Novel pyrolytic graphite vapor deposition device and process

文档序号:940290 发布日期:2020-10-30 浏览:2次 中文

阅读说明:本技术 一种新式热解石墨气相沉积装置及工艺 (Novel pyrolytic graphite vapor deposition device and process ) 是由 付善任 张红 夏倩倩 于 2020-08-28 设计创作,主要内容包括:本发明公开了一种新式热解石墨气相沉积装置及工艺,包括支撑机构、进气机构、罩壳和石墨电阻发热体。该新式热解石墨气相沉积装置及工艺,将碳素件摆放在支撑机构的载物托盘上,然后控制第二气缸带动支撑台面上升,从而使得载物托盘带动碳素件上升到工作时的位置;打开真空系统阀门,通过真空泵将罩壳内的气压抽真空,开始加热,控制石墨电阻发热体开始升温,恒温结束后进气管及石墨隔挡板下降到发热体二分之一位置处;此时由进气管供给碳氢气体原料,当热解石墨气象沉积10-30分钟之后,控制电机开始工作,电机带动载物托盘以十分钟每转的速度;当气相沉积过程结束后,进气管及石墨隔挡板上升回到初始位置后,开始通过水冷排管降温。(The invention discloses a novel pyrolytic graphite vapor deposition device and a novel pyrolytic graphite vapor deposition process. According to the novel pyrolytic graphite vapor deposition device and the novel pyrolytic graphite vapor deposition process, the carbon element is placed on the carrying tray of the supporting mechanism, and then the second cylinder is controlled to drive the supporting table to ascend, so that the carrying tray drives the carbon element to ascend to the position of the carbon element during working; opening a valve of a vacuum system, vacuumizing the air pressure in the housing through a vacuum pump, starting heating, controlling the graphite resistance heating element to start heating, and after the constant temperature is finished, lowering the air inlet pipe and the graphite baffle plate to a position which is one half of the heating element; at the moment, a hydrocarbon gas raw material is supplied by an air inlet pipe, and after the pyrolytic graphite gas is deposited for 10-30 minutes, a motor is controlled to start working, and the motor drives a carrying tray to rotate at the speed of ten minutes per revolution; after the vapor deposition process is finished, the air inlet pipe and the graphite baffle plate rise to the initial position, and then the temperature is reduced through the water-cooling calandria.)

1. A novel pyrolytic graphite vapor deposition device comprises a bracket (1), and is characterized in that: the top surface of the support (1) is fixedly provided with a housing (2), a gas supply mechanism (3) is arranged above the housing (2), a support mechanism (4) is arranged below the housing (2), a graphite resistance heating body (5) is arranged on the inner side of the housing (2), a graphite electrode (6) inserted into the housing (2) is fixedly connected to the outer wall of the upper part of the housing (2), one end of the graphite electrode (6) is fixedly connected with the graphite resistance heating body (5), the gas supply mechanism (3) comprises a mounting frame (7), a first cylinder (8), a transverse plate (9), an air inlet pipe (10), a first thread block (11), a second thread block (12), a graphite baffle plate (13) and a temperature thermocouple (14), the support mechanism (4) comprises a second cylinder (15), a support table board (16), a carrying tray (17), a pipe arranging base (18), a water-cooling pipe (19) and a motor, a carbon element (20) is arranged above the supporting mechanism (4), and a temperature controller (21) is fixedly arranged on the outer wall of the housing (2).

2. The novel pyrolytic graphite vapor deposition apparatus according to claim 1, wherein: the mounting rack (7) is fixedly mounted on the top surface of the housing (2), the first cylinder (8) is symmetrically and fixedly mounted on the inner side of the top of the mounting rack (7), the transverse plate (9) is fixedly connected with the telescopic end of the first cylinder (8), the air inlet pipe (10) and the temperature thermocouple (14) simultaneously penetrate through the transverse plate (9), the housing (2) and the graphite baffle plate (13) are slidably connected with the housing (2), the air inlet pipe (10) is circumferentially and equidistantly arranged on the outer side of the temperature thermocouple (14), the outer walls of the top of the air inlet pipe (10) and the temperature thermocouple (14) are fixedly connected with the transverse plate (9), the air inlet pipe (10) and the temperature thermocouple (14) are slidably connected with the housing (2), the graphite baffle plate (13) is slidably sleeved on the outer sides of the lower parts of the air inlet pipe (10) and the temperature thermocouple (14), the graphite baffle plate (13) is arranged in the, the graphite baffle plate (13) is arranged above the first threaded block (11), the first threaded block (11) is in threaded connection with the outer wall of the bottom of the air inlet pipe (10), the second threaded block (12) is in threaded connection with the outer wall of the upper portion of the air inlet pipe (10), and the second threaded block (12) is arranged between the transverse plate (9) and the housing (2).

