ICMCTF2012 Session F2-2: High Power Impulse Magnetron Sputtering

Tuesday, April 24, 2012 1:50 PM in Room Sunset

Tuesday Afternoon

Time Period TuA Sessions | Abstract Timeline | Topic F Sessions | Time Periods | Topics | ICMCTF2012 Schedule

Start Invited? Item
1:50 PM F2-2-1 HIPIMS Discharge Dynamics: Evolution and Origin of Plasma Instabilities
Ante Hecimovic (Institut for Experimental Physics II, Research Department Plasma, Ruhr-Universität Bochum, Germany); Teresa de los Arcos (Ruhr Universität Bochum, Germany); Volker Schulz-von der Gathen, Marc Böke, Jörg Winter (Institut for Experimental Physics II, Research Department Plasma, Ruhr-Universität Bochum, Germany)

High power impulse magnetron sputtering (HIPIMS) combines impulse glow discharges at power levels up to the MW range with conventional magnetron cathodes to achieve a highly ionised sputtered flux. If observed with a low time resolution, the optical emission from the HIPIMS discharge may appear to be homogeneous during the pulse. However, we have shown recently that the HIPIMS plasma may develop drift wave type instabilities [1]. They are characterized by well defined regions of high and low plasma emissivity along the racetrack of the magnetron and cause periodic shifts in floating potential. The structures rotate in ExB direction at velocities of ~10 kms-1 and frequencies up to 200 kHz. It has already been shown in literature that the magnetron configuration may exhibit two-stream instabilities due to the difference in confinement of electron and ions and the associated differences in particle fluxes [2]. However the characteristic frequency of these instabilities is of the order of a few MHz, well above drift wave type instabilities we have observed.

In this paper a detailed analysis of the temporal evolution of the saturated instabilities using four consequently triggered fast ICCD cameras is presented. The influence of mass of the target material and working gas on the instability properties was investigated using titanium (Ti) and aluminium (Al) targets in either Ar or Kr gases. Furthermore working gas pressure and discharge current variation showed that the shape and the speed of the instability strongly depend on the working gas and target material combination. In order to better understand the mechanism of the instability, different optical interference band pass filters (of metal and gas atom, and ion lines) were used to observe the spatial distribution of each species within the instability. It was found that the optical emission from the instabilities comprises ion emission (both target material and gas ion lines) with strong depletion of the emission lines of the target material atom lines, concluding that instabilities are of generalised ion drift wave type.

[1] A. Ehiasarian, A. Hecimovic, T. de los Arcos, J. Winter, R. New, V. Schulz-von der Gathen, M. Böke, Appl. Phys. Lett. submitted

[2] D. Lundin, P. Larsson, E. Wallin, M. Lattemann, N. Brenning and U. Helmersson, Plasma Sources Science and Technology, 2008, (17), 035021

Acknowledgement: This work was funded within Subproject A5 of SFB-TR 87. We gratefully acknowledge valuable discussions with Prof. A. Ehiasarian and the kindness of Prof. H. Soltwisch and Dr. P. Kempkes on borrowing us the four cameras setup.

