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The goal for this project was to analyze and understand the noise of the ion beam analysis technique, Elastic Recoil Detection Analysis (ERDA). This was done by examining two models: Classical models and a prediction model. The prediction model is a parameterized noise distribution model. After examining the models, we concluded that both models had advantages and disadvantages for ERDA analysis. This information could be applicable to our understanding of how ERDA could improve for our analysis of wall materials, which could lead to the overall development of fusion reactors. / Målet för detta projekt var att analysera och förstå brus från jonstråleanalystekniken, Elastic Recoil Detection Analysis (ERDA). Detta gjordes genom att granska två modeller: Klassiska brusreduceringsmodeller och en förutsägelsemodell. Förutsägelsemodellen är en parametrerad brusfördelningsmodell. Efter granskningen av modellerna drog vi slutsatsen att båda modellerna hade fördelar och nackdelar för ERDA-analys. Denna information kan vara tillämplig på vår förståelse av hur ERDA kan förbättras för vår analys av väggmaterial, vilket kan leda till den övergripande utvecklingen av fusionsreaktorer. / Kandidatexjobb i elektroteknik 2021, KTH, Stockholm

Human bone tissue has an inherent hierarchical structure, which is integral to its material properties. It is primarily composed of a collagen fiber matrix that is mineralized with hydroxyapatite. A comprehensive understanding of bone and the linkages between structural and cellular organization is imperative to developing fundamental knowledge that can be applied to better our understanding of bone disease manifestations and its interaction with implant devices. Herein, this thesis investigated non-traditional methods for evaluating bone structure across the nano- and meso-length scales. Firstly, due to the inhomogeneous organization of collagen fibrils and mineral platelets of bone ultrastructure, a suitable methodology for the investigation of both phases needed to be generated. In this work, focused ion beam (FIB) microscopy was employed to create site-specific scanning transmission electron microscopy (STEM) lift-outs of human osteonal bone that could be visualized with correlatively with STEM and small angle X-ray scattering (SAXS). Samples were successfully characterized using both techniques, and minimal visual damage was induced during data acquisition. This work is the first to demonstrate the potential for bone to be investigated correlatively using both STEM and SAXS. Secondly, this work is the first to employ a dual-beam plasma FIB (PFIB) equipped with a scanning electron microscope (SEM), to investigate bone tissue across the mesoscale. This equipment enables large volume three-dimensional (3D) imaging at nanoscale resolution across larger mesoscale volumes. This thesis aimed to reduce ion beam-based artifacts, which presents as curtain-like features by adjusting the composition of protective capping layers. Subsequently, large volume tomograms of bone tissue were acquired, demonstrating the effectiveness of the PFIB to reveal mesoscale features including the cellular network of bone tissue. Overall, this thesis has developed methods that allow for the application of advanced microscopy techniques to enhance the understanding of bone tissue across the nanoscale and mesoscale. / Thesis / Master of Applied Science (MASc) / Bone tissue has a unique structure that perplexes both biologists and materials scientists. The hierarchical structure of bone has garnered the interest of materials scientists since the body’s skeletal strength and toughness are governed by the nanoscale (millionth of centimetres) to macroscale (centimeters) organization of bone. In this work, the intricate organization of bone is investigated using advanced electron and ion beam microscopy techniques, which achieve high-resolution imaging of bone structure. Firstly, this work developed a sample preparation workflow to correlate electron and X-ray imaging of the same bone tissue. Secondly, this work was the first to apply serial-sectioning plasma focused ion beam tomography to human bone tissue to investigate its structure at high resolution across micron-sized volumes. Here, previously unexplored methodologies to image bone are demonstrated with the hopes of applying such techniques to investigate healthy and pathological bone tissue in the future.

