CN115961238B - Film plating device and film plating method for inner wall of pipe body - Google Patents
Film plating device and film plating method for inner wall of pipe body Download PDFInfo
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Abstract
The invention discloses a film plating device for the inner wall of a pipe body, which comprises a furnace body, wherein the furnace body is a double-layer vacuum furnace and serves as an anode, the furnace wall is cooled by circulating water, a furnace bottom tray is arranged at the inner side of the bottom of the furnace body, the furnace bottom tray is connected with a rod-shaped anode and a workpiece bearing tray, a hollow target and an auxiliary tool are arranged on the workpiece bearing tray, the hollow target penetrates through the rod-shaped anode, the auxiliary tool is used for preserving heat and supporting the hollow target, a tubular workpiece is arranged at the outer side of the hollow target and at the inner side of the auxiliary tool, a workpiece cathode and a target cathode are also arranged in the furnace body, the workpiece cathode is connected with the workpiece bearing tray, the workpiece bearing tray is connected with the tubular workpiece in a conductive manner, the target cathode is connected with the hollow target through a connecting guide rod, the workpiece cathode and the second power supply form a loop, and the furnace body forms glow discharge. When the invention is used for treating tubular workpieces, the coating has strong designability, and the elements can be selected from various types, such as metals, alloys thereof or conductive ceramics.
Description
Technical Field
The invention belongs to a coating device and a coating method, in particular to a coating device and a coating method for the inner wall of a pipe body.
Background
The inner wall of the metal pipe fitting is easy to generate the problems of corrosion, abrasion, oxidation and the like in the working environment, and the inner wall of the metal pipe fitting is required to be prepared with a protective coating in actual use. Such components have complicated structure, and the inner wall surface of the components is difficult to protect, and the large-scale protection is mainly plating or paint coating. For components under severe environments, such as weapon barrels, automobile sleeve cylinders and the like, not only the protection effect of the current method needs to be improved, but also along with the increasing serious environmental and energy problems, the development of green and efficient tubular component inner wall surface modification technology and equipment is more and more necessary.
Over decades, plasma surface modification techniques have been focused on with their unique advantages, however, the techniques currently known to those skilled in the relevant industry still have problems and cannot be widely used. For example, plasma chemical vapor deposition has a large limit on the types of coatings, and the uniformity of the coatings prepared on the components is poor, magnetron sputtering has a wide range of types of films which can be deposited, but the combination mode of a film layer and a pipe wall is mechanical combination and does not meet the use requirement under the action of stress, and arc ion plating has a high speed and high deposition quality, but as the pipe depth increases, plasma is reduced, coating is difficult to perform, and the length of the pipe is strictly limited.
Chinese patent application No. 202210997864.X discloses a method of spin-wave plume accelerated alloy powder sputter coating in an elongated metal tube, where a spin-wave plasma plume and molten droplets are sprayed onto an alloy sputter target in the metal tube to produce negatively charged alloy droplets capable of being sputtered to cover 360 ° angular degrees and having a diameter less than 35um, a positive voltage is applied between the sputter target and the metal tube to accelerate the alloy droplets so that the velocity of the alloy droplets reaches 2000m/s, and the high-speed alloy droplets melt the substrate on the inner wall of the metal tube and form a metallurgical molten alloy coating. However, the inner wall coating prepared by the method has rough surface, insufficient overall uniformity and larger internal stress of the coating after solidification of the metal liquid drops.
Therefore, the development of new surface modification technology which has good binding force, is clean and efficient, is suitable for uniformly coating the inner wall of a tubular member, and particularly the coating of the inner wall of a pipe fitting which needs high-quality coating is a problem to be solved.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and aims to provide a green, efficient and uniform coating device for the inner wall of a pipe body.
