CN108570642B - Low-temperature controllable deposition method and device for carbon film - Google Patents
Low-temperature controllable deposition method and device for carbon film Download PDFInfo
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- CN108570642B CN108570642B CN201810828339.9A CN201810828339A CN108570642B CN 108570642 B CN108570642 B CN 108570642B CN 201810828339 A CN201810828339 A CN 201810828339A CN 108570642 B CN108570642 B CN 108570642B
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- 238000000151 deposition Methods 0.000 title claims abstract description 63
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 38
- 230000008021 deposition Effects 0.000 claims abstract description 36
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 32
- 238000004140 cleaning Methods 0.000 claims abstract description 11
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 8
- 150000004767 nitrides Chemical group 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims description 70
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 56
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 40
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 37
- 229910052786 argon Inorganic materials 0.000 claims description 28
- 239000010408 film Substances 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 229910052757 nitrogen Inorganic materials 0.000 claims description 17
- 239000010409 thin film Substances 0.000 claims description 16
- 229910002804 graphite Inorganic materials 0.000 claims description 11
- 239000010439 graphite Substances 0.000 claims description 11
- 239000000498 cooling water Substances 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 6
- 230000007246 mechanism Effects 0.000 claims description 6
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 3
- 238000005137 deposition process Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 14
- 230000008569 process Effects 0.000 abstract description 11
- 238000000576 coating method Methods 0.000 abstract description 8
- 239000011248 coating agent Substances 0.000 abstract description 6
- 238000009825 accumulation Methods 0.000 abstract description 5
- 229910000831 Steel Inorganic materials 0.000 abstract description 3
- 239000010959 steel Substances 0.000 abstract description 3
- 230000002349 favourable effect Effects 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 5
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 230000013011 mating Effects 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000005299 abrasion Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 230000006870 function Effects 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- QRRWWGNBSQSBAM-UHFFFAOYSA-N alumane;chromium Chemical compound [AlH3].[Cr] QRRWWGNBSQSBAM-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000027648 face development Effects 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 238000007733 ion plating Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000011165 process development Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000005496 tempering Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0605—Carbon
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3485—Sputtering using pulsed power to the target
-
- 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
- C23C16/272—Diamond only using DC, AC or RF discharges
Abstract
The invention discloses a carbon film low-temperature controllable deposition method, which comprises the following steps: (1) vacuumizing; (2) a cleaning step; (3) A step of depositing a bonding layer by a high-power pulse magnetron sputtering column target; (4) Depositing a nitride bearing layer by high-power pulse magnetron sputtering and direct-current magnetron sputtering; (5) a medium-frequency magnetron sputtering auxiliary chemical vapor deposition step. The invention also discloses a device for realizing the carbon film low-temperature controllable deposition method. The method provided by the invention can effectively improve the coating speed, reduce the deposition temperature, inhibit heat accumulation, realize low-temperature (130 ℃) deposition under the condition of batch coating, and is favorable for keeping the mechanical property of the bearing steel without loss in the process of preparing the film on the surface of the bearing steel.
Description
Technical Field
The invention relates to the field of film deposition and surface protection, in particular to a carbon film low-temperature controllable deposition method and device.
Background
The high-pressure common rail system of the diesel engine is one of the preferred energy conservation and emission reduction of the diesel engine, and the high-performance high-pressure common rail fuel injection system can save more than 20 percent of fuel.
But 90% of the common rail market in China is monopoly in bosch, deluxe and electric charge; ethnic enterprises face development dilemma. The reason is mainly that the common rail oil injection system is characterized in that the matching clearance of the matching parts is smaller than 2.5 microns and the speed is higher than 5000 revolutions per minute because of the requirement of high pressure, so that the problems of abrasion pressure relief and friction fusion welding are caused, and the common rail oil injection system becomes a bottleneck problem for restricting the development of autonomous brand high pressure common rail systems in China.
The key mating parts of the high-pressure common rail oil injector, the oil needle and the high-pressure plunger pump plunger (piston) are main sealing mating parts of the common rail system, and the abrasion and the service life of the main sealing mating parts are related to the service performance of the common rail system.
The carbon-based film with high performance is used in foreign countries such as bosch, electric clothes and the like, and the problems of friction pressure relief and friction fusion welding are solved. Because of the technical competition, the technology is tightly blocked abroad, so that the low-friction carbon film batch deposition of key components such as plungers, oil needles and the like is urgently needed to be broken through in China.