2:10 PM F2-2-2 Modes of operation in HiPIMS: Understand and optimize the discharge pulse
Daniel Lundin, Catalin Vitelaru (Université Paris-Sud 11, France); Nils Brenning (Royal Institute of Technology); Ulf Helmersson (Linköping University, Sweden); Tiberiu Minea (Université Paris-Sud 11, France)
High power impulse magnetron sputtering (HiPIMS) is one of the most promising sputtering-based ionized physical vapor deposition (IPVD) techniques and is already making its way to industrial applications. The major difference between HiPIMS and conventional magnetron sputtering processes is the mode of operation. In HiPIMS the power is applied to the magnetron (target) in unipolar pulses at a low duty factor (< 10 %) and low frequency (< 10 kHz) leading to peak target power densities of the order of kW cm-2. These conditions result in the generation of a highly dense plasma discharge, where a large fraction of the sputtered material is ionized and thereby providing new and added means for the synthesis of tailor-made thin films. In this work we dissect the HiPIMS discharge and thereby expose several important physical mechanisms operating during different stages of the discharge pulse. Recent experimental results on the evolution of the process gas (neutral Ar and Arm) and in-situ measurements of the transport of charged particles have been combined with HiPIMS plasma modeling of the dense plasma region in front of the target to establish a more coherent picture of the HiPIMS discharge, which includes time- and space-resolved characteristics on mechanisms such as process gas depletion, gas and metal sputtering, degree of ionization, as well as current distribution. Special attention is paid to how these internal pulse features can be influenced by the choice of discharge pulse configuration.
2:30 PM F2-2-3 High-rate reactive deposition of multifunctional Ta-O-N films using high power impulse magnetron sputtering
Jaroslav Vlcek, Jiri Rezek, Jiri Houska, Radomir Cerstvy (University of West Bohemia, Czech Republic)
High power impulse magnetron sputtering of a planar tantalum target (diameter of 100 mm) in various argon-oxygen-nitrogen gas mixtures was investigated at a fixed average target power density of 50 Wcm-2 in a period. A strongly unbalanced magnetron was driven by a pulsed dc power supply (HMP 2/1, Huettinger Elektronik) operating at the repetition frequency of 500 Hz and the average target power density of up to 2.4 kWcm-2 in a pulse with a fixed 50 μs duration. The nitrogen fractions in the reactive gas flow were in the range from 0 to 100% at the argon partial pressure of 1.5 Pa and the total pressure of the argon-oxygen-nitrogen gas mixture around 2 Pa. The Si (100) and glass substrates were at a floating potential, and the substrate temperature was less than 250°C. The target-to-substrate distance was 100 mm. An effective reactive gas flow control made it possible to produce high-quality Ta-O-N films of various elemental compositions with high deposition rates (97 to 190 nm/min). Their compositions (in at. %) were varied from Ta27O72 with a low content (less than 1%) of hydrogen to Ta38O4N55 with 3% of hydrogen. The former films were nanocrystalline with high optical transparency (extinction coefficient less than 10-4 at 550 nm), refractive index of 2.12, band gap of 4.0 eV, very low electrical conductivity (resistivity of 7.7x109 Ωcm) and hardness of 7 GPa. The latter films exhibited a more pronounced crystallinity, they were opaque with relatively high electrical conductivity (resistivity of 4.2x10-2 Ωcm) and hardness of 19 GPa. The Ta27O40N31 films with 2% content of hydrogen, produced at the 50% nitrogen fraction in the reactive gas flow with the highest deposition rate of 190 nm/min achieved, were nanocrystalline with the band gap of 2.4 eV, electrical resistivity of 5.5x106 Ωcm and hardness of 8 GPa. Such films seem to be suitable candidates for visible-light responsive photocatalysts. Details of the deposition process and measured properties of the films will be presented.
2:50 PM F2-2-4 Variation of high power pulsed / modulated pulsed power magnetron sputtering based on oscillatory voltage wave forms for the deposition of carbon and aluminum oxide coatings
William Sproul (Reactive Sputtering, Inc., US); Jianliang Lin (Colorado School of Mines, US); Bassam Abraham (Zond, Inc. / Zpulser, LLC, US); John Moore (Colorado School of Mines, US); Roman Chistyakov (Zond, Inc. / Zpulser, LLC, US)
A new plasma generator with its roots in the HiPIMS/MPP sputtering technology that now produces oscillatory waveforms was used for the deposition of carbon and aluminum nitride coatings. The amplitude and the frequency of the voltage oscillations control the discharge current and the plasma ionization: Id = f (Ud, fω). At constant discharge voltage achieved by adjusting the frequency of the voltage oscillations, the discharge current could be increased by a factor of up to 7 times. With this new plasma generator, DLC coatings that are hydrogen free could be deposited with hardnesses that approach superhard values. The hardness of the DLC films is a function of the substrate bias voltage, substrate temperature, frequency of the voltage oscillations, and the field strength of the magnetron design. The new plasma generator has also been used for the reactive deposition of such films as AlN. A very interesting side effect of this new plasma generator is that at constant discharge voltage it is possible to generate a near arc free discharge for reactive sputtering processes while still producing a stream of ions from the sputtered material. An arc free process removes one of the disadvantages of HiPIMS sputtering as originally practiced. More will be presented about reactive sputtering using this new plasma source at the meeting.
3:10 PM F2-2-5 The development and the application of a high power impulse inverted cylindrical magnetron sputtering system for the elaboration of nanomaterials on wires or fibers.
Patrick Choquet, David Duday, Antoine Lejars, Olek Vozniy, Tom Wirtz (CRP Gabriel Lippmann, Luxembourg)

The elaboration of new nanomaterials on wires and on fibers is of great interest for industry. One possibility to manufacture these innovative products is to deposit thin films in a continuous way on wires or fibers. This solution offers possibility to synthesize new materials with a large flexibility for the process utilization.

