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At least 73 records · Page 4

Investigation of PTFE transfer films by infrared emission spectroscopy and phase-locked ellipsometry

When a PTFE sheet was rubbed unidirectionally over a smooth surface of stainless steel an essentially monomolecular transfer film was formed. by ellipsometric and emission infrared spectroscopic techniques it was shown that the film was 10 to 15 A thick and birefringent. From the intensity differences of infrared bands obtained with a polarizer passing radiation polarized in mutually perpendicular planes, it was possible to deduce transfer film orientation with the direction of rubbing. After standing in air for several weeks the transfer films apparently increased in thickness by as much as threefold. At the same time both the index of refraction and the absorption index decreased. Examination of the surfaces by optical and electron microscopies showed that the films had become porous and flaky. These observations were consistent with previous tribological measurements. The coefficients of friction decreased with the formation of the transfer film but increased again as the film developed breaks. The applicability of the ellipsometric and polarized infrared emission techniques to the identification of monomolecular tribological transfer films of polymers such as PTFE has been demonstrated.

Lauer, James L.↗

Thin film characterization using spectroscopic ellipsometry

The application of the multiple angle and wavelength (MAW) technique to measure the dielectric function of semiconducting films is discussed. This technique evaluates unambiguously the complex dielectric function, epsilon (E), of the film without any pre-assumptions. In some cases the effective medium approximation (EMA) was used to determine the volume fraction of the film components. Application of the MAW technique to several semiconducting films was published previously. Different applications and examples are given, including metal and insulator films.

Alterovitz, Samuel A.↗

Use of Variable Angle Spectroscopic Ellipsometry in Order to Determine Contaminant Optical Properties

In order to measure contaminant levels found in the manufacture of the Redesigned Solid Rocket Motor (RSRM), optical properties of the contaminants are needed to develop standards for calibration purposes. Specific to our efforts is the determination of the complex index of refraction for a hydrocarbon mixture and a commercial methyl siloxane. Using ellipsometric measurements with multiple angles of incident and a range of wavelengths in the near infrared a determination of the index of refraction and the extinction coefficient were made for the contaminants. This paper will present the optical techniques and modeling approach used to determine these optical constants of the hydrocarbon mixture and the methyl siloxane studied.

Hughes, C.↗

Analysis of Molecular Contamination on Genesis Collectors Through Spectroscopic Ellipsometry

Before the spacecraft returned to Earth in September, the Genesis mission had a preliminary assessment plan in place for the purpose of providing information on the condition and availability of collector materials to the science community as a basis for allocation requests. One important component of that plan was the evaluation of collector surfaces for molecular contamination. Sources of molecular contamination might be the on-orbit outgassing of spacecraft and science canister components, the condensation of thruster by-products during spacecraft maneuvers, or the condensation of volatile species associated with reentry. Although the non-nominal return of the Genesis spacecraft introduced particulate contamination to the collectors, such as dust and heatshield carbon-carbon, it is unlikely to have caused any molecular deposition. The contingency team's quick action in returning the damaged payload the UTTR cleanroom by 6 PM the evening of recovery help to ensure that exposure to weather conditions and the environment were kept to a minimum.

McNamara, K. M.↗

Genesis Preliminary Examination: Ellipsometry Overview

The Genesis spacecraft returned to Earth on September 8, 2004, experiencing a non-nominal reentry in which both the drogue and main parachutes failed to deploy causing the capsule to impact the surface of the UTTR desert at a speed of approximately 310 kph (193 mph). The impact caused severe damage to the capsule and a breach of the science canister in the field. The science canister was recovered and transported to the cleanroom at UTTR within approximately 8 hours of reentry. Although the ground water table did not rise to canister level before removal, damp soil and debris from the heat shield and other spacecraft components did enter the canister and contaminate some collector surfaces. The objective of preliminary examination of the Genesis collectors is to provide the science community with the information necessary to request the most useful samples for their analysis.

Stansbery, E. K.↗

Small modulation ellipsometry

In an ellipsometer, a phase-modulated, polarized light beam is applied to a sample, electrical signals are obtained representing the orthogonal planes of polarization of the light after it has interacted with the sample and the constants of the sample are calculated from the two resulting electrical signals. The phase modulation is sufficiently small so that the calibration errors are negligible. For this purpose, the phase modulator phase modulates the light within a range of no more than ten degrees modulations peak to peak. The two electrical signals are expanded by Fourier analysis and the coefficients thereof utilized to calculate psi and delta.

