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At least 37 records · Page 2
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Solvent-Induced Swelling Behaviors of Microphase-Separated Polystyrene- block -Poly(ethylene oxide) Thin Films Investigated Using In Situ Spectroscopic Ellipsometry and Single-Molecule Fluorescence Microscopy

Block copolymers have attracted considerable interest in the fields of nanoscience and nanotechnology, because these polymers afford well-defined nanostructures via self-assembly. An in-depth understanding of solvent effects on the physicochemical properties of these microdomains is crucial for their preparation and utilization. Herein, we employed in situ spectroscopic ellipsometry and single-molecule fluorescence techniques to gain detailed insights into microdomain properties in polystyrene-block-poly(ethylene oxide) (PS-b-PEO) films exposed to ethanol- and water-saturated N 2 . We observed a quick increase and a subsequent gradual decrease in the ellipsometric thickness of PS-b-PEO films upon exposure to ethanol-saturated N 2 . This observation was unexpected because ethanol-saturated N 2 induced negligible thickness change for PS and PEO homopolymer films. The similarity in maximum thickness gain observed under ethanol- and water-saturated N 2 implied the swelling of PEO microdomains. Ethanol vapor permeation through the PEO microdomains was supported by the red-shift of the ensemble and single-molecule fluorescence emission of Nile red in PS-b-PEO films. Single-molecule tracking data showed the initial enhancement and subsequent reduction of the diffusion of hydrophilic sulforhodamine B molecules in PS-b-PEO films upon exposure to ethanol-saturated N 2 , consistent with the spectroscopic ellipsometry results. Furthermore, the higher ethanol susceptibility of the PEO microdomains was attributable to their amorphous nature, as shown by FTIR data.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2014

Evolution of optical properties of tin film from solid to liquid studied by spectroscopic ellipsometry and ab initio calculation

The temperature dependent optical properties of tin film from solid to liquid were studied by spectroscopic ellipsometry and ab initio molecular dynamics simulations. The dielectric function of liquid Sn was different from solid, and an interband transition near 1.5 eV was easily observed in solid while it apparently disappeared upon melting. From the evolution of optical properties with temperature, an optical measurement to acquire the melting point by ellipsometry was presented. From first principles calculation, we show that the local structure difference in solid and liquid is responsible for this difference in the optical properties observed in experiment.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Crystallographic orientation of uniaxial calcite and dolomite determined using reflection generalized ellipsometry

In this study, using the two-modulator generalized ellipsometry microscope (2-MGEM), it is shown that it is possible to determine the direction of the optic axis of crystallites of the high birefringence materials calcite and dolomite. 2-MGEM measurements are performed in reflection at near-normal incidence, so sample preparation requires only an optically polished surface. For uniaxial materials, the 2-MGEM measures the direction of the fast axis and the diattenuation, which can then be related to the tilt angle of the optic axis with respect to the surface normal once the maximum diattenuation is known. The optical resolution of the present instrument is 4-6 μm, and areas as large as 1 cm 2 can be measured without distortion. Additionally, the 2-MGEM measures the depolarization, which is a measure of the quality of the data. Using this information, an optical pole figure can be determined. The 2-MGEM results are compared with electron backscatter diffraction (EBSD) measurements on the same samples. Lastly, additional standard spectroscopic generalized ellipsometry measurements at a large angle of incidence were performed on single crystal calcite and dolomite to determine the spectroscopic ordinary and extraordinary refractive indices from 220 nm to 850 nm from which the maximum diattenuation can be determined.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Crystallographic orientation of orthorhombic aragonite using reflection generalized ellipsometry

