CN210506520U - Device for preparing DLC film on surface of super martensitic stainless steel - Google Patents
Device for preparing DLC film on surface of super martensitic stainless steel Download PDFInfo
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- CN210506520U CN210506520U CN201921658204.9U CN201921658204U CN210506520U CN 210506520 U CN210506520 U CN 210506520U CN 201921658204 U CN201921658204 U CN 201921658204U CN 210506520 U CN210506520 U CN 210506520U
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Abstract
The utility model relates to a device for preparing DLC film on the surface of super martensitic stainless steel, which comprises a vacuum cavity, a metal net cage, a sample rack, a molecular pump and a mechanical pump, wherein a hollow glass brick with an opening is fixed in the vacuum cavity of a sealing structure, the metal net cage is placed on the hollow glass brick, the metal net cage is a hollow rectangular structure woven by metal wires, and the metal net cage is provided with openings all around, so that electrons escape to form a loop; the sample frame is used for supporting the base body to be arranged in the center of the metal mesh cage, the sample frame penetrates through the metal mesh cage, two ends of the sample frame are arranged outside the metal mesh cage, and the bottom of the sample frame is supported on the vacuum cavity; an air inlet is arranged on the vacuum cavity; the vacuum cavity is connected with the gas cylinder through a pipeline with a valve. The advantages are that: the DLC film deposited by the device improves the film-substrate binding force so as to prolong the service life of the DLC film as the tubing steel.
Description
Technical Field
The utility model belongs to chemical vapor deposition preparation film field especially relates to a device at super martensite stainless steel surface preparation DLC film.
Background
The super martensitic stainless steel has good obdurability, excellent corrosion resistance and low cost, and can be used as a substitute material of super duplex stainless steel in a plurality of stainless steel application fields. Compared with the traditional martensitic stainless steel, the content of C is reduced by below 0.03 percent, the welding performance is greatly improved, the tensile strength is higher, and the large-scale production and application can be carried out. The Cr content is controlled to be 12-13%, the corrosion resistance is improved while the pitting sensitivity is reduced, the delta ferrite is reduced, and the toughness and the stress corrosion resistance of the super martensite are ensured. Therefore, the super martensitic stainless steel is mainly applied to the fields of petroleum gas transportation pipelines and the like which need high strength and toughness, can be produced in a large scale and have good corrosion resistance.
With the gradual reduction of non-renewable energy sources such as petroleum, natural gas and the like, the exploitation environment is increasingly severe, and the requirements on various performances of petroleum pipeline materials are also increasingly severe. In order to bear the requirements of deep wells and ultra-deep wells on yield strength and impact toughness, the method has important practical significance for the research of improving the toughness of the super martensitic stainless steel. CN101956146A introduces a high-strength and high-toughness super martensitic stainless steel which can be used in a deep well environment, reduces the production cost by designing the percentage of chemical components, and simplifies the heat treatment process to improve the production efficiency. The obtained steel is a low-carbon tempered martensite and inverted austenite complex phase structure, and the high strength and toughness of the super martensitic stainless steel suitable for deep wells and ultra-deep well environments are ensured.
With the increasing exploitation depth of oil-gas wells and the like, the use environment of the tubing steel is more severe, and the requirements on the corrosion resistance and the wear resistance of the surface of the steel are further improved. How to improve the corrosion resistance and the wear resistance of the super martensitic stainless steel on the basis of not influencing other properties is still the main focus of current research. Depositing a DLC film on the surface of super martensitic stainless steel and lowering the film deposition temperature requires a special apparatus.
Disclosure of Invention
In order to overcome the defects of the prior art, the utility model aims to provide a device for preparing DLC film on the surface of super martensitic stainless steel, which has reasonable structure and convenient use.