Ducharme, Stephen P.↗

Enhancement of Aviation Fuel Thermal Stability Characterization Through Application of Ellipsometry

ASTM D3241/Jet Fuel Thermal Oxidation Tester (JFTOT) procedure, the standard method for testing thermal stability of conventional aviation turbine fuels is inherently limited due to the subjectivity in the color standard for tube deposit rating. Quantitative assessment of the physical characteristics of oxidative fuel deposits provides a more powerful method for comparing the thermal oxidation stability characteristics of fuels, especially in a research setting. We propose employing a Spectroscopic Ellipsometer to determine the film thickness and profile of oxidative fuel deposits on JFTOT heater tubes. Using JP-8 aviation fuel and following a modified ASTM D3241 testing procedure, the capabilities of the Ellipsometer will be demonstrated by measuring oxidative fuel deposit profiles for a range of different deposit characteristics. The testing completed in this report was supported by the NASA Fundamental Aeronautics Subsonics Fixed Wing Project

Browne, Samuel Tucker↗

Sputter process investigation: Material and environment interaction processes investigation

The multilayer Ellipsometry program has been developed with which the thickness and the optical properties of top layer can be determined with the additional information obtained from other measurement such as the optical constant of the middle layer film. Once the proper parameters are input into the program, the multilayer Ellipsometry program which was developed by H. Kim and Dr. Fromhold gives the best possible set of the solutions for the top layer thickness or its optical index graphically on a PC screen. In this report the basic two layer Ellipsometry theory will be summarized briefly as well as the one layer case. All the code is written in Microsoft Quickbasic version 4.5 for IBM PC with a VGA color graphics monitor so that the measurement could be cross-checked out graphically on the screen.

Williams, John R.↗

Ellipsometric studies of sputtered silicon nitride on n-GaAs

Ellipsometry, which is the study of optical systems through their effect on polarized light, is a nondestructive technique offering extremely high sensitivity and in situ operation. One of the intriguing possibilities is to make use of the high sensitivity of ellipsometry for studying the very thin interface between an insulating film and a semiconductor substrate. Researchers have been especially interested in native or anodic oxides. In a recent study, Aspnes and Theeten used ellipsometry to study the interface between silicon and its thermally grown oxide, SiO2. These authors were able to conclude that the interface consisted of a 7 +/- 2 A graded region of atomically mixed silicon and oxygen. In this paper we report both analysis and experimental results for the system: sputtered silicon nitride on (100) n-type gallium arsenide.

Peng, Y. K.↗

Materials, structures, and devices for high-speed electronics

Advances in materials, devices, and instrumentation made under this grant began with ex-situ null ellipsometric measurements of simple dielectric films on bulk substrates. Today highly automated and rapid spectroscopic ellipsometers are used for ex-situ characterization of very complex multilayer epitaxial structures. Even more impressive is the in-situ capability, not only for characterization but also for the actual control of the growth and etching of epitaxial layers. Spectroscopic ellipsometry has expanded from the research lab to become an integral part of the production of materials and structures for state of the art high speed devices. Along the way, it has contributed much to our understanding of the growth characteristics and material properties. The following areas of research are summarized: Si3N4 on GaAs, null ellipsometry; diamondlike carbon films; variable angle spectroscopic ellipsometry (VASE) development; GaAs-AlGaAs heterostructures; Ta-Cu diffusion barrier films on GaAs; GaAs-AlGaAs superlattices and multiple quantum wells; superconductivity; in situ elevated temperature measurements of III-V's; optical constants of thermodynamically stable InGaAs; doping dependence of optical constants of GaAs; in situ ellipsometric studies of III-V epitaxial growth; photothermal spectroscopy; microellipsometry; and Si passivation and Si/SiGe strained-layer superlattices.

Woollam, John A.↗

Gold Nanoparticle Labels Amplify Ellipsometric Signals

The ellipsometric method reported in the immediately preceding article was developed in conjunction with a method of using gold nanoparticles as labels on biomolecules that one seeks to detect. The purpose of the labeling is to exploit the optical properties of the gold nanoparticles in order to amplify the measurable ellipsometric effects and thereby to enable ultrasensitive detection of the labeled biomolecules without need to develop more-complex ellipsometric instrumentation. The colorimetric, polarization, light-scattering, and other optical properties of nanoparticles depend on their sizes and shapes. In the present method, these size-and-shape-dependent properties are used to magnify the polarization of scattered light and the diattenuation and retardance of signals derived from ellipsometry. The size-and-shape-dependent optical properties of the nanoparticles make it possible to interrogate the nanoparticles by use of light of various wavelengths, as appropriate, to optimally detect particles of a specific type at high sensitivity. Hence, by incorporating gold nanoparticles bound to biomolecules as primary or secondary labels, the performance of ellipsometry as a means of detecting the biomolecules can be improved. The use of gold nanoparticles as labels in ellipsometry has been found to afford sensitivity that equals or exceeds the sensitivity achieved by use of fluorescence-based methods. Potential applications for ellipsometric detection of gold nanoparticle-labeled biomolecules include monitoring molecules of interest in biological samples, in-vitro diagnostics, process monitoring, general environmental monitoring, and detection of biohazards.

