Disclosure of Invention
In order to solve the technical problems, the invention provides a deposition device which is simple in structure and convenient to operate and can be used for depositing pyrolytic carbon with large thickness and uniform structure. The invention also provides a method for preparing the pyrolytic carbon, which can be used for depositing the pyrolytic carbon with large thickness, uniform structure and high density.
The utility model provides a deposition device, includes axis of rotation, inlet channel, barrel, is located deposition substrate in the barrel, be equipped with the apron on the barrel, the through-hole has been seted up on the apron, deposition substrate with the apron sets up relatively, deposition substrate with axis of rotation fixed connection, the barrel with inlet channel intercommunication.
The deposition device preferably further comprises a guide rod, the guide rod is fixedly connected with the deposition substrate, the guide rod extends out of the cylinder from the opening of the cover plate, and the guide rod and the rotating shaft are respectively located on two sides of the deposition substrate.
In the deposition apparatus, preferably, the guide rod is coaxial with the rotation shaft, and the rotation shaft is perpendicular to the plane of the deposition substrate.
The deposition device preferably further comprises a furnace body, and the furnace body is located outside the barrel.
The deposition device preferably further comprises a motor, wherein the rotating shaft is connected with the motor, and the motor is used for driving the rotating shaft to rotate.
In the deposition apparatus, preferably, the diameter of the through hole ranges from 25mm to 125mm, and the diameter of the deposition substrate ranges from 50mm to 200 mm.
In the deposition apparatus, preferably, the gas inlet channel is used for introducing a carrier gas and a carbon source gas.
The method for preparing the pyrolytic carbon by using the deposition device comprises the following steps:
s1, introducing carrier gas into the cylinder;
s2, raising the temperature in the cylinder to 1300-1500 ℃, raising the pressure in the cylinder to 70-100 MPa, adjusting the rotating speed of the rotating shaft to 10-30 r/min, introducing carbon source gas into the cylinder, and depositing for 20-40 h;
and S3, stopping introducing the carbon source gas, continuing introducing the carrier gas, and cooling to obtain the pyrolytic carbon.
In the method for preparing pyrolytic carbon, preferably, the flow rate of the mixed gas composed of the carrier gas and the carbon source gas is 15-30L/min, wherein the mass concentration of the carbon source gas is 40-70%.
In the method for preparing pyrolytic carbon, preferably, the carbon source gas is one or more of propylene, propane and acetylene.
The deposition device provided by the invention drives the deposition substrate to rotate through the rotating shaft, so that the uniform deposition of the carbon source gas on the deposition substrate can be ensured, and the uniform distribution of the thickness of the deposition film can be ensured. The deposition time is prolonged, the pyrolytic carbon with large thickness and uniform density can be obtained, and meanwhile, the structure of the invention is simple, and the production cost is reduced. The method for preparing the pyrolytic carbon is realized by the deposition device provided by the invention, and the high-density pyrolytic carbon can be obtained by adjusting technological parameters such as pressure and the like while the pyrolytic carbon with large thickness and uniform density can be prepared.
Detailed Description
In order to make those skilled in the art better understand the technical solutions in the present application, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, 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 application.
As shown in fig. 1, a deposition apparatus according to a preferred embodiment of the present invention includes: axis of rotation 5, inlet channel 7, barrel 1 and the deposit base plate 4 that is located barrel 1 are equipped with apron 3 on the barrel 1, have seted up through-hole 9 on the apron 3, deposit base plate 4 and axis of rotation 5 fixed connection, and deposit base plate 4 sets up with apron 3 relatively, barrel 1 and inlet channel 7 intercommunication.
The deposition device provided by the invention drives the deposition substrate 4 to rotate through the rotating shaft 5, so that the carbon source gas can be ensured to be uniformly deposited on the deposition substrate 4, and the thickness distribution of the deposited film is ensured to be uniform. By extending the deposition time, pyrolytic carbon having a large thickness and a uniform density can be obtained.
