<p>The object of this thesis is to apply scanning probemicroscopy (SPM) to the field of advanced powder processing.Measurement of interparticle surface forces at conditionsrelevant to ceramic processing has been performed together withthorough studies of powder friction.</p><p>Surface force measurements between silicon nitride andsilica surfaces in 1-bromonaphtalene and diiodomethane resultedin an attractive van der Waals force in both media for thesymmetric systems and a repulsive van der Waals force for theasymmetric systems. This agreed well with theoreticalpredictions from Lifshitz theory. Measurements in electrolytesolutions between silicon nitride surfaces with a varyingdegree of oxidation showed that silanol groups dominated theinteractions at a high degree of oxidation, whereas theinfluence of amine species became stronger after surfaceetching. Surface charge, surface potential and density ofsurface groups have been extracted from DLVO computer modellingof the experimental force curves. Surface force measurementshave been carried out using a nitrided silica sphere as acolloidal probe, representative for commercial silicon nitridepowders. Adsorption of poly(acrylic acid) above the isoelectricpoint generated a thin polymer layer of an essentially flatconformation.</p><p>Friction force measurements were attainable via novelcalibration procedures of both the lateral photodetectorresponse and the cantilever torsional spring constant.Combining the method for detector calibration with evaluationof static friction slopes simplified the choice of appropriatecontact mechanics theory to evaluate the friction measurements.Applying the method on friction measurements between ironsurfaces coated with commercial lubricants showed a substantialsurface deformation not seen from the friction force alone. Thenanorheological properties of silica surfaces coated with twodifferent stearic acids have been evaluated from friction forcemeasurements. Steady sliding motion was replaced by highlyregular stick-slip motion at a critical load and velocity. Thestick-slip motion was successfully described and fitted to aphenomenological model. The contact area evaluated fromMaugis-Dugdale theory revealed the contact diameter to be veryclose to the stick-slip periodicity.</p><p>Friction measurements were carried out between individualspray-dried ceramic granules as a function of binderconcentration and relative humidity. The hygroscopic nature ofthe binder resulted in a higher adhesion force but lowerfriction coefficient with increasing humidity. This effect wasascribed to softening of the binder and a lowering of the shearstrength of the binder rich surface layer on the granules.Comparison of the friction force between two granules and agranule and a hard metal surface confirmed that resistance toflow during the initial stages of powder pressing is dominatedby granule-wall friction and adhesion.</p><p>Keywords: Atomic force microscope, AFM, SPM, van der Waalsinteraction, DLVO-theory, surface forces, colloidal probe,force curve, friction, adhesion, stick-slip, cantilever,calibration, spring constant, silicon nitride, iron,silica.</p>

No description available.

Zr-Si-N thin films were deposited by reactive magnetron sputtering to study silicon influence in the structure, morphology and properties such as hardness and oxidation resistance. Six thin films with silicon concentrations from 2.8 to 14.9 at.% were selected. Thin films morphology shows that there are no columnar grains, structure that is commonly observed in films deposited by sputtering. It was identified amorphous and crystalline areas in films microstructure, creating a structure composed by crystalline grains embedded in an amorphous phase, which were characterized by EDS as Zr and Si rich areas, respectively. XRD results indicate ZrN peaks intensity reduction and a broadening increase due silicon nitride segregation to grain boundaries, which is responsible for grain size reduction, that was calculated by Scherrer and reached magnitudes lower than 10 nm. XRD peaks displacement are observed for all samples and it can be explained due formation of a solid solution in which Si replaces Zr atoms in ZrN crystal lattice and due a strong interface between crystalline phase and amorphous one. XPS data reinforce the presence of compounds like ZrN and Si3N4 and it is also possible to infer the formation of a solid solution of Si in ZrN lattice. Oxidation tests were performed at temperatures in the range of 500°C to 1100°C. ZrN film is almost fully oxidized at 