Venkatasubbarao, Srivatsa↗

Scalable aqueous-phase fabrication of reduced graphene oxide nanofiltration membranes by an integrated roll-to-roll (R2R) process

Economic fractionation of multicomponent biomass-derived streams is a key challenge in biobased fuels and chemicals production. Kraft black liquor (BL) is generated at ~1 billion tons/yr globally from biomass pulping and contains ~15wt% total solids including lignin, hemicellulose fragments, and inorganics. Membrane-based BL concentration is attractive but challenged by low solute rejections and poor stability in BL, which combines alkaline pH (~13), high dissolved solids content (15+ wt%) and high temperature (70–85°C). Here we discuss the scaled fabrication and characterization of reduced graphene oxide (rGO) nanofiltration membranes by slot die coating on a roll-to-roll (R2R) with integrated vacuum filtration. Here, we obtain high-quality 90×30 cm rGO membranes (referred to as “R2R-rGO membranes” in this work) with ~100 nm average thickness supported on porous poly(ethersulfone) (PES) sheets, and an effective area of 2700cm 2 . We present characterizations of their microstructure and uniformity as mapped over large areas by scanning electron microscopy (SEM), ellipsometry, adhesion test and X-ray photoelectron spectroscopy (XPS). The constructed ellipsometry model for the rGO membrane/PES substrate composite was successfully applied to 48 different locations of the R2R-rGO membranes. The R2R-rGO membranes showed >98% lignin rejection with a steady state flux of ~12 LMH at 50bar in a 15.7wt% total solids (TS) kraft BL stream at 72°C and 2–3 gal/min crossflow rates. Slot die coating on a R2R platform with integrated vacuum filtration can enable rapid fabrication of high-quality GO membranes at scale without organic solvents or volatile organic compounds.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Tackling Disorder in γ‐Ga 2 O 3

Abstract Ga 2 O 3 and its polymorphs are attracting increasing attention. The rich structural space of polymorphic oxide systems such as Ga 2 O 3 offers potential for electronic structure engineering, which is of particular interest for a range of applications, such as power electronics. γ‐Ga 2 O 3 presents a particular challenge across synthesis, characterization, and theory due to its inherent disorder and resulting complex structure–electronic‐structure relationship. Here, density functional theory is used in combination with a machine‐learning approach to screen nearly one million potential structures, thereby developing a robust atomistic model of the γ‐phase. Theoretical results are compared with surface and bulk sensitive soft and hard X‐ray photoelectron spectroscopy, X‐ray absorption spectroscopy, spectroscopic ellipsometry, and photoluminescence excitation spectroscopy experiments representative of the occupied and unoccupied states of γ‐Ga 2 O 3 . The first onset of strong absorption at room temperature is found at 5.1 eV from spectroscopic ellipsometry, which agrees well with the excitation maximum at 5.17 eV obtained by photoluminescence excitation spectroscopy, where the latter shifts to 5.33 eV at 5 K. This work presents a leap forward in the treatment of complex, disordered oxides and is a crucial step toward exploring how their electronic structure can be understood in terms of local coordination and overall structure.

36 MATERIALS SCIENCE↗

Atomic Layer Deposition of Nickel Using Ni(dmamb)2 and ZnO Adhesion Layer Without Plasma

Abstract In this study, a novel deposition technique that utilizes diethylzinc (C 4 H 10 ZnO) with H 2 O to form a ZnO adhesion layer was proposed. This technique was followed by the deposition of vaporized nickel(II) 1-dimethylamino-2-methyl-2-butoxide (Ni(dmamb) 2 ) and H 2 gas to facilitate the deposit of uniform layers of nickel on the ZnO adhesion layer using atomic layer deposition. Deposition temperatures ranged from 220 to 300 °C. Thickness, composition, and crystallographic structure results were analyzed using spectroscopic ellipsometry, scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and X-ray diffraction (XRD), respectively. An average growth rate of approximately 0.0105 angstroms per cycle at 260 °C was observed via ellipsometry. Uniform deposition of ZnO with less than 1% of Ni was displayed by utilizing the elemental analysis function via SEM, thereby providing high-quality images. XPS revealed ionizations consistent with nickel and ZnO through the kinetic and binding energies of each detected electron. XRD provided supplemental information regarding the validity of ZnO by exhibiting crystalline attributes, revealing the presence of its hexagonal wurtzite structure.

