FG Experimentalphysik und funktionale Materialien
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This thesis addresses the electro-optical properties of silicon, containing dislocations. The interest in those properties is driven mainly by two practical reasons. One is the optical characterisation of multicrystalline silicon for solar cells, and the other is the design of light emitting diodes based on silicon by enhancement of silicon radiative properties via introduction of dislocations. The work demonstrates that dislocation specific radiation may provide a means for optical diagnostics of solar cell grade silicon. It provides insight into the mechanisms governing the dislocation recombination activity, their radiation, and how are they influenced by other defects present in silicon. We demonstrate that photoluminescence mapping is useful for monitoring the recombination activity in solar cell grade silicon and can be applied for identification of contaminants, based on their photoluminescence signatures. It is shown that the recombination at dislocations is strongly influenced by the presence of metals at the dislocation sites. The dislocation radiation activity correlates with their electrical activity. Thus, photoluminescence mapping at room temperature may provide a means for revealing and characterising of dislocation-rich regions in multicrystalline silicon. It is shown that the dislocation and band-to-band luminescence are essentially anti-correlated. The band-to-band intensity being related to the diffusion length of minority carriers can be used for measurements of diffusion length, as long as the surface recombination rate is controlled. Moreover, photoluminescence mapping can be used for the detection of optically active defects in solar grade materials. Thus, betaFeSi2 precipitates, with a luminescence at 0.8 eV, were detected within the grains of block cast materials. They exhibit a characteristic feature of quantum dots, namely blinking. The second aspect of the thesis concerns the topic of silicon based light emitters for on-chip optical interconnects. The goal is an enhancement of sub-band-gap or band-to-band radiation by controlled formation of dislocation-rich areas in microelectronics-grade silicon as well as understanding of the processes governing such enhancement. For light emitters based on band-to-band emission it is shown, that internal quantum efficiency of nearly 2 % can be achieved, but the emission is essentially generated in the bulk of the wafer. On the other hand, light emitters utilizing the emission from dislocation-rich areas of a well localized wafer depth were explored. Three different methods for reproducible formation of a dislocation-rich region beneath the wafer surface were investigated and evaluated in view of their room temperature sub-band-gap radiation: (1) silicon implantation and annealing, (2) epitaxially grown SiGe buffer, and (3) direct wafer bonding. The most promising dislocation-based emitter appears the utilization of a dislocation network produced by wafer bonding. It is shown, that monochromatic D1 radiation (wavelength 1.5 µm) can be generated in a well localised depth of the wafer. The radiation is not absorbed in silicon and such localized emitter can, potentially, be coupled with silicon waveguides and Ge-based detectors for optical interconnects.
This thesis addresses fundamental physical processes which take place at the surface region of a target during and after the interaction with ultra-short laser pulses. The general goal is to bring together different phenomena and discuss the non-equilibrium nature of the interaction of femtosecond laser pulses (tp < 100 fs) with various materials, in particular dielectrics and semiconductors. Different experiments, using various techniques, are designed to explore the basic mechanisms of laser ionization, defect creation, electron-lattice energetic transfer, charged particles desorption, optical breakdown, phase transformations and surface morphological changes. Such processes are shown to depend strongly on the laser intensity. Thus, they are analyzed for intensities over four orders of magnitude (10^11-10^14 W/cm2), around the surface optical breakdown (damage) threshold intensity. First, experimental studies using time-of-flight mass spectrometry indicate that non-resonant intense ultra-short laser pulses can efficiently ionize a dielectric (semiconducting) material leading to emission of electrons as well as charged particles, i.e. atomic ions and large clusters, and neutral particles. Under these irradiation conditions, the ionization processes can be at best described by multiphoton ionization and ionization at defects sites. The structural defects provide the means for an increased positive ion desorption rate. A multiple pulse incubation effect in the ion yield can be well related with the reduction of the multi-pulse damage threshold with increasing intensity. Following the initial electron excitation and emission, positive ions are released from the surface in a substantial amount with high ion velocities indicative of a localized microscopic electrostatic expulsion. With increasing intensity, the amount of ions gets larger and larger and their velocity distribution exhibits a bimodal structure. Also, in these conditions, negative ions are detected. The ion desorption can arise from a combination of a localized electrostatic repulsion (macroscopic Coulomb explosion) and a thermal ‘explosive’ mechanism. The later becomes more important with increasing intensity. The very fast energy input and particle emission result in a transient perturbation and deformation of the target lattice. Using pump-probe experiments the temporal evolution of lattice dynamics can be analyzed upon single-pulse excitation for many different target materials. This deformation is indicated to be a material characteristic. It is associated with the generation of transient defects in dielectrics or fast phase transitions in semiconductors and metals. Therefore, it could well give estimates of lifetime of transient defect states or electron-phonon relaxation times.At last the surface morphology after ablation is analyzed, with emphasis on the laser-induced surface periodic patterns (ripples). The patterns observed appear to be very different from the ‘classical’ ripples formed after long pulse ablation. They can have periods much smaller than the incident wavelength and are rather insensitive to the variation of the laser wavelength and angle of incidence. We show that control factors are laser beam polarization and the irradiation dose. Additionally, the patterns exhibit features pointing toward a chaotic origin. Their possible formation mechanism is likely linked with the non-equilibrium nature of the interaction.
