CN108220901B - Plasma sputtering coating method - Google Patents
Plasma sputtering coating method Download PDFInfo
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- CN108220901B CN108220901B CN201810115318.2A CN201810115318A CN108220901B CN 108220901 B CN108220901 B CN 108220901B CN 201810115318 A CN201810115318 A CN 201810115318A CN 108220901 B CN108220901 B CN 108220901B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/354—Introduction of auxiliary energy into the plasma
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3485—Sputtering using pulsed power to the target
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Abstract
The invention discloses a novel plasma sputtering coating method, which comprises a control system, a high-voltage energy storage unit, a low-voltage energy storage unit, a negative polarity high-voltage pre-ionization pulse circuit, a bipolar low-voltage main pulse circuit, a pulse synthesis circuit and a plasma load, wherein the control system comprises a control system, a high-voltage energy storage unit, a low-voltage energy storage unit, a negative polarity high-voltage pre-ionization pulse circuit, a bipolar; a design method of high-voltage short pulses for plasma pre-ionization and high-power bipolar pulse magnetron sputtering is provided, multiple times of high-voltage short pulse pre-ionization and high-power bipolar pulse electric field treatment are carried out on a plasma load according to a certain repetition frequency, and the time interval between negative high-voltage short pulses and high-power positive and negative bipolar low-voltage main pulses is reduced, so that the coupling between voltage pulses and the plasma load is enhanced, and the problem of inconsistent target ionization time is solved. The width and the voltage amplitude of the negative high-voltage short pulse can be adjusted according to the difference of the sputtering target material and the plasma gas, the working air pressure of the gas in the magnetron sputtering device can be reduced, the low-air-pressure sputtering coating is realized, and the deposition rate of particles is improved and the surface roughness of the film is reduced.
Description
Technical Field
The invention belongs to the technical field of micro-electronics, optical films and material surface treatment research, and particularly relates to a novel plasma sputtering coating method and device.
Background
In recent years, the preparation method of the coating mainly adopts a Physical Vapor Deposition (PVD) technology, and a thin film coating is deposited on the surface of a substrate by utilizing a glow discharge process, an arc discharge process, a thermal evaporation process or other physical discharge processes. PVD techniques mainly include three types of vacuum evaporation, vacuum sputtering and ion plating. The magnetron sputtering technology is one of the widely adopted technologies for preparing hard coatings due to its unique advantages, such as low deposition temperature, high film density, easy control of film thickness, etc., as one of the vacuum sputtering technologies. The magnetron sputtering process requires a magnetron sputtering power supply to quickly ionize working gas to form stable plasma, and form stable incident ion flow on the surface of a target material. Because the direct current magnetron sputtering technology has low metal ionization rate and poor particle controllability, the direct current magnetron sputtering technology is no longer suitable for preparing novel films, and the current technology for developing high-power pulse magnetron sputtering power sources has the following two types: the power supply has two characteristics of high-power pulse peak value and no pretreatment, and the power supply cannot ensure that each high-power pulse under the repeated frequency work can enable the plasma to generate ionization and successfully sputter particles; the ionization moments of each high-power pulse are not consistent; the arcing and sparking phenomena are easy to occur, and the voltage and the power are difficult to control. The high-power pulse power supply has the characteristics of high-power pulse peak value and direct-current pretreatment, the power supply realizes the arc starting pretreatment by a direct-current part, but the high-power pulse duty ratio is less than the duty ratio of the direct-current part, the power supply is large in size and low in efficiency, the particle deposition rate in practical application is relatively low, and the sputtering efficiency is low.
Disclosure of Invention
The invention aims to provide a novel plasma sputtering coating method and a novel plasma sputtering coating device aiming at the problems in the prior art, and provides a design method for plasma pre-ionization and high-power bipolar pulse magnetron sputtering by adopting high-voltage short pulses. By applying a negative-polarity high-voltage short-pulse electric field to the plasma load, the gas in the ionization of the working gas is quickly ionized to form a stable weak-ionization discharge channel with lower impedance; then, the target is subjected to a high-power negative-polarity low-voltage pulse electric field for sputtering the target; the positive polarity low-voltage pulse electric field is applied to introduce electrons to clean the surface of the niobium target and neutralize the positive charges accumulated on the surface of the target.
