FG Experimentalphysik und funktionale Materialien
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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.
Historically, Ge is one of the oldest materials in the semiconductor industry and its (001) surface has been the subject of extensive investigations by photoelectron spectroscopy. I am going to challenge the predominant attribution of a semi-conducting nature of the Ge(001) surface in this thesis. My investigations reveal the presence of a Ge(001) surface state above the Fermi-level, occupied at room temperature. Employing time- and temperature-dependent angle-resolved photoelectron spectroscopy, I will demonstrate that the presence of this surface state is evidence for the conducting nature of the surface at room temperature.
Sparked by the remarkable properties of the GeSn-alloy and a trend towards Ge-Sn-related multiquantum well fabrication, I investigate the surface electronic structure of Ge(001) after adsorption and incorporation of Sn. With an in-depth analysis of surface core-level shifts, I will extend the growth model of the Sn wetting layer formation by also detailing structural changes in the subsurface region. At the same time, the modifications of the electronic structure will be detailed, observing the removal of the Ge(001) surface states, the creation of a new, Sn-related surface state and the initial stages of the Schottky barrier formation.
β-Ga2O3 is a transparent semi-conducting oxide that has sparked a lot of interest over the last decade, because it offers an ultra-wide band gap and high break down voltage. However, due to its monoclinic crystal structure, device fabrication is rather challenging and researchers are already looking into alternative materials. One of these candidates is ϵ-Ga2O3 and this work presents a combined study by photoelectron spectroscopy and ab initio calculations of its electronic structure. (Hard) X-rays reveal the impact of photoelectron recoil and the absence of a band bending to the surface, while the dispersion of experimentally determined valence states compares favorably with the calculations based on hybrid density-functional theory.
Another alternative to β-Ga2O3 could be ZnGa2O4 and I will present an investigation on the electronic structure of its (100) surface. Due to the novelty of ZnGa2O4 single-crystals, I am first going to explore the preparation of a clean and well-ordered surface by standard in-situ sputtering and annealing. I will show that already low annealing temperatures induce Zn-deficiency, leading to non-stoichiometric surfaces, further exacerbated by sputtering. By changing the sputtering parameters and the annealing conditions, the preparation of a surface with sufficient quality for subsequent investigations will be demonstrated. The results by photoemission techniques compare favorably with the expectations from theory and allowing the first fundamental insights into the surface electronic structure.
This thesis focuses on the investigation and characterization of the surfaces and interfaces of chalcopyrite-based Cu(In,Ga)Se2 (CIGSe) thin film solar cells using various x-ray and electron spectroscopies. In particular, the impact of alkali post deposition treatments (PDT) on the chemical and electronic surface and interface structure of CdS/CIGSe absorbers is studied.
The structure of “real world” CdS/CIGSe interfaces and how they are impacted by different alkali PDTs was investigated by a combination of different x-ray spectroscopies. The interface formation is characterized by studying sample sets with different CdS thicknesses. The chemical environment for indium and cadmium is revealed by deriving the modified Auger parameter α'(In) and α'(Cd) using the kinetic energy of most prominent Auger line together with the binding energy of the chosen core level. A more complex situation is found for CdS/CIGSe samples that underwent NaF+KF PDT, where a K-In-Se compound is initially present on top of the chalcopyrite absorber. The conversion of the K-In-Se type species into a Cd-In-(O,OH,S,Se) interface compound is recorded at short CBD-CdS deposition times. It appears the majority of K that is present at the surface of the NaF+KF PDT CIGSe absorber is dissolved in the CBD and partially re-deposited as K-O type species. The Cd/S ratio clearly deviates from the stoichiometry expected for CdS, and a Cd(O,OH,S)-like compound is likely formed. The electronic structure of CdS/CIGSe interface is similarly more complex for the NaF+KF PDT compared to the NaF PDT case, where only Cd(O,OH,S) buffer was formed.