500°C, while films with high silicon content maintain ZrN grains stable at 700°C. When oxidized, ZrN films form monoclinic ZrO2 phase, but, in films with silicon addition, the stable phase is the tetragonal one. This happens due ZrN grain size reduction, because tetragonal phase has the lowest surface energy. Oxidation tests results confirm that there is a mechanism acting as diffusion barrier in films, preventing grains coalescence and oxygen diffusion into film structure. This mechanism is a direct consequence of silicon segregation process to grain boundaries, which ensures the formation of a nanostructure composed of ZrN grains embedded by an amorphous Si3N4 layer (nc-ZrN/a-Si3N4), allowing oxidation resistance improvement in at least 200°C. / Filmes finos de Zr-Si-N foram depositados por magnetron sputerring reativo para estudar a influência do teor de silício na estrutura, morfologia e propriedades como dureza e resistência a oxidação. Para tal, foram selecionados seis filmes com teor de Si entre 2,8 e 14,9 at.%. A morfologia demonstra que a estrutura colunar característica dos filmes depositados por sputtering não existe. A estrutura é composta por áreas cristalinas e outras amorfas, na qual os grãos cristalinos estão envolvidos pela fase amorfa, sendo que EDS detectou que estas fases são ricas em Zr e Si, respectivamente. Há redução de intensidade e alargamento dos picos de difração do ZrN, efeito provocado pela segregação do Si3N4 para região dos contornos, fato que propicia a redução do tamanho de grão, o qual foi calculado por Scherrer e atinge magnitude inferior a 10 nm. Os picos do DRX estão deslocados, fato justificado pela formação de uma solução sólida na qual o Si substituiu o Zr no reticulado do ZrN e pela forte interface formada entre as fases cristalina e amorfa. Dados de XPS reforçam a formação de uma estrutura bifásica de ZrN e Si3N4 e mostra indícios de que há uma solução sólida de Si no ZrN. Os ensaios de oxidação foram realizados em temperaturas de 500°C até 1100°C. O filme de ZrN praticamente se oxida a 500°C, enquanto nos filmes com altos teores de silício os grãos de ZrN se mantém estáveis até 700°C. Quando oxidado, os filmes de ZrN formam predominantemente ZrO2 na fase monoclínica, mas, nos filmes com adição de Si há a inversão para a fase tetragonal. Tal fato é fruto da redução do tamanho de grão, pois a fase tetragonal possui menor energia de superfície. Tais resultados ratificam que existe mecanismo atuando como barreira a difusão, o qual impede a coalescência dos grãos e a difusão do oxigênio. Este mecanismo é resultado do processo de segregação do silício para os contornos, o qual assegura a formação da nanoestrutura composta de grãos de ZrN embebidos por camada amorfa de Si3N4 (nc- ZrN/a-Si3N4) e permite aprimorar a resistência a oxidação em pelo menos 200°C.

This diploma thesis deals with measuring touches problems in industrial metrology. Thesis describes adhesive wear and tear which is caused by measuring probes when dynamical measuring is being concluded. Measuring of damaged component made of silumin and its different changes of texture by different measuring probes are evaluated. Measuring touches are made of titanium nitride, silicon nitride, zirconium, bearing chrome steel, ruby, experimental composite material and nanocrystalline diamond.

This document is final report of an expertise project lead for ALPHA Company. The project focuses on the machinability characterization and comparison of various lamellar cast irons metallurgies. The comparison is performed in order to improve the casting process and the cast irons composition of brake and hub disk, to increase their machinability. The characterization of the metallurgies was made by tool life test with measurements of the cutting forces. Hardness and surface roughness measurements were performed too. Several Silicon nitride tools were tested. First an adjustment test has been performed to validate the machining parameters, and the methodology of characterization. Secondly, a reference test on Alpha’s cast iron brought reference data for the comparison of the various metallurgies to be tested. This test has improved the method of characterization. Cutting forces recording appeared as the most relevant and irrelevant measurements such as surface roughness were eliminated from the method. A test performed on a second cast iron showed that it has a lower machinability. Project succeeded to characterize and compare cast irons’ machinabilities, allowing the improvement of the composition by further tests.