Die internationale Temperaturskala von 1990 wird im Bereich von -38,8344°C bis 961,78°C neben dem Wasser- und dem Quecksilber-Tripelpunkt durch Schmelz- und Erstarrungstemperaturen von Reinstmetallen definiert. Die Unsicherheiten bei der Darstellung und Weitergabe der Basiseinheit Kelvin des Internationalen Einheitensystems in diesem Bereich (und somit auch der Einheit Grad Celsius und aller abgeleiteten Einheiten) werden dominiert von den Unsicherheiten der Realisierung dieser Fixpunkte und diese wiederum von einem Beitrag, der vom Einfluss in den Metallen gelöster Verunreinigungen herrührt und bis jetzt nur pauschal abgeschätzt wurde. Zwar wird versucht, noch reineres Fixpunktmetall zu verwenden, aber wesentliche Verbesserungen bezüglich der Reproduzierbarkeit der Fixpunkttemperaturen können nur durch eine Korrektion dieser Beiträge erreicht werden. Voraussetzungen für diese Korrektion sind nicht nur eine chemische Spurenanalyse der Fixpunktmetalle mit Unsicherheiten und Detektionsgrenzen am aktuellen technischen Limit, sondern auch die Kenntnis der Auswirkungen jeder einzelnen Verunreinigung auf die Fixpunkttemperatur. Diese Abhängigkeit der Phasenübergangstemperatur von der Konzentration der jeweiligen Verunreinigung wird auf Grund fehlender Kenntnisse im Bereich kleinster Konzentrationen von 10^-9 bis 10^-5 (mol/mol) experimentell durch gezielte Dotierung der Fixpunktmetalle bestimmt. Um die dargestellten Probleme grundlegend zu lösen, wurden im Rahmen dieser Arbeit zwei verschiedene Fixpunktzelldesigns entwickelt. Beide erlauben eine Messung und Kontrolle des Drucks der Gasatmosphäre und sind außerdem wiederverschließbar, wodurch sie eine chemische Analyse des Fixpunktmaterials ermöglichen, das sich in der Zusammensetzung wesentlich von dem unterscheiden kann, mit dem die Zelle befüllt worden ist. Während der eine Zelltyp für Kalibrierzwecke konstruiert worden ist und den herkömmlichen Zellen ähnelt, wurde der zweite Typ auf die Verwendung von deutlich weniger Fixpunktmetall hin optimiert, so dass er sich unter anderem gut für die erwähnten Dotierungsexperimente eignet. Zunächst allerdings bringen die Veränderungen im Design gegenüber den üblichen Fixpunktzellen unvermeidlich eine Vergrößerung unerwünschter parasitärer Wärmeflüsse mit sich, welche als sogenannte thermische Effekte die gemessene Fixpunkttemperatur verfälschen. Diese fallen bei der angestrebten Verwendung von höchstreinem Fixpunktmetall relativ zu den anderen Einflussgrößen umso mehr ins Gewicht, deswegen wurde ihre Untersuchung zu einem weiteren Schwerpunkt der Arbeit. Dabei konnte ein Verfahren zur Quantifizierung und Korrektion und ein besseres Verständnis dieser Effekte entwickelt werden, welche für Metallfixpunktzellen jeder Bauart nützlich sind. Im Ergebnis liegen die Unsicherheiten bei