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Paper des Monats
- ja (2)
We compare standard and inverted bulk heterojunction solar cells composed of PCPDTBT:PC70BM
blends. Inverted devices comprising 100 nm thick active layers exhibited short circuit currents of
15 mA/cm², 10% larger than in corresponding standard devices. Modeling of the optical field distribution
in the different device stacks proved that this enhancement originates from an increased absorption of
incident light in the active layer. Internal quantum efficiencies (IQEs) were obtained from the direct
comparison of experimentally derived and modeled currents for different layer thicknesses, yielding IQEs
of ~70% for a layer thickness of 100 nm. Simulations predict a significant increase of the light harvesting
efficiency upon increasing the layer thickness to 270 nm. However, a continuous deterioration of the
photovoltaic properties with layer thickness was measured for both device architectures, attributed to
incomplete charge extraction. On the other hand, our optical modeling suggests that inverted devices
based on PCPDTBT should be able to deliver high power conversion efficiencies (PCEs) of more than
7% provided that recombination losses can be reduced.
The aim of this study is to develop nanometer-thin epoxy-based films on aluminium alloy AA2024-T3 as a model coating system for high resolution corrosion studies. Spin coating was used for the layer-by-layer (LbL) deposition of poly-(ethylenimine) (PEI) and poly([o-cresyl glycidyl ether]-co-formaldehyde) (CNER) bilayers. The film chemistry and the cross-linking process were characterized by means of Fourier-transform infrared spectroscopy (FTIR).
Ellipsometric data confirmed the linear increase of film thickness. The potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) results indicate the improvement of the film barrier properties with increasing film thickness. Mapping of the topography and the volta potential was performed by means of scanning Kelvin probe force microscopy (SKPFM).
The results indicate the presence of a homogeneous film structure, while the intermetallic phases can still be identified below the coating. The SKPFM Analysis confirmed that the model films are suitable for investigation of corrosion processes at the coating/metal interface.
Mechanical stress often accelerates the failure of polymer materials. The aim of this research is to study the interaction between the sealing material FKM and biofuels B10 (heating oil with 10% biodiesel). The mechanical stress test was carried out in a special apparatus. Both mechanical and non-mechanical stress tests were conducted on specimens at 20, 40, and 70 °C for 28 days to document changes in mass, volume, and tensile properties. Both increasing temperature and mechanical stress have a significant effect on the tensile strength of the FKM polymer when exposed to B10. The combination of increasing temperature and mechanical stress induced rupture within 2 h. It was also established that FKM polymer with pre-exposure in B10 survived longer during mechanical stress compared to specimens exposed only to air. With the support of infrared (IR) spectroscopy, we were able to confirm the penetration of B10 into the FKM polymer.
Auf dem Weg zu Industrie 4.0: Bestimmung von Messunsicherheitsbudgets in der Oberflächentechnik
(2019)
Vorgestellt wurde die Bestimmung von Messunsicherheitsbudgets für sehr unterschiedliche physikalische Größen, die in der Oberflächentechnik von hoher Relevanz sind: Stufenhöhe h, Schichtdicke d, Eindringhärte HIT und Haftfestigkeit. Die Unterschiede betreffen die Art der Prüfmethodik (optisch zerstörungsfrei vs. mechanisch invasiv/zerstörend), die laterale Größe des Integrationsgebietes der Messung (lokal: nano bis sub-mikro vs. global: mikro bis makro) und die Art der Bestimmung von Messunsicherheitsbudgets (physikalische Größen: direkt rückführbar; Werkstoffkenngröße: genormt; Systemkenngröße: genormt).
