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At least 829 records · Page 46
All sourcesNASA NTRSDOE OSTI
DOE OSTI2014

Optical characteristics of nanocrystalline Al{sub x}Ga{sub 1−x}N thin films deposited by hollow cathode plasma-assisted atomic layer deposition

Gallium nitride (GaN), aluminum nitride (AlN), and Al{sub x}Ga{sub 1−x}N films have been deposited by hollow cathode plasma-assisted atomic layer deposition at 200 °C on c-plane sapphire and Si substrates. The dependence of film structure, absorption edge, and refractive index on postdeposition annealing were examined by x-ray diffraction, spectrophotometry, and spectroscopic ellipsometry measurements, respectively. Well-adhered, uniform, and polycrystalline wurtzite (hexagonal) GaN, AlN, and Al{sub x}Ga{sub 1−x}N films were prepared at low deposition temperature. As revealed by the x-ray diffraction analyses, crystallite sizes of the films were between 11.7 and 25.2 nm. The crystallite size of as-deposited GaN film increased from 11.7 to 12.1 and 14.4 nm when the annealing duration increased from 30 min to 2 h (800 °C). For all films, the average optical transmission was ∼85% in the visible (VIS) and near infrared spectrum. The refractive indices of AlN and Al{sub x}Ga{sub 1−x}N were lower compared to GaN thin films. The refractive index of as-deposited films decreased from 2.33 to 2.02 (λ = 550 nm) with the increased Al content x (0 ≤ x ≤ 1), while the extinction coefficients (k) were approximately zero in the VIS spectrum (>400 nm). Postdeposition annealing at 900 °C for 2 h considerably lowered the refractive index value of GaN films (2.33–1.92), indicating a significant phase change. The optical bandgap of as-deposited GaN film was found to be 3.95 eV, and it decreased to 3.90 eV for films annealed at 800 °C for 30 min and 2 h. On the other hand, this value increased to 4.1 eV for GaN films annealed at 900 °C for 2 h. This might be caused by Ga{sub 2}O{sub 3} formation and following phase change. The optical bandgap value of as-deposited Al{sub x}Ga{sub 1−x}N films decreased from 5.75 to 5.25 eV when the x values decreased from 1 to 0.68. Furthermore, postdeposition annealing did not affect the bandgap of Al-rich films.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Radiochromic film calibration for low-energy seed brachytherapy dose measurement

Purpose: Radiochromic film dosimetry is typically performed for high energy photons and moderate doses characterizing external beam radiotherapy (XRT). The purpose of this study was to investigate the accuracy of previously established film calibration procedures used in XRT when applied to low-energy, seed-based brachytherapy at higher doses, and to determine necessary modifications to achieve similar accuracy in absolute dose measurements. Methods: Gafchromic EBT3 film was used to measure radiation doses upwards of 35 Gy from 75 kVp, 200 kVp, 6 MV, and (∼28 keV) I-125 photon sources. For the latter irradiations a custom phantom was built to hold a single I-125 seed. Film pieces were scanned with an Epson 10000XL flatbed scanner and the resulting 48-bit RGB TIFF images were analyzed using both FilmQA Pro software andMATLAB. Calibration curves relating dose and optical density via a rational functional form for all three color channels at each irradiation energy were determined with and without the inclusion of uncertainties in the measured optical densities and dose values. The accuracy of calibration curve variations obtained using piecewise fitting, a reduced film measurement area for I-125 irradiation, and a reduced number of dose levels was also investigated. The energy dependence of the film lot used was also analyzed by calculating normalized optical density values. Results: Slight differences were found in the resulting calibration curves for the various fitting methods used. The accuracy of the calibration curves was found to improve at low doses and worsen at high doses when including uncertainties in optical densities and doses, which may better represent the variability that could be seen in film optical density measurements. When exposing the films to doses > 8 Gy, two-segment piecewise fitting was found to be necessary to achieve similar accuracies in absolute dose measurements as when using smaller dose ranges. When reducing the film measurement area for the I-125 irradiations, the accuracy of the calibration curve was degraded due to the presence of localized film heterogeneities. No degradation in the calibration curves was found when reducing the number of calibration points down to only 4, but with piecewise fitting, 6 calibration points as well as a blank film are required. Variations due to photon energy in film optical density of up to 3% were found above doses of 2 Gy. Conclusions: A modified procedure for performing EBT3 film calibration was established for use with low-energy brachytherapy seeds and high dose exposures. The energy dependence between 6 MV and I-125 photons is significant such that film calibrations should be done with an appropriately low-energy source when performing low-energy brachytherapy dose measurements. Two-segment piecewise fitting with the inclusion of errors in measured optical density as well as dose was found to result in the most accurate calibration curves. Above doses of 1 Gy, absolute dose measurements can be made with an accuracy of 1.6% for 6 MV beams and 5.7% for I-125 seed exposures if using the I-125 source for calibration, or 2.3% if using the 75 kVp photon beam for calibration.