The invention adopts the technical scheme that the film plating device for the inner wall of the pipe body comprises a furnace body, wherein the furnace body is a double-layer vacuum furnace and serves as an anode, the furnace wall is cooled by circulating water, a furnace bottom tray is arranged at the inner side of the bottom of the furnace body, the furnace bottom tray is connected with a rod-shaped anode and a workpiece bearing tray, a hollow target and an auxiliary tool are arranged on the workpiece bearing tray, the hollow target penetrates through the rod-shaped anode, the auxiliary tool is used for preserving heat and supporting the hollow target, a tubular workpiece is arranged at the outer side of the hollow target and at the inner side of the auxiliary tool, a workpiece cathode and a target cathode are also arranged in the furnace body, the workpiece cathode is connected with the workpiece bearing tray, the workpiece bearing tray is connected with the tubular workpiece in a conductive way and is used for bearing and positioning the workpiece, the workpiece electrode rod is prevented from being excessively deformed, the target cathode is connected with the hollow target through a connecting guide rod, the workpiece cathode and the second power supply and the furnace body form a loop, glow discharge is generated, the target cathode and the first power supply and the furnace body form a loop, glow discharge is used for generating sputtering elements and depositing on the surface of the workpiece, the target cathode and the workpiece cathode generate double-hollow effect, and the glow effect of elements are accelerated.
Further, the hollow target is in a cylindrical shape formed by uniformly winding a wire-shaped target, and each circle is connected with the hollow target by spot welding on the outer side by using the same material as the hollow target. The hollow cathode effect is utilized to accelerate the coating speed, the material is any metal simple substance and alloy thereof, and particularly, the advantage of high-melting point metal is obvious, and the diameter of the wire can be adapted to the diameter of a tubular workpiece to change.
Further, the surface of the hollow target is provided with a ceramic connecting hole and an electronic channel hole, the diameter of the electronic channel hole is 1-2 mm, plasma is uniformly discharged, uniformity of a film layer is improved, the ceramic connecting hole is used for penetrating a ceramic connecting rod and is connected with an auxiliary tool, and the ceramic connecting rod is made of insulating ceramic.
Further, the wall thickness of the hollow target is 3-5 mm, and the outer wall of the hollow target is 5-25 mm away from the inner wall of the tubular workpiece. The hollow target is made of metal or conductive ceramic.
In order to avoid the point discharge, the workpiece cathode, the target cathode and the hollow target are all cylindrical.
In order to prevent material contamination, the connecting guide rod is the same material as the hollow target.
Further, the lower bottom of the workpiece bearing tray is supported by insulating ceramics and is arranged on the bottom tray, and the bottom tray shields the air extraction opening to prevent pollution.
Further, the diameter of the rod-shaped anode is 3-5 mm, and the rod-shaped anode is made of one or more of Ta, W and Mo. The rod-shaped anode is used for absorbing electrons, so that the target is uniformly discharged, and the coating quality is improved.
The coating method of the coating device for the inner wall of the pipe body comprises the following steps:
Firstly, polishing the inner wall of a tubular workpiece to 1500 meshes by using sand paper, and then wiping, cleaning and airing the tubular workpiece, a hollow target, a workpiece bearing tray, a rod-shaped anode and a furnace bottom tray by using ethanol with concentration of more than 95%;
step two, sequentially loading all the cleaned parts into a furnace body;
Turning on a mechanical pump, pumping the air pressure of the furnace body to below 1Pa, then filling argon to above 200Pa, pumping to below 1Pa, repeatedly washing the air, and filling the argon to maintain the pressure of 20-80 Pa;
Step four, slowly increasing the cathode voltage of the workpiece to 300-500V, and cleaning and heating the tubular workpiece for 30-60 min by using plasma glow;
Step five, opening and slowly increasing the cathode voltage of the target to 600-950V, and simultaneously increasing the cathode voltage of the workpiece to 450-700V, so that the working air pressure is 20-80 Pa, the distance between the hollow target and the inner wall of the tubular workpiece is 5-25 mm, and the heat preservation time is 3-6 h;
Step six, after the heat preservation is finished, the voltage of the hollow target material and the tubular workpiece is reduced to 0V, the time of the process is more than 30min, then the vacuum is pumped to below 0.1Pa, and the hollow target material and the tubular workpiece are taken out after being cooled along with a furnace.
The device takes the whole furnace body grounded as an anode, and two negative potential electrodes as two cathodes, namely a target cathode and a workpiece cathode, are placed in the furnace. The target cathode is connected with a sputtering target material for sputtering coating elements and depositing the coating elements on the surface of the workpiece. During operation, the cathode potential of the target is more negative than that of the workpiece cathode (i.e. the voltage of the target electrode is higher), ionized argon ions sputter more surface elements of the target, meanwhile, electrons accumulated on the surface can be transferred to the rod-shaped anode through the electron channel due to the special hollow target structure, so that the whole is uniformly discharged, and the effect of high-quality uniform coating of the inner wall is achieved. The target cathode and the workpiece cathode glow simultaneously to generate a hollow cathode effect, so that the element sputtering and the technological process are accelerated.