Im Rahmen von Industrie 4.0 werden ausgehend der geforderten Spezifikation des beschichteten Produkts (Mittelwert mit Vertrauensbereich oder Mindestwert) durchgehende Toleranzbänder zur Oberflächenmodifizierung/Beschichtung des Substrats, einhergehend mit Prozessfenstern, die diese Toleranzbänder garantieren, erforderlich, die zuverlässig erfasst werden müssen. Die Frage der anzuwendenden Mess- und Prüftechnik und die damit notwendige Betrachtung von Messunsicherheitsbudgets ist für die Digitalisierung von Konditionierungs-, Zustands-, Regel- und Steuergrößen unverzichtbar. Mit Blick auf die Einhaltung von Prozessfenstern und die dafür notwendige Prozessführung wird technologisches Kern-Know-how digitalisiert, das es unbedingt zu schützen gilt. Nur lokale Netze können diese Sicherheit garantieren, in globalen Netzen ist die Datensicherheit bestenfalls maximierbar
In this work, thin iron doped tin oxide layers (3–6 nm) were investigated with regard to gas sensitivity by means of surface plasmon resonance (SPR) effect with ellipsometric readout. The experimental set-up was a Kretschmann configuration with gold as metal layer. The sensor system was exposed to different concentrations of methane in the low ppm range and the sensor response of an uncoated gold layer compared to a gold layer coated with iron doped tin oxide. The additional layer effects stability with regard to drift behavior of the sensor and an increase in sensitivity. Furthermore, the sensor is able to detect the toxic gas carbon monoxide in low concentration range (down to 0.5 ppm). The thin layers were investigated by X-ray photoelectron spectroscopy, secondary electron microscopy and spectroscopic ellipsometry. The possible mechanisms taking place on the surface are discussed.
Standardisation of ellipsometry is mainly based on three documents: pioneering work at NIST [1] on film standards, a publicly available specification and stan-dard testing procedure [2] for real-world samples by BAM and a standard specification for integrated metrology by SEMI [3]. Other activities refer to inter-laboratory comparisons for selected layer/substrate systems and analytical methods including ellipsometry [4] and the development of combined standards for thickness d and step height h [5].
Generally, precision of ellipsmetry in terms of raw data Ψ and Δ meets the major demands for all ellipsometric principles (RPE, RAE, PME, RCE, NE).
As a result, fingerprint capabilty is al-most perfect for various layer/substrate systems. However, this is not true for accuracy in terms of physical quantities such as thickness d, optical (n, k) and dielectric constans (ε1, ε2,) as modelling is required. Hence, the layer/substrate and material dependent validation of models is nowadays a key issue.
In contrast to the sub-nanometer sensi-tivity in vertical direction, the effective lateral resolution of almost all ellipso-metric principles except for imaging null
ellipsometry is rather poor, usually be-yond 100 µm.
Hence, nanometer-scaled homogeneity testing and the measurement of micro- and nanopatterned structures is not feasible by standard configurations.
Functionality of optical systems requires optical coatings of
high quality which have to be adapted to the application in
terms of the performance of optical parameters such as
reflectivity (AR, low, defined, high), the substrate material of
interest (polymers, ceramics, and glass), the environmental
conditions (such as temperature or humidity), and the service
conditions (such spectral range and power density). Moreover,
in many cases, additional non-optical requirements have
to be met, including mechanical features such as scratch
resistance, hardness and modulus.
Consequently, thickness and overall uniformity requirements
are steadily increasing. In general, these demands can usually
not be achieved by a single film or coating. Instead, films with
specific design features (such as gradients), layer stacks and
multilayers are a prerequisite for high quality layers and their
reliability. For the development of such layer systems, a
versatile cluster deposition system consisting of three clusters
and a cluster-to-cluster handler has been designed. Besides a
PECVD cluster for DLC coatings, two PVD clusters implement
ion assisted electron beam evaporation and plasmabased
sputter technology. In addition to metallic films, preparation
of oxide and nitride optical coatings (SiO2, TiO2, Ta2O5,
ITO, Al2O3, TiN, AlN) in various process modifications (nonreactive,
partially reactive, full-reactive; rf-, dc-, mf- mode;
PEM control) has been carried out.
Within this paper, the effect of several process parameters on
layer quality (optical constants, density, and uniformity) is
discussed for selected applications examples (AR- and HR
coatings, applications at elevated temperatures and applications
of enhanced mechanical performance).