den Messungen mit den verkleinerten Zellen unverändert im Bereich weniger hundert Mikrokelvin. Die Zellen eignen sich daher sehr gut, die Beeinflussung der Phasenübergangstemperatur der Metallfixpunkte durch die Dotierung mit anderen Elementen im Konzentrationsbereich von 10^-7 bis 10^-5 zu bestimmen. Bevor dies abschließend auch experimentell mit Untersuchungen an ausgewählten binären Systemen gezeigt wird, werden thermodynamische Berechnungen dargestellt, die erstmals eine Vielzahl von möglichen Verunreinigungen in den Fixpunktzellen ausschließen, so dass sich nicht nur die Anzahl zu untersuchender möglicher Verunreinigungen in den Fixpunkten erheblich reduziert, sondern auch die Anzahl zu berücksichtigender Beiträge bei der angestrebten Korrektion der Fixpunkttemperaturen. Alles in allem steht nun eine Methodik zur Verfügung, die Unsicherheit bei der Darstellung der internationalen Temperaturskala im industriell besonders wichtigen Bereich von -40°C bis 1000°C mindestens um den Faktor 3 zu reduzieren.
Titanium nitride (TiN) is a complementary metal-oxide-semiconductor (CMOS) compatible material with large potential for the fabrication of plasmonic structures suited for device integration. However, the comparatively large optical losses can be detrimental for application. This work reports a CMOS compatible TiN nanohole array (NHA) on top of a multilayer stack for potential use in integrated refractive index sensing with high sensitivities at wavelengths between 800 and 1500 nm. The stack, consisting of the TiN NHA on a silicon dioxide (SiO2) layer with Si as substrate (TiN NHA/SiO2/Si), is prepared using an industrial CMOS compatible process. The TiN NHA/SiO2/Si shows Fano resonances in reflectance spectra under oblique excitation, which are well reproduced by simulation using both finite difference time domain (FDTD) and rigorous coupled-wave analysis (RCWA) methods. The sensitivities derived from spectroscopic characterizations increase with the increasing incident angle and match well with the simulated sensitivities. Our systematic simulation-based investigation of the sensitivity of the TiN NHA/SiO2/Si stack under varied conditions reveals that very large sensitivities up to 2305 nm per refractive index unit (nm RIU−1) are predicted when the refractive index of superstrate is similar to that of the SiO2 layer. We analyze in detail how the interplay between plasmonic and photonic resonances such as surface plasmon polaritons (SPPs), localized surface plasmon resonances (LSPRs), Rayleigh Anomalies (RAs), and photonic microcavity modes (Fabry-Pérot resonances) contributes to this result. This work not only reveals the tunability of TiN nanostructures for plasmonic applications but also paves the way to explore efficient devices for sensing in broad conditions.