Compared with the prior art, the invention has the following remarkable characteristics:
1. When a tubular workpiece is processed, the coating has strong designability, the element can be selected in various types, and can be any metal, alloy thereof or conductive ceramic, and the coating has obvious advantages especially in the selection of high-melting-point metal and conductive ceramic and can be combined arbitrarily;
2. The hollow target material can accelerate the coating speed by utilizing the hollow cathode effect, and the electron channel and the rod-shaped anode structure can lead the plasma discharge to be more uniform and controllable;
3. the inner wall coating of the tubular workpiece is uniform and controllable, has strong binding force with the tubular workpiece, is metallurgically bonded, has gradient distribution of coating components, small stress and good protection effect;
4. The preparation method is green and efficient, has no environmental pollution, saves resources, has simple equipment and process, is clean and efficient, and is suitable for industrialized popularization.
Drawings
FIG. 1 is a schematic diagram of the structure of the present invention;
Fig. 2 is a schematic structural view of a first hollow target 9 according to the present invention;
Fig. 3 is a schematic structural view of a second hollow target 9 according to the present invention;
FIG. 4 is a scanning electron microscope image of a sampling section of embodiment 1 of the present invention;
FIG. 5 is a distribution diagram of elements of a sampling section according to example 1 of the present invention;
FIG. 6 is a scanning electron microscope image of a sampling section according to example 2 of the present invention;
FIG. 7 is a distribution diagram of elements of a sampling section according to example 2 of the present invention.
Detailed Description
As shown in FIG. 1, the furnace body 3 of the film plating device on the inner wall of the pipe body is a double-layer vacuum furnace and is grounded as a whole as an anode, and the furnace wall is cooled by circulating water. The opening mode of the furnace body 3 is not limited, and can be manufactured into any shape according to the requirements. The inner side of the bottom of the furnace body 3 is provided with a furnace bottom tray 7, the exhaust opening is shielded to prevent pollution, the furnace bottom tray 7 is connected with a rod-shaped anode 8 and is connected with a workpiece bearing tray 6 in a ceramic insulation manner, and the functions of connecting the rod-shaped anode 8 and supporting the workpiece bearing tray 6 are achieved. The hollow target 9 and the auxiliary tool 11 are arranged on the workpiece bearing tray 6, the rod-shaped anode 8 penetrates through the hollow target 9, the auxiliary tool 11 is used for preserving heat and supporting the hollow target 9, and the tubular workpiece 10 is arranged on the outer side of the hollow target 9 and the inner side of the auxiliary tool 11. The furnace body 3 is also internally provided with a workpiece cathode 4 and a target cathode 5, the tubular workpiece 10 is electrically connected with the workpiece cathode 4 and the workpiece bearing tray 6, and a cylindrical shape is adopted for avoiding the point discharge. The workpiece bearing tray 6 is electrically connected with the tubular workpiece 10, the target cathode 5 is electrically connected with the hollow target 9 through the connecting guide rod 12, and the connecting guide rod 12 is the same as the hollow target 9 in order to prevent material pollution. The workpiece cathode, the power supply II and the furnace body 3 form a loop to generate glow discharge for activating and heating the surface of the tubular workpiece 10, the target cathode 5, the power supply I and the furnace body form another loop to generate glow discharge for sputtering target elements and depositing the target elements on the surface of the workpiece, and the target cathode 5 and the workpiece cathode 4 generate double glow hollow cathode effect to accelerate the sputtering and technological process of the elements. The workpiece cathode 4, the target cathode 5 and the hollow target 9 are all cylindrical. The lower bottom of the workpiece bearing tray 6 is supported by insulating ceramics and is arranged on the furnace bottom tray 7. The diameter of the rod-shaped anode 8 is 3-5 mm, and the rod-shaped anode is made of one or more of Ta, W and Mo.
