CN115786847A - Method for performing magnetron sputtering in elongated tube by using direct-current composite bipolar pulse - Google Patents
Method for performing magnetron sputtering in elongated tube by using direct-current composite bipolar pulse Download PDFInfo
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- CN115786847A CN115786847A CN202211599296.4A CN202211599296A CN115786847A CN 115786847 A CN115786847 A CN 115786847A CN 202211599296 A CN202211599296 A CN 202211599296A CN 115786847 A CN115786847 A CN 115786847A
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Abstract
A method for carrying out magnetron sputtering in a slender pipe barrel by direct current composite bipolar pulse belongs to the field of magnetron sputtering coating. The device solves the problems of difficult internal discharge, poor stability and poor film quality of the existing pipe fittings. The tube to be plated and the columnar target are respectively connected with the positive electrode and the negative electrode of the power supply, and dipolar discharge is carried out between the tube to be plated and the columnar target. The discharge power supply adopts a direct current composite bipolar pulse power supply, the discharge mode can be switched among direct current, pulse, bipolar pulse and the discharge mode of direct current composite bipolar pulse, and the discharge stability and the deposition rate are enhanced through a direct current part; enhancing ionization by negative pulse discharge to prepare for the traction of subsequent positive pulses; ions in the plasma are accelerated to move towards the pipe to be plated through positive pulse traction, the film layer is bombarded and tamped, the quality of the film layer is improved, and finally the rapid and high-quality magnetron sputtering film layer preparation of the inner wall of the slender pipe barrel is realized. The invention is suitable for the field of magnetron sputtering coating of the inner wall of the slender pipe barrel.
Description
Technical Field
The invention belongs to the field of magnetron sputtering coating, and particularly relates to a method for performing magnetron sputtering in a slender pipe barrel by using direct-current composite bipolar pulses.
Background
The magnetron sputtering technology is widely applied to the surface strengthening fields of medical treatment, petrochemical engineering, electric power engineering, ocean engineering and the like by the characteristics of low deposition temperature, good film layer quality and the like. In the medical field, the DLC film layer prepared on the surface of the artificial joint can adjust the hydrophilicity and reduce the friction coefficient, thereby greatly prolonging the service life of the material; the TiN film layer prepared on the surface of the material can not only improve the wear resistance of the material, but also obtain various colors by adjusting the components of the film layer, thereby improving the aesthetic property of the workpiece; the TiN, tiAlN and other film layers are prepared on the surface of the cutter, so that the hardness of the cutter can be improved, the wear resistance of the cutter can be improved, the service life of the cutter can be prolonged, and the performance of the cutter can be improved.
In the above applications, the film layer is prepared mainly on the outer surface of the material. This does not mean that the requirement for a film layer on the inner surface of the material is low, but in practical applications, the film has a wide application prospect on the inner surface of the material, especially on the inner surface of the pipe barrel, for example, in the chemical industry, a large number of pipes are used for conveying high-temperature corrosive chemical media, and the inner surface of the pipe becomes the initial position for the failure of the pipe barrel material relative to the outer surface. The preparation of the high temperature and corrosion resistant film layer on the inner surface of the film layer can greatly improve the service life of the film layer. But the inner wall protection research is slow due to limited space in the pipe barrel and large length-diameter ratio. The protection method of the inner wall of the tube barrel material adopted at present is mainly to add a liner tube or adopt an electroplating method. The former forms weak points at the welded joint, while the latter has poor film quality and causes great environmental pollution. Therefore, the application of the magnetron sputtering technology to the coating of the inner wall of the tube barrel material is greatly developed.