Wherein the barrel 1 is preferably provided in a cylindrical shape, the deposition substrate 4 is preferably provided in a circular plate, and the deposition substrate 4 is used to support the deposited pyrolytic carbon. Because the deposition substrate 4 is fixedly connected with the rotating shaft 5, the rotating shaft 5 can drive the deposition substrate 4 to rotate when rotating, so that the pyrolytic carbon is deposited on the deposition substrate 4. The interface of the air inlet channel 7 and the cylinder 1 is preferably arranged on the bottom plate of the cylinder 1, the air inlet channel 7 is used for conveying air into the cylinder 1, preferably, the air inlet channel can be provided with an air inlet 8, and the air inlet 8 is used for introducing the same or different air. The through hole 9 opened on the cover plate 3 is used for making the redundant gas in the cylinder 1 flow out. The deposition substrate 4 is disposed opposite to the cover plate 3, preferably in parallel. During deposition, gas including carbon source gas enters the barrel 1 from the gas inlet channel 7, the rotating shaft 5 drives the deposition substrate 4 to rotate, carbon source gas particles are deposited above the deposition substrate 4, and redundant gas flows out from a through hole 9 formed in the cover plate 3.
The deposition device of the present invention may further include a guide rod 6, wherein the guide rod 6 is fixedly connected to the deposition substrate 4, the guide rod 6 extends out of the barrel 1 from the opening of the cover plate 3, and the guide rod 6 and the rotation shaft 5 are respectively located at two sides of the deposition substrate 4.
The guide rod 6 is preferably a cylindrical rod body, the guide rod 6 is located on the deposition substrate 4 and extends out of the barrel 1 from the opening of the cover plate 3, the guide effect on gas escaping from the barrel 1 in the barrel 1 can be achieved, and the gas in the barrel 1, particularly the gas above the deposition substrate 4, is uniformly and stably led out from the through hole 9 in the direction, so that the deposition thickness and density of pyrolytic carbon are prevented from being different, and the technical effect of uniform deposition of pyrolytic carbon is achieved.
Preferably, the guide rods 6 are arranged coaxially with the rotation axis 5, and the rotation axis 5 is perpendicular to the plane of the deposition substrate 4. Through setting up guiding rod 6 and axis of rotation 5 to coaxial and guiding rod 6 and axis of rotation 5 all perpendicular to deposition substrate 4 plane for guiding rod 6 can be with gaseous from leading out barrel 1 with deposition substrate 4 perpendicular direction, thereby makes the pyrolytic carbon deposit more even.
The deposition apparatus described in this embodiment further includes a furnace body 2, and the furnace body 2 is located outside the cylinder 1. The heating device is arranged in the furnace body 2 and can play a role in heating the temperature of the cylinder body 1 and the temperature of the heat preservation cylinder body 1.
The deposition apparatus of this embodiment further includes a motor, the rotating shaft 5 is connected to the motor, and the motor is used to drive the rotating shaft 5 to rotate. Because deposition substrate 4 and axis of rotation 5 fixed connection, so when motor drive axis of rotation 5 rotated, axis of rotation 5 can drive deposition substrate 4 rotatory, realized the even deposit of pyrolytic carbon on deposition substrate 4, and the rotation of axis of rotation 5 should keep even as far as possible to make the deposit of pyrolytic carbon more even.
In the deposition apparatus of this embodiment, the diameter of the through-hole 9 is preferably set to be 25 to 125mm, and the diameter of the deposition substrate 4 is preferably set to be 50 to 200 mm.
In the deposition apparatus of the present embodiment, the gas inlet channel 7 is used for introducing carrier gas and carbon source gas. The carrier gas can be hydrogen or inert gas, the carrier gas is introduced before the carbon source gas is introduced, the air in the cylinder 1 can be driven away, the carrier gas is introduced while the carbon source gas is introduced, the deposition of the carbon source gas can be protected, and the carbon source gas is prevented from reacting with oxygen.
The invention also provides a method for preparing pyrolytic carbon by using the deposition device, which mainly comprises the following steps:
s1, introducing carrier gas into the cylinder 1;
s2, raising the temperature in the cylinder 1 to 1300-1500 ℃, raising the pressure in the cylinder 1 to 70-100 MPa, adjusting the rotating speed of the rotating shaft 5 to 10-30 r/min, introducing carbon source gas into the cylinder 1, and depositing for 20-40 h;
and S3, stopping introducing the carbon source gas, continuing introducing the carrier gas, and cooling to obtain the pyrolytic carbon.
Wherein, the flow range of the mixed gas composed of the carrier gas and the carbon source gas is preferably set to be 15-30L/min, and the mass concentration of the carbon source gas is preferably set to be 40-70%.
The carbon source gas is one or more of propylene, propane and acetylene, and can also be other hydrocarbon gases.