3. The novel pyrolytic graphite vapor deposition apparatus according to claim 1, wherein: second cylinder (15) symmetry fixed mounting is inboard in the bottom of support (1), support mesa (16) fixed mounting and serve at the flexible of second cylinder (15), it connects the top surface at support mesa (16) to carry thing tray (17) rotation, motor (22) fixed mounting is in the bottom surface of supporting mesa (16), the output shaft of motor (22) passes support mesa (16) and through the shaft coupling with carry the bottom surface fixed connection of thing tray (17), it adorns to carry thing tray (17) for the I-shaped, calandria base (18) rotate the cover and establish the middle part outside of carrying thing tray (17), establish in calandria base (18) water-cooling calandria (19), it establishes in encloser (2) to carry thing tray (17), and carry the outer wall of thing tray (17) and the inner wall sliding connection of encloser (2).

4. The novel pyrolytic graphite vapor deposition apparatus according to claim 1, wherein: the utility model discloses a graphite heating device, including housing (2), graphite resistance heat-generating body (5), graphite electrode (6), intake pipe (10), first screw thread piece (11), second screw thread piece (12), graphite separate baffle (13) and carry the material of thing tray (17) and be three high graphite materials, support (1), mounting bracket (7), diaphragm (9), support mesa (16), calandria base (18) and water-cooling calandria (19) are the stainless steel material.

5. The novel pyrolytic graphite vapor deposition apparatus according to claim 1, wherein: the outer wall of the temperature thermocouple (14) is a silicon carbide ceramic tube, a tungsten-rhenium thermocouple wire is assembled inside the temperature thermocouple (14), and the middle position of the graphite resistance heating body (5) is an area with the highest temperature.

6. The novel pyrolytic graphite vapor deposition apparatus according to claim 1, wherein: the vacuum system which is communicated with the housing (2) and comprises a valve and a vacuum pump is arranged on the outer side of the housing, the first cylinder (8) and the second cylinder (15) are externally connected with a control air source, temperature control cold water circulation equipment is arranged outside the water cooling calandria (19), and a hydrocarbon gas supply equipment is externally connected with the air inlet pipe (10).

7. The novel pyrolytic graphite vapor deposition apparatus according to claim 1, wherein: graphite electrode (6) and motor (22) all are external to have the power, graphite electrode (6) and graphite resistance heat-generating body (5) electric connection, and temperature control appearance (21) are through electric wire and graphite resistance heat-generating body (5) electric connection, and temperature thermocouple (14) are through electric wire and temperature control appearance (21) electric connection.

8. The novel pyrolytic graphite vapor deposition process according to claim 1, wherein: the process comprises the following steps:

the method comprises the following steps: placing the carbon element (20) on a carrying tray (17) of the supporting mechanism (4), and then controlling a second air cylinder (15) to drive a supporting table surface (16) to ascend, so that the carrying tray (17) drives the carbon element (20) to ascend to a position in work;

step two: opening the valve of the vacuum system, and vacuumizing the air pressure in the housing (2) to 6 x 10 by using a vacuum pump-3Pa-10 Pa, and then closing the vacuum pump;

step three: heating is started, the graphite resistance heating body (5) is controlled to start heating at the speed of 50-300 ℃/h, the process is a pyrolytic graphite process, the temperature detected by the temperature thermocouple (14) is heated to 2200 ℃, then the temperature is kept for 2-6 h, and the temperature of process water in the water-cooling calandria (19) is controlled to be 60-70 ℃;

step four: after the constant temperature is finished, the air inlet pipe (10) and the graphite baffle (13) descend to the position of one half of the heating body;

step five: at the moment, the hydrocarbon gas raw material is supplied by the gas inlet pipe (10), and the gas inlet flow of each gas inlet pipe is 50 ml/min-5L/min;

step six: after the hydrocarbon gas raw material is sprayed out from the air inlet pipe (10), carbon atoms in the hydrocarbon gas raw material are decomposed at high temperature and deposit and attach to the surface of the carbon element (20) along with the airflow direction, the gravity direction and the condensation driving direction, and meanwhile, the temperature of the process water of the water-cooling calandria (19) is adjusted to be 25 ℃ at the moment in order to increase the condensation driving force due to the principle of entropy increase;

