Engineering Papers⌕ Search

SEARCH · Engineering Papers

Results for “Ellipsometry”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 73 records · Page 4

Optical properties of amorphous and crystalline Sb-doped SnO{sub 2} thin films studied with spectroscopic ellipsometry: Optical gap energy and effective mass

We investigated the optical properties of amorphous and crystalline antimony (Sb)-doped tin dioxide (SnO{sub 2}) thin films grown using the co-sputtering deposition method at room temperature. We used undoped and Sb-doped (8 wt. %) SnO{sub 2} targets. Varying the relative power ratio of the two targets, we controlled the Sb-composition of the SnO{sub 2}:Sb thin films up to 2.3 at. % of Sb contents. Through annealing, the as-grown amorphous SnO{sub 2}:Sb thin films were transformed to crystalline thin films. Dielectric functions were obtained from the measured ellipsometry angles, Ψ and Δ, using the Drude and parametric optical constant models. We determined the absorption coefficients and optical gap energies of the SnO{sub 2}:Sb thin films from the dielectric functions. We found increasing optical gap energy with increasing Sb composition. Increases in the Drude tail amplitudes, a signature of free carrier concentrations, were found in annealed, crystalline thin films with increasing Sb composition. The increase in the optical gap energy with increasing Sb composition was mainly attributed to the Burstein-Moss effect. Using Hall effect measurements, we obtained Hall carrier concentrations (N{sub Hall}) and electron Hall mobilities (μ{sub Hall}). The carrier concentrations and mobilities increased from 2.6 × 10{sup 19 }cm{sup −3} and 1.0 cm{sup 2}/(V s) to 2.0 × 10{sup 20 }cm{sup −1} and 7.2 cm{sup 2}/(V s), respectively, with increasing Sb contents. This result suggests that the nominally undoped SnO{sub 2} films are unintentionally n-type doped. Assuming that the N{sub Hall} and optical carrier concentrations (N{sub opt}) were the same, we obtained the effective masses of the SnO{sub 2}:Sb thin films with increasing Sb compositions. The effective masses of the SnO{sub 2}:Sb thin films increased from 0.245 m{sub 0} to 0.4 m{sub 0} with increasing Sb doping contents, and the nonparabolicity of the conduction band was estimated. We discussed the relation between the optical (μ{sub opt}) and Hall (μ{sub Hall}) mobilities as a function of Sb contents and grain sizes.

36 MATERIALS SCIENCE↗

Detection of a MoSe{sub 2} secondary phase layer in CZTSe by spectroscopic ellipsometry

We demonstrate the application of Spectroscopic Ellipsometry (SE) for identification of secondary phase MoSe{sub 2} in polycrystalline Cu{sub 2}ZnSnSe{sub 4} (CZTSe) samples. A MoSe{sub 2} reference sample was analyzed, and its optical constants (ε{sub 1} and ε{sub 2}) were extracted by SE analysis. This dataset was implemented into an optical model for analyzing SE data from a glass/Mo/CZTSe sample containing MoSe{sub 2} at the back side of the absorber. We present results on the n and k values of CZTSe and show the extraction of the thickness of the secondary phase MoSe{sub 2} layer. Raman spectroscopy and scanning electron microscopy were applied to confirm the SE results.

36 MATERIALS SCIENCE↗

Effect of Ta concentration on the refractive index of TiO{sub 2}:Ta studied by spectroscopic ellipsometry

We have investigated optical properties of Ta-doped TiO{sub 2} thin film on LaAlO{sub 3} (LAO) substrate using Spectroscopic Ellipsometry (SE) at room temperature. Amplitude ratio Ψ and phase difference L1 between p- and s- polarized light waves are obtained by multiple incident angles measurement (60°, 70°, and 80°) at energy range of 0.5 – 6.5 eV. In order to obtain optical properties for every Ta concentrations (0.01, 0.4, and 5 at. %), multilayer modelling was performed simultaneously by using Drude-Lorentz model. Refractive index and optical dispersion parameters were determined by Wemple-DiDomenico relation. In general, refractive index at zero photon energy n(0) increases by increasing Ta concentration. Furthermore, optical band gap shows a significant increasing due to presence of Ta dopant. In addition, other optical constants are discussed as well.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Spectroscopic ellipsometry investigations of optical anisotropy in obliquely deposited hafnia thin films