The main difficulties in depositing the film on the inner wall of the elongated tubular member are: 1. the pipe orifice with a smaller caliber has a shielding effect on external plasma, the plasma generated by an external plasma source can only enter the interior of the pipe orifice, the distribution uniformity of the plasma in the interior of the pipe orifice is sharply reduced along with the increase of the length-diameter ratio of the pipe barrel, and the effective and uniform preparation of the film layer is difficult to realize. 2. The caliber of the pipe barrel limits the generation of plasma in the pipe barrel; such as 40mm internal diameter tubing, the ultimate target base distance for internal discharge is typically only a dozen millimeters. The space in the tube is small, so that an additional electrode structure cannot be applied, and only a dipolar discharge structure can be adopted.
The energy of conventional direct current dipolar discharge particles is low, and positive pulses in the bipolar discharge process utilize a tube to be plated as cathode traction ions, so that bombardment on a film layer is realized, and the quality of the film layer is improved. In the narrow-spacing discharge process, plasma dissipates very fast, bipolar discharge has poor stability, and ignition and glow extinction are easy to realize. The method combines high deposition rate and high discharge stability of direct current, high ionization rate and high particle energy of bipolar discharge, is applied to coating in a slender tube, and has good application prospect.
Disclosure of Invention
The invention provides a method for performing magnetron sputtering in a slender pipe barrel by direct current composite bipolar pulse, aiming at the problems of difficult discharge, poor stability and poor film quality in the existing slender pipe barrel inner film coating process.
A method for carrying out magnetron sputtering in a slender pipe barrel by using direct current composite bipolar pulses is based on the existing two-stage discharge magnetron sputtering method, a power supply in the magnetron sputtering process adopts a direct current composite bipolar pulse power supply, the direct current composite bipolar pulse power supply comprises three parts of direct current power supply, negative pulse power supply and positive pulse power supply, the on-off of each part can be independently controlled, the three parts are controlled by combining a single chip microcomputer with a semiconductor switch bridge circuit, negative pulses and positive pulses in the same period jointly form bipolar pulses, the negative pulses and the positive pulses are alternately distributed, N negative pulses and M positive pulses can exist in the same pulse period, wherein N =0,1,2, … … and 100; m =0,1,2, … …,100, the DC power supply is turned off during the action of the bipolar pulse and is turned on intermittently in the pulse;
further, the range of the current value of the direct current power supply is 0-100A, and the range of the power supply voltage is 0-2000V;
furthermore, the pulse width and the voltage of the positive and negative pulses of the bipolar pulse can be controlled independently, and the frequency range is 0-50kHz;
furthermore, the first pulse in the period of the bipolar pulse is a negative pulse, the pulse width range of the positive pulse and the negative pulse is 0-1ms, and the voltage range is 0-2000V;
further, the method comprises the following steps:
1. sample preparation: ultrasonic cleaning the pipe to be plated with acetone and absolute ethyl alcohol for 5-60min, taking out, drying, and placing in a vacuum chamber to be coaxially mounted with the columnar target;
2. pretreatment before film coating: vacuum pumping the vacuum chamber to the pressure of 8 x 10 -3 Heating and drying under Pa for 10-60min, and vacuumizing to 8 × 10 -3 Introducing argon below Pa until the pressure is 0.5-10Pa, and then carrying out plasma sputtering cleaning on the inner wall of the pipe to be plated for 5-60min to obtain the pretreated pipe to be plated;
3. sputtering and coating: introducing mixed gas of working gas and reaction gas after the plasma cleaning is finished, turning on a power supply, setting gas parameters and power supply parameters, and carrying out magnetron sputtering coating on the pretreated pipe to be coated for 10-3000 min;
further, in the step one, the inner diameter of the pipe to be plated is 15-2000mm, the wall thickness is 0.1-100mm, and the pipe to be plated is made of a magnetic or non-magnetic conductive material;
further, the outer diameter of the target tube of the columnar target in the step one is 8-100mm, and the columnar target is made of a non-magnetic conductive material;
further, in the third step, the columnar target is connected with the negative electrode of the power supply in the magnetron sputtering coating process, and the treated pipe to be coated is connected with the positive electrode of the power supply;
further, in the third step, the working gas is Ar; the reaction gas is N 2 、H 2 And O 2 One or more gases;
further, the gas parameters in step three are as follows: the gas flow is 1-3000sccm, and the gas pressure is 0.1-10Pa.