The broad theme of the present research investigation is on the preparation and characterization of the ultra thin films. The emerging field of nano science and technology demands the realization of different materials in nanometer dimension and a comprehensive understanding of their novel properties. Especially, the properties of the semiconducting materials in the nano dimensions are quite different from their bulk phase. A phase transition from semimetalic to semiconducting nature occurs at a thickness < 5nm of Sb ultra thin films. These facts emphasize the need for preparing these materials as nano layers and studying their properties as a function their size. Among the various characterization methods available to study the structure and the interfaces, Raman spectroscopy has proved to be a useful technique. In addition to revealing the structural information, Raman spectroscopy can bring out the quantum size effects in the lattice vibrational spectra of lower dimensional solids, stress state of the film in the initial growth stages, chemical nature of materials etc. Raman spectroscopy studies on the quantum structure of Ge and Sb are limited. This is attributed to the two serious limitations of the conventional backscattering of Raman signal. 1. The back scattered Raman signal intensity from the ultra thin layer could be below the detection limit. 2. The lower penetration depth of the lasers could inhibit the information from the buried layers. These limitations could be overcome to a major extent by employing an optical interference technique called IERS. This is basically an anti-reflection structure consisting minimum of three layers. These three layers are essential for achieving the interference conditions. The thicknesses of each layer were calculated using a matrix method. IERS structure consists of 1. A reflecting layer at the bottom of the stack (Platinum or Aluminum) 2. The second layer which is grown above the reflecting layer is a transparent dielectric layer, which introduces the necessary phase shift and hence it is called phase layer.(SiO2 or CeO2) 3. The top ultra thin layer which is to be investigated (Ge or Sb), is grown over the dielectric film and it is the layer which absorbs the most of the incident exciting light and it is called the absorbing layer. In this trilayer structure the thickness of the phase layer and the absorbing layer are adjusted in such a way that the light reflected from the air-ultra thin layer interface and the dielectric-reflector interface are equal in amplitude but opposite in phase. This leads to the destructive interference and a perfect anti-reflection condition is achieved. This enhances the near surface local field and results in the enhanced Raman signal. Regarding the reflection layer, thermally evaporated Al films were used. But the surface studies revealed a large surface roughness of 2.7nm for area of 2 µm×2µm. Also Al is known to react with oxygen and formation of an oxide layer is favored. In an effort to overcome these problems, a platinum layer was chosen instead of Al as a reflecting layer. Dual ion beam sputter deposition was employed to prepare the platinum films and to study the surface property of the films prepared at different secondary ion current density. Thus the process parameters to get the Pt film with the required surface properties were optimized. To prepare the required phase layer, optical thin films of Ceria were used. The optical and structural property of ceria is found to be sensitive to the process parameters. Hence a new deposition technique for preparing the CeO2 thin films was adopted. This technique is called Dual ion beam Sputter Deposition (DIBSD). This technique involves, two ion sources (Kaufman type). One source is used to sputter the target, which is called the primary ion source and the other one is used to assist the growing film, which is called the secondary ion source. Both argon and oxygen were fed into the secondary ion source and oxygen ions in the mixture of the gases (Ar +O2) react with the growing film and the oxygen stoichiometry in the film is maintained. Also the secondary ion bombardment of the growing film helps in the densification and it leads to the increase in the refractive index of the ceria films. The films were found to grow with a preferential orientation along (111) direction. The optical properties of the films were studied by using the transmission spectra of the films from the spectrophotometer. Powder X-Ray diffraction, and Raman spectroscopy, were employed to study the structural properties. Atomic Force Microscopy was used to examine the surface topography and to estimate the surface statistics. A stress free ceria film with a high refractive index of 2.36 at 600nm was prepared for a secondary ion beam current density of 150µA/cm2 and a beam energy of 150 eV. Raman spectra and X-ray diffraction data of these films have revealed the formation of point defects in these films as a function of secondary ion current density. Germanium (Ge) ultra thin layers were prepared by using Ion Beam Sputter Deposition (IBSD) as this technique has a good control over the rate of deposition apart from various other advantages. The Ge ultra thin films were prepared on the multilayer stacks with Al or Pt as a reflecting layer. The germanium films were prepared for the various thicknesses ranging from 1-10 nm. These films were prepared on the multilayer stack of reflecting layer and phase layer. The films were prepared for the different substrate temperatures from 40 °C to 300 °C. The films thus prepared have been analyzed by Interference Enhanced Raman Spectroscopy (IERS) for the structural and quantum size effects, by RBS for the thickness and to study interface diffusion, and Atomic Force Microscopy (AFM) for the analysis of nano structure of the grown films and also for the surface statistics. The thickness of the Ge films was found to be same as that had been calculated from the rate of deposition of the films. The films showed increase in the grain sizes with increase in the thickness of the films. The nanostructure of the films from AFM images confirms this observation. IERS of the films shows the transition from the compressive to stress free nature of the film for the nominal thickness of 1 & 2 nm. The quantum size effects of the films show the asymmetric broadening and peak shift and these observations were studied using the