In der Promotionsarbeit wurde ein Züchtungsverfahren zur Herstellung strukturell hochqualitativer AlN-Volumenkristalle mittels PVT-Methode entwickelt. Wesentliche Grundvoraussetzungen dafür sind ein thermisch und chemisch stabiles Tiegelmaterial, ein AlN-Quellmaterial mit Sauerstoffverunreinigungen <300 ppm und AlN-Keime mit hoher kristalliner Perfektion. Unter den getesteten potenziellen Tiegelmaterialien (BN, TaC, TaN, NbC, NbN, TaB2, W) zeigten sich TaC und mit Abstrichen W unter AlN-Züchtungsbedingungen ausreichend stabil und wurden für die Wachstumsversuche verwendet. Zur effektiven Reduzierung der Sauerstoffverunreinigungen im AlN-Quellmaterial wurde ein karbothermischer Reduktionsprozess entwickelt, welcher eine Restsauerstoffkonzentration im Quellmaterial von <300 ppm gewährleistet. AlN-Keime für die Homoepitaxie von AlN-Volumenkristallen wurden durch heteroepitaktisches Wachstum auf SiC-Substraten und über spontane Nukleation freistehender AlN-Kristalle hergestellt. Beim heteroepitaktischen Wachstum auf SiC zeigte sich eine starke Abhängigkeit von der Substratpolarität. Wachstum auf C-polarem SiC ist mit geringeren Ätzgrubendichten von 5*10^4 - 10^6 cm^(-2) gegenüber Si-polarem Wachstum mit Ätzgrubensdichten von 5*10^6 - 10^7 cm^(-2) gekennzeichnet. Für beide Substratpolaritäten wurden Modelle des Anwachsstadiums entwickelt. AlN-Kristalle mit bis zu 35 mm im Durchmesser wurden gezüchtet. Die hohe Rissneigung aufgrund von Abkühlspannungen und Si-Konzentrationen von mehreren Prozent im gewachsenen AlN-Kristall vermindern aber die Kristallqualität erheblich. Eine sehr hohe kristalline Perfektion kann hingegen durch spontane Nukleation freistehender AlN-Kristalle auf einer Zwischenebene in der Tiegelmitte gewährleistet werden. Bei Nukleationstemperaturen von 2200 °C wurden isometrische Kristalle mit 12*12*14 mm^3 gezüchtet. Die Kristalle weisen eine zonare Struktur auf, welche durch einen in [000-1]-Richtung gewachsenen Kernbereich mit Versetzungsdichten <10^2 cm^(-2) und einem senkrecht um den Kernbereich gewachsenen Randbereich mit Versetzungsdichten von 10^2 - 10^4 cm^(-2) gekennzeichnet ist. Strukturell hochqualitative (000-1)-Keime wurden aus spontan nukleierten isometrisch gewachsenen AlN-Kristallen präpariert und für die homoepitaktische Volumenkristallzüchtung verwendet. Unter Zuhilfenahme numerischer Temperaturfeldsimulationen wurde ein angepasster Keimhalter entwickelt, welcher ein leicht konvexes Temperaturfeld am Keim gewährleistet und Parasitärwachstum unterdrückt. Somit konnten AlN-Volumenkristalle homoepitaktisch gezüchtet werden, welche eine Durchmesservergrößerung unter Beibehaltung der hohen strukturellen Qualität der Keimkristalle zeigen. Dieses Verfahren bietet die Grundlage, durch die Züchtung mehrerer Kristallgenerationen eine Durchmesseraufweitung auf industriell relevante Größen von 1-2" zu erreichen.
The LHC is the largest particle accelerator and storage ring in the world, used to investigate fundamentals of particle physics and to develop at the same time the technology of accelerators and detectors. Four main experiments (ATLAS, ALICE, CMS and LHCb) , located around the LHC ring, provide insight into the nature of particles and search for answers to as yet unexplained phenomena in the universe. Two proton or heavy ion beams circulate in the LHC and are brought into collision in the four experiments.
The physics potential of each experiment is determined by the luminosity, which is a ratio of the number of the events during a certain time period to the cross section of a physics process. A measurement of the luminosity is therefore essential to determine the cross section of interesting physics processes.
In addition, safe and high-quality data-taking requires stable beam conditions with almost no beam losses. Each experiment has its own detectors to measure beam losses, hereafter called machine induced background. One such detector is installed in CMS, BCM1F. Based on diamond sensors it was designed and built to measure both, the luminosity and the machine induced background. BCM1F ran smoothly during the first LHC running period from 2009-2012 and delivered valuable beam loss and luminosity information to the control rooms of CMS and LHC. At the end of 2012 the LHC was shut down to improve the performance by increasing the proton energy to 7TeV and decreasing the proton bunch spacing to 25ns. Due to the success of BCM1F an upgrade of its sensors and readout components was planned in order to fulfil the new requirements.
The upgrade of the sensors comprises a two pad instead of one pad metallization. 24 instead of the previous 8 single crystal diamond sensors were foreseen for the new BCM1F to enhance the robustness and redundancy. To instrument BCM1F, 59 sensors were electrically characterized by measuring the leakage current, signal stability and charge collection efficiency. Quality criteria were defined to select sensors for the final installation. An overview of these measurements including a summary of the results is given in this thesis. In addition, an upgraded amplifier was developed within the collaboration in 130nm CMOS technology. It has a peaking time of 7ns instead of the 22ns of the one previously installed. A BCM1F prototype comprising a two pad sensor and the upgraded amplifier was tested at the DESY-II accelerator in a 5GeV electron beam. Results of these test-beam measurements are presented in this thesis as well as simulations to interpret the measurements.