In order to achieve the purpose, the invention adopts the following technical scheme:
A novel plasma sputtering coating method and a novel plasma sputtering coating device are composed of a control system, a high-voltage energy storage unit, a low-voltage energy storage unit, a negative polarity high-voltage pre-ionization pulse circuit, a low-voltage bipolar main pulse circuit, a pulse synthesis circuit and a plasma load. The parameters such as voltage amplitude, pulse width, maximum output current and the like output by the negative polarity high-voltage prepulse and the low-voltage bipolar main pulse are individually controllable and do not interfere with each other.
In the scheme, the negative polarity high-voltage short pulse and the high-power positive and negative bipolar low-voltage electric pulses are applied to the plasma load, so that the plasma load is subjected to the circulating action of the negative polarity high-voltage short pulse electric field, the high-power negative polarity low-voltage pulse electric field and the positive polarity low-voltage pulse electric field, the plasma load can be ionized successfully, the particle target can be sputtered successfully, and the sputtering success rate is improved.
In the scheme, the negative high-voltage short pulse is loaded on the plasma load, the voltage amplitude of the high-voltage short pulse is generally more than 3 times of that of the high-power negative low-voltage main pulse, the width of the negative high-voltage short pulse is less than or equal to 10 microseconds, the width and the voltage amplitude of the negative high-voltage short pulse can be adjusted according to the difference between the sputtering target and the plasma gas, the working pressure of the gas in the magnetron sputtering device can be reduced, the low-pressure sputtering coating is realized, the deposition rate of particles is improved, and the surface roughness of the film is reduced.
In the scheme, the novel plasma sputtering coating device adopts a method of pre-ionizing the plasma by the negative polarity high-voltage short pulse, so that the duty ratio of the high-power bipolar main pulse is improved, the volume of the sputtering coating power supply is reduced, the working efficiency is improved, and the problems of large volume and low efficiency of the power supply are solved.
In the scheme, the time interval between the negative polarity high-voltage short pulse and the high-power positive and negative bipolar low-voltage main pulses is required to be as short as possible so as to enhance the coupling between the voltage pulse and the plasma load, quickly ionize the working gas to form a plasma channel, ensure that the negative polarity low-voltage main pulses discharge in a stable weak ionization channel with lower impedance, and ensure that each high-power pulse can enable the plasma to be successfully ionized to sputter particles and the consistency of the ionization time of each high-power pulse under the repeated frequency operation.
In the scheme, the novel plasma sputtering coating method and the novel plasma sputtering coating device are characterized in that high-power positive and negative bipolar low-voltage electric pulses are loaded on a plasma load. The pulse width of the output high-power negative-polarity low-voltage pulse is generally 20-200 microseconds, and the voltage amplitude is 400-; outputting positive polarity low voltage pulse with amplitude of 0-400V for introducing electrons to clean the surface of the target material and neutralize the positive charge accumulated on the surface of the target material.
In the scheme, the plasma load is subjected to high-voltage short-pulse pre-ionization and high-power bipolar pulse electric field treatment for multiple times according to a certain repetition frequency, and the repetition frequency and the maximum output current for loading negative-polarity low-voltage pulses are determined according to the characteristics of different plasma loads. The general recommended parameter ranges are: the repetition frequency is between 0Hz and 60Hz, and the maximum output current of the negative polarity low-voltage pulse is between 0A and 150A.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
The novel plasma sputtering coating method and the novel plasma sputtering coating device solve the problems existing in the prior high-power magnetron sputtering: 1) under the repeated frequency work, the plasma sometimes can not be ionized, and particles can not be successfully sputtered; 2) the ionization moments of each high-power pulse are not consistent; 3) the arcing and ignition phenomena are easy to generate during sputtering, and the target surface is poisoned; 4) voltage and power are difficult to control; 5) the power supply has larger volume and lower efficiency, and the particle deposition rate in practical application is relatively lower; 6) the sputtering efficiency is low. The working pressure of gas in the magnetron sputtering device can be reduced, low-pressure sputtering coating is realized, the sputtering efficiency of the target material is improved, and the surface roughness of the film is reduced.
Drawings
The invention will now be described, by way of example, with reference to the accompanying drawings, in which:
FIG. 1 is a block diagram of a novel plasma sputter coating apparatus;
FIG. 2 shows the voltage and current waveforms output by the novel plasma sputter coating apparatus under the load of the niobium target;
FIG. 3 shows the voltage and current waveforms output by the novel plasma sputter coating device under the load of a tin target.
