ICMCTF2004 Session B9/TS1: Pulsed Plasmas for Vapor Deposition

Wednesday, April 21, 2004 1:30 PM in Room Sunset

Wednesday Afternoon

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1:30 PM B9/TS1-1 Advances in High Power Pulsed Magnetron Sputtering Driven by Novel Pulsed Power Supply Technology.
D.J. Christie, W.D. Sproul, D.C. Carter, F. Tomasel (Advanced Energy Industries, Inc.)

High power pulsed magnetron sputtering (HPPMS) has created growing interest, because it can generate highly ionized plasmas with high target material ion content. HPPMS applies a high power pulse (up to several megawatts) with short pulse width to the target. The result is a high degree of ionization of the plasma, consisting of sputtered species and process gas. The ions can improve the structure and properties of the deposited film. It has been shown that a significant flux of low energy ions to the substrate can result in dense equi-axed films. The HPPMS technique can generate large numbers of ions with essentially conventional magnetron sputtering apparatus. An experimental power supply was built in order to investigate HPPMS. It is capable of peak powers up to 3 megawatts with nominal pulse widths of 100-150 µsec. Average delivered power is up to 20 kW, at frequencies from single shot to 500 Hz. Temporally resolved optical spectroscopy of the plasma provides evidence of the ionization of the sputtered species. The degree of ionization is a function of the peak power delivered to the process. Very thin carbon films for potential hard disk applications have been deposited by HPPMS. The films have a density of 2.7 g/cm3, very high for sputtered carbon.1 The power supply can detect and suppress arcs which enables HPPMS deposition of important materials which are prone to arcing, such as carbon and aluminum. In addition, the pulsing power supply circuitry incorporates wave-shaping to prevent arcing. This enables the pulse to transition directly from the glow to the highly ionized state without accessing the arc regime. Pulse discharge circuit considerations, optical spectra, electrical waveforms, process characteristics, and deposited film properties will be presented.

1B. M. DeKoven, et al., accepted for publication in the Proceedings of the Society of Vacuum Coaters Technical Conference, San Francisco, May 2003.

2:10 PM B9/TS1-3 Influence of Interface Preparation on the Adhesion and Sliding Wear Performance of Chromium Nitride Coatings
A.P. Ehiasarian (Sheffield Hallam Univeristy, United Kingdom); P.Eh. Hovsepian (Sheffield Hallam University, United Kingdom); U. Helmersson, L. Hultman (Linköping University, Sweden); I. Petrov (University of Illinois); A. Anders (Lawrence Berkeley National Laboratory)
The effect of adhesion and macroparticle-induced growth defects on the performance of coatings in wear tests is presented. Adhesion enhancing pretreatment of the substrates was realised by ion bombardment in four different plasma environments: Ar ions generated in a glow discharge, Cr metal ions produced in a steered cathodic arc discharge, Cr metal ions from steered cathodic arc discharge with macroparticle filter, and Cr metal ions + Ar ions from high power impulse magnetron sputtering (HIPIMS). Subsequently, CrN coatings were deposited by unbalanced magnetron (UBM) sputtering and HIPIMS. Cross-sectional transmission electron microscopy revealed a columnar voided microstructure for the UBM deposited coatings and a dense structure for the HIPIMS deposited coatings. Depending on the type of pretreatment used, the coatings exhibited different values of the critical load, LC, in scratch tests: Ar glow discharge - LC = 40 N, Cr arc - LC = 60 N, Cr filtered arc - LC = 82 N, and HIPIMS Cr - LC = 85 N. All coatings showed similar coefficient of friction of 0.45 ± 0.1 and Knoop hardness in the range HK0.025 2100-2800. However, the incorporation of a macroparticle filter during the arc pretreatement reduced the grooving in the wear track and improved the sliding wear coefficients for the coatings (Kc) from 1.3x10-15 m3N-1m-1 to 5x10-16 m3N-1m-1. A further improvement by factor of two to Kc = 2x10-16 m3N-1m-1 was measured for the HIPIMS pretreatment and HIPIMS coating.
2:30 PM B9/TS1-4 Reactive High Power Pulsed Magnetron Sputtering of Aluminum Oxide
W.D. Sproul, D.J. Christie, D.C. Carter (Advanced Energy Industries, Inc.)