The invention provides a method for carrying out magnetron sputtering in a slender pipe barrel by direct current composite bipolar pulse, which can effectively solve the problems of difficult discharge, poor stability, poor film quality and the like in the traditional slender pipe barrel inner film coating process, thereby realizing the rapid and high-quality preparation of the magnetron sputtering film layer on the slender pipe barrel inner wall.
The invention has the advantages that:
the inner wall of the slender cylinder is coated with film, so that the conventional coated multi-electrode structure is difficult to apply. If the tube to be plated is used as the anode and the columnar target is used as the cathode in the conventional direct current dipolar discharge mode, the particle energy is lower, and the film layer cannot be bombarded and tamped and has poorer quality. The positive pulse in the bipolar discharge process utilizes the tube to be plated as a cathode to pull ions, so as to realize bombardment on the film layer and improve the quality of the film layer. However, the space in the slender tube is small, the target base distance is narrow, plasma in the discharge process is very fast to dissipate, the bipolar discharge stability is poor, and the ignition and the glow extinction are easy to occur. The invention combines the high deposition rate and high discharge stability of direct current with the high ionization rate and high particle energy of bipolar discharge, thereby realizing the rapid preparation of high-quality film layers in the slender pipe barrel and promoting the development of the industry.
According to the method for carrying out magnetron sputtering in the elongated tube by the direct current composite bipolar pulse, the discharge mode can be switched among the discharge modes of direct current, pulse, bipolar pulse and direct current composite bipolar pulse, and the method is suitable for the field of magnetron sputtering coating of the inner wall of the elongated tube.
Drawings
Fig. 1 is a schematic diagram of discharge waveforms of the dc composite bipolar pulse power supply of the present invention, wherein (a) is a waveform diagram when N =1 and M =1, (b) is a waveform diagram when N =2 and M =1, (c) is a waveform diagram when N =2 and M =2, and (d) is a waveform diagram of a symmetrical bipolar pulse mode;
FIG. 2 is a graph showing the change in thickness of the film layer at each position of the TiN film deposited by the DC composite bipolar pulse on the inner surface of the stainless steel pipe with an inner diameter of phi 50mm in example 1.
FIG. 3 is a sectional view of the inner surface of a carbon steel pipe with an inner diameter of phi 40mm deposited with a Cr film in example 2, wherein (a) is a pure DC deposition result graph and (b) is a DC composite bipolar pulse deposition result graph.
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 obtained by a person skilled in the art without inventive efforts based on the embodiments of the present invention, shall fall within the scope of protection of the present invention. It should be noted that the embodiments and features of the embodiments of the present invention may be combined with each other without conflict.
The first embodiment is as follows: a method for carrying out magnetron sputtering in a slender pipe barrel by using direct current composite bipolar pulses is based on the existing two-stage discharge magnetron sputtering method, a power supply in the magnetron sputtering process adopts a direct current composite bipolar pulse power supply, the direct current composite bipolar pulse power supply comprises three parts of direct current power supply, negative pulse power supply and positive pulse power supply, the on-off of each part can be independently controlled, the three parts are controlled by combining a single chip microcomputer with a semiconductor switch bridge circuit, negative pulses and positive pulses in the same period jointly form bipolar pulses, the negative pulses and the positive pulses are alternately distributed, N negative pulses and M positive pulses can exist in the same pulse period, wherein N =0,1,2, … … and 100; m =0,1,2, … …,100, the dc supply is turned off during bipolar pulsing and turned on intermittently during the pulsing.
The second embodiment is as follows: the difference between this embodiment and the first embodiment is that the current value of the dc power supply ranges from 0 to 100A, and the power supply voltage ranges from 0 to 2000V. The rest is the same as the first embodiment.