Here, the 2-modulator generalized ellipsometry microscope (2-MGEM) has been used to study a natural crystal of aragonite. Like its polymorph calcite, aragonite has a large refractive index difference between light polarized parallel to the c-axis and light polarized perpendicular to the c-axis. Unlike calcite, aragonite is orthorhombic, so there is also a very small difference between the refractive indices polarized along the a- and b-directions. As a result, it is not possible to use the 2-MGEM to obtain a definitive map of the optic axis directions of a sample as was possible with calcite, but it is possible to determine approximately the orientation of the c-axis with respect to the surface normal. If the c-axis is in the sample surface plane, it is possible to measure very small deviations of the c-axis direction with an accuracy of ~0.2°. If the c-axis is oriented normal to the sample surface, 2-MGEM data can be used to identify different crystallites due to rotations about the c-axis. For comparison, the orientations of some of the crystallites have also been measured using X-ray Laue and electron beam backscatter diffraction. In addition, spectroscopic generalized ellipsometry measurements have been used to determine the refractive indices of aragonite.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Anisotropic index of refraction and structural properties of hexagonal boron nitride epilayers probed by spectroscopic ellipsometry

The anisotropic index of refraction of 200 μm thick boron-10 enriched hexagonal boron nitride (h-BN) freestanding epilayers grown by metalorganic chemical vapor deposition has been measured using spectroscopic ellipsometry in the UV (4.0–5.1 eV) spectral range. It was found that the index of refraction for the polarization mode with an electric field perpendicular to the c-axis (ordinary, n o ) is much higher than that with an electric field parallel to the c-axis (extraordinary, n e ). By inclusion of turbostratic- (t-) phase layers within h-BN having an average inclination angle (θ) with respect to the ideal c-plane, a simple method for quantifying θ has been deduced. Our results revealed that the presence of t-phase layers decreases the optical anisotropy of h-BN and that a signature of improved crystalline quality is an increase in the ordinary index of refraction (n o ) as a result of the average incline angle θ approaching 0° and predicted that n o = 2.7 and n e = 1.5 at 280 nm for single crystalline h-BN epilayers. More importantly, our results demonstrated that spectroscopic ellipsometry is an effective technique for characterizing the crystalline quality of h-BN epilayers with the advantages of being noninvasive and highly sensitive.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2024

High-field/high-frequency electron spin resonances of Fe-doped β − Ga 2 O 3 by terahertz generalized ellipsometry: Monoclinic symmetry effects

We demonstrate detection and measurement of electron paramagnetic spin resonances (EPR) of iron defects in β − Ga 2 O 3 utilizing generalized ellipsometry at frequencies between 110 and 170 GHz. The experiments are performed on an Fe-doped single crystal in a free-beam configuration in reflection at 45 ∘ and magnetic fields between 3 and 7 T. In contrast with low-field, low-frequency EPR measurements, we observe all five transitions of the s = 5 / 2 high-spin state Fe 3 + simultaneously. We confirm that ferric Fe 3 + is predominantly found at octahedrally coordinated Ga sites. We obtain the full set of fourth-order monoclinic zero-field splitting parameters for both octahedrally and tetrahedrally coordinated sites by employing measurements at multiple sample azimuth rotations. The capability of high-field EPR allows us to demonstrate that simplified second-order orthorhombic spin Hamiltonians are insufficient, and fourth-order terms as well as consideration of the monoclinic symmetry are needed. These findings are supported by computational approaches based on density-functional theory for second-order and on ligand-field theory for fourth-order parameters of the spin Hamiltonian. Terahertz ellipsometry is a way to measure spin resonances in a cavity-free setup. Its possibility of varying the probe frequency arbitrarily without otherwise changing the experimental setup offers unique means of truly disentangling different components of highly anisotropic spin Hamiltonians. Published by the American Physical Society 2024

Materials Science↗
DOE OSTI2019

Evaluation of optical parameters and characterization of few layer sputtered MoS{sub 2} film by spectroscopic ellipsometry

