CN104451578A - Direct current coupling type high energy pulse magnetron sputtering method - Google Patents
Direct current coupling type high energy pulse magnetron sputtering method Download PDFInfo
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- CN104451578A CN104451578A CN201410652546.5A CN201410652546A CN104451578A CN 104451578 A CN104451578 A CN 104451578A CN 201410652546 A CN201410652546 A CN 201410652546A CN 104451578 A CN104451578 A CN 104451578A
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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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Abstract
The invention discloses a direct current coupling type high energy pulse magnetron sputtering method. The method comprises the following steps: coupling low direct current voltage into high energy pulse magnetron sputtering voltage, thus forming magnetron sputtering coupled voltage; providing stable low ionization rate plasma by virtue of constant low voltage, so that the film deposition rate is improved and instantaneous high ionization of the plasma is realized by virtue of the high energy pulse voltage; coordinating the operating time sequence of the coupled voltage, regulating the peak value, frequency and duty ratio of the pulsed high voltage under the condition that the direct current constant voltage is fixed, and changing impulse waveform of the coupled voltage so that the deposition rate and the ionization rate are regulated and controlled. The direct current voltage is preset, so that the pulse current hysteresis time is effectively reduced; stable direct current magnetron sputtering is coupled in, so that the film deposition rate is effectively guaranteed; and moreover, an HIPIMS technology with an adjustable plasma ionization rate is established and a technical support is provided for related scientific research.
Description
Technical field
What the present invention relates to is a kind of direct current coupling type high energy pulse magnetron sputtering (HIPIMS) film coating method, can reduce plasma glow retardation time, and it is controlled to realize ionization level while the high ionization level plasma body of acquisition.
Background technology
Magnetron sputtering, as the physical gas phase deposition technology of a very advantageous, is applied widely in multiple fields such as microelectronics, optical thin film and material surface process.But because ionization level is lower, this technology also has some limitations in raising film quality, shows as the loose porous and poor film-substrate cohesion of membrane structure.
Improve plasma body ionization level, the controllability increasing film process is the great demand of surperficial domain engineering application always.High energy pulse magnetron sputtering (HIPIMS) is exactly the new surface modifications technology grown up under this background, be that Surface Engineering studies the most significant breakthrough in history in 30 years, to modern film preparation and the development accurately controlled, there is huge pushing effect.In HIPIMS, high-octane pulse action can make the electron density around magnetic controlling target reach 10
19m
-3, the high-density of electronics adds the ionizing collision probability of sputtered atom and high-energy electron, thereby is achieved the sputter material particle of high ionization, the ionization level of metallic plasma can be brought up to more than 80% by 5%.Owing to controlling and affecting means mainly electricity, the magnetic field of projectile lotus energy state and spatial distribution, therefore, improve plasma body ionization level, make neutral uncontrollable particle change ion into, human intervention film process will be conducive to, and obtain high quality thin film.
The restriction that traditional magnetically controlled DC sputtering melts by magnetic controlling target heating, can only be operated in 25 W/cm
2below energy density.High energy pulse as the HIPIMS system core then can provide 1000 ~ 3000 W/cm on magnetic controlling target
2peak energy denisty, instantaneous power can reach MW class, but its frequency is low, and dutycycle is little, and mean power only has tens kilowatts, can not cause damage to magnetic controlling target.
But in the discharge process of standard HIPIMS power supply, magnetron current rises and is difficult to synchronous with voltage pulse, especially in subatmospheric situation, in same sputtering pulse the generation time of high ionization level plasma glow comparatively voltage delay reach tens microseconds (as Fig. 1).In addition, compared with sputtering with conventional magnetron, the sedimentation rate under HIPIMS same average power is lower, mainly because under high ionization level, a large amount of sputter material ion is sucked back into negative electrode, and does not arrive matrix surface.Therefore, can obtain the plasma body of high ionization level, the sedimentation rate not damaging again film is the development trend of HIPIMS technology.