step seven: after the pyrolytic graphite is deposited for 10-30 minutes in a meteorological manner, controlling a motor (22) to start working, wherein the motor (22) drives a carrying tray (17) to rotate 90 degrees clockwise at the speed of ten minutes per rotation, other process parameters are unchanged in the rotating process, after the rotation is finished, the pyrolytic graphite is continuously deposited for 10-30 minutes in a static meteorological manner, then is rotated 90 degrees clockwise, and the like, the thickness of the pyrolytic graphite is controlled finely, the thickness ranges from 1 mu m to 10 mu m, and carbon elements form a grid-shaped multilayer coating with a hexagonal molecular structure on a carbon element (20), wherein the thickness of the grid-shaped multilayer coating is 360-720 degrees in total in one preparation period;

step eight: after the vapor deposition process is finished, after the air inlet pipe (10) and the graphite baffle plate (13) rise to the initial position, the supply of gas raw materials of the air inlet pipe (10) is closed, the temperature is reduced through the water-cooling calandria (19), the temperature reduction rate is not too fast, the surface coating of the carbon element (20) is prevented from cracking or falling off, the temperature reduction rate is 50-100 ℃/h, and the power is cut off when the temperature is reduced to 300 ℃;

step nine: and after the interior of the housing is completely cooled, opening the housing, taking out the prepared carbon element, and finishing the whole preparation period.

9. The novel pyrolytic graphite vapor deposition process according to claim 8, wherein: the process temperature of the pyrolytic carbon coating in the third step is 1600-1800 ℃, the process temperature of the pyrolytic graphite is 1900-2300 ℃, and the raw material of the carbon hydrogen gas in the fifth step comprises methane, acetylene, other carbon hydrogen gas and the like.

Technical Field

The invention relates to the technical field of pyrolytic graphite coatings, in particular to a novel pyrolytic graphite vapor deposition device and a novel pyrolytic graphite vapor deposition process.

Background

Pyrolytic graphite is a novel carbon material, is a carbon material coating with high crystal orientation, which is prepared by chemical vapor deposition of high-purity hydrocarbon gas on a graphite substrate at 1800-2000 ℃ under a certain furnace pressure, and has high density, high purity and anisotropy of thermal, electric, magnetic and mechanical properties. The vacuum degree of 10mmHg can be maintained at 1800 ℃.

The conventional pyrolytic graphite coating is usually produced by adopting a vapor deposition method, but the situation of uneven deposition and disordered crystal orientation easily occur in the production process, and the performance of the pyrolytic graphite coating is seriously influenced.

Disclosure of Invention

The invention aims to provide a novel pyrolytic graphite vapor deposition device and a novel pyrolytic graphite vapor deposition process so as to solve the problems in the background technology.

In order to achieve the purpose, the invention provides the following technical scheme:

the utility model provides a new-type pyrolysis graphite vapor deposition device, which comprises a bracket, the top surface fixed mounting of support has the housing, the top of housing is equipped with air feed mechanism, the below of housing is equipped with supporting mechanism, the inboard of housing is equipped with graphite resistance heat-generating body, the upper portion outer wall fixedly connected with of housing inserts the graphite electrode in it, the one end and the graphite resistance heat-generating body fixed connection of graphite electrode, air feed mechanism includes the mounting bracket, first cylinder, the diaphragm, the intake pipe, first thread piece, second thread piece, graphite separates baffle and temperature thermocouple, supporting mechanism includes the second cylinder, support the mesa, carry the thing tray, the calandria base, water-cooling calandria and motor, supporting mechanism's top is equipped with the carbon element, the outer wall fixed mounting of housing has temperature controller.

As a further scheme of the invention: the mounting frame is fixedly arranged on the top surface of the housing, the first cylinders are symmetrically and fixedly arranged on the inner side of the top of the mounting frame, the transverse plate is fixedly connected with the telescopic end of the first cylinder, the air inlet pipe and the temperature thermocouple simultaneously penetrate through the transverse plate, the housing and the graphite baffle plate, the circumference of the air inlet pipe is equidistantly arranged on the outer side of the temperature thermocouple, the outer walls of the top of the air inlet pipe and the temperature thermocouple are fixedly connected with the transverse plate, the air inlet pipe and the temperature thermocouple are connected with the housing in a sliding manner, the graphite baffle plate is sleeved on the outer sides of the lower, and the graphite baffle is arranged between the graphite resistance heating bodies, the graphite baffle is arranged above the first thread block, the first thread block is in threaded connection with the outer wall of the bottom of the air inlet pipe, the second thread block is in threaded connection with the outer wall of the upper part of the air inlet pipe, and the second thread block is arranged between the transverse plate and the housing.

