<p>The work presented in this thesis involves experimental and theoretical studies related to plasma properties in high power impulse magnetron sputtering (HiPIMS), and more specifically plasma transport. HiPIMS is an ionized PVD method based on conventional direct current magnetron sputtering (dcMS). In dcMS very little of the sputtered material is ionized since the plasma power density is not high enough. This is not the case for HiPIMS, where a substantial part is ionized, and thus presents many new opportunities for thin film growth. Understanding the dynamics of the charged species in the HiPIMS discharge is therefore of essential value when producing high-quality thin film coatings.</p><p>In the first part of the work a new type of anomalous electron transport was found. Investigations of the transport resulted in the discovery that this phenomenon could quantitatively be described as being related and mediated by highly nonlinear waves, likely due to the modified two-stream instability (MTSI), resulting in electric field oscillations in the MHz-range (the so-called lower hybrid frequency). Measurements in the plasma confirmed these oscillations as well as trends predicted by the theory of these types of waves. The degree of anomalous transport in the plasma could also be determined by measuring the current density ratio between the azimuthal current density (of which the Hall current density is one contribution) and the discharge current density, <em>J</em><em>φ</em><em> / J</em><em>D</em>. The results provided important insights into understanding the mechanism behind the anomalous transport.</p><p>It was furthermore found that the current ratio <em>J</em><em>φ</em><em> / J</em><em>D</em> is inversely proportional to the transverse resistivity, eta_perpendicular , which governs how well momentum is transferred from the electrons to the ions in the plasma. By looking at the forces involved in the charged particle transport it was expected that the azimuthally rotating electrons would exert a volume force on the ions tangentially outwards from the circular race track region. The effect of having an anomalous transport would therefore be a large fraction of highly energetic ions being transported sideways and lost to the walls. In a series of experiments, deposition rates as well as incoming ion energy distributions were measured directly at the side of the magnetron. It was found that a substantial fraction of sputtered material is transported radially away from the cathode and lost to the walls in HiPIMS as well as dcMS, but more so for HiPIMS giving one possible explanation to why the deposition rate for substrates placed in front of the target is lower for HiPIMS compared to dcMS. Furthermore, the recorded, incoming ion energy distributions confirmed theoretical estimations on this type of transport regarding energy and direction.</p>

Cette étude a pour but la mise au point d'un procédé de dépôt en vue de réaliser des fibres piézoélectriques. Ces fibres pourront être utilisées soit comme jauge de déformation (extensomètre) soit comme système de récupération d'énergie liée au mouvement d'un utilisateur (tissu) pour alimenter un dispositif d'électronique embarqué. Une fibre piézoélectrique constituée d'un dépôt cylindrique d'oxyde de zinc sur un fil d'acier inoxydable a été réalisée par pulvérisation magnétron à impulsion de haute puissance (HiPIMS) à l'aide d'un prototype de traitement au défilé conçu, réalisé et décrit lors de cette étude. Une caractérisation précise des échantillons réalisés dans différentes conditions expérimentales a permis de décrire et comprendre en partie les mécanismes de croissance des dépôts, ceci de manière, en particulier, à déterminer les conditions de fonctionnement optimum pour l'élaboration de dépôts possédant une orientation cristalline préférentielle hors plan. Pour envisager le traitement de fibres ne supportant pas les hautes températures nous avons montré qu'il était possible de contrôler cette température en ajustant certains paramètres du procédé, tel que la pression et la puissance moyenne. Un mécanisme de germination préférentielle suivi d'une croissance par auto-épitaxie a été proposé afin d'expliquer la très forte orientation préférentielle des films réalisés à faible température. Pour des fortes valeurs de courant crête, le phénomène de germination préférentielle associé à la croissance évolutionnaire pourrait favoriser l'orientation (101)*. Pour les plus fortes valeurs de courant, aucune orientation préférentielle n'est observée et les fortes contraintes mesurées ont été attribuées à l'excès d'oxygène détecté dans les couches / A piezoelectric fiber constituted of ZnO cylindrical coating on a stainless steel wire has been achieved by High Power Impulse Magnetron Sputtering (HiPIMS) by using a prototype designed and assembled during this PhD work. The piezoelectric fiber can be used as a strain probe or as a vibration harvesting generator for embedded electronics. The analyses of deposited layer allow to understand ZnO growth mechanism in order to optimize to deposition process. A special emphasis has been placed on the selection of preferential orientation during the growth. The low volume of steel wire, allow to control his temperature by adjusting some process parameters, like the pressure and the average power. Temperature sensitive wires (e.g. polymer) can be treated in the mildest conditions. Preferential nucleation followed by self-epitaxy have been proposed to explain the very strong preferential orientation identified in coatings deposited at low temperature. At high peak current, preferential nucleation and evolutionary growth can promote the (101)* orientation. At highest peak currents no preferential orientation was identified and the high residual stress has been attributed to the excess of oxygen in the coating