In order to achieve the above object, the utility model discloses a following technical scheme realizes:
a device for preparing a DLC film on the surface of super martensitic stainless steel comprises a vacuum cavity, a metal mesh cage, a sample rack, a molecular pump and a mechanical pump, wherein a hollow glass brick with an opening is fixed in the vacuum cavity of a sealing structure, the metal mesh cage is placed on the hollow glass brick, the metal mesh cage is a hollow rectangular structure woven by metal wires, and the metal mesh cage is provided with openings at the front, the back, the left and the right;
the sample frame is used for supporting the base body to be arranged in the center of the metal mesh cage, and the bottom of the sample frame is abutted against the inner bottom wall of the metal mesh cage; an air inlet is arranged on the vacuum cavity; the vacuum cavity is connected with the gas cylinder through a pipeline with a valve; the vacuum cavity is respectively connected with the mechanical pump and the molecular pump through pipelines, the other side of the molecular pump is connected with a front-stage valve, and the pipelines are communicated with external air;
the pulse power supply provides power for the vacuum cavity and the metal mesh cage.
The vacuum cavity is characterized by further comprising a heating wire, wherein more than two layers of aluminum foil paper are covered on the inner surface of the vacuum cavity, and the heating wire is arranged between the aluminum foil paper layers.
The sample holder is made of metal material.
Compared with the prior art, the beneficial effects of the utility model are that:
the utility model discloses rational in infrastructure, facilitate the use, utilize the sedimentary DLC membrane of this device, improved membrane base cohesion to prolong its life as the oil pipe steel. And a metal mesh cage with an opening is adopted to form an electron escape loop, so that the quality of the DLC film is ensured. The DLC film prepared on the surface of the super martensitic stainless steel by utilizing the device has compact structure, and obviously improves the performances of matrix hardness, friction reduction, corrosion resistance and the like.
Drawings
Fig. 1 is a schematic structural diagram of the present invention.
In the figure: 1-pulse power supply 2-vacuum cavity 3-air inlet 4-molecular pump 51-mechanical pump 52-backing valve 6-control box 7-base body 8-metal net cage 9-sample rack 10-gas cylinder.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings, but it should be noted that the present invention is not limited to the following embodiments.
Referring to fig. 1, the device for preparing the DLC film on the surface of the super martensitic stainless steel comprises a vacuum cavity 2, a metal mesh cage 8, a sample holder 9, a molecular pump 4 and a mechanical pump 51, wherein a hollow glass brick with an opening is fixed in the vacuum cavity 2 of a sealing structure, the metal mesh cage 8 is placed on the hollow glass brick, the metal mesh cage 8 is a hollow rectangular structure woven by metal wires, and the metal mesh cage 8 is provided with openings at the front, the back, the left and the right, so that electrons escape to form a loop; the sample frame 9 is used for supporting the base body 7 to be arranged in the center of the metal mesh cage 8, the middle part of the sample frame 9 supports the base body 7, and two ends of the bottom of the sample frame are abutted against the inner bottom wall of the metal mesh cage; the vacuum cavity 2 is provided with an air inlet 3 for pressure relief and balancing the pressure inside and outside the vacuum cavity; the vacuum cavity 2 is connected with the gas cylinder 10 through a pipeline with a valve; the vacuum cavity 2 is respectively connected with the mechanical pump 51 and the molecular pump 4 through pipelines, the other side of the molecular pump 4 is connected with a front-stage valve 52, and the pipelines are communicated with the outside air; the pulse power supply 1 supplies power to the metal mesh cage 8.
Wherein, the inner surface of the vacuum cavity 2 is coated with aluminum foil paper, the aluminum foil paper has more than two layers of structures, and heating wires are distributed among the layers. The sample holder 9 is made of a metal material. And a control box 6 is arranged outside the vacuum cavity and used for controlling the opening and closing of the mechanical pump, the molecular pump, the valve and the power supply. In the use process, the pulse power supply provides a cathode power supply for the metal mesh cage and the sample frame and provides an anode power supply for the vacuum cavity. The sample holder 9 is in contact with the metal mesh cage 8 and is at the same potential.