The study involves spectroscopic ellipsometry analysis of sputter deposited few layer MoS{sub 2} grown on three different substrates (ITO coated glass, n-silicon and p-silicon) for diverse deposition time. We have investigated optical parameters such as refractive index, extinction coefficient and dielectric constant of MoS{sub 2} layers in the visible region of electromagnetic spectrum. For such purpose of investigation we have involved Cauchy dispersion model (for the film deposited on n-silicon and p-silicon) and hybrid of Lorentz and Drude model (for the film deposited on ITO coated glass). Furthermore, comparative analysis at the diverse growth time of 5, 10, 15 and 20 min has been performed on the basis of optical parameters and surface morphology.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2017

Non-destructive characterization of corroded glass surfaces by spectroscopic ellipsometry

Characterization of the alteration layers that form on glass surfaces during corrosion processes provides valuable information on both the mechanisms and rate of glass alteration. In recent years, state-of-the-art materials and surface characterization techniques have been employed to study various aspects of the alteration layers that result from corrosion. In most cases, these techniques are destructive and thus can only be employed at the end of the corrosion experiment. We show that the alteration layers can be investigated by non-destructive spectroscopic ellipsometry (SE), which provides pertinent information on alteration layer thickness, morphology, and, through correlation of the index of refraction, porosity. SE measurements of silicate glass coupons altered in aqueous solutions of pH 3, 5, 7, 9, and 11 at 90 °C for 7 days are compared to cross-sectional secondary electron microscopy images. In most cases, quantitative agreement of the alteration layer thickness is obtained. The fractional porosity calculated from the index of refraction is lower than the porosity calculated from elemental analysis of the aqueous solutions, indicating that the alteration layer has compacted during corrosion or the subsequent supercritical CO 2 drying process. Our results confirm the utility of performing non-destructive SE measurements on corroded glass surfaces.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Optical properties of a nanostructured glass-based film using spectroscopic ellipsometry

Nanostructured glass films, which are fabricated using spinodally phase-separated low-alkali glasses, have several interesting and useful characteristics, including being robust, non-wetting and antireflective. Spectroscopic ellipsometry measurements have been performed on one such film and its optical properties were analyzed using a 5-layer structural model of the near-surface region. Since the glass and the film are transparent over the spectral region of the measurement, the Sellmeier model is used to parameterize the dispersion in the refractive index. To simulate the variation of the optical properties of the film over the spot size of the ellipsometer (~ 3 × 5 mm), the Sellmeier amplitude is convoluted using a Gaussian distribution. The transition layers between the ambient and the film and between the film and the substrate are modeled as graded layers, where the refractive index varies as a function of depth. These layers are modeled using a two-component Bruggeman effective medium approximation where the two components are the layer above and the layer below. Lastly, the fraction is continuous through the transition layer and is modelled using the incomplete beta function.

36 MATERIALS SCIENCE↗
DOE OSTI2015

In Situ Infrared Ellipsometry for Protein Adsorption Studies on Ultrathin Smart Polymer Brushes in Aqueous Environment

The protein-adsorbing and -repelling properties of various smart nanometer-thin polymer brushes with high potential for biosensing and biomedical applications are studied by in-situ infrared-spectroscopic ellipsometry (IRSE). IRSE as a highly sensitive non-destructive technique allows us to investigate protein adsorption on polymer brushes in aqueous environment in dependence of external stimuli like temperature and pH. These stimuli are, for instance, relevant in switchable mixed brushes containing poly(N-isopropyl acrylamide) and poly(acrylic acid), respectively. We use such brushes as model surfaces for controlling protein adsorption of human serum albumin and human fibrinogen. IRSE can distinguish between polymer-specific vibrational bands, which yield insights into the hydration state of the brushes, and changes in the protein-specific amide bands, which are related to changes of the protein secondary structure.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Dielectric function of sol-gel prepared nano-granular zinc oxide by spectroscopic ellipsometry