[ES] Esta tesis se ha centrado en el modelado, diseño y demostración experimental de un sensor espectroscópico integrado basado en un AWG (del inglés Arrayed Waveguide Grating). El dispositivo ha sido diseñado y fabricado en una nueva plataforma de nitruro de silico (Si3N4) en oxido de silico (SiO2) desarrollada en España. El trabajo realizado en esta tesis se puede dividir en dos secciones principalmente. En la primera parte, se describe el panorama general de las plataformas de Si3N4 existentes y su estado del arte, junto con la descripción de los procesos de fabricación y caracterización de nuestra plataforma de Si3N4 con 300 nm de altura en la capa de guiado. En la segunda parte, se presenta el dispositivo bautizado como Integrated Optical Spectroscopic Sensor (IOSS). El IOSS consiste en un AWG cuyo conjunto de guías de onda está dividido en dos subgupos diseñados para replicar los canales del AWG. Las guías de uno de los subgrupos contienen ventanas de sensado, que están definidas por secciones en las que el núcleo de las guías está al descubierto y, por tanto, en contacto con el medio que las rodea. De esta manera, el sensado se lleva a cabo mediante la interacción del campo evanescente con la muestra depositada. Las guías del segundo subconjunto permanecen inalteradas. Por lo tanto, el dispositivo proporciona al mismo tiempo los espectros de sensado y de referencia. El modelo matemático del IOSS, su procedimiento de diseño y la prueba de concepto del sensor configurado para espectroscopía de absorción se describen en esta tesis. / [CAT] La present tesi s'ha centrat en el modelatge, disseny i demostració experimental d'un sensor espectroscòpic integrat basat en un AWG (de l'anglès Arrayed Waveguide Grating). El dispositiu ha sigut dissenyat i fabricat en una nova plataforma de nitrur de silici (Si3N4) en òxid de silici (SiO2) desenvolupada a Espanya. El treball realitzat en aquesta tesi es pot dividir en dues seccions principalment. En la primera part, es descriu el panorama general de les plataformes de Si3N4 existents i el seu estat de l'art, juntament amb la descripció dels processos de fabricació i caracterització de la nostra plataforma de Si3N4 amb 300 nm d'altura en la capa de guiat. En la segona part, es presenta el dispositiu batejat com Integrated Optical Spectroscopic Sensor (IOSS). El IOSS consisteix en un AWG en el que el seu conjunt de guies d'ona està dividit en dos subgrups dissenyats per a replicar els canals del AWG. Les guies d'un dels subgrups conté finestres de detecció, que estan definides per seccions en les quals el nucli de les guies d'ona està al descobert i en contacte amb el mitjà que li envolta. D'aquesta manera, la detecció es duu a terme mitjançant la interacció del camp evanescent amb la mostra depositada. Les guies del segon subconjunt romanen inalterades. Per tant, el dispositiu proporciona al mateix temps els espectres de detecció de referència. El model matemàtic del IOSS, el seu procediment de disseny i la prova de concepte del sensor configurat per a espectroscopia d'absorció es descriuen en aquesta tesi. / [EN] This thesis is focused on the model, design and experimental demonstration of an integrated spectroscopic sensor based on a modified Arrayed Waveguide Grating (AWG). The device has been designed and fabricated in a new silicon nitride (Si3N4) on silicon oxide (SiO2) platform developed in Spain. The work performed for this thesis can be then divided into two main sections. In the first part, an overview of the existing Si3N4 platforms and their state of art is described, alongside the report on the fabrication and characterization of our 300 nm guiding film height Si3N4 platform. On the second part, the device named Integrated Optical Spectroscopic Sensor (IOSS) is presented. The IOSS consists of an AWG which arrayed waveguides are divided into two sub-sets engineered to replicate the AWG channels. The waveguides of one of the sub-sets contain sensing windows, defined as waveguides sections which core is in contact with the surrounding media. Thus, the sensing is performed through evanescent field interaction with the sample deposited. The waveguides from the second sub-set remain isolated. Therefore, the device provides both sensing and reference spectra. The IOSS mathematical model, design procedure and proof of concept configured for absorption spectroscopy are reported in this thesis. / Micó Cabanes, G. (2020). Integrated Spectroscopic Sensor fabricated in a novel Si3N4 platform [Tesis doctoral]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/159381