High power pulsed magnetron-sputtering (HPPMS) offers the opportunity of producing a highly ionized metal plasma. The degree of ionization of the plasma is a function of the peak power in the pulse, and for sputtered metals such as aluminum the degree of ionization can exceed 50%. Previous work1 with the reactive sputtering of aluminum oxide in an ionized PVD system demonstrated that it is possible to deposit crystalline alumina at temperatures below 500 degrees C. In this study, an experimental high power pulse power supply with special arc handling and pulse rise time features combined with partial pressure control of the reactive gas was used to evaluate the feasibility of reactively depositing crystalline alumina in an HPPMS system. Target arcing is particularly debilitating to the control of any reactive sputtering process, and the experimental power supply was capable of detecting and quenching arcs, which brought stability to the deposition process. In addition, the rising edge of the pulse was controlled to prevent the plasma from going from the abnormal glow discharge mode into the arc regime. The combination of these features allowed the reactive sputter deposition of aluminum oxide films using HPPMS. Details of the deposition process and results of the characterization of the deposited films will be reported.

1J. M. Schneider, W. D. Sproul, A. A. Voevodin, and A. Matthews, "Crystalline Alumina Deposited at Low Temperature by Reactive Ionized Magnetron Sputtering," J. Vac. Sci. Technol. A, 15(3) (1997) 1084.

2:50 PM B9/TS1-5 Magnetic Disturbance in a Pulsed High Current Magnetron Discharge
J. Bohlmark (Thin Film Physics, IFM, Sweden); J. Alami (Linköping University, Sweden); M. Van Zeeland (UCLA Large Plasma Device (LAPD)); U. Helmersson (Linköping University, Sweden)
We demonstrate the change of the magnetron's magnetic field in a high current and high plasma density discharge. The high-density plasma is created by applying a high power pulse (up to 2 MW peak power) to a conventional planar magnetron, resulting in a magnetron current of several hundreds of amperes. The pulse length is about 100 µs and the repetition frequency is 50Hz, i.e., a duty factor of about 1%, which reduces the problem of target heating. The temporal and spatial magnetic environment of the magnetron in a vicinity of the target is investigated using a coil type magnetic probe. Spatially resolved measurements of the change in the magnetron's magnetic field show that circulating currents confined in the magnetic field dominate the picture. Comparisons between electron currents measured with a flat probe and the magnetic field change also indicate that the expanding high-density plasma created by the discharge close to the target weakly affects the magnetron's magnetic field. Furthermore, we quantify the magnetic disturbance for different applied magnetron powers. A connection between magnetron impedance and magnetic field change is shown and explained by reduced magnetron confinement for high discharge power.
3:10 PM B9/TS1-6 Pulsed Magnetron Sputter Deposition of High Performance Magnesium Aluminate Spinel Coatings for Cutting Tools
E. Lugscheider, K. Bobzin, M. Maes (RWTH-Aachen, Germany); R. Cremer, G. Erkens (CemeCon AG, Germany)
Ever increasing tool performance has led to a variety of requirements on high performance tool coatings. Oxidic coatings show most promising properties in this matter. High oxidation resistance, hot hardness, low friction and anti-sticking are just a few benefits of these coatings. However oxidic coatings have been avoided for a long time since coating equipment was unable to produce the required quality in high deposition rates. Pulsed power supplies offer an excellent opportunity to deposit non-conductive, high quality coatings with outstanding deposition rates. Focal point of this paper is the process technology required for the deposition of these complex coatings. A dual cathode arrangement was used for deposition. The required composition of aluminum to magnesium was attained by aluminum targets with magnesium inserts in an optimized target surface ratio. After deposition, these coatings were characterized with common coating test methods. Additionally the deposited coatings were compared and evaluated to common industrial coatings in standard cutting tests.
3:30 PM B9/TS1-7 Time-resolved Characterization of Pulsed Magnetron Discharges using Langmuir Probes
F. Richter, Th. Welzel, Th. Dunger, H. Kupfer (Chemnitz University of Technology, Germany)