It has been shown that specific features of ion and plasma
assisted PVD processes, including ion-beam and plasma preand
post-treatment of substrates and layer systems, may
widen the application range and improve functionality features
of given coating/substrate systems.
Die Oberflächentechnik ist eine Schlüsseltechnologie in nahezu zu allen industriellen Branchen. Mit Ausnahme der mechanischen Stabilität, die das Substrat bereitstellt, werden verschiedenartigste Funktionen materialsparend, zum Teil hochintegriert mit maßgeschneiderten Schichtdesigns unter Ausnutzung von Nano- und Quanteneffekten auf Oberflächen appliziert. Ein Großteil der Fertigungskosten in der Mikro- und Nanotechnik wird durch Reinräume und die Umsetzung ausgeklügelter Reinigungsstrategien zur Vermeidung von Restverschmutzungen und partikulären Belegungen
verursacht, da diese unweigerlich zum Bauteilversagen führen. Die Validierung des Reinigungszustandes ist somit von zentraler Bedeutung für die Schichtqualität und Produktfunktionalität. Dies gilt in Abhängigkeit von der Applikation und den vertikalen Schicht- bzw. lateralen Strukturdimensionen sowohl für Fertigungsprozesse im Reinraum als auch für solche in robuster Umgebung. In der Praxis kommt es häufig vor, dass man mikroskopisch scheinbar saubere Substrate erst durch die Beschichtung „enttarnt" und dann Defekte oft mit bloßem Auge sichtbar werden. Noch problematischer ist der Einbau von Verunreinigungen während der Schichtabscheidung, die zunächst nicht sichtbar sind, dann aber zum Bauteilversagen führen.
Public, hidden, and forensic features either encoded or directly legible are used for authentication. Fabry-Perot layer stacks as information carriers in combination with imaging ellipsometry as optical read-out system provide all-in-one anti-counterfeiting capability that may establish the new security level 'encoded forensic'. Different layer designs are described with regard to all three security levels: public features (e.g. color and tilt effect) perceptible by the human eye, hidden features (e.g. spectroscopic response in the UV or IR), and forensic features (ellipsometric quantities Ψ and Δ as a function of wavelength λ and angle of incidence AOI). Physically uncloneable functions (PUF) could be realized as a result of a multi-material and a multi-parameter deposition approach as well as by means of specific design features of the Fabry-Perot layer stack. Hence, they are not subject to any reverse engineering strategies. Examples of stratified, micro-structured, and laser-modified Fabry-Perot layer systems are considered that may be used at all perception levels (e.g. human eye, bar code reader, and imaging ellipsometry) for authentication against product counterfeiting and related areas. --------------------------------------------------------------------------------------------------------------------
Zur Authentifizierung werden offene, versteckte und forensische Merkmale entweder codiert oder direkt auslesbar verwendet. Mit Fabry-Perot Schichtsystemen als Informationsträger in Kombination mit der abbildenden Ellipsometrie als optischem Auslesesystem steht ein 'all-in-one' Fälschungsschutz-System zur Verfügung, das ein neues Sicherheitsniveau 'kodiert-forensisch' darstellt. Es werden unterschiedliche Schichtdesigns beschrieben, mit denen alle drei Sicherheitsniveaus realisiert werden können: offene Merkmale (z.B. Farbe und Kippeffekt), die mit dem menschlichen Auge wahrnehmbar sind, versteckte Merkmale (z.B. die spektrale Antwort im Sichtbaren oder im IR) sowie forensische Merkmale (ellipsometrische Größen Ψ und Δ als Funktion der Wellenlänge λ und des Einfallswinkels AOI).