The wall thickness of the hollow target 9 is 3-5 mm, the outer wall being spaced from the tubular shape the inner wall of the workpiece 10 is 5-25 mm. The hollow target 9 is made of conductive metal or ceramic. The hollow target 9 can be of two structures. As shown in fig. 2, a ceramic connecting hole 901 and an electronic channel hole 902 are formed in the surface of a first hollow target 9, the diameter of the electronic channel hole 902 is 1-2 mm, the vertical distance is 10-15mm, and the ceramic connecting hole 901 is used for penetrating through a ceramic connecting rod and connecting with an auxiliary tool 11. As shown in fig. 3, the second hollow target 9 is a cylindrical tube formed by uniformly winding a wire-shaped target, and each ring is connected by spot welding with the same material as the hollow target 9 at the outer side. Preferably a hollow target 9 of fig. 2.
Example 1
The coating method of the coating device for the inner wall of the pipe body comprises the following steps:
Firstly, polishing the inner wall of a tubular workpiece to 1500 meshes by using sand paper, and then wiping, cleaning, airing and the like components of a pure copper pipe fitting (99.99%), a pure Ta hollow target material 4 (99.95%), a stainless steel workpiece bearing tray 6, a pure Ta rod-shaped anode 8, a stainless steel furnace bottom tray 7 and the like with the inner diameter of 40mm, the outer diameter of 20mm and the wall thickness of 3mm by using industrial ethanol with the concentration of 95%;
Step two, all the cleaned parts are sequentially arranged in a furnace body 3 from bottom to top according to a stainless steel furnace bottom tray 7, a workpiece cathode 4, a target cathode 5, a pure copper tubular workpiece 10, a pure Ta hollow target 9, an auxiliary tool 11 and a pure Ta rod-shaped anode 8;
Turning on a mechanical pump, pumping the air pressure of the furnace body 3 to below 1Pa, performing gas washing operation, filling argon with the purity of 99.999% to 200Pa, pumping to below 1Pa, repeating the operation for two times, and filling the argon to be maintained at 35Pa;
step four, slowly raising the voltage of the cathode 4 of the workpiece to 300V, and cleaning and heating the tubular workpiece 10 for 30min by using plasma glow;
step five, opening and slowly increasing the voltage of the target cathode 5 to 850V, and simultaneously increasing the voltage of the workpiece cathode 4 to 600V, so that the working air pressure is 35Pa, the distance between the hollow target 9 and the inner wall of the tubular workpiece 10 is 10mm, and the heat preservation time is 3h;
Step six, after the heat preservation is finished, the voltage of the hollow target 9 and the tubular workpiece 10 is reduced to 0V, the process takes 40min, then the vacuum is pumped to below 0.1Pa, and the hollow target is taken out after being cooled for 8h along with a furnace.
Performance test:
As shown in FIG. 4, the sample section of the tubular workpiece 10 coated with the coating film of the embodiment is photographed by a scanning electron microscope, and the result shows that the coating is very uniform and compact, and the coating inside and the transition part of the substrate are defect-free. As shown in FIG. 5, the effective thickness of the coating is 17 mu m, and the coating elements are distributed in a gradient manner, so that the bonding force of the coating is effectively improved. .
The inner wall of the pipe fitting is contacted with molten cerium metal in a vacuum environment at 1000 ℃, the pure copper component 3h is severely corroded, and the coating component obtained in the embodiment 1 is still intact after 60h, so that the metal corrosion resistance is improved by more than 20 times.