In present work, HfO{sub 2} thin films have been deposited at various oblique incidences on Si substrates by electron beam evaporation. These refractory oxide films exhibited anisotropy in refractive index predictably due to special columnar microstructure. Spectroscopic ellipsometry being a powerful tool for optical characterization has been employed to investigate optical anisotropy. It was observed that the film deposited at glancing angle (80°) exhibits the highest optical anisotropy. Further, anisotropy was noticed to decrease with lower values of deposition angles while effective refractive index depicts opposite trend. Variation in refractive index and anisotropy has been explained in light of atomic shadowing during growth of thin films at oblique angles.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Influence of annealing temperature and Sn doping on the optical properties of hematite thin films determined by spectroscopic ellipsometry

Hematite (α-Fe{sub 2}O{sub 3}) thin films were prepared by sol-gel route and investigated for application in H{sub 2} generation by photo-assisted water splitting. The photoelectrochemical (PEC) performance was shown to increase significantly for films deposited on SnO{sub 2}:F/glass subjected to high temperature (T) annealing (>750 °C). Strong correlation was found between photogenerated current, donor concentration, and Sn concentration as determined by Mott-Schottky analysis and X-ray photoelectron spectroscopy. The effects of thermal annealing and Sn addition in the resulting microstructure and optical properties of hematite films deposited on fused silica substrates were determined by a combination of structural characterization techniques and spectroscopic ellipsometry. Thermal annealing (>600 °C) induces a higher optical absorption that is associated directly to film densification and grain growth; however, it promotes no changes in the energy positions of the main Fe{sub 2}O{sub 3} electronic transitions. The band gap energy was found to be 2.21 eV and independent of microstructure and of Sn concentration for all studied films. On the other hand, Sn can be incorporated in the Fe{sub 2}O{sub 3} lattice for concentration up to Sn/Fe ∼2%, leading to an increase in energy split of the main absorption peak, attributed to a distortion of the Fe{sub 2}O{sub 3} lattice. For higher concentrations, Sn incorporation leads to a reduction in absorption, associated with higher porosity and the formation of a secondary Sn-rich phase. In summary, the variation in the optical properties induced by thermal annealing and Sn addition cannot account for the order of magnitude increase of the current density generated by photoanodes annealed at high T (>750 °C); thus, it is concluded that the major contribution for the enhanced PEC performance comes from improved electronic properties induced by the n-type doping caused by Sn diffusion from the SnO{sub 2}:F substrate.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Effects of oxygen partial pressure, deposition temperature, and annealing on the optical response of CdS:O thin films as studied by spectroscopic ellipsometry

Ex-situ spectroscopic ellipsometry measurements are made on radio frequency magnetron sputtered oxygenated cadmium sulfide (CdS:O) thin films. Films are deposited onto glass substrates at room temperature and at 270 °C with varying oxygen to total gas flow ratios in the sputtering ambient. Ellipsometric spectra from 0.74 to 5.89 eV are collected before and after annealing at 607 °C to simulate the thermal processes during close-space sublimation of overlying cadmium telluride in that solar cell configuration. Complex dielectric function (ε = ε{sub 1} + iε{sub 2}) spectra are extracted for films as a function of oxygen gas flow ratio, deposition temperature, and post-deposition annealing using a parametric model accounting for critical point transitions and an Urbach tail for sub-band gap absorption. The results suggest an inverse relationship between degree of crystallinity and oxygen gas flow ratio, whereas annealing is shown to increase crystallinity in all samples. Direct band gap energies are determined from the parametric modeling of ε and linear extrapolations of the square of the absorption coefficient. As-deposited samples feature a range of band gap energies whereas annealing is shown to result in gap energies ranging only from 2.40 to 2.45 eV, which is close to typical band gaps for pure cadmium sulfide.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Surface roughness estimation of MBE grown CdTe/GaAs(211)B by ex-situ spectroscopic ellipsometry