spatial correlation model. The TEM studies on the samples with Pt as a reflecting layer show influence of the underlying layer of CeO2 by the formation Moiré fringes. Antimony (Sb) films were prepared for the different thicknesses (3-10nm) and at different substrate temperatures (40 °C - 200 °C) on the Pt/CeO2 multilayer stacks as the absorbing layer. IERS studies on the films were performed and the results are as follows. Sb films show crystallization with increase in thickness from 3nm to 4nm. The films show amorphous to crystalline transition for the substrate temperature of 200 °C. Quantum size effects on the samples due to the phonon confinement were analyzed by the spatial correlation model. The atomic force microscopic measurements for the nanostructural information on the samples showed that the grain sizes of the films increase with increase in the thickness. Also the surface morphology shows a definite change in the features for the transition of amorphous to crystallization phase. Chapter 1 introduces the importance of Ge and Sb in the present day technologies. The current state of research on these two materials has been discussed. The importance of ceria and Pt films has been highlighted in the context of IERS and for the applications elsewhere. The advantages and disadvantages of ion beam sputter deposition have been described. The importance of Raman spectroscopy as a characterization tool for the nano structures has been shown in this chapter along with an introduction on Raman spectroscopy. Also, the importance of the other complimentary characterization techniques has been discussed. Chapter 2 presents the experimental details used to deposit and characterize the thin films. Details of IBSD and DIBSD processes are given. The characterization pertaining to structural, surface, optical and compositional properties are dealt in detail. Method to compute the optical constants of a transparent film is also given. Chapter 3 presents the properties of reflecting layers. Structural, surface and the compositional (presence of Ar ion) properties of the DIBSD platinum thin films are presented. Chapter 4 presents the optical, structural and surface properties of DIBSD ceria thin films as a function of process parameters. Chapter 5 deals with the growth and Raman analysis of ultra thin Ge films with Al and Pt as reflecting layers. Chapter 6 deals with the growth and Raman analysis of ultra thin Sb films. Chapter 7 gives the summary of the thesis and the future scope of the work.

Nowadays, the systems that allow simultaneous employment of both focused electron and ion beams are very important tools in the field of micro- and nanotechnology. In addition to imaging and analysis, they can be used for lithography, which is applied for preparation of structures with required shapes and dimensions at the micrometer and nanometer scale. The first part of the thesis deals with one lithographic method – focused electron or ion beam induced deposition, for which a suitable adjustment of exposition parameters is searched and quality of deposited metal structures in terms of shape and elemental composition studied. Subsequently, attention is paid also to other types of lithographic methods (electron or ion beam lithography), which are applied in preparation of etching masks for the subsequent selective wet etching of silicon single crystals. In addition to optimization of mentioned techniques, the application of etched silicon surfaces for, e.g., selective growth of metal structures has been studied. The last part of the thesis is focused on functional properties of selected 2D or 3D structures.

<p>This thesis is based on a selection of six different experimental techniques used for studies in atomic and molecular physics. The techniques analysed in the thesis are compared to find similarities in strategies and ways to avoid sources of error.</p><p>Paper 1 deals with collision based spectroscopy with 60 keV Xe6+ ions on sodium and argon gas targets. Information on energy of Rydberg states in Xe5+ is unveiled by optical spectroscopy in the wavelength range from vacuum ultraviolet (VUV) to visible. In paper 2, the fast ion-beam laser spectroscopy (FIBLAS) is adapted for measuring hyperfine structure of barium isotopes in an isotopically pure ion-beam. This techniques involves changing the isotope during the measurement to minimize sources of error in measurement and enhance the signal from lesser abundant isotopes. The FIBLAS technique is used in paper 3 to study samarium ions. The ions are optically pumped and the recorded optical nutation is used to measure transition probabilities. This technique eludes the difficulties inherent in relative intensity measurements of all the radiative transitions from an excited state. In Paper 4, optical emission spectroscopy is used in the VUV region to study noble gas mixture discharges. The source of the emission bands near the resonance lines of krypton and xenon are found to be heteronuclear dimers. In paper 5, radiation from a pulsed argon plasma with admixture of nitrogen is studied with time resolved spectroscopy in the VUV and ultraviolet wavelength ranges to investigate the mechanism of energy transport. A metastable state of atomic argon is found to be an important source of energy to many radiative processes. In Paper 6, photoelectron spectroscopy (PES) on thiophene, on 3-bromothiophene and on 3,4-dibromothiophene using time-of-flight photoelectron-photoelectron coincidence technique and conventional PES to investigate the onset of double ionisation compared to the onset of single ionisation in molecules.</p>