The third concrete implementation mode: the difference between the present embodiment and the first embodiment is that the pulse width and voltage of the positive and negative pulses of the bipolar pulse can be controlled individually, and the frequency range is 0-50kHz. The rest is the same as the first embodiment.
The fourth concrete implementation mode: the difference between this embodiment and the first embodiment is that the first pulse in the period of the bipolar pulse is a negative pulse, the pulse width of the positive and negative pulses ranges from 0 ms to 1ms, and the voltage ranges from 0V to 2000V. The rest is the same as the first embodiment.
The fifth concrete implementation mode: in a difference from the first embodiment, the method includes the steps of:
1. sample preparation: ultrasonic cleaning the pipe to be plated with acetone and absolute ethyl alcohol for 5-60min, taking out, drying, and placing in a vacuum chamber to be coaxially mounted with the columnar target;
2. pretreatment before film coating: vacuum pumping the vacuum chamber to the pressure of 8 x 10 -3 Heating and drying under Pa for 10-60min, and vacuumizing to 8 × 10 -3 Introducing argon below Pa until the pressure is 0.5-10Pa, and then carrying out plasma sputtering cleaning on the inner wall of the pipe to be plated for 5-60min to obtain the pretreated pipe to be plated;
3. sputtering and coating: and introducing mixed gas of working gas and reaction gas after the plasma cleaning is finished, turning on a power supply, setting gas parameters and power supply parameters, and performing magnetron sputtering coating on the pretreated pipe to be coated for 10-3000 min.
The rest is the same as the first embodiment.
In the third step of this embodiment, the power supply is a dc composite bipolar pulse power supply, and the discharge waveform of the power supply is schematically shown in fig. 1.
The sixth specific implementation mode: the difference between the present embodiment and the fifth embodiment is that, in the first step, the inner diameter of the tube to be plated is 15-2000mm, the wall thickness is 0.1-100mm, and the material is a magnetic or non-magnetic conductive material. The rest is the same as the fifth embodiment.
The seventh embodiment: the difference between the present embodiment and the fifth embodiment is that, in the first step, the outer diameter of the target tube of the columnar target is 8-100mm, and the material is a non-magnetic conductive material. The rest is the same as the fifth embodiment.
The specific implementation mode is eight: the difference between the fifth embodiment and the fifth embodiment is that in the third step, the columnar target is connected with the negative electrode of the power supply in the magnetron sputtering coating process, and the treated pipe to be coated is connected with the positive electrode of the power supply. The rest is the same as the fifth embodiment.
The specific implementation method nine: the difference between this embodiment and the fifth embodiment is that the working gas in the third step is Ar; the reaction gas is N 2 、H 2 And O 2 One or more gases. The rest is the same as the fifth embodiment.
In the present embodiment, when the reaction gas is a mixed gas, the components are mixed at an arbitrary ratio.
The detailed implementation mode is ten: the difference between this embodiment and the fifth embodiment is that the gas parameters in step three are as follows: the gas flow is 1-3000sccm, and the gas pressure is 0.1-10Pa. The rest is the same as the fifth embodiment.
The beneficial effects of the present invention are demonstrated by the following examples:
example 1:
1. sample preparation: sequentially ultrasonically cleaning a stainless steel tube with the inner diameter of 50mm, the outer diameter of 55mm and the length of 240mm for 15min by using acetone and absolute ethyl alcohol respectively, taking out the stainless steel tube, drying the stainless steel tube, and then placing the stainless steel tube in a vacuum chamber to be coaxially installed with a columnar Ti target with the outer diameter of 25mm and the length of 280 mm;
2. pretreatment before film coating: vacuum pumping the vacuum chamber to the pressure of 8 x 10 -3 Heating and drying under Pa for 30min, and vacuumizing to 8 × 10 -3 Introducing argon gas to the pressure of 5Pa below, and then carrying out plasma sputtering cleaning on the inner wall of the stainless steel pipe for 30min to obtain a pretreated stainless steel pipe;
3. sputtering and coating: introducing Ar and N after the plasma cleaning is finished 2 Mixed gas, flow ratio is 5:1, turning on a power supply, and setting power supply parameters as follows: the direct current is 0.5A, the frequency of the pulse part is 100Hz, the number of negative pulses is 1, the voltage is 500V, the pulse width is 100 mus, the number of positive pulses is 1, the voltage is 50V, the pulse width is 50 mus, and the deposition time is 20min.