Example 1
The method for preparing the DLC film on the surface of the super martensitic stainless steel by utilizing the device comprises the following steps:
1) preparation of the substrate 7: the 13Cr super martensitic stainless steel is selected as the substrate 7 for coating.
The substrate 7 was cut into a sample having a size of 15 × 15 × 8mm, polished to a mirror surface with metallographic sandpaper until the surface thereof had no visible scratches.
And immersing the prepared sample into absolute ethyl alcohol for ultrasonic cleaning, wherein the heating temperature is 50 ℃, the ultrasonic frequency is 50Hz, and the cleaning is carried out for 20-30 min. And taking out after cleaning and drying.
2) See fig. 1, equipment installation: the rubber gloves are worn for operation, aluminum foil paper is fully paved on the inner surface of the vacuum cavity 2 to ensure that the aluminum foil paper is tightly adhered to the inner wall of the cavity and the electrical conductivity of the cavity is not influenced, the aluminum foil paper is divided into two layers, heating wires are arranged between the two layers, and parts of the heating wires, the air supply port, the air outlet, the valve and the like are exposed; the insulating glass brick and the metal mesh cage 8 are cleaned by absolute ethyl alcohol and are placed in a drying box for drying. After cooling, the metal mesh cage 8 is erected by using a hollow glass brick with an opening for explosion prevention, so that the metal mesh cage 8 is insulated from the vacuum cavity 2. The metal mesh cage 8 is opened at the front, rear, left and right sides to form an electron escape loop. The substrate 7 is placed on a conductive sample holder 9 inside a metal mesh cage 8. The coating surface faces upwards and is opposite to the metal mesh cage 8, and is connected with the negative bias of the pulse power supply 1 to ensure that the coating surface and the metal mesh cage 8 have the same potential. The metal mesh cage 8 is insulated from the vacuum cavity 2 and has the same potential with the matrix 7 by using a universal meter for detection, so that the phenomenon of short circuit or point discharge in the preparation process is prevented. The interior of the vacuum cavity 2 is dedusted, and the vacuum cavity 2 is closed after a sealing ring on the door of the vacuum cavity 2 is wiped by absolute ethyl alcohol.
3) Vacuumizing: when the pressure of the vacuum cavity 2 is lower than 2Pa, the molecular pump 4 is started; when the rotation speed of the molecular pump 4 reaches more than 2000r/min, the front-stage valve (flap valve) 52 is fully opened, and when the vacuum degree in the cavity reaches 10-4～10-3And when the pressure is Pa, heating, continuously vacuumizing the molecular pump 4, and removing residual water vapor in the cavity.
4) Internal high-pressure cleaning: when the vacuum degree in the cavity is reduced to 10-3～10-4And after Pa, opening an argon gas cylinder 10, setting the flow of argon gas to be 50-100 sccm, controlling the vacuum degree in the vacuum cavity 2 to be 2-4 Pa, and degassing for 20-30 min.
The pulse power supply 1 is turned on, the pulse bias voltage is set to 3000-3500V, the frequency is 1000-1200 Hz, and the pulse width is 15-20 mus. The pulse bias voltage needs to be increased slowly from 800-1000V with the increment of 300V every ten minutes until 3000-3500V, and the high-pressure cleaning of the substrate 7 is started. The voltage reduction caused by point discharge and overcurrent protection during cleaning needs to be manually set to the voltage before reduction.
5) Preparation of the transition layer and the DLC film: and closing argon, introducing tetramethylsilane, setting the gas flow to be 40-50 sccm, controlling the vacuum degree in the vacuum cavity 2 to be 1-2 Pa, controlling the temperature to be 110-150 ℃, and depositing for 30-40 min. Setting the flow rate of the tetramethylsilane gas to be 10-20 sccm; and opening an acetylene gas cylinder 10, introducing acetylene, and setting the flow of acetylene gas to be 10-20 sccm. Controlling the vacuum degree in the cavity to be 0.8-1 Pa, controlling the temperature to be 110-150 ℃, and depositing for 10-20 min. Two transition layers are deposited to play a role in buffering, stress generated in the film deposition process is slowed down, and the film-substrate binding force is improved.