According to the method for preparing the pyrolytic carbon, provided by the invention, when the pyrolytic carbon is prepared, the deposition substrate 4 is driven to rotate through the rotating shaft 5, so that the carbon source gas is ensured to be uniformly deposited on the deposition substrate 4, the thickness distribution of the deposited film is ensured to be uniform, the pyrolytic carbon with uniform density and structure can be obtained, when the deposition time is prolonged, the pyrolytic carbon with large thickness can be obtained, and the pyrolytic carbon which is suitable for requirements can be obtained by adjusting technological parameters such as pressure, the size of the cover plate 3 and the through hole 9, temperature and the like.
In the following 3 preferred embodiments are given.
Example 1
The deposition device with the deposition substrate 4 having a diameter of 80mm and the cover plate 3 having the through hole 9 having a diameter of 30mm was previously cleaned to remove graphite particles attached to the surface of the substrate during the previous processing, and the deposition device was dried to remove moisture, thereby checking the sealing property of the device.
Introducing nitrogen into the cylinder 1, setting the temperature in the cylinder 1 to be 1300-1400 ℃ under the nitrogen protection atmosphere, setting the absolute pressure of the system to be 90-100 MPa, turning on the motor to drive the rotating shaft 5 to rotate, and adjusting the rotating speed of the motor to be 20-30 r/min. And when the temperature and the system absolute pressure reach set values and are kept stable, opening a methane valve, filling propane gas into the cylinder body 1, and adjusting the flow values of the nitrogen and the propane to ensure that the flow range of mixed gas consisting of the nitrogen and the methane gas is 15-30L/min, wherein the mass concentration of the methane gas is 40-70%.
After 25 hours of deposition, the methane valve was closed and nitrogen was continued to stop the deposition. After the power is cut off and the temperature is reduced, a pyrolytic carbon part is formed on the deposition substrate 4. The density of the obtained pyrolytic carbon material is 1.82g/cm3The elastic modulus is 11.5GPa, the deposition thickness is 12mm, and the diameter is 70 mm.
Example 2
The deposition device with the diameter of the deposition substrate 4 being 120mm and the diameter of the through hole 9 of the cover plate 3 being 40mm was previously cleaned to remove graphite particles attached to the surface during the previous processing, and the deposition device was dried to remove moisture and to check the sealing property of the device.
Introducing hydrogen into the cylinder 1, setting the temperature in the cylinder 1 to 1400-1500 ℃ and the absolute pressure of the system to 80-100 MPa in a hydrogen protective atmosphere, turning on a motor to drive a rotating shaft 5 to rotate, and adjusting the rotating speed of the motor to 20 r/min. And when the temperature and the system absolute pressure reach set values and are kept stable, opening a propane valve, filling propane gas into the cylinder body 1, and adjusting the flow values of hydrogen and propane to ensure that the flow range of mixed gas consisting of the hydrogen and the propane gas is 20-30L/min, wherein the mass concentration of the propane gas is 40-70%.
After 30 hours of deposition, the propane valve was closed and hydrogen was continued to stop the deposition. After the power is cut off and the temperature is reduced, a pyrolytic carbon part is formed on the deposition substrate 4. The density of the obtained pyrolytic carbon material is 1.85g/cm3The elastic modulus is 11.9GPa, the deposition thickness is 15mm, and the diameter is 100 mm.
Example 3
The deposition apparatus having the deposition substrate 4 with a diameter of 150mm and the cover plate 3 with the through-hole 9 with a diameter of 50mm was previously cleaned to remove graphite particles attached to the surface during the previous processing, and the deposition apparatus was dried to remove moisture, and the sealing property of the apparatus was examined.
Introducing hydrogen into the cylinder 1, setting the temperature in the cylinder 1 to 1400-1500 ℃ and the absolute pressure of the system to 70-90 MPa in a hydrogen protective atmosphere, turning on a motor to drive a rotating shaft 5 to rotate, and adjusting the rotating speed of the motor to 20 r/min. And when the temperature and the system absolute pressure reach set values and are kept stable, opening an acetylene valve, filling acetylene gas into the cylinder 1, and adjusting the flow values of the hydrogen and the acetylene to ensure that the flow range of mixed gas consisting of the hydrogen and the acetylene gas is 20-30L/min, wherein the mass concentration of the acetylene gas is 40-70%.
After 20 hours of deposition, the acetylene valve was closed, and hydrogen was continuously introduced to stop the deposition. After the power is cut off and the temperature is reduced, a pyrolytic carbon part is formed on the deposition substrate 4. The density of the obtained pyrolytic carbon material is 1.91g/cm3The elastic modulus is 12.8GPa, the deposition thickness is 11mm, and the diameter is 140 mm.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.