As a still further scheme of the invention: second cylinder symmetry fixed mounting is inboard in the bottom of support, support mesa fixed mounting is served at the flexible of second cylinder, it connects the top surface at the support mesa to carry the thing tray rotation, motor fixed mounting is in the bottom surface of supporting the mesa, the output shaft of motor passes the bottom surface fixed connection that supports the mesa and pass through shaft coupling and year thing tray, it is the I dress to carry the thing tray, the calandria base rotates the cover and establishes the middle part outside of carrying the thing tray, the water-cooling calandria is established in the calandria base, it establishes in the housing to carry the thing tray, and carry the outer wall of thing tray and the inner wall sliding connection of housing.

As a still further scheme of the invention: the cover shell is externally provided with a door body, the material of the cover shell is graphite felt, the material of the graphite resistance heating body, the graphite electrode, the air inlet pipe, the first thread block, the second thread block, the graphite baffle and the loading tray is three-high graphite material, and the support, the mounting frame, the transverse plate, the support table board, the calandria base and the water-cooling calandria are made of stainless steel.

As a still further scheme of the invention: the outer wall of the temperature thermocouple is a silicon carbide ceramic tube, a tungsten-rhenium thermocouple wire is assembled inside the temperature thermocouple, and the middle position of the graphite resistance heating body is an area with the highest temperature.

As a still further scheme of the invention: the outer side of the housing is provided with a vacuum system which is communicated with the housing and comprises a valve and a vacuum pump, the first cylinder and the second cylinder are both externally connected with a control air source, a temperature control cold water circulating device is arranged outside the water cooling calandria, and a carbon hydrogen gas supply device is externally connected with the air inlet pipe.

As a still further scheme of the invention: the graphite electrode and the motor are externally connected with a power supply, the graphite electrode is electrically connected with the graphite resistance heating body, the temperature controller is electrically connected with the graphite resistance heating body through an electric wire, and the temperature thermocouple is electrically connected with the temperature controller through an electric wire.

As a still further scheme of the invention: a novel pyrolytic graphite vapor deposition process comprises the following steps:

the method comprises the following steps: placing the carbon element on a carrying tray of the supporting mechanism, and then controlling a second cylinder to drive the supporting table to ascend, so that the carrying tray drives the carbon element to ascend to a working position;

step two: opening the valve of the vacuum system, and vacuumizing the air pressure in the housing to 6 x 10 by using a vacuum pump-3Pa-10 Pa, and then closing the vacuum pump;

step three: heating, controlling a graphite resistance heating element to start heating at a speed of 50-300 ℃/h, wherein the heating is a pyrolytic graphite process, the temperature is kept for 2-6 h after the detection temperature of a temperature thermocouple is increased to 2200 ℃, and the temperature of process water of a water-cooling calandria is controlled to be 60-70 ℃;

step four: after the constant temperature is finished, the air inlet pipe and the graphite baffle plate descend to the position of one half of the heating body;

step five: at the moment, the carbon hydrogen gas raw material is supplied by the gas inlet pipe, and the gas inlet flow of each gas inlet pipe is 50 ml/min-5L/min;

step six: after the hydrocarbon gas raw material is sprayed out from the air inlet pipe, carbon atoms in the hydrocarbon gas raw material are decomposed at high temperature and deposit and attach to the surface of a carbon element along with the air flow direction, the gravity direction and the condensation driving direction, and simultaneously, the temperature of the process water of the water-cooling calandria is adjusted to be 25 ℃ at the moment in order to increase the condensation driving force due to the principle of entropy increase;

step seven: after the pyrolytic graphite is deposited for 10-30 minutes in a meteorological manner, controlling a motor to start working, driving a carrying tray to rotate 90 degrees clockwise at the speed of ten minutes per rotation by the motor, keeping other process parameters unchanged in the rotating process, continuing to deposit for 10-30 minutes in a static state after the rotation is finished, then rotating 90 degrees clockwise, and so on, wherein the thickness of the pyrolytic graphite in the meteorological deposition range is 1-10 microns after the static state is formed in a preparation cycle, and the carbon element forms a grid-shaped multilayer coating with a hexagonal molecular structure on a carbon element;

