In this master thesis, performed at Sandvik Coromant Västberga (Stockholm), a comprehensive study has been made to investigate the wear on textured alumina (Inveio™) coated cutting tools when turning low-alloy steels. Specifically, wear studies have been made on tools’ rake faces when turning two separate batches of SS2541, after an initial turning time of 4 min. A particular focus has been given to elucidate what particular role the inclusions might have for the wear of the alumina coating onthe tools. Evaluation of tool wear has been made by employing several different analytical techniques, such as LOM, SEM, Wyko, Auger-spectrometry (AES), EPMA and XRD. The results shows that the arisen wear marks on both tested tool types may be divided into three separate and highly distinguishable wear zones, denoted here in thiswork as “wear bands”. Largest amount of wear tended to occur initially at the topmost part of the 3rd wear band. This was true for both tested tool types. This area demonstrated a characteristic 'lamellar' wear pattern, composed of narrow andstructured ridges. All the tools tested demonstrated the adhesion of workpiece materials of various composition that formed into smeared layers in these formed ridges. Depth-profiling Auger-spectrometry revealed that a significant amount of calcium was present in the machined alumina coating layers. This suggests that a reaction between the calcium-containing inclusions found in the steel and the aluminacoating layer had occurred during the performed turning tests.These results arecontradictory to the general belief that alumina is chemical inert during machiningand has previously, to the authors knowledge, not yet been published. Based on the results from this thesis and from a literature review concerning thebehavior of α-alumina during deformation, a new theoretical wear model has been developed. In this model, it is emphasised that the sliding of hard inclusions from the steel may activate pyramidal slip systems in the textured alumina coating. This causes a nano-crystallisation and/or amorphisation in the topmost part of the coating, which facilitates the further wear of these coated tools. / I detta examensarbete, som har utförts vid Sandvik Coromant i Västberga (Stockholm), har en omfattande studie gjorts i syfte att undersöka slitaget på texturerad aluminiumoxid-belagda skärverktyg (Inveio™) vid svarvningen av låglegerade stålsorter. Förslitningsstudier har framförallt gjorts på verktygens spånsidor vid svarvningen av två separata batcher av stålsorten SS2541 efter en inledande ingreppstid på 4 min. Ett särskilt fokus har även ägnats åt att belysa vilken roll stålets inneslutningar kan ha för slitaget av aluminiumoxidbeläggningen. Utvärderingen av verktygsslitaget har gjorts med hjälp av flera olika analytiska tekniker, däribland LOM, SEM, Wyko, Auger-spektrometri (AES), EPMA samt XRD. Resultaten från detta examensarbete visar på att det uppkomna slitaget på de verktyg som har testats kan uppdelas till tre separata och mycket distinkta ”slitagezoner”. Dessa zoner har för detta arbete benämnts som ”nötningsband”. Störst förslitning framträdde initialt i den översta delen av det 3:e nötningsbandet på de testade skärverktygen. Detta område uppvisade ett karaktäristiskt ”lamell”-liknande utseende, bestående av smala och strukturerade åsar och skåror. Vidare uppvisade samtliga undersökta verktyg på förekomsten av påsmetat arbetsmaterial av varierande sammansättning i dessa bildade åsar. När de slitna verktygen undersöktes med djuprofilerande Auger-spektrometri påvisades det att en signifikant mängd kalcium fanns inuti aluminiumoxidbeläggningen. Detta tyder på att en reaktion mellan de kalciuminnehållande inneslutningarna (som finns inuti stålet) och aluminiumoxidbeläggningen har reagerat med varandra under bearbetningsförloppet. Dessa resultat är motsägande till den allmänna uppfattningen om att aluminiumoxid är kemiskt inert vid bearbetningen av stål. Därutöver har dessa resultat även, till författarens kännedom, aldrig tidigare publicerats. Baserat på de resultat som har erhållits från detta examensarbete, och från en omfattande litteraturstudie gällande deformationen av α-aluminiumoxid, har en ny teoretisk förslitningsmodell utarbetats. I denna modell betonas det särskilt att glidningen av hårda inneslutningar från stålet kan aktivera s.k. pyramidala glidsystem i den texturerade aluminiumoxidbeläggningen. Detta orsaker en nano-kristallisering och/eller amorfisering av den översta delen av aluminiumoxidbeläggningen.  Denna omvandling tros kunna underlätta den fortsatta förslitningen av dessa belagda skärverktyg.