Accurate knowledge of stopping powers is essential for these for quantitative analysis and surface characterization of thin films using ion beam analysis (IBA). These values are also of interest in radiobiology and radiotherapy, and in ion- implantation technology where shrinking feature sizes puts high demands on the accuracy of range calculations. A theory that predicts stopping powers and ranges for all projectile-target combinations is needed. The most important database used to report the stopping powers is the SRIM/TRIM program developed by Ziegler and coworkers. However, other researchers report that at times, these values differ significantly from experimental values. In this study the stopping powers of Si, P and S ions have been measured in Ni, Cu, Ge and GaAs absorbers in the energy range ~ 2-10 MeV. For elemental films of Ni, Cu and Ge, the stopping of heavy ions was measured using a novel ERD (Elastic Recoil Detection) based technique. In which an elastically recoiled lighter atom is used to indirectly measure the energy of the incoming heavy ion using a surface barrier detector. In this way it was possible to reduce the damage and to improve the FWHM of the detector. The results were compared to SRIM-2000 predictions and other experimental measurements. A new technique derived from Molecular Beam Epitaxy (MBE) was developed to prepare stoichiometric GaAs films on thin carbon films for use in transmission ion beam experiments. The GaAs films were characterized using X-ray Photoelectron Spectroscopy (XPS) and Particle Induced X-ray Emission (PIXE). These films were used to investigate the stopping powers of energetic heavy ions in GaAs and to provide data for the calculation of Bethe-Bloch parameters in the framework of the Modified Bethe-Bloch theory. As a result of this study, stopping power data are available for the first time for Si and P ions in the energy range 2-10 MeV stopping in GaAs absorbers.

A system is presented that is capable of confining an ion beam or plasma within a region that is essentially free of applied fields. An Artificially Structured Boundary (ASB) produces a spatially periodic set of magnetic field cusps that provides charged particle confinement. Electrostatic plugging of the magnetic field cusps enhances confinement. An ASB that has a small spatial period, compared to the dimensions of a confined plasma, generates electro- magneto-static fields with a short range. An ASB-lined volume thus constructed creates an effectively field free region near its center. It is assumed that a non-neutral plasma confined within such a volume relaxes to a Maxwell-Boltzmann distribution. Space charge based confinement of a second species of charged particles is envisioned, where the second species is confined by the space charge of the first non-neutral plasma species. An electron plasma confined within an ASB-lined volume can potentially provide confinement of a positive ion beam or positive ion plasma. Experimental as well as computational results are presented in which a plasma or charged particle beam interact with the electro- magneto-static fields generated by an ASB. A theoretical model is analyzed and solved via self-consistent computational methods to determine the behavior and equilibrium conditions of a relaxed plasma. The equilibrium conditions of a relaxed two species plasma are also computed. In such a scenario, space charge based electrostatic confinement is predicted to occur where a second plasma species is confined by the space charge of the first plasma species. An experimental apparatus with cylindrical symmetry that has its interior surface lined with an ASB is presented. This system was developed by using a simulation of the electro- magneto-static fields present within the trap to guide mechanical design. The construction of the full experimental apparatus is discussed. Experimental results that show the characteristics of electron beam transmission through the experimental apparatus are presented. A description of the experimental hardware and software used for trapping a charged particle beam or plasma is also presented.

In recent years a great deal of interest has been focused on the synthesis of transitional metal (e.g. Ag, Cu, Fe, Au) nanosystems at the surface to sub-surface regions of Si and SiO2 matrices for fundamental understanding of their structures as well as for development of technological applications with enhanced electronic and optical properties. The applications of the metal nanoparticle or nanocluster (NC) systems range from plasmonics, photovoltaic devices, medical, and biosensors. In all of these applications; the size, shape and distribution of the metallic NCs in the silicon matrix play a key role. Low energy ion implantation followed by thermal annealing (in vacuum or gas environment) is one of the most suitable methods for synthesis of NCs at near surfaces to buried layers below the surfaces of the substrates. This technique can provide control over depth and concentration of the implanted ions in the host matrix. The implanted low energy metal ions initially amorphizes the Si substrates while being distributed at a shallow depth near the substrate surface. When subject to thermal annealing, the implanted ions agglomerate to form clusters of different sizes at different depths depending upon the fluence. However, for the heavier ions implanted with high fluences (~1×1016 - 1×1017 atoms/cm2), there lies challenges for accurately predicting the distribution of the implanted ions due to sputtering of the surface as well as redistribution of the implants within the host matrix. In this dissertation, we report the investigation of the saturation of the concentration of the implanted ion species in the depth profiles with low energies (< 80 keV) metal ions (Ag and Au) in Si (100), while studying the dynamic changes during the ion implantation. Multiple low energies (30-80 keV) Ag ions with different fluences were sequentially implanted into commercially available Si wafers in order to facilitate the formation of Ag NCs with a wide ion distributions range. The light absorption profile according to different sizes of NCs at the near-surface layers in Si were investigated. We have investigated the formation of Ag NCs in the Si matrix as a function of implantation and thermal annealing parameters. The absorbance of light is increased in Ag implanted Si with a significant increase in the current collection in I-V (current-voltage) photo switching measurements. The experimental photovoltaic cells fabricated with the Ag implanted Si samples were optically characterized under AM (air mass) 1.5 solar radiation conditions (~1.0 kW/m2). An enhancement in the charge collection were measured in the annealed samples, where prominent Ag NCs were formed in the Si matrix compared to the as-implanted samples with the amorphous layer. The characterization techniques such as Rutherford Backscattering Spectroscopy, XPS-depth profiling, transmission electron microscopy, optical absorption, and I-V (current-voltage) photo switching measurements were employed to understand the underlying science in the observed properties. The results of these investigations are discussed in this research.