With the increasing popularity of pulsed plasma discharges a growing interest in time-resolved process characterization arose. Langmuir single and double probes enable one to determine plasma density and electron temperature as well as (in case of single probes) the plasma potential. Owing to the dimensions of the probe tips (typically 1 - 10 mm) a certain spatial resolution can be achieved. During the past years, time-resolved Langmuir probe technuiques have been developed and applied to pulsed magnetron sputtering processes. The talk is organised as follows:

i) As an introduction, a concise description of the Langmuir probe measurement and data evaluation techniques is given and it is shown how plasma parameters can be derived from the current-voltage characteristics of the probe. Peculiarities of Langmuir single and double probes are presented and practical problems to be faced in depositing plasma are discussed.

ii) In the past years, few groups have done time-resolved Langmuir probe investigations of pulsed magnetron discharges. These results are shortly reviewed, including own results of a time-resolved Langmuir double probe technique which was applied to a pulsed magnetron discharge at several 100 kHz used for MgO deposition. The tungsten probe tips were 500 µm in diameter, 10 mm in length and where placed parallel to each other in a distance of 5 mm. The time-resolved measurement was done by fixing the probe voltage and recording the probe current as a function of time. This was repeated for different voltages. Then, the matrix of the IU(t) curves was transposed with a computer to yield for each time step the usual I(U) characteristic, from which plasma density and electron temperature were determined.

iii) All results are critically discussed in connection with the discharge characteristics as well as time-dependent processes in the plasma which may influence the time-resolved measurement.

4:10 PM B9/TS1-9 Argon Plasma Modelling in a RF Magnetron Sputtering System
A. Palmero, E.D.van Hattum, W.M. Arnoldbik, A.M. Vredenberg, F.H.P.M. Habraken (Utrecht University, The Netherlands)
Argon plasma properties in a radio-frequency magnetron sputtering system have been studied, both theoretically and experimentally. A Langmuir probe has been used to meassure the ion density, electron temperature and plasma potential in front of the race track, and particulary nearby the cathode. Hence, the influence of the magnetic field on the Langmuir probe data were taken into account. From a theoretical point of view, the plasma equations have been solved. We find a good agreement between theoretical and experimental data for several conditions of rf power and pressure. This agreement helps to understand the dynamics of the sputtering process, and particulary the interaction between the plasma and the cathode.
4:30 PM B9/TS1-10 Experimental Characterization of the Deposition Process of Silicon Suboxide Thin Films in a Radio-frequency Magnetron Reactive Sputtering System
E.D.van Hattum, A. Palmero, W.M. Arnoldbik, A.M. Vredenberg, F.H.P.M. Habraken (Utrecht University, The Netherlands)
The particle flows reaching the anode in a radio-frequency magnetron reactive sputtering system have been determined using an energy resolved mass spectrometer. The cathode is made of polycrystalline silicon, while the plasma is composed of argon and oxygen. The deposition rate and stoichiometry of deposited silicon (SiOx) sub-oxide thin films have been obtained using the high-energy ion beam techniques Elastic Recoil Detection and Rutherford Backscattering Spectroscopy. The atomic structure of the films is investigated with in situ X-ray Photoelectron Spectroscopy and Infrared Absorption Spectroscopy. We especially focused on the relation between energy and particle flows from the plasma and this atomic structure, in view of the instability of a homogeneous SiOx network against Si/SiO2 phase separation. This relation has been studied for several deposition pressures and incident radio-frequency power.
4:50 PM B9/TS1-11 Pulsed DC Operation of an Opposed Target Magnetron
D. Cameron, T. Moiseev (Dublin City University, Ireland)
The cylindrical opposed target magnetron in which the magnetic field is perpendicular to the targets rather than parallel in conventional planar magnetron was originally proposed for sputtering ferromagnetic materials. We have investigated the characteristics of an opposed target magnetron with rectangular configuration, more suitable for industrial use. With a copper target and DC power, as the magnetron current is increased, the I-V characteristic shows an initial increase in voltage followed by decrease and then a further increase. As the pulsed DC 'off' time is increased, the negative resistance part of the characteristic becomes less significant and eventually disappears. The relation between this behaviour and the evolution of the time resolved optical emissions from the plasma will be presented. Time resolved optical emission spectroscopy of the excited and ionised species shows a difference in the time constants between the argon and the copper excitation. The copper excitation has a slower rise time than that of argon and also a slower decay with evidence of more than one time constant in the process. These results will be reported and the differences which occur in the magnetron characteristics and plasma emissions when using ferromagnetic and non-ferromagnetic targets will be discussed.
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