Various types of carbon films have been developed in laboratories by scientific research institutions and universities in China, but in the aspect of mass production, the mass production is not realized because of the dislocation of laboratory process development and coating machine design and preparation. Although some film plating equipment manufacturers develop carbon-based thin film processes themselves, high bias or arc ion plating is often used because of the need to increase the bonding force, and deposition temperatures above 200 degrees limit their scale application. The parts such as the plunger, the oil needle and the like are mostly bearing steel, and the tempering temperature is usually 160 or 180 degrees, so that the preparation process cannot be changed at will because of the requirements of the industrial chain flow.
Aiming at the problems, a new low-temperature deposition technology needs to be developed, and the problem of batch application of the low-friction carbon film in common rails and engine key parts is solved.
Disclosure of Invention
One of the technical problems to be solved by the invention is to provide a carbon film low-temperature controllable deposition method mainly aiming at the blank situation of the low-temperature deposition technology at present.
The second technical problem to be solved by the invention is to provide a carbon film low-temperature controllable deposition device mainly aiming at the blank situation of the current low-temperature deposition technology.
The low-temperature controllable deposition method for the carbon film as the first aspect of the invention comprises the following steps:
(1) Vacuumizing;
(2) A cleaning step;
(3) A step of depositing a bonding layer by a high-power pulse magnetron sputtering column target;
(4) Depositing a nitride bearing layer by high-power pulse magnetron sputtering and direct-current magnetron sputtering;
(5) Intermediate frequency magnetron sputtering assisted chemical vapor deposition.
In a preferred embodiment of the invention, the evacuation step is performed to a vacuum of 1.0x10 -4 Pa.
In a preferred embodiment of the present invention, the cleaning step is specifically to turn on a high-power pulse power supply, a voltage of 800V, a pulse current of 400A, a bias voltage of 500V, an anode of 300V, and a cleaning time of 15 minutes, and argon of 1Pa;
in a preferred embodiment of the present invention, the step of depositing the bonding layer by the high-power pulse magnetron sputtering target specifically reduces the bias voltage to 120V, 200V for the anode, 1Pa for argon, and 0.15Pa for nitrogen; deposit for 120 minutes.
In a preferred embodiment of the present invention, the step of depositing the nitride bearing layer by high-power pulse magnetron sputtering+direct-current magnetron sputtering is specifically a high-power pulse power source, a voltage of 600V, a pulse current of 300A, a bias voltage of 120V, an anode of 200V, argon of 1Pa, nitrogen of 0.15Pa, methane of 0.30Pa, and an intermediate frequency graphite target power source of 10A, and depositing for 30 minutes.
In a preferred embodiment of the present invention, the intermediate frequency magnetron sputtering auxiliary chemical vapor deposition step specifically turns off the high power pulse power supply, biases to 120V, anode 200V, argon 1Pa, methane 0.40Pa, intermediate frequency graphite target power supply 10A, and deposits for 120 minutes.
The carbon film low-temperature controllable deposition device as the second aspect of the invention comprises a double-layer water-cooling cavity and a top cover covered on the double-layer water-cooling cavity, wherein the double-layer water-cooling cavity comprises an inner-layer water-cooling cavity with a circular radial cross section and an annular outer-layer water-cooling cavity surrounding the periphery of the inner-layer water-cooling cavity;
The carbon film low-temperature controllable deposition device also comprises a plurality of magnetic control cylindrical targets arranged in the outer water-cooling cavity, a central water-cooling cylindrical anode arranged at the central position of the inner water-cooling cavity, and a tool clamp arranged in the inner water-cooling cavity and positioned at the periphery of the central water-cooling cylindrical anode; the magnetic control cylindrical targets are divided into two groups, one group of magnetic control cylindrical targets is powered by a high-power pulse power supply, and the other group of magnetic control cylindrical targets is powered by an intermediate-frequency power supply; the central water-cooled cylindrical anode is powered by an intermediate frequency pulse power supply; the tool clamp is connected with the top cover; the double-layer water-cooling cavity is also connected with a vacuum system through a vacuumizing joint and a vacuumizing tube, and is also connected with an argon flow meter, a nitrogen flow meter and a methane flow meter through an air pipe joint and an air pipe respectively; the argon flow meter is connected with an argon gas source, the nitrogen flow meter is connected with a nitrogen gas source, and the methane flow meter is connected with a methane gas source;
The carbon film low-temperature controllable deposition device also comprises an industrial personal computer PLC controller and a signal acquisition device in the double-layer water cooling cavity, wherein the signal acquisition device is used for acquiring water cooling signals in the double-layer water cooling cavity; the industrial personal computer PLC controller is in signal connection with the signal acquisition device, and is in control connection with the argon flow meter, the nitrogen flow meter, the methane flow meter, the high-power pulse power supply, the intermediate-frequency power supply and the intermediate-frequency pulse power supply.