Spectroscopic ellipsometry (SE) ranging from 1.24 eV to 5.05 eV is used to obtain the film thickness and optical properties of high index (211) CdTe films. A three-layer optical model (oxide/CdTe/GaAs) was chosen for the ex-situ ellipsometric data analysis. Surface roughness cannot be determined by the optical model if oxide is included. We show that roughness can be accurately estimated, without any optical model, by utilizing the correlation between SE data (namely the imaginary part of the dielectric function, <ε{sub 2} > or phase angle, ψ) and atomic force microscopy (AFM) roughness. <ε{sub 2} > and ψ values at 3.31 eV, which corresponds to E{sub 1} critical transition energy of CdTe band structure, are chosen for the correlation since E{sub 1} gives higher resolution than the other critical transition energies. On the other hand, due to the anisotropic characteristic of (211) oriented CdTe surfaces, SE data (<ε{sub 2} > and ψ) shows varieties for different azimuthal angle measurements. For this reason, in order to estimate the surface roughness by considering these correlations, it is shown that SE measurements need to be taken at the same surface azimuthal angle. Estimating surface roughness in this manner is an accurate way to eliminate cumbersome surface roughness measurement by AFM.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Nucleation and growth of MgO atomic layer deposition: A real-time spectroscopic ellipsometry study

The atomic layer deposition (ALD) of MgO thin films from bis(cyclopentadienyl) magnesium and H{sub 2}O was studied using in-situ real-time spectroscopic ellipsometry (SE), ex-situ x-ray photoelectron spectroscopy, and grazing-incidence x-ray diffraction. It is found that the initial growth is not linear during the first ten cycles, and magnesium silicate forms spontaneously on the SiO{sub 2}/Si substrates at 250 °C. Submonolayer sensitivity of SE is demonstrated by the analysis of each half-cycle and self-limiting adsorption, revealing characteristic features of hetero- and homo-MgO ALD processes.

36 MATERIALS SCIENCE↗

Using spectroscopic ellipsometry and single-angle reflectance to derive accurate optical constants for chemical forms of aspartame

Variable angle spectroscopic ellipsometry and single-angle infrared reflectance methods have been used to derive the complex optical constants n and k in the mid-infrared spectral region for aspartame. Aspartame exists in four unique forms – three of which incorporate water into the lattice, as well as the anhydrate form. The different forms can induce splitting or slight wavenumber shifts in the spectral features. Pressed pellets of neat powder were prepared and measured using both methods to derive the optical constants. Different n and k values were obtained depending on the percentage of the forms of aspartame, which was determined using powder X-ray diffraction (XRD) analysis.

optical constants, refractive index, extinction co↗

Optical Properties of Nonstoichiometric Tantalum Oxide TaO{sub x} (x < 5/2) According to Spectral-Ellipsometry and Raman-Scattering Data

Optical properties of amorphous nonstoichiometric tantalum-oxide films of variable composition (TaO{sub x}, x = 1.94–2.51) in the spectral range of 1.12–4.96 eV, obtained by ion-beam sputtering-deposition of metallic tantalum at different partial oxygen pressures (0.53–9.09 × 10{sup –3} Pa), have been investigated. It is shown by spectral ellipsometry that the character of dispersion of the absorption coefficient and refractive index in TaO{sub x} of variable composition suggests that light-absorbing films with dispersion similar to that in metals are formed at oxygen pressures in the growth chamber below 2.21 × 10{sup –3} Pa, whereas transparent films with dielectric dispersion are formed at pressures above 2.81 × 10{sup –3} Pa. According to the data of quantumchemical simulation, the absorption peak at a photon energy of 4.6 eV in TaO{sub x} observed in the absorptioncoefficient dispersion spectrum is due to oxygen vacancy. The peak in the Raman-scattering spectra of TaO{sub x} films with metallic dispersion at frequencies of 200–230 cm{sup –1} is presumably related to tantalum nanoclusters.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Spectral ellipsometry as a method for characterization of nanosized films with ferromagnetic layers