[ES] Esta tesis aborda la caracterización de circuitos fotónicos integrados (PIC) usando interferometría óptica en el domino de las frecuencias (OFDI). OFDI tiene una implementación razonablemente simple e interroga al dispositivo bajo test (DUT) proporcionando su respuesta en el dominio del tiempo, en la que los distintos caminos ópticos seguidos por la luz se manifiestan en contribuciones que contienen información de posición, amplitud y fase. Junto con un "setup" OFDI construido en nuestros laboratorios y estructuras de test integradas que involucran anillos resonantes, interferómetros, etc., proponemos e implementamos técnicas para obtener parámetros ópticos cruciales tales como el índice de grupo, dispersión cromática, rotación de polarización y pérdidas de propagación en guías de onda. También para caracterizar acopladores ópticos. Se realizan evaluaciones directas de fase óptica en diferentes experimentos para, entre otras aplicaciones, caracterizar efectos de calor en chips. En la culminación de la tesis, se aborda la integración conjunta de los interferómetros de OFDI junto con el DUT, concibiéndolo como una estructura de caracterización integrada. El uso de guías de onda integradas proporciona una alta estabilidad y adaptación al DUT, además de un mecanismo inherente de compensación de la dispersión. Se realiza un análisis y prueba de concepto experimental caracterizando un "arrayed waveguide grating" en tecnología de nitruro de silicio. Seguidamente, se da un paso adelante proponiendo una arquitectura interferométrica de tres brazos novedosa que permite reducir la complejidad de la medida. Se lleva a cabo una validación experimental amplia usando distintos equipos de laboratorio, acoplamiento horizontal y vertical al chip, y diferentes DUTs en tecnologías de nitruro de silicio y "silicon-on-insulator". / [CAT] Aquesta tesi aborda la caracterització de circuits fotònics integrats (PIC) usant interferometria òptica al domini de les freqüències (OFDI). OFDI té una implementació raonablement simple i interroga el dispositiu sota test (DUT) proporcionant la seva resposta en el domini del temps, en què els diferents camins òptics seguits per la llum es manifesten en contribucions que contenen informació de posició, amplitud i fase. Juntament amb un "setup" OFDI construït als nostres laboratoris i estructures de test integrades que involucren anells ressonants, interferòmetres, etc., proposem i implementem tècniques per obtenir paràmetres òptics crucials com ara l'índex de grup, dispersió cromàtica, rotació de polarització i pèrdues de propagació en guies d'ona. També per caracteritzar acobladors òptics. Es fan avaluacions directes de fase òptica en diferents experiments per, entre altres aplicacions, caracteritzar efectes de calor en xips. A la culminació de la tesi, s'aborda la integració conjunta dels interferòmetres d'OFDI juntament amb el DUT, concebent-ho com una estructura de caracterització integrada. L'ús de guies d'ona integrades proporciona una alta estabilitat i adaptació al DUT, a més d'un mecanisme inherent de compensació de la dispersió. Es realitza una anàlisi i prova de concepte experimental caracteritzant un "arrayed waveguide grating" en tecnologia de nitrur de silici. Seguidament, es fa un pas avant proposant una arquitectura interferomètrica de tres braços nova que permet reduir la complexitat de la mesura. Es du a terme una validació experimental àmplia usant diferents equips de laboratori, acoblament horitzontal i vertical al xip, i diferents DUTs en tecnologies de nitrur de silici i "silicon-on-insulator". / [EN] This PhD thesis covers