In a preferred embodiment of the invention, a columnar water cooling structure is arranged in each magnetic control cylindrical target, and the columnar water cooling structure is connected with a cooling water source through a cooling water pipeline; through setting up the column water-cooling structure in every magnetic control cylinder target inside, increase effective water-cooling area 2 times, show reduction indoor temperature.
In a preferred embodiment of the invention, a high-pressure pump is connected to the cooling water pipeline to increase the water flow speed and pressure and remove more heat of the target surface.
In a preferred embodiment of the invention, the working target surface of the magnetically controlled cylindrical target is one fifth of the total target surface, which has a higher cooling efficiency relative to a planar target.
In a preferred embodiment of the present invention, the magnetron cylindrical target is a magnetron sputtered graphite cylindrical target.
In a preferred embodiment of the invention, the tool holder is connected to the top cover by a planetary gear train; the planetary gear train is characterized in that a sun wheel and a planet wheel in the planetary gear train are both arranged on the top cover in a shaft mode, the tool clamp is connected with the planet wheel and driven by the planet wheel to rotate, the sun wheel shaft in the sun wheel stretches out of the top cover and is connected with a driving mechanism, and the driving mechanism is connected with a PLC (programmable logic controller) controller of an industrial personal computer in a control mode and drives the sun wheel to rotate.
In a preferred embodiment of the present invention, the carbon thin film low temperature controllable deposition apparatus further comprises a plurality of indoor water-cooled cylindrical targets disposed in the outer water-cooled cavity, each indoor water-cooled cylindrical target being disposed between two adjacent magnetic control cylindrical targets. By adding the indoor water-cooling cylindrical target, the cooling effect is accelerated, and the heat accumulation is reduced.
Due to the adoption of the technical scheme, compared with the conventional magnetron sputtering technology, the magnetron sputtering method has the following advantages:
1. And an indoor water-cooling cylindrical target is added between two adjacent magnetic control cylindrical targets, so that cooling is accelerated, and heat accumulation is reduced.
2. The cooling water pipeline of each magnetic control cylindrical target is connected with a high-pressure pump, so that the water flow speed is accelerated, and the temperature of the cylindrical targets is reduced.
3. The working target surface of each magnetic control cylindrical target is only one fifth of all target surfaces, and the magnetic control cylindrical target has higher cooling efficiency compared with a planar target.
4. According to the invention, each magnetic control cylindrical target is internally provided with a cylindrical water cooling structure, so that the effective water cooling area is increased by 2 times, and the indoor temperature is obviously reduced.
5. The invention adopts the central water-cooled cylindrical anode to effectively attract heavy electrons of plasma, prevent the deposition rate from being reduced caused by charge accumulation, and simultaneously improve the ionization rate due to the relative reduction of electrons in a plasma region, thereby accelerating the deposition rate and shortening the film coating period.
6. The invention adopts the industrial PLC controller to control the vacuum acquisition, measurement, process implementation and detection of the whole coating system, the system has the functions of memory and learning, each point of the fixed process can be calibrated, the coating process is detected according to the calibration in the repeated process, the process repeatability is realized by adjusting the flow control process deviation, and the low-temperature (130 ℃) deposition under the condition of batch coating is realized.
7. According to the invention, an industrial control PLC controller is adopted to record each customized process key node parameter database through the memory and tracking functions, parameter adjustment is carried out on the target database in the repeated deposition process, and the repeated stability of multiple batches is ensured through controlling and fine-tuning each flowmeter.