07 ISOTOPE AND RADIATION SOURCES↗
DOE OSTI2014

SU-E-T-637: Age and Batch Dependence of Gafchromic EBT Films in Photon and Proton Beam Dosimetry

Purpose: Gafchrmoic films have undergone significant changes in characteristic over time reflected by HS, EBT, EBT2, EBT3 name. Interand intra- EBT film variability have been studied and found to be significant. However, age and lot/batch type have not been studied in various radiation beams that are investigated in this study. Methods: Thirteen sets of films; 2 EBT, 6 EBT2 and 5 EBT3 films with different lot number and expiration date were acquired. Films were cut longitudinally in 3 cm width and sandwiched between two solid water slabs that were placed in a water phantom to eliminate air gap. Each set of films were irradiated longitudinally at dmax with 6 and 15 MV photon beams as well as in reference condition (16 cm range, 10 cm SOBP) in our uniform scanning proton beam. Films were scanned using an Epson flatbed scanner (ES-10000G) after 48 hours to achieve full polymerization. The profiles were compared with the depth-dose measured with ionization chamber and net optical density (net OD) were calculated. Results: The net OD versus dose for EBT, EBT2 and EBT3 films of different age showed similar trend but with different slope. Even after calibration, differences are clearly visible in net OD in proton and photon beams. A net OD difference of nearly 0.5 is observed in photon but this was limited to 0.2–0.3 in proton beam. This relates to 20% and 15% dosimetric difference in photon and proton beam respectively over age and type of film. Conclusion: Net OD related to dose is dependent on the age and lot of the film in both photon and proton beams. It is concluded that before any set of film is used, a calibration film should be used for a meaningful dosimetry. The expired films showed larger OD variation compared to unexpired films.

07 ISOTOPE AND RADIATION SOURCES↗
DOE OSTI2015

SU-E-T-386: Evaluation of EBT3 Film Response in Different Batches

Purpose: To investigate the uniformity of film response of EBT3 film of two different film batches. It has been reported that the response of the EBT film family is not homogenous between film batches. The later may have an impact in the dosimetry of small radiotherapy beams. Methods: A solid water phantom was used for dosimetric measurements. EBT3 film irradiation was performed with a 6 MV photon beam at 5 cm depth with a SAD of 100 cm. All irradiations were performed perpendicularly to the film plane covering the dose range 1 to 10 Gy. Three square field sizes were used to analyze the film response energy dependence: 10, 5 and 1 cm{sup 2}. Two batches of film EBT3 were used #A03181302 (B1) and #03031403 (B2). Film read out was carrying out with an Epson Perfection V750-Pro flatbed scanner in transmission mode with a spatial resolution of 72 dpi, with all post-processing and colour management options turned off, using 48 bits RGB colour depth. The scans were analyzed with the red channel. Results: The results shown that there were differences between the film response for each batch. The differences between batches for 1 Gy were 2%, 6% and 12% for 10, 5 and 1 cm2 square field sizes, respectively. The differences found for 10 Gy were 13%, 14% and 13% for 10, 5 and 1 cm{sup 2} square field sizes, respectively. It can be observed that the dependence with field size dismissed for higher doses. The later may be due to film response saturation at 10 Gy. Conclusion: The EBT3 film -as its predecessors-, it suffer for inter-batch variability in the film response. Further research is required to assess the possible impact in small beam dosimetry.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2021

Thin-film chemical expansion of ceria based solid solutions: laser vibrometry study