La coloration d'un béton, matériau faiblement chromatique, est obtenue soit par introduction de pigments dans son volume, soit par application d'un revêtement coloré sur sa surface. Ces travaux de thèse s'intéressent à une voie de coloration alternative innovante, qui consiste à introduire les pigments dans l'agent de décoffrage afin qu'ils soient transférés durablement vers la surface du béton frais au moment où celui-ci est coulé dans le coffrage. Cette méthode s'apparente beaucoup à la technique de peinture à fresque, qui a largement fait ses preuves en terme de durabilité. Dans un premier temps, l'étude de fresques sur chaux et sur ciment anciennes, ainsi que de reconstitutions, a permis d'identifier les principaux paramètres qui régissent le dépôt des pigments et leur adhésion durable au support : compatibilité du liant avec l'eau capillaire de l'enduit, granulométrie des pigments,cisaillement du pinceau à la surface de la fresque. Dans un second temps, la transposition de ces paramètres au cas du béton a conduit à l'identification de solutions satisfaisantes en terme de transfert et de durabilité de la couleur, mais aussi d'état de surface du béton (rugosité, porosité, homogénéité) : remplacement de l'huile de décoffrage par des tensioactifs non ioniques de faible viscosité et emploi de pigments correctement dispersés dans l'agent décoffrant. Finalement, l'étude des interfaces béton- agent décoffrant - coffrage a montré que le transfert durable des pigments repose sur un double mécanisme de démouillage de l'agent décoffrant par le béton en écoulement et de mélange des deux phases au niveau du front de la coulée, qui aboutit à la formation d'une inter phase pigments - béton de plusieurs dizaines de micromètres d'épaisseur. La profondeur de pénétration des pigments sous la surface a pu être quantifiée grâce à la combinaison d'observations en microscopie électronique à balayage et d'analyses en spectroscopie de rétrodiffusion Rutherford. La durabilité de la coloration a été évaluée par des mesures colorimétriques dans l'espace CIELab. / Concrete is an achromatic material that can be coloured through two main techniques: introduction of pigments in the bulk of the material, or application of a coloured layered on the hardened surface. This work focuses on an innovating alternative technique: the pigments are mixed with the demoulding agent, so that they can be transferred to the fresh concrete while it is poured into the mould. This method is ver y similar to the long-lasting fresco painting technique. The first par t of this work was dedicated to the study of ancient frescoes on lime or cement, in order to identify the main parameters responsible for the transfer and durable adhesion of the pigments to the plaster : compatibility between the binder and the capillar y water of the plaster, grain size of the pigments and shear stress between the brush and the plaster surface. In the second par t, these parameters were transposed to the case of concrete, which lead to satisfactor y solutions in terms of colour transfer and durability as well as surface proper ties of the concrete: the demoulding oil was replaced by low-viscosity non-ionic surfactants and the pigments were chosen to be finely dispersed in the demoulding solution. The last part consisted of a study of the mould - demoulding agent - concrete system and showed that the pigments are transferred to the concrete through the dewetting of the demoulding agent by the flowing concrete and the mixing of the two phases. This mechanism leads to the formation of a pigments - concrete interphase with a thickness of several tens micrometers. The depth of the pigments was quantified through a combination of scanning electron microscopy and Rutherford back-scattering spectroscopy. The durability of the colour was evaluated by colour measurements in the CIELab colorimetric space.