8. The process part of the invention modulates high-power pulse magnetron sputtering by the assistance of the pulse anode, increases the flexibility of a coating process, and prepares a multilayer structure by modulating the change of pulse time sequence.
9. The process part of the invention uses anode auxiliary bias to carry out chemical vapor deposition, modulates and forms a nano structure, and improves the toughness and strength of the carbon film.
Drawings
FIG. 1 is a schematic view of a part of a low-temperature controllable deposition device for carbon films.
Detailed Description
Referring to fig. 1, the carbon thin film low-temperature controllable deposition device shown in the drawing comprises a double-layer water-cooling cavity 1 and a top cover (not shown in the drawing) covering the double-layer water-cooling cavity 1, wherein the double-layer water-cooling cavity 1 comprises an inner-layer water-cooling cavity 1a with a circular radial cross section and an outer-layer water-cooling cavity 1b which surrounds the periphery of the inner-layer water-cooling cavity 1a and is annular.
The carbon film low-temperature controllable deposition device further comprises four magnetic control cylindrical targets 2 arranged in the outer water-cooling cavity 1b, four indoor water-cooling cylindrical targets 3 arranged in the outer water-cooling cavity 1b, a central water-cooling cylindrical anode 4 arranged in the central position of the inner water-cooling cavity 1a, and a plurality of tool fixtures 5 arranged in the inner water-cooling cavity 1a and positioned on the periphery of the central water-cooling cylindrical anode 4.
A columnar water cooling structure (not shown) is arranged in each magnetic control cylindrical target 2, and the columnar water cooling structure is connected with a cooling water source (not shown) through a cooling water pipeline (not shown). According to the invention, the columnar water cooling structure is arranged in each magnetic control cylindrical target 2, so that the effective water cooling area is increased by 2 times, and the indoor temperature is obviously reduced. The invention also connects a high-pressure pump (not shown in the figure) to the cooling water pipeline to increase the water flow speed and pressure and take away more heat of the target surface.
The magnetron cylindrical target 2 is a magnetron sputtering graphite cylindrical target, the working target surface of the magnetron cylindrical target is one fifth of the whole target surface, and the magnetron cylindrical target has higher cooling efficiency compared with a planar target.
The four magnetic control cylindrical targets 2 are divided into two groups, one group of the magnetic control cylindrical targets 2 is powered by a high-power pulse power supply, and the other group of the magnetic control cylindrical targets 2 is powered by an intermediate-frequency power supply.
Each indoor water-cooling cylindrical target 3 is arranged between two adjacent magnetic control cylindrical targets 2. By adding the indoor water-cooling cylindrical target, the cooling effect is accelerated, and the heat accumulation is reduced.
The central water-cooled cylindrical anode 4 adopts an intermediate frequency pulse power supply to supply power; the double-layer water-cooling cavity 1 is also connected with a vacuum system through a vacuum-pumping joint and a vacuum-pumping pipe, and the double-layer water-cooling cavity 1 is also connected with an argon flow meter 8a, a nitrogen flow meter 8b and a methane flow meter 8c through an air pipe joint and an air pipe respectively; the argon flow meter 8a is connected with an argon gas source, the nitrogen flow meter 8b is connected with a nitrogen gas source, and the methane flow meter 8c is connected with a methane gas source.
The carbon film low-temperature controllable deposition device also comprises an industrial personal computer PLC controller 7 and a signal acquisition device 6 in the double-layer water cooling cavity, wherein the signal acquisition device is used for acquiring water cooling signals in the double-layer water cooling cavity; the industrial personal computer PLC controller 7 is in signal connection with the signal acquisition device 6, and the industrial personal computer PLC controller 7 is in control connection with the argon flow meter 8a, the nitrogen flow meter 8b, the methane flow meter 8c, the high-power pulse power supply, the intermediate-frequency power supply and the intermediate-frequency pulse power supply.
A plurality of tool clamps 5 are connected with the top cover through a planetary gear train (not shown in the figure); the sun wheel and the planet wheel in the planetary gear train are both arranged on the top cover in a shaft mode, each tool clamp is connected with the planet wheel and driven by the planet wheel to rotate, the sun wheel shaft in the sun wheel extends out of the top cover and is connected with a driving mechanism, and the driving mechanism is connected with the PLC controller of the industrial personal computer in a control mode and drives the sun wheel to rotate.