The chemical expansion of Pr 0.1 Ce 0.9 O 2-δ (PCO) and CeO 2-δ thin films is investigated in the temperature range between 600 °C and 800 °C by laser Doppler vibrometry (LDV). It enables non-contact determination of nanometer scale changes in film thickness at high temperatures. The present study is the first systematic and detailed investigation of chemical expansion of doped and undoped ceria thin films at temperatures above 650 °C. The thin films were deposited on yttria stabilized zirconia substrates (YSZ), operated as an electrochemical oxygen pump, to periodically adjust the oxygen activity in the films, leading to reversible expansion and contraction of the film. This further leads to stresses in the underlying YSZ substrates, accompanied by bending of the overall devices. Film thickness changes and sample bending are found to reach up to 10 and several hundred nanometers, respectively, at excitation frequencies from 0.1 to 10 Hz and applied voltages from 0–0.75 V for PCO and 0–1 V for ceria. At low frequencies, equilibrium conditions are approached. As a consequence maximum thin-film expansion of PCO is expected due to full reduction of the Pr ions. The lower detection limit for displacements is found to be in the subnanometer range. At 800 °C and an excitation frequency of 1 Hz, the LDV shows a remarkable resolution of 0.3 nm which allows, for example, the characterization of materials with small levels of expansion, such as undoped ceria at high oxygen partial pressure. As the correlation between film expansion and sample bending is obtained through this study, a dimensional change of a free body consisting of the same material can be calculated using the high resolution characteristics of this system. A minimum detectable dimensional change of 5 pm is estimated even under challenging high-temperature conditions at 800 °C opening up opportunities to investigate electro-chemo-mechanical phenomena heretofore impossible to investigate. The expansion data are correlated with previous results on the oxygen nonstoichiometry of PCO thin films, and a defect model for bulk ceria solid solutions is adopted to calculate the cation and anion radii changes in the constrained films during chemical expansion. The constrained films exhibit anisotropic volume expansion with displacements perpendicular to the substrate plane nearly double that of bulk samples. The PCO films used here generate high total displacements of several 100 nm’s with high reproducibility. Consequently, PCO films are identified to be a potential core component of high-temperature actuators. They benefit not only from high displacements at temperatures where most piezoelectric materials no longer operate while exhibiting, low voltage operation and low energy consumption.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

Low-cost, highly transparent flexible low-e coating film to enable electrochromic windows with increased energy savings

Five Quads of energy are lost through windows annually in the U.S. Low-e coatings are increasingly employed to reduce the wasted energy. Most commonly, the low-e coating is an oxide material applied directly to the glass at high temperature. With over 100,000,000 existing homes, a retrofit product is crucial to achieve widespread energy savings. Low-e films, i.e. coatings on polymeric substrates, are now also available to meet this need. However, the traditional oxide materials and process is incompatible with low temperature plastics. Alternate high performing low-e films typically incorporate materials that limit visible transmission to 35% or less. Further, the cost is high. The objective of this award was to develop a retrofit, integrated low-e/electrochromic window film to dramatically reduce energy lost through windows. While field testing of state-of-the-art electrochromic (EC) windows show the energy savings are maximized if a low-e coating is used in conjunction with the EC, available low-e films have a low visible transmission (~70% or less) that limits the achievable clear state and therefore, appearance and energy savings potential. Comprehensive energy savings models were completed at Lawrence Berkeley National Lab (LBNL). A parametric approach was used to project energy usage for windows with a large range of low-e properties across all U.S. climate zones, without limiting the study to materials that had already been produced commercially or made in a lab. The model enables projection of energy savings for low-e films as well as integrated low-e/EC products. This project developed a novel low-e film, optimized for compatibility with EC windows, using low temperature, high deposition rate processes for the growth of low-e coatings on plastic films by microwave plasma enhanced chemical vapor deposition. Silica films with good density and optical properties were demonstrated at deposition rates as high as 130Å/sec. A simple bi-layer low-e stack of silica and a transparent conductive oxide demonstrated 90% visible transmission with high thermal infrared reflectivity characteristic of conventional low-e coatings. A slightly more complex stack provided high solar infrared reflection without sacrificing visible transmission or thermal infrared reflection. Successful completion of the effort produced a prototype integrated low-e, dynamic window film with characterized energy saving potential. Cost modeling for the passive bi-layer, low-e film projects a manufacturing cost of ~$0.50/ft2 for a plant with 10M ft2/yr capacity. The novel thin film processes developed here enable high deposition rate (low cost), optical quality oxide coatings at low temperatures. When combined with engineered materials, ITN’s coating will result in low-cost, low-e films that reflect a high degree of infrared radiation without substantially reducing the visible transmission. The resultant window film will improve the U-value and achieve SHGC improvements over bare glass. The new low-e coating will be particularly attractive when combined with an electrochromic film. Low-e coating design guided by energy savings modeling allows customization of the product for different climate zones.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗
DOE OSTI2017

