacuum state by a vacuum pump (13) to ensure that the air pressure value is between 0.8 and 1.5 Pa;
step two: after the vacuum reaction chamber (8) is vacuumized, valves of a hydrogen bottle (1), an argon bottle (2) and a methane bottle (3) are opened, hydrogen, methane and argon are mixed according to the volume ratio of 93:4:3 and then are introduced into the vacuum reaction chamber (8), and the air pressure in the vacuum reaction chamber (8) is kept within the range of 2-5 kPa;
step three: starting the heating power supply (5), heating the hot wire by the electrode assembly (16), measuring the temperature of the hot wire by the infrared thermometer (7), adjusting the heating power supply (5) according to the measured temperature, and further controlling the temperature of the hot wire to be 2200-2500 ℃;
step four: hydrogen and methane in the vacuum reaction chamber (8) generate chemical vapor deposition reaction under the action of a high-temperature hot wire, and the preparation of the diamond coating on the surface of the micro-cutter is completed after 5-7 hours of chemical deposition reaction;
step five: and after the reaction is finished, stopping the work of the heating power supply (5), gradually cooling the vacuum reaction chamber (8) to room temperature under the action of circulating cooling water, closing valves of the hydrogen cylinder (1) and the methane cylinder (3), introducing argon into the vacuum reaction chamber (8) by the gas supply system to enable the interior of the vacuum reaction chamber (8) to reach a normal pressure state, stopping the work of the gas supply system, opening the vacuum reaction chamber (8), checking the quality of the diamond coating on the surface of the micro-cutter, and finishing the deposition process.
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| CN201710900693.3A CN107740067B (en) | 2017-09-28 | 2017-09-28 | Chemical vapor deposition device and method for micro-cutter diamond coating |
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| CN201710900693.3A CN107740067B (en) | 2017-09-28 | 2017-09-28 | Chemical vapor deposition device and method for micro-cutter diamond coating |
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| CN107740067B true CN107740067B (en) | 2020-03-13 |
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| CN113699518B (en) * | 2021-08-27 | 2023-06-20 | 浙江六方碳素科技有限公司 | Low-temperature preparation device for silicon carbide coating on metal surface |
| CN117947404B (en) * | 2024-03-27 | 2024-05-28 | 苏州辉钻纳米新材料有限公司 | PECVD-based fuel cell metal polar plate carbon-based coating preparation device |
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| JP4985919B2 (en) * | 2005-12-22 | 2012-07-25 | 三菱マテリアル株式会社 | Cutting tool made of surface-coated cubic boron nitride-based ultra-high pressure sintered material that provides excellent long-term surface accuracy in high-speed cutting of hardened steel |
| CN101235485A (en) * | 2008-02-29 | 2008-08-06 | 上海大学 | Method for preparing nano diamond thin film window |
| CN105603386A (en) * | 2016-03-01 | 2016-05-25 | 上海科弦精密工具有限公司 | Preparing method of mini-sized milling cutter nanometer diamond coating |
| CN106282964B (en) * | 2016-08-18 | 2018-11-27 | 哈尔滨工业大学 | The electrode system of micro- tool surface hot-filament cvd reactor diamond coatings |
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| JP2002192402A (en) * | 2000-12-26 | 2002-07-10 | Mitsubishi Materials Corp | Surface coated-hard metal cutting tool having superior surface lubricity to chips |
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