The invention discloses a low-temperature controllable deposition method of a carbon film, which comprises the following steps of:
(1) Vacuumizing;
(2) A cleaning step;
(3) A step of depositing a bonding layer by a high-power pulse magnetron sputtering column target;
(4) Depositing a nitride bearing layer by high-power pulse magnetron sputtering and direct-current magnetron sputtering;
(5) Intermediate frequency magnetron sputtering assisted chemical vapor deposition.
In a preferred embodiment of the invention, the evacuation step is performed to a vacuum of 1.0x10 -4 Pa.
The cleaning step is to start a high-power pulse power supply, the voltage is 800V, the pulse current is 400A, the bias voltage is 500V, the anode is 300V, the cleaning time is 15 minutes, and the argon is 1Pa;
The step of depositing the bonding layer by the high-power pulse magnetron sputtering column target is to reduce the bias voltage to 120V, the anode to 200V, the argon to 1Pa and the nitrogen to 0.15Pa; deposit for 120 minutes.
The high-power pulse magnetron sputtering and direct-current magnetron sputtering deposition of the nitride bearing layer comprises the steps of high-power pulse power supply, voltage 600V, pulse current 300A, bias voltage to 120V, anode 200V, argon 1Pa, nitrogen 0.15Pa, methane 0.30Pa, intermediate-frequency graphite target power supply 10A and deposition for 30 minutes.
The intermediate frequency magnetron sputtering auxiliary chemical vapor deposition step is to turn off a high-power pulse power supply, bias the power supply to 120V, anode 200V, argon 1Pa, methane 0.40Pa, intermediate frequency graphite target power supply 10A, and deposit for 120 minutes.
The process of the method of the invention will be described in detail below using a plunger as an example of a workpiece:
(1) Installing the cleaned plunger on a workpiece frame, closing a cavity door, vacuumizing to 1.0x10 -4 Pa, and starting coating;
(2) Starting a high-power pulse power supply, wherein the voltage is 800V, the pulse current is 400A, the bias voltage is 500V, the anode is 300V, the target is metal chromium aluminum, the cleaning time is 15 minutes, and the argon is 1Pa;
(3) Reducing the bias voltage to 120V, wherein the anode is 200V, the argon is 1Pa, and the nitrogen is 0.15Pa; depositing for 120 minutes;
(4) High-power pulse power supply, voltage 600V, pulse current 300A, bias voltage to 120V, anode 200V, argon 1Pa, nitrogen 0.15Pa, methane 0.30Pa, intermediate frequency graphite target power supply 10A, deposition for 30 minutes; turning off a high-power pulse power supply, biasing to 120V, setting the anode at 200V, argon at 1Pa, methane at 0.40Pa, and setting the intermediate-frequency graphite target power supply at 10A for 120 min;
(5) Closing the system after the deposition is finished, cooling for 30 minutes, and taking out the sample;
the test bond showed 47N, a coefficient of friction of 0.04, and a load of 10N.
Claims (12)
1. An apparatus for a low temperature controllable deposition method of a carbon thin film, the low temperature controllable deposition method of a carbon thin film comprising the steps of:
(1) Vacuumizing;
(2) A cleaning step;
(3) A step of depositing a bonding layer by a high-power pulse magnetron sputtering column target;
(4) Depositing a nitride bearing layer by high-power pulse magnetron sputtering and direct-current magnetron sputtering;
(5) A step of intermediate frequency magnetron sputtering auxiliary chemical vapor deposition; the device is characterized by comprising a double-layer water-cooling cavity and a top cover covered on the double-layer water-cooling cavity, wherein the double-layer water-cooling cavity comprises an inner water-cooling cavity with a circular radial section and an outer water-cooling cavity which surrounds the periphery of the inner water-cooling cavity and is annular;
The carbon film low-temperature controllable deposition device also comprises a plurality of magnetic control cylindrical targets arranged in the outer water-cooling cavity, a central water-cooling cylindrical anode arranged at the central position of the inner water-cooling cavity, and a tool clamp arranged in the inner water-cooling cavity and positioned at the periphery of the central water-cooling cylindrical anode; the magnetic control cylindrical targets are divided into two groups, one group of magnetic control cylindrical targets is powered by a high-power pulse power supply, and the other group of magnetic control cylindrical targets is powered by an intermediate-frequency power supply; the central water-cooled cylindrical anode is powered by an intermediate frequency pulse power supply; the tool clamp is connected with the top cover; the double-layer water-cooling cavity is also connected with a vacuum system through a vacuumizing joint and a vacuumizing tube, and is also connected with an argon flow meter, a nitrogen flow meter and a methane flow meter through an air pipe joint and an air pipe respectively; the argon flow meter is connected with an argon gas source, the nitrogen flow meter is connected with a nitrogen gas source, and the methane flow meter is connected with a methane gas source;
The carbon film low-temperature controllable deposition device also comprises an industrial personal computer PLC controller and a signal acquisition device in the double-layer water cooling cavity, wherein the signal acquisition device is used for acquiring water cooling signals in the double-layer water cooling cavity; the industrial personal computer PLC controller is in signal connection with the signal acquisition device, and is in control connection with the argon flow meter, the nitrogen flow meter, the methane flow meter, the high-power pulse power supply, the intermediate-frequency power supply and the intermediate-frequency pulse power supply.