Summary of the invention
The present invention develops based on above background, its objective is to reduce impulse of current lag time in HIPIMS discharge process, while guarantee film deposition rate, sets up the HIPIMS magnetron sputtering coating method that a kind of plasma body ionization level is controlled.To achieve these goals, the present invention adopts following technical proposals:
A kind of direct current coupling type high energy pulse magnetron sputtering coating method, described method is included in high energy pulse magnetron sputtering voltage and is coupled into low dc voltage, forms magnetron sputtering coupled voltages; By coordinating the work schedule of coupled voltages, when DC constant voltage is determined, the peak value of regulation and control high voltage pulse, frequency and dutycycle, change the pulse waveform of coupled voltages, realizes the adjustment to sedimentation rate and ionization level and control.
Further, provide stable low ionization level plasma body by constant low voltage, improve the sedimentation rate of film; And high energy pulse voltage, realize the instantaneous high ionization of plasma body.
Further, preset constant DC low-voltage, plays pre-build-up of luminance effect to magnetic controlling target, the electric current lag time of coupled pulse under effective reduction subatmospheric.
Further, by changing DC low-voltage value, the regulation and control to film deposition rate are realized.
Further, by changing the peak value of high energy pulse voltage, frequency and dutycycle etc., the regulation and control of plasma ionization level are realized.
Beneficial effect of the present invention is:
1) preset volts DS, effectively reduces pulsed current lag time;
2) be coupled into stable magnetically controlled DC sputtering, effectively ensure that film deposition rate;
3) the adjustable HIPIMS magnetron sputtering technique of a kind of plasma body ionization level is set up, for the research of related science provides technical support.
Accompanying drawing explanation
Fig. 1 is the discharge character curve of typical high energy pulse magnetron sputtering power supply;
Fig. 2 is direct current coupling type high energy pulse magnetron sputtering target voltage operation mode;
Fig. 3 is the discharge character curve of direct current coupling type high energy pulse magnetron sputtering power supply;
Fig. 4 is the Ti plasma body typical emission spectra figure of embodiment 1-2;
Fig. 5 is the Ti plasma body typical emission spectra figure of embodiment 3-5;
Fig. 6 is the Ti plasma body typical emission spectra figure of embodiment 3,6-7;
Fig. 7 is Ti film growth rate result figure obtained in embodiment 1-7;
Fig. 8 is Ti plasma body ionization level result figure in embodiment 1-7.
Embodiment
Elaborate below in conjunction with the embodiment of accompanying drawing to direct current coupling type high energy pulse magnetron sputtering (HIPIMS) film coating method disclosed by the invention.The invention provides under one is operated in magnetron sputtering coupled voltages pattern, the HIPIMS magnetron sputtering technique that plasma body ionization level is adjustable.It is pointed out that the following stated embodiment is being convenient to the understanding of the present invention, and any restriction effect is not play to it.
Make means for achieving the above object, in high-power impulse magnetron sputtering voltage, be coupled into low dc voltage, form magnetron sputtering coupled voltages.Adopt PLC (programmable logic controller) as central control unit, regulate and control the peak value of coupled pulse voltage, frequency and dutycycle etc. by the work schedule of coherent system switch, realize the adjustment to sedimentation rate and ionization level and control.
Magnetron sputtering coupled voltages operating mode provided by the invention, as shown in Figure 2.Wherein preset Constant Direct Current low voltage plays the effect of pre-build-up of luminance to magnetic controlling target, the coupled pulse electric current under subatmospheric is made to be reduced to below ten microseconds (as Fig. 3) retardation time, compared with the impulse of current lag time of prior art in Fig. 1, obviously accelerate the lift velocity of pulsed current.In addition, in the coupled voltages waveform of Fig. 2, low-voltage dc power supply is that magnetic controlling target provides conventional magnetically controlled DC sputtering electric current, can obtain stable low ionization level plasma body, to ensure the sedimentation velocity of film.And under PLC cooperation control back to back HIPIMS high-voltage pulse, realize the instantaneous high ionization of plasma body.By adjustment pulse and the power ratio of magnetically controlled DC sputtering, namely when DC constant voltage is determined, the peak value of regulation and control high voltage pulse, frequency and dutycycle, change the pulse waveform of coupling power, realizes the adjustment to sedimentation rate and ionization level and control.