the characterization of complex photonic integrated circuits (PIC) by using Optical Frequency Domain Interferometry (OFDI). OFDI has a fairly simple implementation and interrogates the device under test (DUT) providing its time domain response, in which the different optical paths followed by light manifest in contributions with position, amplitude and phase information. Together with a working OFDI setup built in our laboratory and integrated test structures involving devices such as ring resonators, interferometers, etc., we propose and implement techniques to get crucial optical parameters such as waveguide group refractive index, chromatic dispersion, polarization rotation, and propagation loss. Also, to characterize optical couplers. Direct optical phase assessment is made in different experiments permitting, amongst others, the characterization of on-chip heat effects. In the culmination of the thesis, the co-integration of the OFDI interferometers with the DUT is addressed, conceiving it as an integrated characterization structure. The use of integrated waveguides provide high stability and adaptation to the DUT, as well as an inherent dispersion de-embedding mechanism. It is provided analysis and experimental proof of concept with an arrayed waveguide grating as DUT in a silicon nitride platform. A considerable leap forward is then taken by proposing a novel three-way interferometer architecture, reducing the measurement complexity. Wide experimental validation is carried out using different laboratory equipment, horizontal and vertical chip coupling, and different DUTs in silicon nitride and silicon-on-insulator. / Bru Orgiles, LA. (2022). Optical Frequency Domain Interferometry for the Characterization and Development of Complex and Tunable Photonic Integrated Circuits [Tesis doctoral]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/181635

Es wird eine Alternative zum Ätzen von Siliciumnitrid (SiNx) auf Silicium-Wafern vorgestellt. Herkömmliche Verfahren zum Ätzen von SiNx auf Silicium-Wafern arbeiten mit Flusssäure oder Phosphorsäure. Zu diesen Chemikalien werden alternative organische Komplexbildner zum Ätzen von SiNx vorgestellt, welche im Gegensatz zu den herkömmlichen Substanzen weniger giftig und umweltschädlich sind. Bei den organischen Komplexbildnern handelt es sich um die Stoffgruppen der Hydroxycarbonsäuren und Aminosäuren. Für diese Substanzen wurden die ersten wichtigen Parameter für einen Einsatz in der Halbleiterindustrie untersucht. Dabei handelt es sich um Einflüsse durch die Herstellungsprozesse des SiNx selbst, des pH-Wertes, der chemischen Struktur des organischen Komplexbildners und die Konzentrations- und Temperaturabhängigkeit. Es werden für die Reaktion auch die ersten Reaktionsmechanismen postuliert.:1 Einleitung...................... 1 1.1 NachhaltigkeitinderHalbleiterindustrie................. 2 1.2 Nasschemische Ätzmethoden für Siliciumnitrid (SiNx).......... 5 1.3 ZieledieserForschungsarbeit........................ 9 2 Material und Methoden 11 2.1 Probenkörper ................................ 11 2.2 Ätzversuche ................................. 12 2.3 Charakterisierung.............................. 15 3 Ätzmittel für SiNx 25 3.1 Chemischer Aufbau von organischen Komplexbildnern für Siliciumnitrid.... 25 3.2 UntersuchungderMorphologie....................... 25 3.3 XPS-AnalysederOberfläche........................ 33 3.4 WirksameGruppen............................. 35 4 Methodenentwicklung zur Bestimmung von Ätzraten, Selektivität und Isotropie.... 37 4.1 Ätzrate.................................... 37 4.2 Selektivität................................. 39 4.3 Methoden zur Bestimmung der Schichtdickendifferenz .......... 43 4.4 Fehlerbetrachtung und Zusammenfassung der Methoden........ 46 4.5 Zusammenfassung der Messmethoden................... 51 5 Parameter mit Einfluss auf den Ätzprozess 53 5.1 Einfluss des Herstellungsprozesses..................... 53 5.2 Einfluss des pH-Wertes auf den SiNx-Abbau ................... 55 5.3 Einfluss von Wasser auf die Reaktion ................... 