Detailed Description
All of the features disclosed in this specification, or all of the steps in any method or process so disclosed, may be combined in any combination, except combinations of features and/or steps that are mutually exclusive.
As shown in fig. 1, the novel plasma sputtering coating device is composed of a control system, a high-voltage energy storage unit, a low-voltage energy storage unit, a negative polarity high-voltage pre-ionization pulse circuit, a low-voltage bipolar main pulse circuit, a pulse synthesis circuit and a plasma load. The control system is composed of peripheral circuits such as a touch screen, a Field Programmable Gate Array (FPGA), a Programmable Logic Controller (PLC), an isolation circuit and the like. The touch screen mainly realizes the setting of parameters such as charging voltage, output protection current, optical signal pulse width, optical signal frequency and the like of the high-voltage preionization pulse and the high-power bipolar low-voltage main pulse, and controls the charging unit to charge the energy storage capacitor and control the generation of pulse signals. The PLC converts a 0-1000V voltage set value on the touch screen into a 0-10V analog quantity, and controls the charging unit to charge the energy storage capacitor after passing through the isolating circuit; the FPGA and the peripheral circuit mainly realize the generation of an optical pulse signal with adjustable frequency of 0-60Hz and adjustable pulse width of 20-200 microseconds, detect and sample the current in a negative polarity low-voltage main pulse loop output by the device in real time, compare the current with reference current, if the output pulse current exceeds a set current value, the FPGA turns off the power pulse signal in the period, so that the magnetron sputtering power supply has no voltage pulse output, and the current of a current output end is prevented from sharply rising due to arc striking of a plasma load and short circuit, thereby realizing the protection of the power supply, ensuring the normal work of the next period and ensuring the reliable operation of the power supply device.
As shown in fig. 2, the voltage and current waveforms output by the novel plasma sputter coating device under the load of the niobium target. The device parameters are: the high-voltage pre-ionization pulse voltage amplitude is-3400V, and the pulse width is 6 microseconds; the amplitude of the high-power negative-polarity low-voltage pulse voltage is-700V, and the pulse width is 200 microseconds; the amplitude of the positive low-voltage pulse voltage is 50V, and the pulse width is 200 microseconds; the working frequency is 60Hz, the working gas is argon, the air pressure is 0.44 Pa, and the negative main pulse lags behind the high-voltage pre-ionization pulse for 50 microseconds. The voltage and current signals in the load loop during work are respectively detected by a PEARSON current loop (110 type, 0.1V/A) and a Tek P6015A high-voltage probe. The negative polarity high-voltage pre-ionization pulse quickly ionizes argon to form a weak ionization discharge channel with low impedance and stability, when a high-power negative polarity main voltage pulse is added to the niobium target, the load impedance is immediately and gradually reduced, the current is gradually increased and stabilized at 140A, the main negative polarity high-voltage pre-ionization pulse is mainly used for sputtering the niobium target, and the positive polarity low-voltage main pulse is mainly used for cleaning the surface of the niobium target. Under the repeated frequency operation, the time of each ionization of the niobium target is consistent, and no arcing site appears. The high-power bipolar main pulse is directly increased without adding a high-pressure pre-ionization pulse, the niobium target can not be sputtered under the low-pressure condition, the argon gas pressure is required to be increased if the niobium target is successfully sputtered, and the niobium target is sputtered under the high-pressure condition, so that the surface of a film layer sputtered under the high-pressure condition is rough and the particle sputtering efficiency is low.
As shown in FIG. 3, the voltage and current waveforms output by the novel plasma sputter coating device under the load of the tin target. The device parameters are: the high-voltage pre-ionization pulse voltage amplitude is-3400V, and the pulse width is 6 microseconds; the amplitude of the high-power negative-polarity low-voltage pulse voltage is-800V, and the pulse width is 200 microseconds; the amplitude of the positive low-voltage pulse voltage is 10V, and the pulse width is 200 microseconds; the working frequency is 20 Hz, the working gas is argon, the air pressure is 0.55 Pa, and the negative main pulse lags behind the high-voltage pre-ionization pulse for 50 microseconds. The PEARSON current loop and the Tek P6015A high-voltage probe are used for respectively detecting voltage and current signals in a load loop during work. Under the low-pressure working condition, the tin target successfully sputters tin particles, and the high-power bipolar low-pressure main pulse tin target can not be sputtered without adding high-pressure pre-ionization pulse. Unlike niobium targets, tin targets are difficult to sputter even under high gas pressure conditions, and once sputtering occurs, the current in the sputtering circuit increases immediately, causing arcing.
the invention is not limited to the foregoing embodiments. The invention extends to any novel feature or any novel combination of features disclosed in this specification and any novel method or process steps or any novel combination of features disclosed.