For splash-proofing sputtering metal Ti film, carry out following embodiment:
The scope of DC low-voltage is 0 ~ 1000V, peak power 8KW.The crest voltage of high energy pulse is 2000V, and pulse-repetition is 5HZ ~ 200HZ, and dutycycle is 0.1% ~ 1%.
Embodiment 1:
In the present embodiment, customary DC magnetically controlled sputter method is adopted to prepare metal Ti film.Preparation condition is: highest attainable vacuum 1 × 10
-3pa, operating air pressure 0.5Pa, volts DS 400V, target-substrate distance 10cm, depositing time 60min.
Embodiment 2:
In the present embodiment, high energy pulse magnetically controlled sputter method is adopted to prepare metal Ti film.Preparation condition is: highest attainable vacuum 1 × 10
-3pa, operating air pressure 0.5Pa, high energy pulse crest voltage 800V, pulse-repetition 100HZ, dutycycle 1%, target-substrate distance 10cm, depositing time 60min.
In embodiment 1-2 preparation process, the typical emission spectra figure of Ti plasma body as shown in Figure 4.As seen from Figure 4, in the Ti plasma body adopting DC magnetron sputtering method to obtain, Ti atom accounts for major portion, only has a small amount of Ti
+ion.And in the Ti plasma body adopting high energy pulse magnetically controlled sputter method to obtain, Ti
+ratio shared by ion has remarkable increase, obtains the metallic plasma of high ionization.
Embodiment 3:
In the present embodiment, direct current coupling type high energy pulse magnetically controlled sputter method is adopted to prepare metal Ti film.Preparation condition is: highest attainable vacuum 1 × 10
-3pa, operating air pressure 0.5Pa, volts DS 400V, high energy pulse crest voltage 800V, pulse-repetition 100HZ, dutycycle 1%, target-substrate distance 10cm, depositing time 60min.
Embodiment 4:
In the present embodiment, direct current coupling type high energy pulse magnetically controlled sputter method is adopted to prepare metal Ti film.Preparation condition is: highest attainable vacuum 1 × 10
-3pa, operating air pressure 0.5Pa, volts DS 400V, high energy pulse crest voltage 700V, pulse-repetition 100HZ, dutycycle 1%, target-substrate distance 10cm, depositing time 60min.
Embodiment 5:
In the present embodiment, direct current coupling type high energy pulse magnetically controlled sputter method is adopted to prepare metal Ti film.Preparation condition is: highest attainable vacuum 1 × 10
-3pa, operating air pressure 0.5Pa, volts DS 400V, high energy pulse crest voltage 600V, pulse-repetition 100HZ, dutycycle 1%, target-substrate distance 10cm, depositing time 60min.
In embodiment 3-5 preparation process, the typical emission spectra figure of Ti plasma body as shown in Figure 5.As seen from Figure 5, when adopting direct current coupling type high energy pulse magnetically controlled sputter method, when DC low-voltage is constant, along with the reduction of high energy pulse crest voltage, Ti in plasma body
+ratio shared by ion has obvious decline, effectively can realize the regulation and control of ionization level.
Embodiment 6:
In the present embodiment, direct current coupling type high energy pulse magnetically controlled sputter method is adopted to prepare metal Ti film.Preparation condition is: highest attainable vacuum 1 × 10
-3pa, operating air pressure 0.5Pa, volts DS 300V, high energy pulse crest voltage 800V, pulse-repetition 100HZ, dutycycle 1%, target-substrate distance 10cm, depositing time 60min.
Embodiment 7:
In the present embodiment, direct current coupling type high energy pulse magnetically controlled sputter method is adopted to prepare metal Ti film.Preparation condition is: highest attainable vacuum 1 × 10
-3pa, operating air pressure 0.5Pa, volts DS 200V, high energy pulse crest voltage 800V, pulse-repetition 100HZ, dutycycle 1%, target-substrate distance 10cm, depositing time 60min.