Baker, Kaiya↗

Mixed Tin-Titanium Oxides by Atomic Layer Deposition on Planar Substrates: Physical and Electronic Structure

Ternary atomic layer deposition of Sn-doped TiO x (Sn:TiO x ) and Ti-doped SnO x (Ti:SnO x ) was performed using tetrakisdimethylamidotitanium (IV) and tin(IV) with water at 150 °C on (1 0 0) Si and quartz substrates. The physical structure of the films was investigated using scanning electron, atomic force, and Kelvin probe force microscopies as well as spectroscopic ellipsometry, Raman spectroscopy, and X-ray diffraction. All as-deposited films are amorphous and possessed flat and conformal topographies with low surface roughness (<1 nm). Annealed Sn:TiO x and Ti:SnO x crystallize into the tetragonal anatase TiO 2 and cassiterite SnO 2 structures, respectively, without large variations to the film topography. The chemical composition of the as-deposited and annealed films was investigated through X-ray photoelectron spectroscopy. While dopants are homogenously mixed, the ternary ALD to form Sn:TiO x and Ti:SnO x surprisingly does not follow the rule of mixtures, despite similarities in both the growth rates of binary SnO x and TiO x and the precursors used. This finding is also supported by spectroscopic ellipsometry. Here, we postulate the deviation from the rule of mixtures is due to non-ideal surface chemistry of the binary ALD of SnO x . The optical bandgap of all films was quantified by the Tauc analysis and the valence band position was investigated by valence band X-ray photoelectron spectroscopy. Intra-bandgap states above the valence band maximum were observed for as-deposited Ti:SnO x and Sn:TiO x and ascribed to 5 s states from Sn 2+ ions. The presence of these intra-bandgap states induces enhanced visible absorption and bathochromic shifts to the apparent bandgap for all as-deposited films. Annealing the films removes the intra-bandgap states and increases the optical bandgap. Simplified band diagrams created using the data available demonstrated that the conduction and valence band positions did not vary between the positions of pure TiO 2 or SnO 2 with monotonic increases to the dopant incorporation.

36 MATERIALS SCIENCE↗

Infrared-active phonon modes in single-crystal thorium dioxide and uranium dioxide

The infrared-active phonon modes, in single-crystal samples of thorium dioxide (ThO 2 ) and uranium dioxide (UO 2 ), were investigated using spectroscopic ellipsometry and compared with density functional theory. Both ThO 2 and UO 2 are found to have one infrared-active phonon mode pair [consisting of one transverse optic (TO) and one associated longitudinal optic (LO) mode], which is responsible for the dominant features in the ellipsometric data. Furthermore, at room temperature, our results for the mode pair’s resonant frequencies and broadening parameters are comparable with previous reflectance spectroscopy characterizations and density functional theory predictions. For ThO 2 , our ellipsometry and density function theory results both show that the LO mode broadening parameter is larger than the TO mode broadening. This signifies mode anharmonicity, which can be attributed to the intrinsic phonon–phonon interaction. In addition to the main mode pair, a broad low-amplitude impurity-like vibrational mode pair is detected within the reststrahlen band for both ThO 2 and UO 2 . Elevated temperature measurements were performed for ThO 2 in order to study the mechanisms by which the phonon parameters evolve with increased heat. The observed change in the TO resonant frequency is in excellent agreement with previous density functional calculations, which only consider volume expansion of the crystal lattice. This suggests that the temperature-dependent change in the TO frequency is primarily due to volume expansion. The change in the main mode pair’s broadening parameters is nearly linear within the temperature range of this study, which indicates the intrinsic anharmonic scattering (via cubic anharmonicities) as the main decay mechanism.