The installation of the upgraded BCM1F was completed in 2014. In 2015 BCM1F was commissioned and started to measure luminosity and machine induced background. At the end, the thesis will describe both types of measurements with the focus on machine induced background demonstrating the functionality of BCM1F.
Das Ziel der vorliegenden Arbeit ist es, einen Beitrag zum Verständnis mikroskopischer Prozesse zu leisten welche an der Laser-Ablation dielektrischer Kristalle mit ultrakurzen Laserpulsen beteiligt sind. Die von den Targets emittierten elektrisch geladenen Partikel werden mit einem Flugzeitmassenspektrometer nachgewiesen, und die resultierende Morphologie der Targetoberfläche wird ex-situ mit Methoden der optischen Mikroskopie bzw. der Raster-Elektronenmikroskopie charakterisiert. Die Absorption der Laserstrahlung führt zu Multiphotonen-Ionisationsprozessen, so dass es zu einer Coulomb-Explosion der Oberfläche kommt. Bei hohen Laserintensitäten gibt es außerdem thermische Beiträge zu Ablation (Phasen-Explosion). Für die resonante Unterstützung der Photoelektronenemission sind materialabhängige Oberflächenzustände (z. Bsp. F-Zentren) wichtig. An BaF2 (111) Oberflächen wird ein „Layer-by-Layer“ Abtrag beobachtet. Die Partikelemission hinterlässt eine instabile Oberfläche, deshalb kann es im Ablationskrater zur Ausbreitung von Oberflächenwellen und der Bildung von Ripples durch selbst-organisierte Prozesse kommen.
Zur Deckung des stetig steigenden Energiebedarfs und unter Berücksichtigung des Umweltschutzes werden unter anderem Solarzellen genutzt. Defekte in Solarzellen können die Effizienz verringern. In dieser Arbeit wird das Defektverständnis von Silizium basierten Solarzellen erweitert.
Neue experimentelle Erkenntnisse konnten zu folgenden Schwerpunkten gewonnen werden:
• Siliziumnitrid- und Siliziumkarbidausscheidungen in multikristallinem Silizium
• Rekombinationsaktivität in dünnen Siliziumschichten
• Charakterisierung der Rekombinationsaktivität von Germanium als Modellmaterial für die Siliziumkristallisation
• Rekombinationsaktivität und Verspannung an Korngrenzen
Um Ergebnisse experimenteller Defektcharakterisierung auf allgemein gültige Parameter der Rekombination wie z.B. Ladungsträgerdiffusionslänge oder Oberflächenrekombinationsgeschwindigkeit zurückführen zu können, wurden zu folgenden Phänomenen Modelle entwickelt und Simulationen durchgeführt:
• Getterzonen an Korngrenzen
• Ermittlung von Diffusionslänge und Diffusionskoeffizient in Dünnschichtmaterial
• 3D-Raumladungseffekte
Die Nutzung der gewonnenen Erkenntnisse über die Rekombinationseigenschaften der Defekte liegt in einer möglicherweise zukünftigen kontrollierten Defektbeeinflussung und somit einer Effizienzverbesserung von Solarzellen.