The typical emission spectra figure of the Ti plasma body in embodiment 3,6-7 preparation process as shown in Figure 6.As seen from Figure 6, when adopting direct current coupling type high energy pulse magnetically controlled sputter method, when high energy pulse crest voltage is constant, different volts DSs is to Ti
+the ratio of ion does not make significant difference.
Fig. 7 is Ti film growth rate result figure obtained in embodiment 1-7.As seen from Figure 7, the significant parameter affecting film deposition rate is preset constant DC voltage.
Fig. 8 is the result figure of plasma body ionization level in embodiment 1-7.As seen from Figure 8, the significant parameter affecting plasma body ionization level is high energy pulse crest voltage.
Therefore, carry out communication by computer and PLC, regulation and control direct current coupling and the peak value of high energy pulse voltage, frequency and dutycycle etc. just can realize adjustment to film deposition rate and plasma body ionization level and control.
The foregoing is only the preferred embodiments of the present invention, the numerical value mentioned in the description of above-mentioned specification sheets and numerical range are not limited to the present invention, just for the invention provides preferred embodiment, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. a direct current coupling type high energy pulse magnetron sputtering coating method, described method is included in high energy pulse magnetron sputtering voltage and is coupled into low dc voltage, forms magnetron sputtering coupled voltages; By coordinating the work schedule of coupled voltages, when DC constant voltage is determined, the peak value of regulation and control high voltage pulse, frequency and dutycycle, change the pulse waveform of coupled voltages, realizes the adjustment to sedimentation rate and ionization level and control.
2. method according to claim 1, is characterized in that, provides stable low ionization level plasma body by constant low voltage, improves the sedimentation rate of film; High energy pulse voltage, realizes the instantaneous high ionization of plasma body.
3. method according to claim 1, is characterized in that, preset constant DC low-voltage, plays pre-build-up of luminance effect to magnetic controlling target, the electric current lag time of coupled pulse under effective reduction subatmospheric.
4. method according to claim 1, is characterized in that, by changing DC low-voltage value, realizes the regulation and control to film deposition rate.
5. method according to claim 1, is characterized in that, by changing the peak value of high energy pulse voltage, frequency and dutycycle, realizes the regulation and control of plasma ionization level.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108251807A (en) * | 2018-01-02 | 2018-07-06 | 中国科学院宁波材料技术与工程研究所 | The amorphous carbon-base film of nanometer grade thickness is as the application of infrared absorbing material and the preparation method of amorphous carbon-base film |
| CN111378947A (en) * | 2020-04-21 | 2020-07-07 | 中国科学院力学研究所 | Preparation method of diamond-like thin film |
| CN112522672A (en) * | 2020-11-18 | 2021-03-19 | 东莞市华升真空镀膜科技有限公司 | High-energy pulse magnetic control film coating machine with unbalanced magnetic field and manufacturing and processing technology thereof |
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Cited By (4)
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| CN108251807A (en) * | 2018-01-02 | 2018-07-06 | 中国科学院宁波材料技术与工程研究所 | The amorphous carbon-base film of nanometer grade thickness is as the application of infrared absorbing material and the preparation method of amorphous carbon-base film |
| CN108251807B (en) * | 2018-01-02 | 2020-05-08 | 中国科学院宁波材料技术与工程研究所 | Application of amorphous carbon-based film with nanoscale thickness as infrared absorption material and preparation method of amorphous carbon-based film |
| CN111378947A (en) * | 2020-04-21 | 2020-07-07 | 中国科学院力学研究所 | Preparation method of diamond-like thin film |
| CN112522672A (en) * | 2020-11-18 | 2021-03-19 | 东莞市华升真空镀膜科技有限公司 | High-energy pulse magnetic control film coating machine with unbalanced magnetic field and manufacturing and processing technology thereof |
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Application publication date: 20150325 |