La pulvérisation cathodique magnétron pulsée à haute puissance (HiPIMS) est un procédé de dépôt de couches minces dans lequel le flux de dépôt est principalement composé d’ions du matériau pulvérisé. Ce type de décharge permet de contrôler l’énergie et la direction des espèces qui seront déposées, ce qui est favorable à la modification de la structure et des propriétés finales des couches. Malgré tous les travaux de recherches menés pour caractériser et comprendre les conditions de décharge HiPIMS, la nécessité de développer des couches minces utiles à la société reste toujours d’actualité. La finalité de ce travail est l’obtention de couches minces HiPIMS plus performantes que celles obtenues aujourd'hui en utilisant des techniques de dépôt classiques. Pour cela il est indispensable d'identifier et d'optimiser les paramètres de dépôt permettant de modifier à la fois la microstructure des couches, la contrainte résiduelle et les propriétés liées à l'énergie telles que la résistivité électrique et la bande interdite. Trois matériaux sont au cœur de ce travail : le cuivre, le dioxyde de titane et le nitrure de titane. Les études expérimentales ont montré que les paramètres les plus importants pour obtenir les propriétés souhaitées étaient la quantité et l’énergie cinétique des espèces ionisées irradiant la couche au cours de sa croissance. Par ailleurs, les paramètres de croissance optimale entre couches métalliques et couches composées diffèrent considérablement. / High power impulse magnetron sputtering (HiPIMS) is a thin film deposition technique where the deposition flux is predominantly composed of ionized sputtered material. This enables control of energy and direction of the film-forming species and is thereby beneficial for tailoring the film structure and final properties. Although researchers world-wide have spent significant time and efforts characterizing and understanding the plasma process conditions in HiPIMS, research in new and improved HiPIMS-based thin film materials that find applications in areas of importance for society is still required. The goal of this work has been to identify and optimize the deposition parameters that allow tailoring the film microstructure, intrinsic stress and energy-related properties, such as electrical resistivity and optical band gap, to ultimately achieve superior HiPIMS coatings compared to what is achieved today using conventional deposition techniques. Three material systems constitute the core of the work: copper, titanium dioxide, and titanium nitride. From the work carried out it is concluded that the most important parameters affecting the film structure and properties are the amount as well as the kinetic energy of the ionized sputtered species irradiating the film during growth. These parameters differ substantially for optimum growth conditions of metallic and compound films.