In an attempt to shed more light into this complex situation, the impact of evaporated alkali metals (K, Rb, Cs) on the surface structure of CIGSe was studied in-system by synchrotron-based hard x- ray photoelectron spectroscopy (HAXPES), aiming at understanding the underlying mechanism of the interfacial effect of alkalis on the performance of CIGSe devices. In the case of K deposition, two K species are observed by x-ray absorption near-edge structure (XANES) and HAXPES, one of which species disappears at high annealing temperature. Furthermore, three new In contributions (In-O and K-In-Se, metallic In species) can be observed after K evaporation. The evolution of chemical contribution supports the formation of a K-In-Se and Cu-poor CIGSe (1:3:5) bilayer structure that is similar to what was reported for “real world” NaF+KF PDTs. Deposition of heavy alkali metals (Rb, Cs) induced the formation of alkali selenide phases after alkali evaporation and during low temperature annealing. Similar chemical changes as seen for the K composition (i.e. presence of metallic In, In-O, and alkali-O) are observed. However, detailed analysis of the Alk/Se ratio and composition provide direct evidence for the formation of a Alk-(In)-Se and (Cu,Alk)(In, Ga)Se2 bilayer.
The insights from these studies promise to provide crucial aid to fully exploit alkali pre-treatments in scientific and industrial CIGSe production, and will deliberate use of this means of surface/interface tailoring to push efficiencies even further.
Over the past seven decades Si microelectronics have developed rapidly. The success of the growing microelectronic industry is also caused by the expansion of materials in addition to Si. Open challenges are the monolithic integration of group IV devices on Si photonics as well as overcoming the size mismatch between electronic parts in the nm range and photonic parts in the µm scale. In this thesis the future application of GeSn NIs on Si as a photodetector is evaluated. The key element required for high performance optoelectronic devices is the formation of high-quality GeSn nano-islands (NIs), i.e. overcoming growth challenges such as introduction of defects due to lattice and thermal mismatch between GeSn and Si substrate as well as suppression of Sn precipitation caused by the limited solid solubility of Sn in Ge. To achieve high-quality nanostructures, the selective growth of GeSn NIs on Si(001) seeds via molecular beam epitaxy is investigated, exploiting the advantages of nanoheteroepitaxy (NHE), i.e. growth on nano-patterned substrates. The best compromise between selective growth of GeSn on Si nano-pillars at significant higher growth temperature than the eutectic temperature of GeSn and the incorporation of Sn into the Ge lattice was achieved at 600°C. X-ray diffraction studies confirmed the substitutional incorporation of 1.4at.% Sn into the NIs avoiding considerable Si interdiffusion from the substrate. Transmission electron microscopy images have shown that dislocations and stacking faults caused by plastic relaxation of the GeSn NIs are located near the NIs/substrate interface and thus, dislocation-free GeSn NIs can be formed, due to gliding out of the threading arms triggered by the NHE approach.
The high crystal quality of the GeSn NIs, enables the investigation of the bandgap by μ-photoluminescence (PL) analyses, demonstrating the shrinkage of the direct bandgap with increasing Sn content in the quasi-direct semiconductor.
All NIs however feature a β-Sn droplet on their nano-facets. To suppress the out-diffusion of Sn and hence increase the Sn concentration of the GeSn alloy, the GeSn NIs were overgrown with a thin Ge cap layer. The Ge cap successfully hinders the formation of Sn segregates on top of the NIs. Capping at 600 °C and 650°C results in an enrichment of Sn at the surface, forming a GeSn crust with 8±0.5at.% Sn. This wetting layer both enhances the optoelectronic properties of the NI core and exhibits a relatively strong PL emission attributed to direct radiative recombination.
Finally, a first demonstration of a GeSn NIs based photodetector was successful, due to the utilization of Al nano-antennas exhibiting an enhanced light coupling into the GeSn NIs at a wavelength of 700nm. The responsible mechanisms is the local plasmonic field enhancement of the incoming light. The manipulation of the resonance wavelength into the telecommunication regime, i.e. >1550nm, have to be investigated in future studies.
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.