Claims (8)
1. A plasma sputtering coating method is characterized in that:
Negative high-voltage short pulses and high-power positive and negative bipolar low-voltage electric pulses are applied to the plasma load, so that the plasma load is subjected to the circulating action of the negative high-voltage short pulse electric field, the high-power negative low-voltage pulse electric field and the positive low-voltage pulse electric field, and each high-power pulse can ensure that the plasma load is ionized to successfully sputter particles.
2. The plasma sputtering coating method of claim 1, wherein the plasma load is loaded with negative high voltage short pulses, the voltage amplitude of the negative high voltage short pulses is more than 3 times of that of the high power negative low voltage main pulse, and the width of the negative high voltage short pulses is less than or equal to 10 microseconds.
3. The method according to claim 2, wherein the width and the voltage amplitude of the negative polarity high voltage short pulse are adjusted according to the sputtering target and the plasma gas.
4. The plasma sputtering coating method of claim 1, wherein a negative high-voltage short pulse pre-ionization method is adopted for the plasma load, so as to improve the duty ratio of the high-power bipolar main pulse and reduce the volume of the sputtering coating power supply.
5. The plasma sputtering coating method as claimed in claim 1, wherein the plasma load is loaded with high power positive and negative bipolar low voltage pulses, the pulse width of the output high power negative polarity low voltage pulse is 20-200 μ s, the voltage amplitude is 400-800V, and the pulse amplitude of the output positive polarity low voltage pulse is 0-400V.
6. The plasma sputtering coating method of claim 1, wherein the plasma load is subjected to high-voltage short pulse pre-ionization and high-power bipolar pulse electric field treatment for a plurality of times according to a repetition frequency, and the repetition frequency and the maximum output current for loading negative polarity low-voltage pulses are determined according to the characteristics of different plasma loads.
7. The plasma sputtering coating method according to claim 6, wherein the repetition frequency is between 0Hz and 60Hz, and the maximum output current of the negative polarity low voltage pulse is between 0A and 150A.
8. The device for the plasma sputtering coating method according to any one of claims 1 to 7, characterized by comprising a control system, a high-voltage energy storage unit, a low-voltage energy storage unit, a negative polarity high-voltage pre-ionization pulse circuit, a bipolar low-voltage main pulse circuit, a pulse synthesis circuit and a plasma load, wherein parameters such as voltage amplitude, pulse width and output maximum current output by the negative polarity high-voltage pre-pulse and the bipolar low-voltage main pulse are individually controllable and do not interfere with each other.
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| CN110138362B (en) * | 2019-04-10 | 2020-10-27 | 北京航空航天大学 | Novel pulsating plasma power supply for pumping ions out of target material |
| CN110164566B (en) * | 2019-04-25 | 2020-10-30 | 中国科学院合肥物质科学研究院 | Method for protecting plasma current of EAST device |
| CN112888129A (en) * | 2020-12-14 | 2021-06-01 | 北京东方计量测试研究所 | Modulation method and device for homogenizing atmospheric gas discharge |
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| JP2006120234A (en) * | 2004-10-21 | 2006-05-11 | Hitachi Global Storage Technologies Netherlands Bv | Manufacturing method of perpendicular magnetic recording medium |
| CN102108492A (en) * | 2011-01-18 | 2011-06-29 | 中国科学院力学研究所 | Ionization-rate-controllable coating device based on high-power impulse magnetron sputtering |
| CN103248263B (en) * | 2012-02-09 | 2017-02-15 | 中兴通讯股份有限公司 | PWM DC pulse circuit, coating circuit and film coating method |
| CN105803411A (en) * | 2016-05-11 | 2016-07-27 | 魏永强 | Combined method of arc ion plating and twin target bipolar high-power pulsed magnetron sputtering |
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