The ion acceleration process in Bipolar High Power Impulse Magnetron Sputteringis investigated for use in a novel space propulsion system - the BP-HiPIMS thruster.The interest for BP-HiPIMS has recently been growing within the area of thin filmdeposition due to the theorised acceleration of target ions caused by the reversedpulse following the regular HiPIMS pulse. This same acceleration could be usedto produce thrust in a space propulsion system, where the lack of physical gridsand temporal separation of ionisation and acceleration are attractive benefits of thesuggested system. In this paper the physical processes and parameters of importanceare experimentally investigated to gain understanding of the ion acceleration processwith the goal of verifying the theory of BP-HiPIMS thusters.Through plasma potential measurements a beneficial potential structure between themagnetic trap and bulk of the plasma which could potentially accelerate ions is foundat certain discharge conditions and some acceleration of ions is confirmed in massspectrometer measurements. The results are promising for a thruster application butfurther research is needed to evaluate the viability of the proposed system. / Jonaccelerationsprocessen i Bipolar High Power Impulse Magnetron Sputteringundersöks för användning i ett nytt framdrivningssystem för rymdfarkoster: BPHiPIMSthrusters. Intresset för BP-HiPIMS har ökat den senaste tiden inomtunnfilmsfysiken på grund av accelerationen av “target” joner som tros accelererasav den bipolära pulsen som följer den vanliga HiPIMS pulsen. Denna accelerationskulle också kunna användas för att skapa en framdrivande kraft som kan användassom motor på rymdfarkoster, där saknaden av accelererande galler och separationav jonisering och acceleration i tiden är attraktiva fördelar av det föreslagnasystemet. I denna rapport undersöks den fysikaliska processen och viktiga parametrarexperimentellt för att få en förståelse för jonaccelerationsprocessen med målet attverifiera teorin bakom “BP-HiPIMS thrusters”.Genom plasmapotentialmätningar kan en gynnsam potentialstruktur, mellan denmagnetiska fällan nära magnetronen och volymenutanför, som potentiellt kan accelerera joner uppmätas under vissa förhållanden, däracceleration av joner bekräftas av masspektrometri. Resultaten är lovande för ettelektriskt rymdframdrivningssystem, men ytterligare forskning krävs för att evaluerakonkurrenskraften av det föreslagna systemet.

<p>High power impulse magnetron sputtering (HiPIMS) is a novel pulsed power technique. In HiPIMS, high power pulses are applied to the target for short duration with a low duty factor. It provides a high degree of ionization of the sputtered material (in some cases up to 90%) and a high plasma density (10¹⁹ m^-3) which results in densification of the grown films. Recently a large side-transport of the sputtered material has been discovered, meaning that the sputtered material is transported radially outwards, parallel to the cathode surface. In this research, we use this effect and study the side-ways deposition of thin films. We designed a new magnetron sputtering system, consisting of two opposing magnetrons with similar polarity. Ti films were grown on Si using the side-ways transport of the sputtered material. Scanning electron microscope was employed to investigate the microstructure of the grown films. Optical emission spectroscopy (OES) measurements were made for investigating the ionized fraction of the sputtered material while Langmuir probe measurements were made for evaluating the plasma parameters such as electron density. The conclusion is that the system works well for side-ways deposition and it can be useful for coating the interior of cylindrically shaped objects. It is a promising technique that should be used in industry.</p>

<p>A microphone has been used to measure the dynamic pressure inside a vacuum chamber during high power impulse magnetron sputtering with high enough time-resolution (~µs) to track the pressure change during the discharge pulse. An experimental measurement of the dynamic pressure is of interest since it would give information about gas depletion, which is believed to dramatically alter the plasma discharge characteristics. This investigation has shown that the magnitude of the pressure wave, which arises due to the gas depletion, corresponds to a 0.4 - 0.7Pa (3 - 5.5mTorr) pressure difference at a distance of 15cm from the target, with base pressures of 2 - 6mTorr for a peak current of 110A. It has also been shown that another pressure wave, about 250µs later, can be detected. Its explanation is suggested to be that the initial pressure wave is bouncing against the chamber walls and thereby causing another peak.</p>

A microphone has been used to measure the dynamic pressure inside a vacuum chamber during high power impulse magnetron sputtering with high enough time-resolution (~µs) to track the pressure change during the discharge pulse. An experimental measurement of the dynamic pressure is of interest since it would give information about gas depletion, which is believed to dramatically alter the plasma discharge characteristics. This investigation has shown that the magnitude of the pressure wave, which arises due to the gas depletion, corresponds to a 0.4 - 0.7Pa (3 - 5.5mTorr) pressure difference at a distance of 15cm from the target, with base pressures of 2 - 6mTorr for a peak current of 110A. It has also been shown that another pressure wave, about 250µs later, can be detected. Its explanation is suggested to be that the initial pressure wave is bouncing against the chamber walls and thereby causing another peak.