In this example, tiN film can be deposited on the inner surface of stainless steel tube with an inner diameter of phi 50mm, the film is bright golden yellow, and the thickness of the middle 160mm part of the film is 1.4-1.7 μm, the result is shown in FIG. 2.
Example 2:
in this example, the film layers prepared by two methods, namely pure dc deposition and dc composite bipolar pulse deposition, were compared.
The specific process of the coating method is as follows:
1. sample preparation: sequentially ultrasonically cleaning a carbon steel pipe with the inner diameter of 40mm, the outer diameter of 50mm and the length of 240mm for 15min by respectively adopting acetone and absolute ethyl alcohol, taking out the carbon steel pipe, drying the carbon steel pipe, and then placing the carbon steel pipe into a vacuum chamber to be coaxially installed with a columnar Cr target with the outer diameter of 25mm and the length of 280 mm;
2. pretreatment before film coating: vacuum pumping the vacuum chamber to the pressure of 8 x 10 -3 Heating and drying under Pa for 30min, and vacuumizing to 8 × 10 -3 Introducing argon gas to the pressure of 5Pa below, and then carrying out plasma sputtering cleaning on the inner wall of the stainless steel pipe for 30min to obtain a pretreated stainless steel pipe;
3. sputtering and coating: after the plasma cleaning is finished, introducing argon, and turning on a power supply;
the power supply parameters in the pure direct current deposition process are set as follows: direct current 1A, deposition time 120mm;
the power supply parameters in the deposition process of the direct current composite bipolar pulse are set as follows: DC current 0.6A, pulse frequency 100Hz, negative pulse number 1, voltage 700V, pulse width 100 mus, positive pulse number 1, voltage 50V, pulse width 50 mus, deposition time 120min.
This embodiment can deposit a Cr film on the inner surface of a carbon steel pipe with an inner diameter of Φ 40mm, as shown in fig. 3. Fig. 3 (a) shows the pure dc deposition result, and fig. 3 (b) shows the dc composite bipolar pulse deposition result. The comparison shows that the direct current composite bipolar pulse deposition film layer has no obvious thick columnar crystal and is more compact.
Claims (10)
1. A method for carrying out magnetron sputtering in a slender pipe barrel by using direct current composite bipolar pulses is based on the existing two-stage discharge magnetron sputtering method and is characterized in that a power supply in the magnetron sputtering process adopts a direct current composite bipolar pulse power supply, the direct current composite bipolar pulse power supply comprises three parts of direct current power supply, negative pulse power supply and positive pulse power supply, the on-off of each part can be independently controlled, the three parts are controlled by combining a single chip microcomputer with a semiconductor switch bridge circuit, negative pulses and positive pulses in the same period jointly form bipolar pulses, the negative pulses and the positive pulses are alternately distributed, N negative pulses and M positive pulses can exist in the same pulse period, wherein N =0,1,2, … …,100; m =0,1,2, … …,100, the DC supply is turned off during bipolar pulsing and turned on intermittently during the pulsing.
2. The method for magnetron sputtering in the elongated tube by the composite bipolar pulse direct current according to claim 1, wherein the current value of the direct current power supply is in a range of 0-100A, and the power supply voltage is in a range of 0-2000V.