Physikalisch nicht klonbare Funktionen (PUF) können im Ergebnis einer Multi-Material- und Multi-Parameter Beschichtungsstrategie sowie durch spezifische Design-Merkmale des Fabry-Perot Schichtsystems realisiert werden. Folglich sind solche Schichtsysteme dem 'reverse engineering' nicht zugänglich. Es werden Beispiele für lateral ausgedehnte, mikrostrukturierte und Laser modifizierte Schichtsysteme auf verschiedenen Ausleseniveaus (menschliches Auge, Barcode-Lesegerät, abbildendes Ellipsometer) vorgestellt, die zur Authentifizierung von Produkten und verwandte Gebiete geeignet sind.
The irradiation of ~0.9-µm-thick hydrogenated amorphous carbon (a-C:H) layers deposited on silicon substrates with single femtosecond (fs) laser pulses (35 fs pulse duration, 790 nm centre wavelength) in air is studied experimentally. Irradiation spots have been generated with different peak fluences and subsequently investigated by optical topometry, micro Raman spectroscopy and microscale mechanical indentation in order to evaluate their microscopic, topographical, structural and mechanical properties (e.g. elastic modulus). By this multi-method approach, a clear separation of different effects (delamination and graphitisation) becomes possible. The joint application of mechanical and spectroscopic techniques provides unique insights into the effects of the fs-laser radiation on the carbon layer.
The thickness measurement of transparent layers with optical techniques is very problematic. The observed deviations can easily reach 100% of the layer thickness to be measured. In order to analyse these deviations, tactile reference measurements have been developed. The proposed method is based on contact mode measurements with low contact pressure. With stylus instruments, this can be realized either by using the recommended tip radius of 2 µm and very small probing forces in the micronewton range (and low scanning speeds of 50 µm s-1) or by using the recommended probing force of 750 µN, but a large probing tip radius. Three metal layers on silicon or silicon dioxide and two polymer resist materials on a thin chromium adhesive layer on silicon are used as artefacts. The comparison of the optical measurements with the tactile reference values disclosed deviations of the optical measurements of up to 195% of the layer thickness. Layer thicknesses were between 200 nm and 4 µm. This paper analyses the deviations of two white light interference microscopes, one phase shift interference microscope, one confocal microscope, one autofocus sensor, a chromatic sensor, an interferometric film thickness sensor and one spectroscopic ellipsometer. Simple and well-known expressions for the description of the observed deviations are presented and discussed. The order of magnitude of the observed deviations can be described well by these correction formulas but further investigations are necessary in order to better understand the systematic deviations of optical surface measuring instruments on non-cooperating surfaces.
Single-pulse damage thresholds of hydrogenated amorphous carbon (a-C:H) films were measured for 8-ns laser pulses at 532-nm wavelength. Layer thicknesses from below the optical penetration depth to above the thermal diffusion length (60 nm13 µm) were examined. After correction of the damage-threshold values for the fraction of energy effectively absorbed by the material, the damage threshold was found to increase linearly with the layer thickness, also for film thicknesses below the optical penetration depth of a-C:H. The threshold fluence reached the bulk value for a layer thickness equal to the thermal diffusion length. The thermal diffusion coefficient was obtained from fitting the experimental data. Several phenomena like graphitization, blistering, exfoliation, and ablation were observed for different fluence regimes and film thicknesses.
Hybrid optical measurement technique for detection of defects in epitaxially grown 4H-SiC layers
(2022)
Recent developments in power electronics require the use of new wide bandgap compound semiconductor. We demonstrate the use of the ellipsometry and white light interference microscopy to detect defects in epitaxially grown SiC layers on SiC substrates. Such hybrid optical metrology methods can be used to better understand the mechanism of the development of the defects as well as their effects on the material´s optoelectronic properties.
Critical defects, also known as device killers, in wide bandgap semiconductors significantly affect the performance of power electronic devices. We used the methods imaging ellipsometry (IE) and white light interference microscopy (WLIM) in a hybrid optical metrology study for fast and non-destructive detection, classification, and characterisation of defects in 4H–SiC homoepitaxial layers on 4H–SiC substrates. Ellipsometry measurement results are confirmed by WLIM. They can be successfully applied for wafer characterisation already during production of SiC epilayers and for subsequent industrial quality control.