High voltage rotating machines play a significant role in generation and use of electrical energy as the demand for power continues to increase. However, one of the main causes for down times in high voltage rotating machines is related to problems with the winding insulation. The utilities want to reduce costs through longer maintenance intervals and a higher lifetime of the machines. These demands create a challenge for the producers of winding insulations, the manufacturers of high voltage rotating machines and the utilities to develop new insulation materials which can improve the life of the equipment and reduce the maintenance cost. The advent of nanotechnology in recent times has heralded a new era in materials technology by creating opportunities to significantly enhance the properties of existing conventional materials. Polymer nanocomposites belong to one such class of materials that exhibit unique combinations of physical, mechanical and thermal properties which are advantageous as compared to the traditional polymers or their composites. Even though they show tremendous promise for dielectric/electrical insulation applications, there are no studies relating to the long term performance as well as life estimation of the nanocomposites. Considering this, an attempt is made to generate an understanding on the feasibility of these nanocomposites for electrical insulation applications. An epoxy based nanocomposite system is chosen for this study along with alumina (Al2O3) and silica (SiO2) as the nanofillers. The first and the foremost requirement for studies on polymer nanocomposites is to achieve a uniform dispersion of nanoparticles in the polymer matrix, as nanoparticles are known to agglomerate and form large particle sizes. A laboratory based direct dispersion method is used to process epoxy nanocomposites in order to get well dispersed samples. A detailed microscopy analysis of the filler dispersion using Scanning Electron Microscope (SEM) has been carried out to check the dispersion of the nanofiller in the polymer. An attempt is made to characterize and analyze the interaction dynamics at the interface regions in the epoxy nanocomposite by glass transition temperature (Tg) measurements and Fourier transform infrared (FTIR) spectroscopy studies. The values of Tg for the nanocomposites studied decreases at 0.1 wt% filler loading and then starts to increase gradually with increase in filler loading. This Tg variation suggests that there is certainly an interaction between the epoxy chains and the nanoparticles. Also no new chemical bonds were observed in the spectra of epoxy nanocomposite as compared to unfilled epoxy. But changes were observed in the peak intensity and width of the –OH band in the spectrum of epoxy nanocomposite. This change was due to the formation of the hydrogen bonding between the epoxy and the nanofiller. The thermal conductivity of the epoxy alumina and the epoxy silica nanocomposites increased even with the addition of 0.1 wt% of the filler. This increase in thermal conductivity is one of the factors that make these nanocomposites a better option for electrical insulation applications. The dielectric properties of epoxy nanocomposites obtained in this investigation also reveal few interesting behaviors which are found to be unique and advantageous as compared to similar properties of unfilled materials. It is observed that the addition of fillers of certain loadings of nanoparticles to epoxy results in the nanocomposite permittivity value to be lower than that of the unfilled epoxy over the entire range of frequencies [10-2-106 Hz] considered in this study. This reduction has been attributed to the inhibition of polymer chain mobility caused by the addition of the nanoparticles. The tan values are almost the same or lower as compared to the unfilled epoxy for the different filler loadings considered. This behavior is probably due to the influence of the interface as the strong bonding at the interface will make the interface very stable with fewer defects apart from acting as charge trapping centres. From a practical application point of view, the surface discharge resistant characteristics of the materials are very important and this property has also been evaluated. The resistance to surface discharge is measured in the form of roughness on the surface of the material caused by the discharges. A significant enhancement in the discharge resistance has been observed for nanocomposites as compared to unfilled epoxy/ microcomposites, especially at longer exposure durations. The partial discharge (PD) measurements were carried out at regular intervals of time and it is observed that the PD magnitude reduced with discharge duration in the case of epoxy alumina nanocomposites. An attempt was made to understand the chemical changes on the surface by conducting the FTIR studies on the aged surface. For all electrical insulation applications, materials having higher values of dielectric strengths are always desired and necessary. So AC breakdown studies have also been conducted. The AC breakdown strength shows a decreasing trend up to a certain filler loading and then an increase at 5 wt% filler loading for epoxy alumina nanocomposites. It has been also observed that the type of filler as well as the thickness of the filler influences the breakdown strength. The AC dielectric strength of microcomposites are observed to be lower than the nanocomposites. Extensive research by long term aging studies and life estimation are needed before these new nanocomposites can be put into useful service. So long term aging studies under combined electrical and thermal stresses have been carried out on unfilled epoxy and epoxy alumina nanocomposite samples of filler loading 5 wt%. The important dielectric parameters like pemittivity, tan  and volume resistivity were measured before and after aging to understand the performance of the material under study. The leakage current was measured at regular intervals and tan  values were calculated with duration of aging. It was observed that the tan  values increased drastically for unfilled epoxy for the aging duration considered as compared to epoxy alumina nanocomposites. The life estimation of unfilled epoxy as well as epoxy nanocomposites were also performed by subjecting the samples to different stress levels of 6 kV/mm, 7 kV/mm and 8 kV/mm at 60 oC. It is observed that the epoxy alumina nanocomposite has an enhanced life which is nine times the life of the unfilled epoxy. These results obtained for the nanocomposites enable us to design a better material with improved dielectric strength, dielectric properties, thermal conductivity, resistance to surface discharge degradation and enhanced life without sacrificing the flexibility in the end product and the ease of processing. Dry type transformers and stator winding insulation need to be cast with the above material developed and tested before practically implementing these in the actual application.