step eight: after the vapor deposition process is finished, after the air inlet pipe and the graphite baffle plate rise to the initial position, the supply of gas raw materials of the air inlet pipe is closed, the temperature is reduced through the water-cooling calandria, the temperature reduction rate is not too fast, the cracking or the dropping of the surface coating of the carbon element is prevented, the temperature reduction rate is 50-100 ℃/h, and the power is cut off when the temperature is reduced to 300 ℃;

step nine: and after the interior of the housing is completely cooled, opening the housing, taking out the prepared carbon element, and finishing the whole preparation period.

As a still further scheme of the invention: the process temperature of the pyrolytic carbon coating in the third step is 1600-1800 ℃, the process temperature of the pyrolytic graphite is 1900-2300 ℃, and the raw material of the carbon hydrogen gas in the fifth step comprises methane, acetylene, other carbon hydrogen gas and the like.

Compared with the prior art, the invention has the beneficial effects that:

the device can carry out pyrolytic graphite vapor deposition operation by the matching use among the bracket, the housing, the gas supply mechanism, the support mechanism, the graphite resistance heating body and the graphite electrode, the gas inlet position of the gas inlet pipe and the height position of the graphite baffle plate can be adjusted by the matching use among the mounting frame, the first cylinder, the transverse plate, the gas inlet pipe, the first thread bank, the second thread block and the graphite baffle plate, thereby effectively controlling the distance between the carbon gas raw material and the carbon element, effectively controlling the effective working area, reducing the injection amount of the carbon gas raw material, facilitating the gathering of the carbon gas raw material, and leading the carbon element to be capable of lifting and rotating when carrying out pyrolytic graphite vapor deposition by the matching use among the second cylinder, the support table surface, the carrying tray, the calandria base, the calandria and the motor, the coating formed by the pyrolytic graphite vapor deposition of the carbon element is more uniform, so that the novel pyrolytic graphite vapor deposition device and the novel pyrolytic graphite vapor deposition process can make the vapor deposition more uniform, and the quality of the coating on the surface of the carbon element is effectively improved.

Drawings

FIG. 1 is a schematic structural diagram of a novel pyrolytic graphite vapor deposition apparatus and process.

FIG. 2 is a working position diagram of a new pyrolytic graphite vapor deposition apparatus and process.

FIG. 3 is a diagram of a new pyrolytic graphite vapor deposition apparatus and a graphite baffle plate in the process.

In the figure: the device comprises a support 1, a cover 2, an air supply mechanism 3, a support mechanism 4, a graphite resistance heating element 5, a graphite electrode 6, a mounting rack 7, a first cylinder 8, a transverse plate 9, an air inlet pipe 10, a first thread block 11, a second thread block 12, a graphite baffle 13, a temperature thermocouple 14, a second cylinder 15, a support table top 16, a loading tray 17, a calandria base 18, a water-cooling calandria 19, a carbon element 20, a temperature controller 21 and a motor 22.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Referring to fig. 1 to 3, in the embodiment of the present invention, a novel pyrolytic graphite vapor deposition apparatus and process comprises a support 1, a housing 2 is fixedly installed on the top surface of the support 1, a gas supply mechanism 3 is installed above the housing 2, a support mechanism 4 is installed below the housing 2, the support mechanism 4 can be lifted and rotated during the vapor deposition process to improve the preparation efficiency and the coating quality, a graphite resistance heating element 5 is installed inside the housing 2, the graphite resistance heating element 5 is a heating source of the whole thermal field, a graphite electrode 6 inserted into the housing 2 is fixedly connected to the outer wall of the upper portion of the housing 2, one end of the graphite electrode 6 is fixedly connected to the graphite resistance heating element 5, the gas supply mechanism 3 comprises a mounting frame 7, a first cylinder 8, a transverse plate 9, a gas inlet pipe 10, a first thread block 11, a second thread block 12, a graphite baffle 13 and a temperature thermocouple 14, the air supply mechanism 3 can adjust the air outlet position of the air inlet pipe 10, the position of the air outlet of the air inlet pipe 10 can be flexibly adjusted according to the requirements of the quantity, the appearance, the process temperature and the like of coating objects to be prepared, the spraying path of raw material gas is shortened, the spraying pressure is increased, and a better process effect is achieved, the supporting mechanism 4 comprises a second air cylinder 15, a supporting table surface 16, a carrying tray 17, a pipe arranging base 18, a water-cooling pipe arranging pipe 19 and a motor 22, a carbon element 20 is arranged above the supporting mechanism 4, and a temperature controller 21 is fixedly arranged on the outer wall of the housing 2.