An instrumental prototype designed as a continuous air-to-air in-line wire-coating has been set-up with the capability to run with speed lines between 5 to 30m/min. A new Inverted Cylindrical Magnetron (ICM) plasma deposition reactor operated in the HIPIMS mode has been developed. It has been demonstrated both theoretically and experimentally that this configuration allows a high ionization degree of sputtered target material while reaching the same high deposition rate as for planar magnetrons operated in the DC mode. It has been shown that this ICM configuration, which is moreover ideally adapted for a homogeneous wire coating due to its cylindrical symmetry, promotes a better self-assistance with target ions and allow for a repeated use of ionized species to maintain a high ionization degree in metal plasma. Also, the magnetron was intentionally designed with an unbalanced system of magnets to ensure the diffusion of the plasma electrons along the force lines of the magnetic field to the central part of the discharge volume. This magnetic field can permit to form a channel from the target surface to the wire, where the plasma volume can be extended down to the substrate area with minimal losses. It has also been shown that a non-stationary magnetic field allows to a better stabilization of the discharge voltage even at a high degree of the target erosion.

The outstanding performance of the ICM prototype, which is characterized by a much higher deposition rate than in conventional planar systems, was validated in direct measurements. The values of the deposition rate for the ICM were compared with a reactor equipped with 4 planar magnetrons surrounding the wire for the same power input per the cm2 of the target surface. It was concluded that a 10 times higher deposition rate can be achieved with this ICM designed system. Also, in order to demonstrate the performance of the wire coated prototype instrument, elaborations of ZnO and AlTiSiN films on wires have been achieved. The structural and chemical properties of the ceramic films has been established and correlated with end-used performances.

3:30 PM F2-2-6 Low pressure High Power Impulse Magnetron Sputtering systems for deposition of biomedical functional thin films
Vitezslav Stranak (University of Greifswald, Germany); Martin Cada, Zdenek Hubicka (Academy of Sciences, Czech Republic); Steffen Drache, Ann-Pierra Herrendorf, Harm Wulff, Rainer Hippler (University of Greifswald, Germany)

The high ionization of sputtered metal particles is a main advantage of High Power Impulse Magnetron Sputtering (HiPIMS) discharges. Large quantity of ionized sputtered material leads to the growth of smooth and dense films, allows control of the crystallography phase, mechanical and optical properties etc. Because of these positive effects there is reason to develop sputtering sources with high level of metal ionization. It is already known that namely energy of ions and incoming particles to growing film is a key parameter which influences film property. In our contribution we report two novel HiPIMS-based techniques which allow energy control in wide range.

The first system is a unipolar hybrid-dual HiPIMS based on a combination of dual-HiPIMS (the system where two magnetically and electrically confined magnetrons are alternately operated in HiPIMS mode, f = 100 Hz, duty cycle 1 %) with mid-frequency (MF) discharge operated at f = 94 kHz and duty cycle 30 %. The second system is based on sputtering of HiPIMS driven electrode inserted in RF discharge with an additionally superimposed magnetic field (ECWR). The most important feature of these hybrid methods is the pre-ionization effect which causes/allows: (i) significant reduction of working pressure by nearly two orders of magnitude, (ii) intensive ionization of metal atoms with substantial amount of double ionized species, (iii) increase of HiPIMS power density and other discharge parameters, (iv) faster ignition and development of HiPIMS pulses.

Enhanced time-resolved diagnostic of developed plasma sources has been done. From time-resolved Langmuir probe measurements was estimated mean electron energy, electron density and electron energy probability function (EEPF). The plasma density reached values about 5.1018 m-3 during HiPIMS pulses at low pressure (0.04 Pa). The time–resolved measurements of Ion Velocity Distribution Functions (IVDFs) and Ion Energy Distribution Functions (IEDFs) were performed. It was found that ion energies during HiPIMS pulses are strongly enhanced (about 20-30 eV) while in background (MF or RF) discharge were measured much lower values. Parameters from Langmuir probe diagnostic serve also as input for calculation of influx contributions of particular species, e.g. neutral particles. The study of plasma transport effects was done by fast optical emission imaging and spectroscopy.

This work was supported by Deutsche Forschungsgemeinschaft through SFB/TR 24 and by the German Federal Ministry of Education and Research (BMBF) through Campus PlasmaMed. Further projects KAN301370701 of ASCR, 1M06002 of MSMT and project 202/09/P159 of GACR are acknowledged.