Nanosized films with ferromagnetic layers are widely used in nanoelectronics, sensor systems and telecommunications. Their properties may strongly differ from those of bulk materials that is on account of interfaces, intermediate layers and diffusion. In the present work, spectral ellipsometry and magnetooptical methods are adapted for characterization of the optical parameters and magnetization processes in two- and three-layer Cr/NiFe, Al/NiFe and Cr(Al)/Ge/NiFe films onto a sitall substrate for various thicknesses of Cr and Al layers. At a layer thickness below 20 nm, the complex refractive coefficients depend pronouncedly on the thickness. In two-layer films, remagnetization changes weakly over a thickness of the top layer, but the coercive force in three-layer films increases by more than twice upon remagnetization, while increasing the top layer thickness from 4 to 20 nm.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Real Time Spectroscopic Ellipsometry Analysis of First Stage CuIn1-xGaxSe2 Growth: Indium-Gallium Selenide Co-Evaporation

Real time spectroscopic ellipsometry (RTSE) has been applied for in-situ monitoring of the first stage of copper indium-gallium diselenide (CIGS) thin film deposition by the three-stage co-evaporation process used for fabrication of high efficiency thin film photovoltaic (PV) devices. The first stage entails the growth of indium-gallium selenide (In 1-x Gax) 2 Se 3 (IGS) on a substrate of Mo-coated soda lime glass maintained at a temperature of 400 °C. This is a critical stage of CIGS deposition because a large fraction of the final film thickness is deposited, and as a result precise compositional control is desired in order to achieve the optimum performance of the resulting CIGS solar cell. RTSE is sensitive to monolayer level film growth processes and can provide accurate measurements of bulk and surface roughness layer thicknesses. These in turn enable accurate measurements of the bulk layer optical response in the form of the complex dielectric function ε = ε 1 - iε 2 , spectra. Here, RTSE has been used to obtain the (ε 1 , ε 2 ) spectra at the measurement temperature of 400 °C for IGS thin films of different Ga contents (x) deduced from different ranges of accumulated bulk layer thickness during the deposition process. Applying an analytical expression in common for each of the (ε 1 , ε 2 ) spectra of these IGS films, oscillator parameters have been obtained in the best fits and these parameters in turn have been fitted with polynomials in x. From the resulting database of polynomial coefficients, the (ε 1 , ε 2 ) spectra can be generated for any composition of IGS from the single parameter, x. The results have served as an RTSE fingerprint for IGS composition and have provided further structural information beyond simply thicknesses, for example information related to film density and grain size. The deduced IGS structural evolution and the (ε 1 , ε 2 ) spectra have been interpreted as well in relation to observations from scanning electron microscopy, X-ray diffractometry and energy-dispersive X-ray spectroscopy profiling analyses. Overall the structural, optical and compositional analysis possible by RTSE has assisted in understanding the growth and properties of three stage CIGS absorbers for solar cells and shows future promise for enhancing cell performance through monitoring and control.

36 MATERIALS SCIENCE↗

Ellipsometry

Ellipsometry is a technique often used to measure the thickness and properties of a thin film. This article covers the instrumental, theoretical, and practical aspects of this technique. Notably, different types of instruments including nulling ellipsometer, rotating compensator ellipsometer, and photoelastic modulator ellipsometer designs are presented. Elements of proper data analysis are also included, such as the use of an error-based figure of merit.

Complex reflection coefficients↗

Evaluation of the SEI using a multilayer spectroscopic ellipsometry model

A multilayer spectroscopic ellipsometry (SE) model has been developed to characterize SEI formation. The model, which consists of two Cauchy layers, is constructed with an inner layer meant to model primarily inorganic compounds adjacent to an electrode and an outer layer which mirrors polymeric, organic constituents on the exterior of the SEI. Comparison of 1:1 EC:EMC and 1:4 EC:EMC with 1.0 M LiPF6 shows distinct differences in the two modeled layers. The data suggest that the thickness of both layers change over a wide potential range. These changes have been linked with other reports on the growth of the SEI.