The mounting frame 7 is fixedly mounted on the top surface of the housing 2, the first air cylinders 8 are symmetrically and fixedly mounted on the inner side of the top of the mounting frame 7, the transverse plate 9 is fixedly connected with the telescopic end of the first air cylinder 8, the air inlet pipes 10 and the temperature thermocouples 14 simultaneously penetrate through the transverse plate 9, the housing 2 and the graphite baffle 13, the temperature thermocouples 14 are used for monitoring the thermal decomposition temperature of hydrocarbon gas, the heating power of the graphite resistance heating element 5 can be controlled through the temperature controller 21 to achieve the purpose of process adjustment, the air inlet pipes 10 are circumferentially and equidistantly arranged on the outer side of the temperature thermocouples 14, the air passages are more uniformly and reasonably distributed due to the arrangement of the multiple air inlet pipes 10, the influence of radiant heat on the flow direction and speed of the air is weakened, the purpose of uniform and consistent deposition of pyrolytic graphite meteorology is achieved, the outer walls of the top parts of the air inlet pipes, the graphite baffle 13 is sleeved on the outer sides of the lower parts of the air inlet pipe 10 and the temperature thermocouple 14 in a sliding manner, the graphite baffle 13 is arranged in the housing 2, the graphite baffle 13 is arranged between the graphite resistance heating bodies 5, the graphite baffle 13 is arranged above the first thread block 11, and when hydrocarbon gas just rushes out of the air inlet pipe 10, part of the gas escapes to the two sides of the pipeline due to the instant change of pressure difference, flows upwards and is rebounded by the graphite baffle 13. The graphite baffle 13 can further compress the spraying space along with the lifting of the air inlet pipe 10, indirectly increase the spraying pressure on the surface of the carbon element 20 and improve the spraying quality. Meanwhile, the heat preservation and insulation effect is achieved, the energy consumption of the heating body is reduced, the first thread block 11 is in threaded connection with the outer wall of the bottom of the air inlet pipe 10, the first thread block 11 plays a role in hanging the graphite baffle 13, the second thread block 12 is in threaded connection with the outer wall of the upper portion of the air inlet pipe 10, the second thread block 12 is arranged between the transverse plate 9 and the housing 2, the second thread block 12 is limited for the moving position of the air inlet pipe 10 in the process operation process, meanwhile, the safety mechanism can be used, and the air inlet pipe 10 is prevented from falling.

The second cylinder 15 symmetry fixed mounting is inboard in the bottom of support 1, support mesa 16 fixed mounting is on the flexible end of second cylinder 15, it connects the top surface at support mesa 16 to carry thing tray 17 to rotate, motor 22 fixed mounting is in the bottom surface of supporting mesa 16, the output shaft of motor 22 passes support mesa 16 and through shaft coupling and the bottom surface fixed connection who carries thing tray 17, it adorns to carry thing tray 17 to be I, calandria base 18 rotates the cover and establishes the middle part outside at carrying thing tray 17, water-cooling calandria 19 is established in calandria base 18, it establishes in housing 2 to carry thing tray 17, and carry the outer wall of thing tray 17 and the inner wall sliding connection of housing 2.

The door body is arranged outside the housing 2, the housing 2 is made of graphite hard felt, the main effect is heat preservation and insulation, the graphite resistance heating body 5, the graphite electrode 6, the air inlet pipe 10, the first thread block 11, the second thread block 12, the graphite baffle 13 and the carrying tray 17 are made of three-high graphite materials, the support 1, the mounting frame 7, the transverse plate 9, the support table board 16, the calandria base 18 and the water-cooling calandria 19 are made of stainless steel materials, the water-cooling calandria 19 is adjusted through water temperature and plays a role in controlling axial temperature gradient, by utilizing the principle of entropy increase, the graphite decomposed by carbon hydrogen gas is attached to the surface of a carbon device downwards, the phenomenon that hot air flow takes pyrolytic graphite molecules to rise upwards is avoided, the calandria base 18 plays a role in fixing the water-cooling calandria and protects the cala.