Les potentialités du nitrure de gallium (GaN) et notamment de l'hétérostructure AlGaN/GaN, semiconducteur à large bande interdite, en font un matériau particulièrement intéressant en électronique de puissance, notamment pour des applications haute tension, haute température et haute fréquence. L'objectif de ce travail de thèse était de développer et d'optimiser l'étape d'isolation de la grille lors la réalisation de transistors MIS-HEMT de puissance sur hétérostructure AlGaN/GaN, le but étant de réduire les courants de fuite de grille sans perturber les propriétés du transistor. Après avoir évaluation, le choix s'est porté sur l'alumine Al2O3 déposé par ALD comme diélectrique de grille. L'étude s'est d'abord concentrée sur l'analyse de l'influence de traitements, chimiques ou plasma, sur la contamination de la surface d'AlGaN au travers d'analyses XPS et AFM. Puis, l'influence du diélectrique de grille a été évalué à travers la réalisation et la mesure électrique de dispositifs, diodes et transistors, en variant les méthodes de dépôt par ALD. Enfin, l'impact d'un recess par gravure ICP-RIE partielle ou complètes de la barrière d'AlGaN sous la grille a été étudiée. La réalisation d'un HEMT passe par l'étape critique du dépôt du diélectrique de grille sur le semiconducteur, et le contrôle de la qualité de l'interface " diélectrique/AlGaN " est donc une étape fondamentale car elle influe sur les propriétés électriques du composant. Ce contrôle comprend le traitement de surface du semiconducteur, mais aussi la nature et la technique de dépôt du diélectrique. Ainsi il apparaît à travers l'étude qu'un traitement de surface à l'ammoniaque à haute température est le plus efficaces pour retirer les contamination en oxydes natifs. Les mesures électriques, C(V) et Id(Vg), ont quant à elle montrés la supériorité de la PEALD par rapport à un dépôt thermique conventionnel. Ceci peut s'expliquer par le fait que le plasma oxygène qui entre jeu lors du dépôt de l'alumine par PEALD semble nettoyer la surface lors des premiers cycles, retirant notamment la contamination carbone. Cela permet d'avoir une meilleure interface entre l'alumine et le semi-conducteur, limitant les pièges à l'interface et dans l'oxyde. Cela a réduit de manière considérable les courants de fuite de grille, sans détériorer la qualité et la rapidité de la transition entre l'état on et off. De plus, les HEMTs réalisé étant de type normally-off, le recess de grille par gravure ICP-RIE a été implémenté afin de rendre moins négative la tension de pincement. Cela a été réalisé avec succès, notamment avec la réalisation d'un composant de type noramlly-off grâce à un recess total de la barrière d'AlGaN sous la grille. Des résultats à l'état de l'art ont été obtenus à travers une approche simple, et un processus de création de transistors robuste et hautement reproductible, avec une réduction importante des courants de fuite de grille et une pente sous le seuil record. Afin de compléter l'étude il conviendra par la suite de réaliser des études de fiabilité, notamment à travers des mesures dynamiques pour évaluer notamment les phénomènes de dégradation du Ron. / With its large band gap, Gallium Nitride (GaN) semiconductor is one of the most promising materials for new power devices generation thanks to its outstanding material properties for high voltage, temperature and frequency applications. The main objective of this thesis was the development and optimization of the insulating step taking place in the elaboration of MIS-HEMT transistors on an AlGaN/GaN heterstroctructure. In order to reduce gate leakage currents without degrading the device properties, alumina Al2O3 deposited by ALD was chosen as a gate dielectric. The study was first centered on the influence of surface treatments, chemical or plasma, regarding surface contamination. Their impact was analyzed through XPS and AFM. Secondly, electrical measures were performed on complete MIS-HEMT diodes and transistors to evaluate the influence of the alumina insulating layer depending on the ALD deposition method. Lastly, partial and full recess of the AlGaN barrier was studied via ICP-RIE etching. The gate dielectric deposition is one of the crucial steps intervening in the HEMT creation process. The quality and control at the Al2O2/AlGaN interface being paramount, it will directly influence the device's electric properties. This involves control ing the semiconductor surface, but also the nature and deposition technique of the dielectric. As such, an ammonia-based treatment at high temperature appears to be the most efficient in reducing native oxygen contamination. Regarding electric performances, C(V) and Id(Vg) measures showed the superiority of PEALD compared to traditional thermal ALD deposition. This can be explained by the fact that the oxygen plasma used as oxydant during the alumina deposition by PEALD seems to clean the surface during the first cycles, mostly by reducing carbon contamination. This allowed to achieve a better interface between the semiconductor and the insulting layer, thus limiting traps at the interface or in the oxyde. This allows to considerably reduce gate leakage currents, without degrading the quality and transition sharpness between the on and off state. Moreover, the realized HEMTs being normally-off, gate recess etching via ICP-RIE was implemented in order to make the threshold voltage less negative. This was successfully achieved, especially through the realization of a normally-off transistors thanks to a full recess of the AlGaN barrier under the gate. State of the art results were achieved through a simple approach, and a robust and highly reproducible transistor elaboration process, with great reduction of gate leakage currents and a record sub-threshold slope. In order to complete the study, it will be necessary in the future to proceed to viability studies, especially through dynamic electric evaluation, in order to evaluate for instance Ron degradation phenomenons.