56 5.4 Einfluss der Struktur ............................ 57 5.5 Konzentrations- und Temperaturabhängigkeit der Ätzrate von Ätzmitteln 60 5.6 Untersuchung des kinetischen Verlaufs der Reaktion . . . . . . . . . . . 69 5.7 Untersuchung der Isotropie......................... 72 6 Postulierte Reaktionsmechanismen 77 6.1 Abbau des Stickstoffs aus der SiNx-Oberfläche . . . . . . . . . . . . . . 77 6.2 Abbau des Si aus der SiNx-Oberfläche................... 78 6.3 Milchsäure als Katalysator zum Abbau von elementarem Si . . . . . . . 80 6.4 NMR-Analyse................................ 82 7 Zusammenfassung und Ausblick 87 7.1 Zusammenfassung.............................. 87 7.2 Ausblick................................... 89 6.5 Ergebniszusammenfassung der postulierten Reaktionsmechanismen . . . 86

<p dir="ltr">This thesis is about the exciting discovery of a new kind of single photon emitter that<br>is suspected to occur at the interface of silicon nitride SixNy and silicon dioxide SiO2 after<br>being rapidly annealed. Since SixNy is one of the most developed platforms for integrated<br>photonics the discovery of a native emitter in this platform opened up the possibility for<br>seamless integration of these single photon emitters with photonic circuitry for the first<br>time. This seamless integration was demonstrated as is shown in Chapter 3 by creating the<br>emitters and then patterning the SixNy layer into a waveguide. This work demonstrated for<br>the first time the coupling of such single photon emitters with on-chip integrated photonics.<br>However, the integration approach demonstrated was based on the stochastic integration of<br>emitters which limits the efficiency of the devices and the possible types of devices that can<br>be designed. This is why the next stage of research focused on the development of a site-<br>controlled process for creating these single photon emitters. Remarkably, it was found that<br>if the SixNy and SiO2 are nanostructured into nanopillars and then annealed then a single<br>photon emitter forms over 65% of the time within the nanopillar! Due to the lithography<br>defined nature of this process for creating the single photon emitters the first multi-mask<br>integration process was also developed and demonstrated. This fabrication process was used<br>to demonstrate the integration of several thousand single photon emitters with complex<br>integrated photonic structures such as topology optimized couplers. These developments<br>has generated a great deal of excitement due to the inherent scalability of the approach and<br>it’s obvious applications for the development of very large scale integrated (VLSI) on-chip<br>quantum photonic systems.</p>

This thesis deals with the analysis of nano-structured layers deposited by high-frequency magnetron sputtering on the monocrystalline silicon surface. The content of the work focuses on the magnetron sputtering application as an alternative method for passivation and antireflection layers deposition of silicon solar cells. The procedure of pre-deposite silicon surface cleaning by plasma etching in the Ar/H2 gas mixture atmosphere is suggested. In the next step the silicon nitride and aluminum nitride layers with hydrogen content in Ar/N2/H2 gas mixture by magnetron sputtering are deposited. One part of the thesis describes an experimental pseudo-carbide films deposition from a silicon target in the atmosphere of acetylene (C2H2). An emphasis is placed on the research of sputtered layers properties and on the conditions on the silicon-layer interface with the help of the standard as well as special measurement methods. Sputtered layers structure is analyzed by modern X-ray spectroscopy (XPS) and by Fourier infrared spectroscopy (FTIR). Optical ellipsometry and spectrophotometry is used for the diagnostic of the layers optical properties depending upon the wavelength of incident light. A special method of determining the surface lay-out of the charge´s carrier life in the volume and on the surface of silicon is employed to investigate the passivating effects of the sputtered layers.