3. The method for magnetron sputtering in a slender cylinder by using direct current composite bipolar pulses as claimed in claim 1, wherein the pulse width and voltage of the positive and negative pulses of the bipolar pulses can be controlled independently, and the frequency range is 0-50kHz.
4. The method for magnetron sputtering in the elongated tube by the direct current composite bipolar pulse according to claim 1, wherein a first pulse in a period of the bipolar pulse is a negative pulse, pulse widths of the positive pulse and the negative pulse are in a range of 0-1ms, and a voltage is in a range of 0-2000V.
5. The method for magnetron sputtering in the elongated tube by the composite bipolar pulse of the direct current according to claim 1, wherein the method comprises the following steps:
1. sample preparation: ultrasonic cleaning the pipe to be plated with acetone and absolute ethyl alcohol for 5-60min, taking out, drying, and placing in a vacuum chamber to be coaxially mounted with the columnar target;
2. pretreatment before film coating: vacuum pumping the vacuum chamber to the pressure of 8 x 10 -3 Heating and drying under Pa for 10-60min, and vacuumizing to 8 × 10 -3 Introducing argon gas to the pressure of 0.5-10Pa below Pa, and then carrying out plasma sputtering cleaning on the inner wall of the pipe to be plated for 5-60min to obtain the pretreated pipe to be plated;
3. sputtering and coating: and introducing mixed gas of working gas and reaction gas after the plasma cleaning is finished, turning on a power supply, setting gas parameters and power supply parameters, and carrying out magnetron sputtering coating on the pretreated pipe to be coated for 10-3000 min.
6. The method for performing magnetron sputtering in the elongated tube by using the direct current composite bipolar pulse according to claim 5, wherein in the step one, the inner diameter of the tube to be plated is 15-2000mm, the wall thickness is 0.1-100mm, and the material is a magnetic or non-magnetic conductive material.
7. The method according to claim 5, wherein in the first step, the outer diameter of the target tube of the columnar target is 8-100mm, and the material is a non-magnetic conductive material.
8. The method for performing magnetron sputtering in the elongated tube by using the direct current composite bipolar pulse according to claim 5, wherein the columnar target is connected with a negative electrode of a power supply in the magnetron sputtering coating process in the third step, and the pretreated tube to be coated is connected with a positive electrode of the power supply.
9. The method for performing magnetron sputtering inside the elongated tube by using the direct current composite bipolar pulse according to claim 5, wherein in the third step, the working gas is Ar; the reaction gas is N 2 、H 2 And O 2 One or more gases.
10. The method for magnetron sputtering in the elongated tube by the composite bipolar pulse of the direct current according to claim 5, wherein the gas parameters in the step three are as follows: the gas flow is 1-3000sccm, and the gas pressure is 0.1-10Pa.
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| CN202211599296.4A CN115786847A (en) | 2022-12-12 | 2022-12-12 | Method for performing magnetron sputtering in elongated tube by using direct-current composite bipolar pulse |
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| CN202211599296.4A CN115786847A (en) | 2022-12-12 | 2022-12-12 | Method for performing magnetron sputtering in elongated tube by using direct-current composite bipolar pulse |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116855885A (en) * | 2023-07-05 | 2023-10-10 | 哈尔滨工业大学 | Device and method for rapidly and uniformly depositing metal film on inner wall of slender tube piece through electric field auxiliary pulse enhanced columnar cathode arc |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116855885A (en) * | 2023-07-05 | 2023-10-10 | 哈尔滨工业大学 | Device and method for rapidly and uniformly depositing metal film on inner wall of slender tube piece through electric field auxiliary pulse enhanced columnar cathode arc |
| CN116855885B (en) * | 2023-07-05 | 2023-12-08 | 哈尔滨工业大学 | Device and method for rapidly and uniformly depositing metal film on inner wall of slender tube piece through electric field auxiliary pulse enhanced columnar cathode arc |
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