ZnO thin films have been prepared by sol gel and deposited by spin coating. The dielectric function has been determined by spectroscopic ellipsometry. Ellipsometric spectra are inverted by a direct numerical method without using the standard fitting procedures. The obtained dielectric function presents a broad excitonic effect. The dielectric function is studied using Elliot excitonic theory including exciton plus band-to-band Coulomb interactions with standard Lorentzian broadening. A modification of this model dielectric function with independent bound and unbound exciton contributions is empirically proposed to improve modelling of the band gap excitonic peak.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Interband electronic transitions and phase transformation of multiferroic Bi{sub 1−x}La{sub x}Fe{sub 1−y}Ti{sub y}O{sub 3} ceramics revealed by temperature-dependent spectroscopic ellipsometry

Optical properties and phase transition of Bi{sub 1−x}La{sub x}Fe{sub 1−y}Ti{sub y}O{sub 3} (BLFTO) ceramics with different composition (0.02 ≤ x ≤ 0.10, 0.01 ≤ y ≤ 0.06) have been investigated by spectroscopic ellipsometry (SE) in the temperature range of −70–450 °C. The real part of the complex dielectric function ε{sub 1} increases with the temperature. Meanwhile, the imaginary part ε{sub 2} in the low-energy region decreases with the temperature and has an opposite trend in the high-energy side. Four typical interband transitions (E{sub a} ∼ 2.50 eV, E{sub b} ∼ 2.70 eV, E{sub c} ∼ 3.60 eV, and E{sub d} ∼ 4.25 eV) can be observed from the second derivative of the complex dielectric functions with aid of the standard critical point model. The critical point (CP) transition becomes broadening and shifts to a lower energy side as La and Ti compositions increase. Moreover, the CP transition energies show a red-shift trend with increasing the temperature until 320 °C, due to the lattice thermal expansion and electron-phonon interaction. The typical interband transitions and partial spectral weight present anomalies in the proximity of antiferromagnetic transition owing to the coupling between magnetic and ferroelectric order parameters and spin-lattice coupling for BLFTO multiferroic materials. It was found that the Néel temperature of BLFTO ceramics decreases from 364 to 349 °C with increasing doping composition of La and Ti elements. These phenomena can be attributed to the modification of electronic structure and magnetic order because the differences of electronegativity and ionic radii between Bi and La, Fe and Ti induce the variations on the bond angle and bond length between cations and anions. Moreover, the substitution for magnetic Fe{sup 3+} ions with nonmagnetic Ti{sup 4+} ions can reduce the exchange interaction between adjacent magnetic moments. Therefore, SE technique can be sensitive for detecting the phase/structural transitions of multiferroic oxides.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Spectroscopic ellipsometry of homoepitaxial diamond multilayers and delta-doped structures

The optimization of diamond-based unipolar electronic devices such as pseudo-vertical Schottky diodes or delta-doped field effect transistors relies in part on the sequential growth of nominally undoped (p{sup –}) and heavily boron doped (p{sup ++}) layers with well-controlled thicknesses and steep interfaces. Optical ellipsometry offers a swift and contactless method to characterize the thickness, roughness, and electronic properties of semiconducting and metallic diamond layers. We report ellipsometric studies carried out on delta-doped structures and other epitaxial multilayers with various boron concentrations and thicknesses (down to the nanometer range). The results are compared with Secondary Ion Mass Spectroscopy and transport measurements.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Investigation of temperature dependent dielectric constant of a sputtered TiN thin film by spectroscopic ellipsometry

The temperature dependence of optical constants of titanium nitride thin film is investigated using Spectroscopic Ellipsometry (SE) between 1.4 and 5 eV in the temperature range of 300 K to 650 K in steps of 50 K. The real and imaginary parts of the dielectric functions ε{sub 1}(E) and ε{sub 2}(E) marginally increase with increase in temperature. A Drude Lorentz dielectric analysis based on free electron and oscillator model are carried out to describe the temperature behavior. With increase in temperature, the unscreened plasma frequency and broadening marginally decreased and increased, respectively. The parameters of the Lorentz oscillator model also showed that the relaxation time decreased with temperature while the oscillator energies increased. This study shows that owing to the marginal change in the refractive index with temperature, titanium nitride can be employed for surface plasmon sensor applications even in environments where rise in temperature is imminent.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Intrinsic relationship between electronic structures and phase transition of SrBi{sub 2−x}Nd{sub x}Nb{sub 2}O{sub 9} ceramics from ultraviolet ellipsometry at elevated temperatures