Optical-based spectroscopic methods for measuring chemical, optical, and physical properties of thin polymer waveguide films

Non-destructive optical-based spectroscopic methods are needed for analyzing “real world” devices that consist of thin polymer waveguide films. Many applications (e.g., sensors, microelectronics, optics, and biomedical applications, etc.) utilize thin polymer waveguide films, and non-destructive characterization methods based on Fourier transform (FT)-plasmon waveguide spectroscopy (PWR) and scanning angle (SA) Raman spectroscopy are used to extract optical, physical, and chemical properties simultaneously. The FT-PWR method measures reflected light at polymer waveguide interface as both the incident frequency (wavelength) and incident angle are scanned. This method uses p- and s-polarized light to simultaneously extract the polymer waveguide thickness and apparent anisotropic indices of refraction. Polystyrene waveguide films ranging from 360 to 800 nm are used to demonstrate the method and it has an average 0.4% relative error when compared to profilometry and atomic force microscopy measurements. SA Raman spectroscopy is used to measure mixed waveguide polymer films consisting of polystyrene-block-poly(methyl methacrylate) and homopolymer poly(methyl methacrylate) (PS-b-PMMA:PMMA), and poly(2-vinylnapthalene)-block-poly(methyl methacrylate) (P2VN-b-PMMA). PMMA homopolymer is added to the PS-b-PMMA solutions to vary the chemical composition. The chemical composition of each mixed film is quantified (SA Raman peak amplitude ratios) and averaged over all incident angles and is termed the Raman amplitude ratio (rps). This parameter is used to calculate the refractive index of each mixed waveguide polymer film. The refractive index is an input parameter for sum square electric field (SSEF) calculations, which are used to model SA Raman spectra as a function of incident angle to extract the film thickness. The mixed polymer waveguide film thicknesses ranged from 495 to 971 nm, and the SA Raman spectroscopy method has an average 5% difference between the values determined by profilometry. The SA Raman spectroscopy method developed for mixed polymer waveguide films is used to measure the chemical composition and extract interface locations in bilayer and trilayer films consisting of PMMA/PS or PMMA/PS/PMMA, respectively. The rps value is averaged over angle ranges corresponding to waveguide mode 0 and waveguide mode 1 for the bilayer and trilayer films, respectively. Six multilayer films are analyzed and their total thicknesses range from 330 to 1260 nm. Iterative SSEF calculations are used to model the SA Raman spectra as a function of incident angle, and the best fit to the experimental data is used to extract the total thickness and interface location(s). The method has an axial spatial resolution of 7 to 80 nm and provides comparable values to films measured by profilometry with an average 8% and 7% difference for the bilayer and trilayer films, respectively.

36 MATERIALS SCIENCE↗
NASA NTRS2000

The Effect of Radiation on Selected Photographic Film

We conducted this film test to evaluate several manufacturers' photographic films for their ability to acquire imagery on the International Space Station. We selected 25 motion picture, photographic slide, and negative films from three different film manufacturers. We based this selection on the fact that their films ranked highest in other similar film tests, and on their general acceptance by the international community. This test differed from previous tests because the entire evaluation process leading up to the final selection was based on information derived after the original flight film was scanned to a digital file. Previously conducted tests were evaluated entirely based on 8 x 10s that were produced from the film either directly or through the internegative process. This new evaluation procedure provided accurate quantitative data on granularity and contrast from the digital data. This test did not try to define which film was best visually. This is too often based on personal preference. However, the test results did group the films by good, marginal, and unacceptable. We developed, and included in this report, a template containing quantitative, graphical, and visual information for each film. These templates should be sufficient for comparing the different films tested and subsequently selecting a film or films to be used for experiments and general documentation on the International Space Station.