The outer wall of the temperature thermocouple 14 is a silicon carbide ceramic tube, a tungsten-rhenium thermocouple wire is assembled inside the temperature thermocouple 14, and the middle position of the graphite resistance heating body 5 is a region with the highest temperature.

The outer side of the housing 2 is provided with a vacuum system which is communicated with the housing and comprises a valve and a vacuum pump, the first cylinder 8 and the second cylinder 15 are both externally connected with a control air source, a temperature control cold water circulating device is arranged outside the water cooling calandria 19, and the air inlet pipe 10 is externally connected with a hydrocarbon gas supply device.

The graphite electrode 6 and the motor 22 are both externally connected with a power supply, the graphite electrode 6 is electrically connected with the graphite resistance heating element 5, the temperature controller 21 is electrically connected with the graphite resistance heating element 5 through an electric wire, and the temperature thermocouple 14 is electrically connected with the temperature controller 21 through an electric wire.

A novel pyrolytic graphite vapor deposition device comprises a novel pyrolytic graphite vapor deposition production process, and comprises the following process steps:

the method comprises the following steps: placing the carbon element 20 on a carrying tray 17 of the supporting mechanism 4, and then controlling a second air cylinder 15 to drive a supporting table surface 16 to ascend, so that the carrying tray 17 drives the carbon element 20 to ascend to a working position;

step two: the valve of the vacuum system is opened, and the air pressure in the housing 2 is pumped to 6 multiplied by 10 by the vacuum pump-3Pa-10 Pa, and then closing the vacuum pump;

step three: heating, controlling the graphite resistance heating element 5 to start heating at a speed of 50-300 ℃/h, wherein the heating is a pyrolytic graphite process, the temperature of the temperature thermocouple 14 is kept constant for 2-6 h after the temperature rises to 2200 ℃, and the temperature of process water in the water-cooling calandria 19 is controlled to be 60-70 ℃;

step four: after the constant temperature is finished, the air inlet pipe 10 and the graphite baffle 13 descend to the half position of the heating element;

step five: at the moment, the gas inlet pipe 10 is supplied with hydrocarbon gas raw materials, and the gas inlet flow of each gas inlet pipe is 50 ml/min-5L/min;

step six: after the hydrocarbon gas raw material is sprayed out from the air inlet pipe 10, the carbon atoms inside the hydrocarbon gas raw material are decomposed at high temperature, and are deposited and attached to the surface of the carbon element 20 along with the air flow direction, the gravity direction and the condensation driving direction, and simultaneously, the temperature of the process water of the water-cooling calandria 19 is adjusted to be 25 ℃ at the moment in order to increase the condensation driving force due to the principle of entropy increase;

step seven: after the pyrolytic graphite is deposited for 10-30 minutes in a meteorological manner, controlling the motor 22 to start working, driving the carrying tray 17 by the motor 22 to rotate 90 degrees clockwise at the speed of ten minutes per rotation, keeping other process parameters unchanged in the rotating process, continuing to deposit in a static state for 10-30 minutes after the rotation is finished, then rotating 90 degrees clockwise, and so on, rotating 360-720 degrees in total in one preparation period, finely controlling the thickness of the pyrolytic graphite meteorological deposition coating, wherein the thickness ranges from 1 mu m to 10 mu m, and carbon elements form a grid-shaped multilayer coating with a hexagonal molecular structure on the carbon element 20;

step eight: after the vapor deposition process is finished, after the air inlet pipe 10 and the graphite baffle 13 rise to the initial position, the supply of the gas raw material of the air inlet pipe 10 is closed, and the temperature is reduced through the water-cooling calandria 19, the temperature reduction rate is not too fast, the surface coating of the carbon element 20 is prevented from cracking or falling off, the temperature reduction rate is 50-100 ℃/h, and the power is cut off when the temperature is reduced to 300 ℃;

step nine: and after the interior of the housing is completely cooled, opening the housing, taking out the prepared carbon element, and finishing the whole preparation period.

The process temperature of the pyrolytic carbon coating in the third step is 1600-1800 ℃, the process temperature of the pyrolytic graphite is 1900-2300 ℃, and the raw materials of the carbon hydrogen gas in the fifth step comprise methane, acetylene, other carbon hydrogen gas and the like.

Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes in the embodiments and/or modifications of the invention can be made, and equivalents and modifications of some features of the invention can be made without departing from the spirit and scope of the invention.

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