The ferroelectric orthorhombic to paraelectric tetragonal phase transition of SrBi{sub 2−x}Nd{sub x}Nb{sub 2}O{sub 9} (x = 0, 0.05, 0.1, and 0.2) layer-structured ceramics has been investigated by temperature-dependent spectroscopic ellipsometry. Based on the analysis of dielectric functions from 0 to 500 °C with double Tauc-Lorentz dispersion model, the interband transitions located at ultraviolet region have shown an abrupt variation near the Curie temperature. The changes of dielectric functions are mainly due to the thermal-optical and/or photoelastic effect. Moreover, the characteristic alteration in interband transitions can be ascribed to distortion of NbO{sub 6} octahedron and variation of hybridization between Bi 6s and O 2p states during the structure transformation.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Investigation of the optical properties of MoS{sub 2} thin films using spectroscopic ellipsometry

Spectroscopic ellipsometry (SE) characterization of layered transition metal dichalcogenide (TMD) thin films grown by vapor phase sulfurization is reported. By developing an optical dispersion model, the extinction coefficient and refractive index, as well as the thickness of molybdenum disulfide (MoS{sub 2}) films, were extracted. In addition, the optical band gap was obtained from SE and showed a clear dependence on the MoS{sub 2} film thickness, with thinner films having a larger band gap energy. These results are consistent with theory and observations made on MoS{sub 2} flakes prepared by exfoliation, showing the viability of vapor phase derived TMDs for optical applications.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Spectroscopic ellipsometry determination of the optical constants of titanium-doped WO{sub 3} films made by co-sputter deposition

Titanium (Ti) doped tungsten oxide (WO{sub 3}) thin films were grown by co-sputter deposition of W and Ti metal targets. The sputtering powers to the W and Ti were kept constant at 100 W and 50 W, respectively, while varying the growth temperature (T{sub s}) in the range of 25–400 °C. The structural quality of Ti-doped WO{sub 3} films is dependent on T{sub s}. Ti-doped WO{sub 3} films grown at T{sub s} < 400 °C were amorphous. A temperature of 400 °C is critical to promote the structural order and formation of monoclinic, nanocrystalline films. The optical constants and their dispersion profiles determined from spectroscopic ellipsometry indicate that there is no significant inter-diffusion at the film-substrate interface for W-Ti oxide film growth of ∼40 nm. The index refraction (n) at λ = 550 nm varies in the range of 2.15–2.40 with a gradual increase in T{sub s}. Lorentz-Lorenz analysis (n{sub (λ)} = 550 nm) of the data indicates the gradual improvement in the packing density coupled with structural transformation accounts for the observed optical quality of the Ti-doped WO{sub 3} films as a function of T{sub s}. A correlation between the growth conditions and optical constants is discussed.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Modeling ellipsometry and electron energy loss spectroscopy of graphene

Recent studies of electronic excitations in graphene by Electron Energy Loss Spectroscopy (EELS) have revealed massive high-frequency peaks assigned to the π and σ+π plasmons [1], which were semi-quantitatively modeled with a two-dimensional, two-fluid hydrodynamic (HD) model [2]. On the other hand, Spectroscopic Ellipsometry (SE) of graphene covers the region of nearly constant absorbance due to graphene’s universal optical conductivity at infrared frequencies, which is not clearly resolved by EELS, and goes up to cover the π-plasmon peak at ultraviolet frequencies [3]. To attempt to model both the SE and EELS, we amend the HD model by including a low-frequency contribution of graphene’s inter-band transitions, while monitoring the fulfillment of the f-sum rule [4] up to frequencies that cover excitations of all valence electrons.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