Background: Gas sensors are very important in several fields like gas monitoring, safety and environmental applications. In this approach, a new gas sensing concept is investigated which combines the powerful adsorption probability of metal oxide conductive sensors (MOS) with an optical ellipsometric readout. This concept Shows promising results to solve the problems of cross sensitivity of the MOS concept.
Results: Undoped tin oxide (SnOx) and iron doped tin oxide (Fe:SnOx) thin add-on films were prepared by magnetron sputtering on the top of the actual surface plasmon resonance (SPR) sensing gold layer. The films were tested for their sensitivity to several gas species in the surface plasmon resonance enhanced (SPREE) gas measurement. It was found that the undoped tin oxide (SnOx) shows higher sensitivities to propane (C3H8) then to carbon monoxide (CO). By using Fe:SnOx, this relation is inverted. This behavior was explained by a change of the amount of binding sites for CO in the layer due to this iron doping. For hydrogen (H2) no such relation was found but the sensing ability was identical for both layer materials. This observation was related to a different sensing mechanism for H2 which is driven by the Diffusion into the layer instead of adsorption on the surface.
Conclusion: The gas sensing selectivity can be enhanced by tuning the properties of the thin film overcoating. A relation of the binding sites in the doped and undoped SnOx films and the gas sensing abilities for CO and C3H8 was found. This could open the path for optimized gas sensing devices with different coated SPREE sensors.
In this study, thickness related changes of the optical properties of doped tin oxide were studied. Two different sets of samples were prepared. The first set was doped with iron or nickel on silicon substrate with thicknesses of 29–56 nm, the second was iron doped on gold/glass substrate with 1.6–6.3 nm. The optical constants were determined by using spectral ellipsometry (SE) followed by modelling of the dielectric function with an oscillator model using Gaussian peaks. The analysis of the optical constants shows a dependence of the refraction and the absorption on the thickness of the doped tin oxide coating. In addition to the tin oxide absorption in the UV, one additional absorption peak was found in the near-IR/red which is related to plasmonic effects due to the doping. This peak shifts from the near-IR to the red part of the visible spectrum and becomes stronger by reducing the thickness, probably due to the formation of metal nanoparticles in this layer. These results were found for two different sets of samples by using the same optical model. Afterwards the second sample set was tested in the Surface Plasmon Resonance Enhanced Ellipsometric (SPREE) gas measurement with CO gas. It was found that the thickness has significant influence on the sensitivity and thus the adsorption of the CO gas. By increasing the thickness from 1.6 nm to 5.1 nm, the sensing ability is enhanced due to a higher coverage of the surface with the over coating. This is explained by the high affinity of CO molecules to the incorporated Fe-nanoparticles in the tin oxide coating. By increasing the thickness further to 6.3 nm, the sensing ability drops because the layer disturbs the SPR sensing effect too much.
Single Femtosecond Laser-Pulse-Induced Superficial Amorphization and Re-Crystallization of Silicon
(2021)
Superficial amorphization and re-crystallization of silicon in <111> and <100> orientation after irradiation by femtosecond laser pulses (790 nm, 30 fs) are studied using optical imaging and transmission electron microscopy. Spectroscopic imaging ellipsometry (SIE) allows fast data acquisition at multiple wavelengths and provides experimental data for calculating nanometric amorphous layer thickness profiles with micrometric lateral resolution based on a thin-film layer model. For a radially Gaussian laser beam and at moderate peak fluences above the melting and below the ablation thresholds, laterally parabolic amorphous layer profiles with maximum thicknesses of several tens of nanometers were quantitatively attained. The accuracy of the calculations is verified experimentally by high-resolution transmission electron microscopy (HRTEM) and energy dispersive X-ray spectroscopy (STEM-EDX). Along with topographic information obtained by atomic force microscopy (AFM), a comprehensive picture of the superficial re-solidification of silicon after local melting by femtosecond laser pulses is drawn.