Slater, Richard↗
NASA NTRS2004

Gravity Effects in Condensing and Evaporating Films

A general overview of gravity effects in condensing and evaporating films is presented. The topics include: 1) Research Overview; 2) NASA Recognizes Critical Need for Condensation & Evaporation Research to Enable Human Exploration of Space; 3) Condensation and Evaporation Research in Reduced Gravity is Enabling for AHST Technology Needs; 4) Differing Role of Surface Tension on Condensing/Evaporating Film Stability; 5) Fluid Mechanisms in Condensing and Evaporating Films in Reduced Gravity; 6) Research Plan; 7) Experimental Configurations for Condensing Films; 8) Laboratory Condensation Test Cell; 9) Aircraft Experiment; 10) Condensation Study Current Test Conditions; 11) Diagnostics; 12) Shadowgraph Images of Condensing n- pentane Film in Unstable (-1g) Configuration; 13) Condensing n-Pentane Film in Normal Gravity (-1g) at Constant Pressure; 14) Condensing n-Pentane Film in Normal Gravity (-1g) with Cyclic Pressure; 15) Non-condensing Pumped Film in Normal Gravity (-1g); 16) Heat Transfer Coefficient in Developing, Unstable Condensing Film in Normal Gravity; 17) Heat Transfer for Unsteady Condensing Film (-1g); 18) Ultrasound Measurement of Film Thickness N-pentane Film, Stable (+1g) Configuration; and 19) Ultrasound Measurement of Film Thickness N-pentane Film, Unstable (-1g) Configuration.

Hermanson, J. C.↗
DOE OSTI2020

Cyclic Topology Enhancing Structural Ordering and Stability of Comb-Shaped Polypeptoid Thin Films against Melt-Induced Dewetting

We investigated the effect of cyclic chain topology on the molecular ordering and thermal stability of comb-shaped polypeptoid thin films on silicon (Si) substrates. Cyclic and linear poly(N-decylglycine) (PNDG) bearing long n-decyl side chains were synthesized by ring-opening polymerization of N-decylglycine-derived N-carboxyanhydrides. When the spin-coated thin films were subjected to thermal annealing at temperatures above the melting temperature (T > T m ), the cyclic PNDG films exhibited significantly enhanced stability against melt-induced dewetting than the linear counterparts (l-PNDG). When recrystallized at temperatures below the crystallization temperature (T < T c ), the homogeneous c-PNDG films exhibit enhanced crystalline ordering relative to the macroscopically dewetted l-PNDG films. Both cyclic and linear PNDG molecules adopt cis-amide conformations in the crystalline film, which transition into trans-amide conformations upon melting. A top-down solvent leaching treatment of both l/c-PNDG films revealed the formation of an irreversibly physisorbed monolayer with similar thickness (ca. 3 nm) on the Si substrate. The physisorbed monolayers are more disordered relative to the respective thicker crystalline films for both cyclic and linear PNDGs. Upon heating above T m , the adsorbed c-PNDG chains adopt trans-amide backbone conformation identical with the free c-PNDG molecules in the molten film. By contrast, the backbone conformations of l-PNDG chains in the adsorbed layers are notably different from those of the free chains in the molten film. We postulate that the conformational disparity between the chains in the physically adsorbed layers versus the free chains in the molten film is an important factor to account for the difference in the thermal stability of PNDG thin films. These findings highlight the use of cyclic chain topology to suppress the melt-induced dewetting in polymer thin films.

36 MATERIALS SCIENCE↗
DOE OSTI2019

FMR and Magnetic Studies of RF-Sputtered Mn-Zn Ferrite Thin Films

The Manganese–Zinc ferrite (MZF) thin films were deposited on quartz substrates by radio frequency (RF) magnetron sputtering at 10 mTorr of argon gas pressure. The FMR and magnetization measurement were carried out to understand magnetic properties of the as-deposited and annealed MZF films. The resonance field (H{sub r}) of the FMR spectra shifts towards higher magnetic field when angle between applied field and thin film plane is changed from 0 to 90° indicating the existence of uniaxial anisotropy in the film. Whereas, H{sub r} shifts towards lower magnetic field with decrease in temperature of the film. This is due to ferrimagnetic ordering in the films at low temperatures. The magnetization versus field (M-H) plots reveal the soft ferrimagnetic behavior of the films. The post-deposition annealing of the film leads to increase in crystallite size with more uniform film surface and dense columnar growth compared to the as-deposited film. The increase in magnetization and decreases in H{sub r}-values compared to that of as-deposited film are observed for annealed film. The optical band gap of the film is also found to increase with annealing.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Interfacial Strength Evaluation of Oxide Films on Carbon Steel by Using the Laser Shock Adhesion Test