HfO2 is a popular replacement for SiO2 in modern CMOS technology. It is used as the gate dielectric layer isolating the transistor channel from the gate. For this application, certain material property demands need to be met, most importantly, a high static dielectric constant is desirable as this positively influences the effectiveness and reliability of the device. Previous theoretical calculations have found that this property varies with the crystal structure of HfO2; specifically, the tetragonal structure possesses the highest dielectric constant (~70 from theoretical calculations) out of all possible stable structures at atmospheric pressure, with the cubic phase a far second (~29, also calculated). Following the results from previous experimental work on the phase formation of sputtered HfO2, this study investigates the possibility of producing thin films of HfO2 with the cubic or tetragonal structure by the addition of nitrogen to a reactive sputtering process at various deposition temperatures. Also, a new physical vapor deposition method known as High Power Impulse Magnetron Sputtering (HiPIMS) is employed for its reported deposition stability in the transition zone of metal-oxide compounds and increased deposition rate. Structural characterization of the produced films shows that films deposited at room temperature with a low N content (~6 at%) are mainly composed of amorphous HfO2 with mixed crystallization into t-HfO2 and c-HfO2, while pure HfO2 is found to be composed of amorphous HfO2 with signs of crystallization into m-HfO2. At 400o C deposition temperature, the crystalline quality is enhanced and the structure of N incorporated HfO2 is found to be c-HfO2 only, due to further ordering of atoms in the crystal lattice. Optical and dielectric characterization revealed films with low N incorporation (&lt; 6 at%) to be insulating while these became conductive for higher N contents. For the insulating films, a trend of increasing static dielectric constant with increasing N incorporation is found.

In this work, we investigate the relation between the diffusion behavior of Ti1-xAlxN at elevated temperatures and the microstructure. Thinfilm samples are synthesized by reactive co-sputtering with two cathodes. One cathode equipped with Ti target is connected to a highpower impulse magnetron sputtering (HiPIMS) power supply, and the other cathode equipped with Al target is operated with a directcurrent power source. The spinodal decomposition of cubic metastable Ti1-xAlxN controlled by thermally activated diffusion is observe fordiffusion behavior. Various HiPIMS pulsing frequencies are used to achieve different microstructure, while altered power applied to Altarget is used to change the Al content in films. In the phase composition analysis achieved by GI-XRD, the right-shift of (111) film peakalong with increasing Al-power is observed. A saturation of the right-shift and h-AlN peaks are also observed at certain Al-power. Thechemical composition determined by ERDA shows trends of reducing Al solubility limit in metastable phase and O contamination upondecreasing the pulsing frequency. More N deficiency is found in samples deposited with higher frequency. In the 500 Hz and 250 Hzsamples deposited into similar composition and thickness, no apparent difference of the microstructure is observed from the SEM crosssectionalimages. From HT-XRD, we observe higher intensity of TiO2 and h-AlN peaks in 500 Hz sample at elevated temperature ascompared with 250 Hz one. From the reduction of O contamination, denser Ti1-xAlxN films are able to be deposited with lower HiPIMSpulsing frequency. In addition, the higher intensity observed in HT-XRD patterns indicates that the 500 Hz sample is more open todiffusion and therefore allows the new formed phases to grow in larger grains.

High power impulse magnetron sputtering (HiPIMS) is a novel pulsed power technique. In HiPIMS, high power pulses are applied to the target for short duration with a low duty factor. It provides a high degree of ionization of the sputtered material (in some cases up to 90%) and a high plasma density (1019 m-3) which results in densification of the grown films. Recently a large side-transport of the sputtered material has been discovered, meaning that the sputtered material is transported radially outwards, parallel to the cathode surface. In this research, we use this effect and study the side-ways deposition of thin films. We designed a new magnetron sputtering system, consisting of two opposing magnetrons with similar polarity. Ti films were grown on Si using the side-ways transport of the sputtered material. Scanning electron microscope was employed to investigate the microstructure of the grown films. Optical emission spectroscopy (OES) measurements were made for investigating the ionized fraction of the sputtered material while Langmuir probe measurements were made for evaluating the plasma parameters such as electron density. The conclusion is that the system works well for side-ways deposition and it can be useful for coating the interior of cylindrically shaped objects. It is a promising technique that should be used in industry.