Example 2
The coating method of the coating device for the inner wall of the pipe body comprises the following steps:
Firstly, polishing the inner wall of a tubular workpiece to 1500 meshes by using sand paper, and then wiping, cleaning, airing and the like components of an alloy steel pipe fitting (PCrNi 3 MoVA) with the inner diameter of 40mm, a pure Ta hollow target material 4 (99.95%) with the outer diameter of 20mm and the wall thickness of 3mm, a stainless steel workpiece bearing tray 6, a pure Ta rod-shaped anode 8 with the diameter of 3mm, a stainless steel furnace bottom tray 7 and the like by using industrial ethanol with the concentration of 95%;
Step two, all the cleaned parts are sequentially arranged in a furnace body 3 from bottom to top according to a stainless steel furnace bottom tray 7, a workpiece cathode 4, a target cathode 5, a pure copper tubular workpiece 10, a pure Ta hollow target 9, an auxiliary tool 11 and a pure Ta rod-shaped anode 8;
Turning on a mechanical pump, pumping the air pressure of the furnace body 3 to below 1Pa, performing gas washing operation, filling argon with the purity of 99.999% to 200Pa, pumping to below 1Pa, repeating the operation for two times, and filling the argon to be maintained at 40Pa;
Step four, slowly raising the voltage of the cathode 4 of the workpiece to 300V, and cleaning and heating the tubular workpiece 10 by using plasma glow for 40min;
Step five, opening and slowly increasing the voltage of the target cathode 5 to 900V, and simultaneously increasing the voltage of the workpiece cathode 4 to 650V, so that the working air pressure is 40Pa, the distance between the hollow target 9 and the inner wall of the tubular workpiece 10 is 10mm, and the heat preservation time is 3.5h;
Step six, after the heat preservation is finished, the voltage of the hollow target 9 and the tubular workpiece 10 is reduced to 0V, the process takes 40min, then the vacuum is pumped to below 0.1Pa, and the hollow target is taken out after being cooled for 8h along with a furnace.
Performance test:
As shown in FIG. 6, the sample section of the tubular workpiece 10 coated with the coating film of the present example was photographed by a scanning electron microscope, and the results showed that the coating was very uniform and dense, and that the coating was defect-free both in the interior and in the transition with the substrate. As shown in FIG. 7, the overall effective thickness of the coating is approximately 20 mu m, the coating elements are distributed in a gradient manner, and the bonding force of the coating is effectively improved.
The oxidation performance test is carried out on the pipe sample for 40 hours under the atmospheric environment at 650 ℃, and the result shows that the uncoated sample is seriously oxidized, and finally the weight of the uncoated sample is increased by 3.52mg/cm 2, while the weight of the coated pipe sample is increased by 1.26mg/cm 2, and the oxidation resistance is still good and is improved by more than 2.8 times.
Claims (9)
1. A film plating device for the inner wall of a tube body is characterized by comprising a furnace body (3), wherein the furnace body (3) is a double-layer vacuum furnace and is used as an anode, a furnace wall is cooled by circulating water, a furnace bottom tray (7) is arranged at the inner side of the bottom of the furnace body (3), the furnace bottom tray (7) is connected with a rod-shaped anode (8) and a workpiece bearing tray (6), a hollow target (9) and an auxiliary tool (11) are arranged on the workpiece bearing tray (6), the hollow target (9) penetrates through the rod-shaped anode (8), the auxiliary tool (11) is used for preserving heat and supporting the hollow target (9), a tubular workpiece (10) is arranged at the outer side of the hollow target (9) and the inner side of the auxiliary tool (11), a workpiece cathode (4) and a target cathode (5) are further arranged in the furnace body (3), the workpiece cathode (4) is connected with the workpiece bearing tray (6), the workpiece bearing tray (6) is electrically connected with the tubular workpiece (10), the target cathode (5) is connected with the hollow target (9) through a connecting guide rod (12), the workpiece cathode (4) and the tubular workpiece cathode (5) are used for generating a glow circuit (1) and a power supply, a secondary power supply (1) and a secondary power supply (2) and a heating circuit (1) is formed The furnace body (3) forms a loop to generate glow discharge for sputtering target elements and depositing the target elements on the surface of a workpiece;
the surface of the hollow target (9) is provided with a ceramic connecting hole (901) and an electronic passage hole (902), the diameter of the electronic passage hole (902) is 1-2 mm, the vertical distance is 10-15 mm, and the ceramic connecting hole (901) is used for penetrating through a ceramic connecting rod and connecting with an auxiliary tool (11);
the target cathode (5) and the workpiece cathode (4) glow simultaneously to generate a hollow cathode effect.
2. The coating device for the inner wall of the pipe body according to claim 1, wherein the hollow target (9) is in a cylindrical shape formed by uniformly winding a wire-shaped target, and each ring is connected with the hollow target (9) by spot welding on the outer side by using the same material as the hollow target.
3. The coating device for the inner wall of the pipe body according to claim 1, wherein the wall thickness of the hollow target material (9) is 3-5 mm, and the outer wall of the hollow target material is 5-25 mm away from the inner wall of the tubular workpiece (10).