We investigate the adhesion strength (interfacial strength) of the oxide film formed on a carbon steel substrate by using a laser shock adhesion test (LaSAT). A rolled carbon steel (SS400) plate is first heated at high temperature (700 °C) under the atmosphere (heat treatment) to cause the formation of oxide films about 20-50 μm thick on the steel surface. The film consisted of multiple layers, including wustite (FeO), magnetite (Fe{sub 3}O{sub 4}), and hematite (Fe{sub 2}O{sub 3}). Next, the x-ray diffraction method was used to measure the residual stress in the film. We find that compression stress develops in the film because of a mismatch of thermal strain in between the film and substrate after the heat treatment. With LaSAT, strong elastic wave generates by a pulsed laser ablation of the substrate backside, and results in interfacial fractures in the oxide films. To monitor the normal (out-of-plane) displacement of the top surface film, a laser ultrasonic interferometer is simultaneously utilized, such that we detect film delamination and determine the critical laser energy for interfacial fracture to obtain the critical stress (interfacial strength). Furthermore, additional pulsed laser irradiation is conducted against a pre-delaminated specimen in order to examine the growth of delamination area and evaluate the interfacial fracture toughness. Finally, elastic wave propagation in the sample is computed using the finite element method (FEM) in order to evaluate the interfacial stress field, accurately. For the FEM, multiple layers in the oxide film are modeled, and the residual stress due to thermal strain mismatch is introduced. The FEM computations reveal the stress distribution around the interface and evaluate the critical stress and critical stress intensity factor for delamination. We thus quantitatively evaluate the interfacial strength and interfacial fracture toughness of the oxide film formed on carbon steel. The mechanism of interfacial fracture is also discussed on the basis of microstructures in a film with multiple layers. This result may be useful for understanding the adhesion quality of oxide film during the hot-rolling process.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Influence of vanadium incorporation on the microstructure, mechanical and tribological properties of Nb–V–Si–N films deposited by reactive magnetron sputtering

Composite Nb–V–Si–N films with various V contents (3.7–13.2 at.%) were deposited by reactive magnetron sputtering and the effects of V content on the microstructure, mechanical and tribological properties of Nb–V–Si–N films were investigated. The results revealed that a three-phase structure, consisting of face-centered cubic (fcc) Nb–V–Si–N, hexagonal close-packed (hcp) Nb–V–Si–N and amorphous Si{sub 3}N{sub 4}, co-exists in the Nb–V–Si–N films and the cubic phase is dominant. The hardness and critical load (L{sub c}) of Nb–V–Si–N films initially increased gradually and reached a summit, then decreased with the increasing V content in the films and the maximum values were 35 GPa and 9.8 N, respectively, at 6.4 at.% V. The combination of V into Nb–Si–N film led to the fracture toughness linearly increasing from 1.11 MPa·m{sup 1/2} at 3.7 at.% V to 1.67 MPa·m{sup 1/2} at 13.2 at.% V. At room temperature (RT), the average friction coefficient decreased from 0.80 at 3.7 at.% V to 0.55 at 13.2 at.% V for the Nb–V–Si–N films. The wear rate of Nb–V–Si–N films initially decreased and then increased after reaching a minimum value of about 6.35 × 10{sup −} {sup 7} mm{sup 3}/N·mm at 6.4 at.% V. As the rise of testing temperature from 200 °C to 600 °C, the average friction coefficient of Nb–V–Si–N films decreased with the increase of the testing temperature regardless of V content. However, the wear rate gradually increased for all films. The average friction coefficient and wear rate at RT and elevated temperatures were mainly influenced by the vanadium oxides with weakly bonded lattice planes. - Highlight: • Fcc-Nb–V–Si–N, hcp-Nb–V–Si–N and amorphous Si{sub 3}N{sub 4} co-existed in the films. • The amount of Si{sub 3}N{sub 4} decreased with increasing V content in the films. • Hardness of Nb–V–Si–N film (6.4 at.%) reached a maximum value of 35 GPa. • Addition of V led to the increase of fracture toughness. • Tribological properties were influenced by lubricant wear debris.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Preparation and thermochromic properties of Ce-doped VO{sub 2} films