2. The apparatus for low temperature controlled deposition method of carbon thin film according to claim 1, wherein the vacuum is applied to 1.0x10 -4 Pa in the vacuum applying step.
3. The apparatus for low temperature controlled deposition of carbon thin film according to claim 2, wherein the cleaning step is specifically to turn on a high power pulse power supply, voltage 800V, pulse current 400A, bias voltage 500V, anode 300V, cleaning time 15 minutes, argon 1Pa.
4. The apparatus for low temperature controllable deposition method of carbon thin film according to claim 3, wherein said high power pulse magnetron sputtering target deposition bonding layer step is specifically to reduce bias voltage to 120V, anode 200V, argon 1Pa, nitrogen 0.15Pa; deposit for 120 minutes.
5. The apparatus for low temperature controlled deposition of carbon thin film according to claim 4, wherein the high power pulsed magnetron sputtering+dc magnetron sputtering deposition of the nitride bearing layer is performed by high power pulsed power supply, voltage 600V, pulsed current 300A, bias to 120V, anode 200V, argon 1Pa, nitrogen 0.15Pa, methane 0.30Pa, intermediate frequency graphite target power supply 10A, deposition for 30 minutes.
6. The apparatus for low temperature controlled deposition of carbon thin film according to claim 5, wherein the medium frequency magnetron sputtering assisted chemical vapor deposition step is performed by turning off a high power pulse power supply, biasing to 120V, anode 200V, argon 1Pa, methane 0.40Pa, medium frequency graphite target power supply 10A, and depositing for 120 minutes.
7. The apparatus for low temperature controllable deposition method of carbon thin film according to claim 1, wherein each of the magnetically controlled cylindrical targets is provided inside with a cylindrical water cooling structure connected to a cooling water source through a cooling water pipe.
8. The apparatus for low temperature controllable deposition process of carbon thin film as claimed in claim 7, wherein a high pressure pump is connected to said cooling water line.
9. The apparatus for low temperature controlled deposition of carbon thin film according to claim 8, wherein the working target surface of the magnetically controlled cylindrical target is one fifth of the total target surface.
10. The apparatus for low temperature controllable deposition of carbon thin films according to claim 9, wherein the magnetron cylindrical target is a magnetron sputtered graphite cylindrical target.
11. The apparatus for low temperature controlled deposition of carbon thin film according to claim 1, wherein the tool holder is connected to the top cover through a planetary gear train; the planetary gear train is characterized in that a sun wheel and a planet wheel in the planetary gear train are both arranged on the top cover in a shaft mode, the tool clamp is connected with the planet wheel and driven by the planet wheel to rotate, the sun wheel shaft in the sun wheel stretches out of the top cover and is connected with a driving mechanism, and the driving mechanism is connected with a PLC (programmable logic controller) controller of an industrial personal computer in a control mode and drives the sun wheel to rotate.
12. The apparatus for low temperature controlled deposition of carbon thin film according to any one of claims 6 to 11, further comprising a plurality of indoor water-cooled cylindrical targets disposed in the outer water-cooled chamber, each indoor water-cooled cylindrical target being disposed between two adjacent magnetic control cylindrical targets.
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