4. A coating device for the inner wall of a pipe body according to claim 1, characterized in that the hollow target (9) is made of metal or conductive ceramic.
5. The coating device for the inner wall of the pipe body according to claim 1, wherein the workpiece cathode (4), the target cathode (5) and the hollow target (9) are all cylindrical.
6. A coating device for the inner wall of a pipe body according to claim 1, wherein the connecting guide rod (12) is made of the same material as the hollow target (9).
7. A coating apparatus for an inner wall of a pipe body according to claim 1, wherein the lower bottom of said work load-bearing tray (6) is supported by insulating ceramics and placed on a hearth tray (7).
8. The coating device for the inner wall of a pipe body according to claim 1, wherein the diameter of the rod-shaped anode (8) is 3-5 mm, and the rod-shaped anode is made of one or more of Ta, W and Mo.
9. The film plating method of a film plating device for an inner wall of a pipe body according to any one of claims 1 to 8, comprising the steps of:
firstly, polishing the inner wall of a tubular workpiece (10) to more than 1500 meshes by sand paper, and then wiping, cleaning and airing the tubular workpiece (10), a hollow target (9), a workpiece bearing tray (6), a rod-shaped anode (8) and a furnace bottom tray (7) by ethanol with concentration of more than 95%;
Step two, sequentially loading all the cleaned parts into a furnace body (3);
Turning on a mechanical pump, pumping the air pressure of the furnace body (3) to below 1Pa, then filling argon to above 200Pa, pumping to below 1Pa, repeatedly washing, and filling the argon to maintain 20-80 Pa;
Step four, slowly raising the voltage of the workpiece cathode (4) to 300-500V, and cleaning and heating the tubular workpiece (10) for 30-60 min by using plasma glow;
Step five, opening and slowly increasing the voltage of the target cathode (5) to 600-950V, and simultaneously increasing the voltage of the workpiece cathode (4) to 450-700V, so that the working air pressure is 20-80 Pa, the distance between the hollow target (9) and the inner wall of the tubular workpiece (10) is 5-25 mm, and the heat preservation time is 3-6 h;
Step six, after the heat preservation is finished, the voltage of the hollow target material (9) and the tubular workpiece (10) is reduced to 0V, the time of the process is more than 30min, then the vacuum is pumped to below 0.1Pa, and the hollow target material is taken out after being cooled along with the furnace.
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| CN108456854A (en) * | 2018-04-02 | 2018-08-28 | 中国工程物理研究院材料研究所 | A kind of devices and methods therefor of tungsten making Nano surface |
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| JPH06287751A (en) * | 1993-03-31 | 1994-10-11 | Shimadzu Corp | Sputtering equipment |
| RU2194798C2 (en) * | 1996-09-23 | 2002-12-20 | Сименс Акциенгезелльшафт | Part and method of application of heat-insulating coating to it |
| CN1174114C (en) * | 2002-03-18 | 2004-11-03 | 太原理工大学 | Bicathode-high frequency glow ion diffusion coating equipment and its process |
| CN100494482C (en) * | 2006-08-15 | 2009-06-03 | 夏小勇 | Hollow cathode ionization metallization device |
| US9175381B2 (en) * | 2008-07-09 | 2015-11-03 | Southwest Research Institute | Processing tubular surfaces using double glow discharge |
| CN201517130U (en) * | 2009-10-29 | 2010-06-30 | 中国计量学院 | Source electrode used for double-cathode luminance discharging leaked metal |
| US8747631B2 (en) * | 2010-03-15 | 2014-06-10 | Southwest Research Institute | Apparatus and method utilizing a double glow discharge plasma for sputter cleaning |
| US9640359B2 (en) * | 2012-08-09 | 2017-05-02 | Vactronix Scientific, Inc. | Inverted cylindrical magnetron (ICM) system and methods of use |
| US9765726B2 (en) * | 2013-03-13 | 2017-09-19 | Federal-Mogul | Cylinder liners with adhesive metallic layers and methods of forming the cylinder liners |
| CN106756792B (en) * | 2016-12-30 | 2019-01-01 | 南京信息工程大学 | A kind of preparation method of oxide transparent electrode film |
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