The aim of this work is to study the optical properties of crystal defects in multicrystalline solar silicon and poly-/microcrystalline silicon thin films on glass substrate.
First a setup for photoluminescence imaging on multicrystalline silicon solar wafers was developed. This system is suitable for detecting band-to-band luminescence as well as defect-related luminescence at room temperature on large-scale wafers at different stages of their processing.
Spectroscopic photoluminescence investigations of multicrystalline silicon solar wafers indicated a new intense luminescence line at ≈ 0.91 eV at room temperature. The origin of this line is probably found in a specific grain boundary. Furthermore, luminescence in the region of 0.8 eV was investigated in detail, and it was found that probably oxygen is responsible for a peak at 0.77 eV at 80 K.
Electroluminescence investigations at room temperature at both materials exhibit extended defect structures such as grain boundaries. Furthermore, it can be concluded that electroluminescence imaging in reverse bias mode indicate on serious breakdown points in solar cells, which can lead to destruction of solar cells and modules. By comparing defect-related and reverse bias electroluminescence images, a difference in the spatial distribution of defects emitting D1 radiation and defects emitting light under reverse bias beyond -12 V is detectable.
In addition, there seems to be a correlation in the distribution of non-doping impurities and photoluminescence. Concerning this, vertical slabs of two silicon blocks were examined by means of Fourier-transform infrared spectroscopy and photoluminescence. A correlation of the distributions of interstitial oxygen and the band-to-band luminescence profiles could be found. Additionally, a correlation between D3/D4 luminescence profile and nitrogen distribution in the blocks was observed.
Finally, the growth process, particularly the transition from amorphous to microcrystalline silicon by PECVD, was studied by combined photoluminescence and Raman investigations. Formation of silicon nano-grains was detected by means of photoluminescence and Raman spectroscopy.
The aim of this work is to describe and explain the properties of defects in multicrystalline (mc) and thin-film solar silicon (Si). For this reason, investigations with scanning electron microscope methods were performed, namely cathodoluminescence (CL), electron beam induced current (EBIC), electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM). Additionally, photoluminescence (PL) and reverse-biased electro luminescence (ReBEL) measurements were also conducted. Through correlation of PL, ReBEL and EBIC, it was possible to localize breakdown sites at mc-Si solar cells. Problems that occurred during the thin-film EBIC investigations could be demonstrated and explained. For the first time cross sectional EBIC investigations could be performed on thin-film silicon tandem cells. At mc-Si, it was possible to observe the oxygen related P-line next to the common D1-line luminescence at 10 K clearly distinguishable from each other at once. Furthermore, a hitherto not comprehensively discussed intense luminescence line at 0.93 eV could be described in detail. Through correlation of PL, CL, EBIC, EBSD, and TEM measurements, the origin of the now named Di luminescence at 0.93 eV is postulated to be in connection with Frank partial dislocations, with two energetic levels inside the band gap, one at 112±9 meV below the conduction band and the other at 93±10 meV above the valence band. Finally, it was attempted to explain the behavior of twin boundaries at temperatures below 30 K, where these show an enhanced collection efficiency in comparison to the surrounding grains. An alteration of the local “freeze out” temperature, possibly by a local band gap narrowing, is suggested as a reason. Another conceivable explanation is a breakdown of the diode potential at the grains.
Gallium nitride (GaN) is a III-V semiconductor, characterized by direct, wide band gap of 3.4 eV at RT. As a material of particular interest for opto- and power electronics applications, it has been thoroughly studied in recent years. Utilization of GaN homoepitaxy in manufacturing of laser diodes (LDs), light-emitting diodes (LEDs), power devices, etc. would be beneficial in terms of reducing defect density, thus improving their lifetime and performance. Yet cost-effective process for providing native GaN substrates has not been established so far.