Graphical abstract: This effect of doping concentration on the phase transition temperature of VO{sub 2} films demonstrates that the phase transition temperature is decreasing along with the increase of the Ce dopant concentrations. After doping Ce, the transition temperature of VO{sub 2} film changes appreciably. Highlights: ► Ce-doped VO{sub 2} films were prepared on muscovite substrate by inorganic sol–gel method for the first time. ► The cerium existing in the VO{sub 2} films in the form of Ce{sup 4+} and Ce{sup 3+} was substituted for part of V atoms in the lattice. ► Ce doping could remarkably reduce the particle size of the Ce-doped films compared with undoped films. ► The phase transition temperature of Ce-doped VO{sub 2} films decreased appreciably with maintaining high-quality phase transition. - Abstract: Mixture of cerium (III) nitrate hexahydrate and vanadium pentaoxide powder were used as precursor to prepare Ce-doped VO{sub 2} films on the muscovite substrate by inorganic sol–gel method. SEM, XRD and XPS were used to investigate the morphologies and structures of VO{sub 2} films. The results show that the VO{sub 2} films grow on the muscovite substrate with preferred orientated (0 1 1) plane and the Ce exists in the form of Ce{sup 4+} and Ce{sup 3+} replacing part of V atoms in the lattice. The infrared transmittance change was measured from room temperature to the temperature above the metal–insulator transition. The films have excellent thermochromic performance. The metal–insulator transition temperature of VO{sub 2} films changes appreciably with Ce doped, which decreases by 4.5 °C per 1 at.% doping. Furthermore, Ce doping could remarkably reduce the particle size of VO{sub 2} films.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Non-toxic novel route synthesis and characterization of nanocrystalline ZnS{sub x}Se{sub 1−x} thin films with tunable band gap characteristics

Highlights: • A simple, inexpensive, and non-toxic CBD route is used to deposit ZnS thin films. • The ZnS{sub x}Se{sub 1−x} thin films formation takes place via annealing of ZnS thin films in Se atmosphere. • S/(S + Se) ratio found to be temperature dependent and easy tuning of band gap has been done by Se atom deposition. - Abstract: An environmentally benign chemical bath deposition (CBD) route was employed to deposit zinc sulfide (ZnS) thin films. The CBD-ZnS thin films were further selenized in a furnace at various temperatures viz. 200, 300, 400, and 500 °C and the S/(S + Se) ratio was found to be dependent on the annealing temperature. The effects of S/(S + Se) ratio on the structural, compositional and optical properties of the ZnS{sub x}Se{sub 1−x} (ZnSSe) thin films were investigated. EDS analysis showed that the S/(S + Se) ratio decreased from 0.8 to 0.6 when the film annealing temperature increased from 200 to 500 °C. The field emission scanning electron microscopy and atomic force microscopy studies showed that all the films were uniform, pin hole free, smooth, and adhered well to the glass substrate. The X-ray diffraction study on the ZnSSe thin films showed the formation of the cubic phase, except for the unannealed ZnSSe thin film, which showed an amorphous phase. The X-ray photoelectron spectroscopy revealed Zn-S, Zn-Se, and insignificant Zn-OH bonds formation from the Zn 2p{sub 3/2}, S 2p, Se 3d{sub 5/2}, and O 1s atomic states, respectively. The ultraviolet–visible spectroscopy study showed ∼80% transmittance in the visible region for all the ZnSSe thin films having various absorption edges. The tuning of the band gap energy of the ZnSSe thin films was carried out by selenizing CBD-ZnS thin films, and as the S/(S + Se) ratio decreased from 0.8 to 0.6, the band gap energy decreased from 3.20 to 3.12 eV.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Growth and Characterization of Epitaxial FeWO 4 Thin Films with Controlled Oxygen Stoichiometry