And closing stop valves of other working gases and corresponding gas cylinders 10, opening the argon gas and acetylene gas cylinders 10, and setting the flow of the argon gas to be 50-60 sccm and the flow of the acetylene to be 20-30 sccm. The pulse bias voltage is reduced to 1600-2200V. The vacuum degree is controlled to be 1.5-2 Pa. The coating time is 2-3 h. And in the coating process, observing whether the gas discharge condition, the pulse voltage and the vacuum degree in the vacuum chamber change or not, and if so, adjusting in time.
6) Cooling after film coating: and after the film coating is finished, setting the acetylene flow to be 0sccm, and closing the stop valve and the gas cylinder 10. And (3) closing the pulse power supply 1, continuously introducing Ar until the temperature is reduced to 50-80 ℃, and closing the argon, the front-stage valve 52 and the molecular pump 4. After the rotation speed of the molecular pump 4 is about 0r/min, the front-stage valve 52 and the mechanical pump 51 are closed. And opening the air release valve to release air after placing for 3-4 h. And taking out the sample to detect the frictional wear performance and the corrosion performance.
If heating is needed in the whole process, the heating power supply is connected with the heating wire, and the heating power supply is used for electrifying the heating wire, so that the temperature in the vacuum cavity is increased.
Therefore, the antifriction and corrosion-resistant DLC film prepared on the surface of the super martensitic stainless steel by adopting the device can effectively improve the antifriction and corrosion-resistant performance of the super martensitic surface, can completely cover the surface of the substrate 7, improves the surface hardness of the substrate 7 and reduces the roughness.
Claims (3)
1. A device for preparing a DLC film on the surface of super martensitic stainless steel is characterized by comprising a vacuum cavity, a metal mesh cage, a sample rack, a molecular pump and a mechanical pump, wherein a hollow glass brick with an opening is fixed in the vacuum cavity of a sealing structure, the metal mesh cage is placed on the hollow glass brick, the metal mesh cage is a hollow rectangular structure woven by metal wires, and the metal mesh cage is provided with openings at the front, the back, the left and the right, so that electrons escape to form a loop;
the sample frame is used for supporting the base body to be arranged in the center of the metal mesh cage, and the bottom of the sample frame is abutted against the inner bottom wall of the metal mesh cage; an air inlet is arranged on the vacuum cavity; the vacuum cavity is connected with the gas cylinder through a pipeline with a valve; the vacuum cavity is respectively connected with the mechanical pump and the molecular pump through pipelines, the other side of the molecular pump is connected with a front-stage valve, and the pipelines are communicated with external air;
the pulse power supply provides power for the vacuum cavity and the metal mesh cage.
2. The device for preparing the DLC film on the surface of the super martensitic stainless steel as claimed in claim 1, further comprising a heating wire, wherein more than two layers of aluminum foil are coated on the inner surface of the vacuum cavity, and the heating wire is arranged between the layers of the aluminum foil.
3. The apparatus for preparing DLC film on the surface of super martensitic stainless steel as claimed in claim 1 wherein, said sample holder is made of metal material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921658204.9U CN210506520U (en) | 2019-09-30 | 2019-09-30 | Device for preparing DLC film on surface of super martensitic stainless steel |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201921658204.9U CN210506520U (en) | 2019-09-30 | 2019-09-30 | Device for preparing DLC film on surface of super martensitic stainless steel |
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| CN201921658204.9U Active CN210506520U (en) | 2019-09-30 | 2019-09-30 | Device for preparing DLC film on surface of super martensitic stainless steel |
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