The focus of this work is put on development of a new method to grow single crystalline GaN layers from Ga vapour. Our approach exploits microwave (MW) plasma as a source of excited nitrogen species, in contrast to classical physical vapour transport (PVT)-based technique, in which ammonia (NH3) serves as a source of reactive nitrogen. Novelty of MW plasma enhanced growth of GaN from vapour lies in MW nitrogen plasma formation in the vicinity of the seed, at moderate pressure (200 – 800 mbar range), and concurrent physical vapour transport of Ga to the growth zone. Simulations of the growth setup (HEpiGaN software) and of the MW plasma source (CST Microwave software) have followed the extensive investigations of material properties. The growth setup and the MW plasma source, with the resonance cavity being its crucial part, have been constructed and implemented into the existing growth reactor.
The stability of MW plasma in function of temperature and pressure has been studied along with its influence on the seed temperature, and thus on the growth conditions. Furthermore, optical emission spectroscopy (OES) has been utilized for in-situ characterization of the growth atmosphere. Studies on the interaction of Ga vapour with the nitrogen discharge were interpreted on the basis of the level structure of lower excited states of Ga.
Deposition experiments have been conducted, using sapphire seeds, GaN, AlN and AlGaN templates, while GaN single crystalline layers have been grown on sapphire and GaN templates. Characterization of GaN layers have been done by various methods, i.e. structure of layers by scanning electron microscopy (SEM), their composition by energy dispersive X-ray spectroscopy (EDX) and secondary ion mass spectrometry (SIMS), and crystal quality by high resolution X-ray diffraction (HRXRD). Results of the characterization together with outcome of OES measurements revealed importance of carbon for the sub-atmospheric MW plasma enhanced growth of GaN from vapour. In addition, this fact was confirmed by experiments in the setup with reduced carbon content. Possible routes for GaN synthesis have been discussed, with the most probable being CN-assisted GaN formation. While CN was detected in the plasma spectra, there was no evidence for the existence of GaN molecules in vapour phase.
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.
Semiconductor nanowires, also called nanorods or nanowhiskers, are of particular interest for various applications in nanotechnology. Especially, germanium as a CMOS compatible material with its good electronic properties has gained renewed interest in recent years due to the availability of modern gate dielectrics. The present work deals with the vapor-liquid-solid growth of germanium nanowires and their characterization. The Growth has been carried out by means of molecular beam epitaxy using differently oriented germanium and silicon substrates whereas gold has been used to create metal catalyst droplets with radii of typically 100 nm and below. All stages from the substrate preparation to the final growth have been investigated in the frame of this work to find significant control parameters that influence the growth result. The droplet formation by means of gold evaporation onto the heated substrates has been investigated extensively on different substrates and for different surface preparations to identify parameters that are crucial for the resulting size distribution. Thereby sticking effects of the droplet circumference turned out to influence the radius distribution significantly. Germanium nanowires have been observed to grow preferentially along the <011> crystallographic directions on all utilized substrate orientations leading to defined possible inclinations of the wires with respect to the substrate normal. In contrast to the faceting known from silicon wires, the sidewalls mainly exhibit four flat {111} facets whereas the tip is roof shaped consisting of another two {111} facets. Different models which describe the inclined growth are presented and discussed. Furthermore, the material transport during the growth has been investigated. The nanowire length was found to be up to eight times larger than the nominal layer thickness according to the total amount of deposited germanium which is explained by surface diffusion towards the nanowires. The diffusion dominated growth regime was confirmed by length-radius-plot showing a decrease of the nanowire length at increasing radii. A temperature dependent diffusion model has been utilized to describe the observed nanowire length as a function of the substrate temperature. Beside conventional nanowires, so-called in-plane nanowires which grow along the substrate surface have been studied. Like their vertically growing counterparts, they also tend to grow along <011> in-plane directions which is particularly distinct on Ge(011) substrates. However, the fraction of nanowires which are aligned along <011> is influenced by substrate imperfections which was intentionally affected by means of wet-chemical substrate preparation. In addition to the nanowire growth, techniques for selective catalyst removal as well as for nanowire embedding in an insulating, transparent matrix have been established which can be important prerequisites for further nanowire processing in terms of electric or optoelectronic applications.