25 ENERGY STORAGE↗

Combining Spectroscopic Ellipsometry with Transmission Spectroscopy to Derive Accurate Optical Constants for Organic Materials

A method for deriving the optical constants of organic powdered materials in the mid-infrared spectral range is introduced using variable angle spectroscopic ellipsometry and transmission spectroscopy. The approach uses pressed pellets of the powder and is applied to organic solids, which have both strong and weak infrared absorption features. Many powders have significant voids and do not press into smooth, homogenous pellets. To account for pellet non-idealities and to accurately measure both n and k, three different forms of pellets were pressed and measured: A pure analyte pellet, a mixed analyte/KBr pellet with a large analyte percentage, and a KBr transmission pellet with only a small analyte percentage. Using all three pellets in a multi-sample analysis involving both ellipsometric and transmission data, the complex refractive index (n/k) values can be derived for many organic compounds. This method is illustrated to calculate the optical constants for anhydrous lactose from 6000-400 cm-1. The transmission measurements improve the spectral fitting of weak absorption features, and the multi-sample analysis enables a better determination of the significant void space that is present in the pure pellet, leading to lower values for both n and k if not properly accounted for in the multi-oscillator model used to fit the ellipsometric data.

Optical constants, refractive index, extinction co↗

Quantitative measurement of pebble fuel anisotropy using generalized ellipsometry

The renewed development of high-temperature gas-cooled reactors has created a need to modernize pebble fuel quality control methods. One important specification in these methods is the coefficient of thermal expansion (CTE) anisotropy, which reflects graphite grain alignment and affects fuel performance. This study investigates the feasibility of using two-modulator generalized ellipsometry microscopy (2-MGEM) as a potential surrogate metric for CTE anisotropy. Graphite matrix compacts with controlled levels of anisotropy were fabricated by varying pre-pressures during forming and were subsequently characterized using both optical dilatometry and 2-MGEM. Measured responses were compared to an isotropic reference pebble produced using an industrial manufacturing process to provide a practical baseline. The resulting measurements revealed a strong quantitative correlation between the CTE anisotropy ratio and the corresponding diattenuation ratio. However, propagated measurement uncertainties in the optical method were found to limit definitive pass/fail discrimination, highlighting the need for improved precision before qualification as a quality control tool. Still, the results establish a quantitative relationship between optical and CTE anisotropy and support further development of 2-MGEM as a potential surrogate method for evaluating graphite matrix anisotropy in pebble fuel manufacturing.

Raftery, Alicia [ORNL] (ORCID:0000000259076427)↗

Delineating Confinement Regimes for Nafion Thin Films via Simultaneous QCM-D and Spectroscopic Ellipsometry

Proton-conducting ionomers used in electrodes of electrochemical devices form nanometer-scale films covering metallic catalyst surfaces, wherein they experience confinement and interfacial effects absent in the bulk polymer. This confinement alters the physical properties of the ionomer film, which is postulated to increase the density and is attributed to the transport limitations observed in fuel-cell electrodes. Despite studies showing reduced swelling, no systematic measurement has validated this phenomenon by demonstrating both densification and stiffening as the film gets thinner. Here, this study aims to fill this gap by reporting the humidity-driven changes in swelling, mass uptake, and density of Nafion ionomer films cast at varying thicknesses (10–320 nm) onto a gold-plated sensor. The films were simultaneously probed during humidification using spectroscopic ellipsometry (SE) and a quartz crystal microbalance with dissipation (QCM-D), which allowed for determination of the density and shear stiffness. The effects of confinement were prominently observed below ∼30 nm, with films showing increased density along with decreased swelling and mass uptake during hydration. In addition, the confined films show a negative excess volume upon initial water sorption, implying a larger proportion of absorbed water might bound to ionic groups in accord with notion of localized densification.

Espinet, Kevin B. [University of California, Berke↗

Electron Beam Infrared Nano-Ellipsometry of Individual Indium Tin Oxide Nanocrystals

Leveraging recent advances in electron energy monochromation and aberration correction, we record the spatially resolved infrared plasmon spectrum of individual tin-doped indium oxide nanocrystals using electron energy-loss spectroscopy (EELS). Both surface and bulk plasmon responses are measured as a function of tin doping concentration from 1–10 atomic percent. Furthermore, these results are compared to theoretical models, which elucidate the spectral detuning of the same surface plasmon resonance feature when measured from aloof and penetrating probe geometries. We additionally demonstrate a unique approach to retrieving the fundamental dielectric parameters of individual semiconductor nanocrystals via EELS. This method, devoid from ensemble averaging, illustrates the potential for electron-beam ellipsometry measurements on materials that cannot be prepared in bulk form or as thin films.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