Abstract. In power electronics, compound semiconductors with large bandgaps, like silicon carbide (SiC), are increasingly being used as material instead of silicon. They have a lot of advantages over silicon but are also intolerant of nanoscale material defects, so that a defect inspection with high accuracy is needed. The different defect types on SiC samples are measured with various measurement methods, including optical and tactile methods. The defect types investigated include carrots, particles, polytype inclusions and threading dislocations, and they are analysed with imaging ellipsometry, coherent Fourier scatterometry (CFS), white light interference microscopy (WLIM) and atomic force microscopy (AFM). These different measurement methods are used to investigate which method is most sensitive for which type of defect to be able to use the measurement methods more effectively. It is important to be able to identify the defects to classify them as critical or non-critical for the functionality of the end product. Once these investigations have been completed, the measurement systems can be optimally distributed to the relevant defects in further work to realize a hybrid analysis of the defects. In addition to the identification and classification of defects, such a future hybrid analysis could also include characterizations, e.g. further evaluation of ellipsometric data by using numerical simulations.
The different defect types on SiC samples are measured with various measurement methods including optical and tactile methods. The defect types investigated include particles, carrots and triangles and they are analyzed with imaging ellipsometry, coherent Fourier scatterometry and atomic force microscopy. Each of these methods measures different properties of the defects and they all together contribute to a complete analysis.
Surface damage and color centers generated by femtosecond pulses in borosilicate glass and silica
(2003)
Hydrogen-containing amorphous carbon layers as optical materials for the NIR and MIR spectral range
(2006)
On the use of plasma-deposited thin films for gas sensors with read-out based on the SPR effect
(2012)
Qualitätssicherung für Schichtsysteme aus Ionenstrahl- und Plasmaprozessen mit optischen Methoden
(2005)
Optical vs. mivroscopic properties of ECR and RF bias generated amoephous hydrogenated carbon films
(2010)
Ellipsometry has been an extremely successful and fast expanding method in the past decades along with other related techniques using polarisation sensitive measurements. Opening new fields of application for a successful measurement technique brings some requirements and issues that have to be solved. From a metrological point of view, ellipsometry has the problem that uncertainties are difficult to determine for model-based analysis techniques in general. In this presentation, we will explore how the usefulness of polarimetric methods like ellipsometry can be increased.
Ellipsometry as a method could profit from several current developments which will be discussed in this presentation:
• Standardisation initiatives on national and international level developing standards for best practice when using ellipsometry. A series of at least six standards is currently developed on national German and international level covering different levels of sample complexity.
• Projects on traceability of ellipsometry and structured surface spectrometry as well as new dielectric function database initiatives.
• Metadata handling and data ontology providing a better framework for exchange and collaborative use of research data.
We will also explore the quantification of measurement uncertainty using examples from projects in which BAM is involved. Examples will be presented of multilayer and non-ideal materials as well as the determination of layer properties for technical applications such as thin layer catalysts and complex polymers. The definition of reference materials will be discussed.
A competitive advantage in the semiconductors industry is gained through the exploitation of new materials and processes, translating into improved components’ performances. This requires a metrological infrastructure allowing reliable nanoscale characterisation of new materials and devices, particularly in terms of their electrical parameters and properties. Traceability and reliability of nanoscale measurements stand as a major challenge for electrical properties (i.e. resistance, impedance) using conductive atomic force microscopy (C-AFM) and scanning microwave microscopy (SMM) techniques. The non-destructive analysis nature of these two methods is of paramount importance for the characterization of devices and components. However, the state of the art still lacks established measurement protocols, easy to use reference standards, well-defined best practice guides and easy to use 3D models to assess environmental and external stimulation effects. Moreover, costly instrumentation, particularly for high-frequency measurements, still hinders efficient advancements in these directions.
ELENA is a 3-years European project that aims at bringing solutions to the aforementioned difficulties. To achieve this goal, the project uses a combination of nanoscale electrodynamic scanning probe methods in combination with optical tools such as spectroscopic ellipsometry on several lateral length scales to determine the electrical properties of layers and small structures.