Aluminiumschichten werden durch Kaltgasspritzen auf fünf verschiedene poly- und monokristalline keramische Werkstoffe (Al2O3 , AlN, SiC, Si3N4 , MgF2 ) appliziert. Dabei erfolgt eine Variation der Substrattemperatur und der Partikelgröße. Ausgewählte Proben werden einer nachfolgenden Wärmebehandlung unterzogen. Die im Fokus der Arbeit stehende Erforschung der an der Grenzfläche zwischen Aluminium und Keramik wirkenden Haftmechanismen erfolgt sowohl mithilfe einer mechanischen Charakterisierung (Stirnzugversuche) als auch durch verschiedene mikroskopische, spektroskopische und hochauflösende Methoden. Die Bewertung der Untersuchungsergebnisse zeigt, dass im Allgemeinen ein Anstieg der Haftzugfestigkeit mit steigender Substrat- und Wärmebehandlungstemperatur sowie mit zunehmender thermischer Effusivität des Substratwerkstoffs zu verzeichnen ist. Eine vergleichbare Auswirkung hat innerhalb bestimmter Grenzen die Zunahme der Partikelgröße. Mit der Heteroepitaxie wird neben der mechanischen Verklammerung ein weiterer wichtiger Haftmechanismus kaltgasgespritzter metallischer Schichten auf keramischen Substraten identifiziert. Die Ausbildung von quasiadiabatischen Scherbändern und statische Rekristallisationsprozesse wirken dabei als wichtige begleitende Mechanismen. Als Nachweis für heteroepitaktisches Wachstum ist die Existenz von (annähernd) parallelen, senkrecht oder geneigt zur Grenzfläche stehenden Ebenenpaaren, die eine geringe Gitterfehlanpassung aufweisen, zu werten. Der Vergleich mit PVD-Schichten zeigt, dass in Bezug auf die Orientierung von Gitterebenen verschiedene Mechanismen der Heteroepitaxie existieren, die von der atomaren Mobilität des Beschichtungswerkstoffs bestimmt werden.

Aluminiumschichten werden durch Kaltgasspritzen auf fünf verschiedene poly- und monokristalline keramische Werkstoffe (Al2O3 , AlN, SiC, Si3N4 , MgF2 ) appliziert. Dabei erfolgt eine Variation der Substrattemperatur und der Partikelgröße. Ausgewählte Proben werden einer nachfolgenden Wärmebehandlung unterzogen. Die im Fokus der Arbeit stehende Erforschung der an der Grenzfläche zwischen Aluminium und Keramik wirkenden Haftmechanismen erfolgt sowohl mithilfe einer mechanischen Charakterisierung (Stirnzugversuche) als auch durch verschiedene mikroskopische, spektroskopische und hochauflösende Methoden. Die Bewertung der Untersuchungsergebnisse zeigt, dass im Allgemeinen ein Anstieg der Haftzugfestigkeit mit steigender Substrat- und Wärmebehandlungstemperatur sowie mit zunehmender thermischer Effusivität des Substratwerkstoffs zu verzeichnen ist. Eine vergleichbare Auswirkung hat innerhalb bestimmter Grenzen die Zunahme der Partikelgröße. Mit der Heteroepitaxie wird neben der mechanischen Verklammerung ein weiterer wichtiger Haftmechanismus kaltgasgespritzter metallischer Schichten auf keramischen Substraten identifiziert. Die Ausbildung von quasiadiabatischen Scherbändern und statische Rekristallisationsprozesse wirken dabei als wichtige begleitende Mechanismen. Als Nachweis für heteroepitaktisches Wachstum ist die Existenz von (annähernd) parallelen, senkrecht oder geneigt zur Grenzfläche stehenden Ebenenpaaren, die eine geringe Gitterfehlanpassung aufweisen, zu werten. Der Vergleich mit PVD-Schichten zeigt, dass in Bezug auf die Orientierung von Gitterebenen verschiedene Mechanismen der Heteroepitaxie existieren, die von der atomaren Mobilität des Beschichtungswerkstoffs bestimmt werden.