36 MATERIALS SCIENCE↗

The 2022 magneto-optics roadmap

Abstract Magneto-optical (MO) effects, viz. magnetically induced changes in light intensity or polarization upon reflection from or transmission through a magnetic sample, were discovered over a century and a half ago. Initially they played a crucially relevant role in unveiling the fundamentals of electromagnetism and quantum mechanics. A more broad-based relevance and wide-spread use of MO methods, however, remained quite limited until the 1960s due to a lack of suitable, reliable and easy-to-operate light sources. The advent of Laser technology and the availability of other novel light sources led to an enormous expansion of MO measurement techniques and applications that continues to this day (see section 1). The here-assembled roadmap article is intended to provide a meaningful survey over many of the most relevant recent developments, advances, and emerging research directions in a rather condensed form, so that readers can easily access a significant overview about this very dynamic research field. While light source technology and other experimental developments were crucial in the establishment of today’s magneto-optics, progress also relies on an ever-increasing theoretical understanding of MO effects from a quantum mechanical perspective (see section 2), as well as using electromagnetic theory and modelling approaches (see section 3) to enable quantitatively reliable predictions for ever more complex materials, metamaterials, and device geometries. The latest advances in established MO methodologies and especially the utilization of the MO Kerr effect (MOKE) are presented in sections 4 (MOKE spectroscopy), 5 (higher order MOKE effects), 6 (MOKE microscopy), 8 (high sensitivity MOKE), 9 (generalized MO ellipsometry), and 20 (Cotton–Mouton effect in two-dimensional materials). In addition, MO effects are now being investigated and utilized in spectral ranges, to which they originally seemed completely foreign, as those of synchrotron radiation x-rays (see section 14 on three-dimensional magnetic characterization and section 16 on light beams carrying orbital angular momentum) and, very recently, the terahertz (THz) regime (see section 18 on THz MOKE and section 19 on THz ellipsometry for electron paramagnetic resonance detection). Magneto-optics also demonstrates its strength in a unique way when combined with femtosecond laser pulses (see section 10 on ultrafast MOKE and section 15 on magneto-optics using x-ray free electron lasers), facilitating the very active field of time-resolved MO spectroscopy that enables investigations of phenomena like spin relaxation of non-equilibrium photoexcited carriers, transient modifications of ferromagnetic order, and photo-induced dynamic phase transitions, to name a few. Recent progress in nanoscience and nanotechnology, which is intimately linked to the achieved impressive ability to reliably fabricate materials and functional structures at the nanoscale, now enables the exploitation of strongly enhanced MO effects induced by light–matter interaction at the nanoscale (see section 12 on magnetoplasmonics and section 13 on MO metasurfaces). MO effects are also at the very heart of powerful magnetic characterization techniques like Brillouin light scattering and time-resolved pump-probe measurements for the study of spin waves (see section 7), their interactions with acoustic waves (see section 11), and ultra-sensitive magnetic field sensing applications based on nitrogen-vacancy centres in diamond (see section 17). Despite our best attempt to represent the field of magneto-optics accurately and do justice to all its novel developments and its diversity, the research area is so extensive and active that there remains great latitude in deciding what to include in an article of this sort, which in turn means that some areas might not be adequately represented here. However, we feel that the 20 sections that form this 2022 magneto-optics roadmap article, each written by experts in the field and addressing a specific subject on only two pages, provide an accurate snapshot of where this research field stands today. Correspondingly, it should act as a valuable reference point and guideline for emerging research directions in modern magneto-optics, as well as illustrate the directions this research field might take in the foreseeable future.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Challenges in atomic layer etching of gallium nitride using surface oxidation and ligand-exchange

Two atomic layer etching (ALE) methods were studied for crystalline GaN, based on oxidation, fluorination, and ligand exchange. Etching was performed on unintentionally doped GaN grown by hydride vapor phase epitaxy. For the first step, the GaN surfaces were oxidized using either water vapor or remote O 2 -plasma exposure to produce a thin oxide layer. Removal of the surface oxide was addressed using alternating exposures of hydrogen fluoride (HF) and trimethylgallium (TMG) via fluorination and ligand exchange, respectively. Several HF and TMG super cycles were implemented to remove the surface oxide. Each ALE process was monitored in situ using multiwavelength ellipsometry. X-ray photoelectron spectroscopy was employed for the characterization of surface composition and impurity states. Additionally, the thermal and plasma-enhanced ALE methods were performed on patterned wafers and transmission electron microscopy (TEM) was used to measure the surface change. The x-ray photoelectron spectroscopy measurements indicated that F and O impurities remained on etched surfaces for both ALE processes. Ellipsometry indicated a slight reduction in thickness. TEM indicated a removal rate that was less than predicted. In conclusion, we suggest that the etch rates were reduced due to the ordered structure of the oxide formed on crystalline GaN surfaces.

36 MATERIALS SCIENCE↗