In this work, the electrical and luminescence properties of a series of Si based materials used for photovoltaics, microelectronics and nanoelectronics have been investigated by means of electron beam induced current (EBIC), cathodoluminescence (CL), photoluminescence (PL) and electroluminescence (EL). Photovoltaic Si produced by block casting has been investigated by EBIC on wafers sliced from different parts of the ingot. The impact of selected solar cell processing steps on the material properties has been evaluated by EBIC utilizing adjacent wafers from the ingot. The temperature dependence of dislocations’ EBIC contrast was measured to assess the degree of dislocation contamination with impurities, yielding low dislocation contamination for the middle of the block and high contamination in the top and bottom regions. This is in agreement with the impurity distribution in the block. It was found that phosphorus diffusion gettering (PDG) followed by SiN firing greatly reduces the recombination activity of extended defects at room temperature, and improves the bulk property simultaneously. The improvement is attributed to both PDG of metal impurities and a passivation effect of SiN firing. In order to better understand the factors limiting the properties of thin polycrystalline Si layers prepared by the Aluminum induced layer exchange (Alile) technique, epilayers grown on (111) and (100) monocrystalline Si substrates were used as a model system to investigate the impact of processing temperature (Ts) and type of substrate. It was found that no dislocations are formed for epilayers on (100) Si, while a high density of dislocations was detected on epilayers prepared on (111) Si at 450 °C. The dislocation density decreases with increasing TS. The diffusion lengths extracted from the energy dependent EBIC collection efficiencies reveal an improvement of the epilayer quality with increasing TS during growth from 450 °C to 650 °C, and a decrease of the epilayer quality at 700 °C. This is attributed to a reduction of the dislocation density with increasing TS and a formation of precipitates during the process. Precipitate formation of at 700 °C is limited because the metal impurities are very mobile at high TS, resulting in a homogeneous distribution of the impurities. Because the impurities are effective lifetime killers of the minority carriers, so the diffusion length decreases. PL measurements on epilayers grown on Si substrates revealed no characteristic dislocation-related luminescence (DRL) lines at room temperature and 77 K, while intense characteristic DRL lines D1 - D4 have been detected in the sample prepared by the Alile technique. This indicates that dislocations in the Alile sample are relatively clean. The possible reason for the purification of the Alile samples is Al induced gettering during the polycrystalline Si layer growth. The diffusion length in the thin top layer of Si-on-insulator (SOI) samples has been successfully measured by EBIC employing suppression of the surface recombination at the buried oxide layer and at surface of the top layer by biasing. The measured diffusion length is several times larger than the layer thickness. Dislocation networks produced by Si wafer direct bonding have been investigated with regard to their electrical properties by EBIC. The networks were observed to show charge carrier collection and electrical conduction. Inhomogeneities in the charge collection were detected in n- and p-type samples under appropriate beam energy. The EBIC contrast behavior can be understood under the consideration of the positively charged oxide precipitates along with dislocations charged with majority carriers, where the appearance of the contrast in dark or bright depends strongly on the ratio of the collection and the recombination loss of the carriers.The luminescence properties of Si nanostructures (Si nanowires, Si nano rods, porous Si, and Si/SiO2 multi quantum wells (MQWs)) are another important subject of this work. Sub-bandgap infrared (IR) luminescence around 1570 nm has been found in Si nanowires, nano rods and porous Si. PL measurements with samples immersed in different liquid media, for example, in aqueous HF (50%), concentrated H2SO4 (98%) and H2O2 established that the sub-bandgap IR luminescence originates from the Si/SiOx interface. Its origin was explained in terms of a simple recombination model through radiative interface states. EL in the sub-bandgap IR range has been observed in simple diodes prepared on porous Si and MQWs at room temperature. The results show the possibility to fabricate an efficient light emitter around 1570 nm wavelength based on the radiative recombination at the Si/Si oxide interface. Based on the knowledge about radiative transitions via the interface states, an improved understanding of luminescence in dislocated samples was proposed.
The aim of this work is to establish tools for optical characterization of defects in thin-film silicon solar cells. This is related to a challenging process of setup adjustments and careful interpretation of the measured raw data because of several artifacts and effects, which are typical for thin films. They are caused by the low layer/sample thickness and the related high impact of interfaces. Therefore, different thin-film samples were investigated to establish a process to correct/minimize these thin-film effects. The possibility of a knowledge transfer from mc-Si wafers with bulk thickness to thin Si films was checked. This would simplify a successful interpretation of the corrected data. Defects in mc-Si were investigated for many decades without the parasitic impact of thin films. Other Si phases, which are limited to thin-film samples, were investigated to learn details about their specific physical properties. These Si phases are amorphous and microcrystalline silicon. Additional to that electroluminescence investigations were performed on mc-Si solar cells. These investigation deals with topics, which are not even understood on bulk materials up to now. This could offer a basic for further knowledge transfers to thin-film Si.