4:10 PM F2-2-8 Material properties of Aluminum Metal (Titanium/Chromium) Nitride coatings deposited by High Power Impulse Magnetron Sputtering (HIPIMS+) technology.
Frank Papa, Anna Campiche, Roel Tietema, Thomas Krug (Hauzer Techno Coating, BV, Netherlands); Tomoya Sasaki, Takeshi Ishikawa (Hitachi Tool Engineering, Ltd., Japan)
Aluminum Metal (Titanium/Chromium) Nitride coatings have been deposited from targets consisting of tiles from 4 different aluminum metal compositions using HIPIMS+ technology. In such a configuration, the changes in material properties such as hardness and crystal orientation can be analyzed for many coating compositions while keeping the plasma conditions constant. The peak cathode current has been used as the control variable as this has a strong influence on the metal ion content within the plasma and the plasma density. As the peak cathode current is increased, the crystal size and structure change significantly. The effect of varying the plasma density on the proportion of the cubic/hexagonal phase for such materials as Al(Ti/Cr)N is of great interest for hard coatings for cutting tool applications.
4:30 PM F2-2-10 On the Influence of superimposed MF and HPPMS/HiPIMS pulsed packages on the deposition rate and properties of TiN
Jones Alami, Zeljko Maric (INI Coatings Ltd., Germany); Martin Malzer, Martin Fenker (FEM Forschungsinstitut Edelmetalle & Metallchemie, Germany); Michael Mark, Jonathan Löffler, Erick Parra Maza, Günter Mark (MELEC GmbH, Germany)

High Power Pulse Magnetron Sputtering, HPPMS (also known as HiPIMS), is a promising pulsed plasma technology for deposition of high quality thin films. HPPMS has been shown to exhibit very high electron density and ionization of the sputtered material. The plasma charged particles are easily affected by magnetic and electric fields and present therefore conditions for the thin film developer to control the energy bombardment and subsequently the properties of the deposited thin films. Even if HPPMS has a great potential for bringing new and interesting solutions to the PVD market, it is still inconsistent and not standardized as is always the case for new technologies or techniques. It has been established that in order for HPPMS to function in an optimal fashion, it is of importance to understand not only the plasma condition of the process but also how the different parts of a coating system interact with each other in order to give the right process conditions needed for the deposition.

A number of works have characterized and attempted to correlate the effect of pulsing on the HPPMS process, especially on the deposition rate. These have used different power supplies as well as different power supply combinations in order to achieve the different modes of operation. They found that the pulsing configuration and frequency affect to a large extent the coating process as well as the resulting thin film properties.

Recent approaches supply power to the magnetron source by super-imposing a medium frequency (MF) and a HPPMS power unit. The main advantage of such an approach is to provide means to even better architect the plasma conditions that best enable a suitable compromise between deposition rate and ionization. Moreover, the combination of MF and HPPMS allows better tuning of the process parameters and therewith the resulting thin film’s properties. This new approach for using the HPPMS technique is appropriate for single and dual magnetron sputtering and synchronized pulsed bias. It is therefore possible to perform stable reactive depositions in continuous operating systems such as inline glass coaters.

The present work investigates the influence of the pulsed power controllers and the mechanisms for producing the very high peak currents needed for the HPPMS process. The influence of MF and HPPMS superimposed pulse packages on the deposition rate during reactive sputtering of titanium in an Ar/N2 atmosphere will be presented. Additionally the resulting TiN film microstructure and phase/texture composition will be discussed with respect to the corresponding plasma conditions.

4:50 PM F2-2-11 Angle-resolved energy flux measurements of a HIPIMS-powered rotating cylindrical magnetron in reactive and non-reactive atmosphere.
Stephanos Konstantinidis (University of Mons, Belgium); Wouter Leroy (Ghent University, Belgium); Rony Snyders (University of Mons, Belgium); Diederik Depla (Ghent University, Belgium)
Energy flux measurements were carried out using a passive thermal probe during sputtering of titanium in a reactive Ar/O2 atmosphere with a rotating cylindrical magnetron. The data were collected 90° around the cylindrical magnetron cathode. The rectangular voltage pulses had a duration of either 5 or 20 µs and target voltage was set to 600V in order to reach a time-averaged power density over the racetrack of 30 W/cm². As a reference, the energy flux was also measured during DC magnetron under the same working conditions. The energy flux per adparticle was calculated by measuring the deposition rate for all sputter modes and regimes. The lowest deposition rate was measured during reactive HiPIMS, with 20µs-long pulses. However the highest energy per adparticle was measured for that particular case. This result can be understood based on the increased ion and electron fluxes on the probe surface during the HiPIMS experiments. A possible contribution to the energy flux could also originate from the presence of fast oxygen ions (0-) emitted from the target surface and accelerated in the cathode sheath. A difference in the angular distribution of the energy deposited per arriving adparticle is noticed when comparing the dc and the HIPIMS discharges. The dc mode has a maximum arriving energy per adparticle at around 50°, while the maximum is located at 60° for the HIPIMS mode.
Time Period TuA Sessions | Abstract Timeline | Topic F Sessions | Time Periods | Topics | ICMCTF2012 Schedule