Here, we report the growth of single-phase epitaxial FeWO 4 thin films, using plasma-assisted molecular beam epitaxy, and investigate structural, optical, and electronic properties. The FeWO 4 films grow in (100) orientation on c-plane sapphire (0001) substrates and exhibit 3 rotational twin variants where FeWO 4 [001] is aligned to sapphire [100] equivalent in-plane directions. X-ray diffraction measurements indicate that the epitaxial FeWO 4 (100) structure is optimized when 80-100 W of rf power is applied to an atomic oxygen source during growth, yielding films with minimal strain and impurity phases or other orientations. In films grown with 120 W of rf power, FeWO 4 crystallites develop inhomogeneous and homogeneous strains and are potentially contaminated with Fe 3+ oxide phase impurities. In films grown with 60 W of rf power, FeWO 4 crystallites do not form fully epitaxial layers. X-ray photoelectron spectroscopy indicates that the structural changes are correlated with the Fe 3+ /Fe 2+ oxidation state ratio increasing from 0.6-1.4 with rf power from 60-120 W. X-ray fluorescence spectroscopy indicates that the Fe/W composition ratio is also increasing from 1.1-1.8 with rf power from 60-120 W. Ultraviolet and visible optical absorption spectra indicate a 1.8 ± 0.1 eV band gap with an additional interband absorption feature at 3.1 ± 0.1 eV in the 80-100 W films, with similar onsets observed in the 60 W films. In the 120 W films, the higher lying transition is shifted to 2.7 ± 0.1 eV due to the Fe 3+ enrichment. Electrical resistivity decreases over 2 orders of magnitude with oxidation from 10 4 -10 5 Ω cm in 60 W films to 120 ± 10 Ω cm in 120 W films. Thermopower measurements show p-type to n-type conductivity conversion when oxidation states shift from Fe 2+ majority in the 100 W films to Fe 3+ majority in the 120 W films. We conclude that electron polaron hopping driven by Fe 3+ is a dominant transport mechanism and a source of n-type conductivity in overoxidized FeWO 4 films.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2013

Characteristics of ultra low-k nanoporous and fluorinated silica based films prepared by plasma enhanced chemical vapor deposition

Low dielectric constant (low-k) silica based films were deposited on p-type silicon and polycarbonate substrates by radio frequency (RF) plasma enhanced chemical vapor deposition method at low temperature. A mixture of tetraethoxysilane vapor, oxygen, and tetrafluoromethane (CF{sub 4}) was used for the deposition of the films in forms of two structures called as SiO{sub x}C{sub y} and SiO{sub x}C{sub y}F{sub z}. Properties of the films were controlled by amount of porosity and fluorine content in the film matrix. The influence of RF power and CF{sub 4} flow on the elemental composition, deposition rate, surface roughness, leakage current, refractive index, and dielectric constant of the films were characterized. Moreover, optical emission spectroscopy was applied to monitor the plasma process at the different parameters. Electrical characteristics of SiO{sub x}C{sub y} and SiO{sub x}C{sub y}F{sub z} films with metal-oxide-semiconductor structure were investigated using current-voltage analysis to measure the leakage current and breakdown field, as well as capacitance-voltage analysis to obtain the film's dielectric constant. The results revealed that SiO{sub x}C{sub y} films, which are deposited at lower RF power produce more leakage current, meanwhile the dielectric constant and refractive index of these films decreased mainly due to the more porosity in the film structure. By adding CF{sub 4} in the deposition process, fluorine, the most electronegative and the least polarized atom, doped into the silica film and led to decrease in the refractive index and the dielectric constant. In addition, no breakdown field was observed in the electrical characteristics of SiO{sub x}C{sub y}F{sub z} films and the leakage current of these films reduced by increment of the CF{sub 4} flow.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Additive to regulate the perovskite crystal film growth in planar heterojunction solar cells

We reported a planar heterojunction perovskite solar cell fabricated from MAPbI{sub 3−x}Cl{sub x} perovskite precursor solution containing 1-chloronaphthalene (CN) additive. The MAPbI{sub 3−x}Cl{sub x} perovskite films have been characterized by UV-vis, SEM, XRD, and steady-state photoluminescence (PL). UV-vis absorption spectra measurement shows that the absorbance of the film with CN additive is significantly higher than the pristine film and the absorption peak is red shift by 30 nm, indicating the perovskite film with additive possessing better crystal structures. In-situ XRD study of the perovskite films with additive demonstrated intense diffraction peaks from MAPbI{sub 3−x}Cl{sub x} perovskite crystal planes of (110), (220), and (330). SEM images of the films with additive indicated the films were more smooth and homogenous with fewer pin-holes and voids and better surface coverage than the pristine films. These results implied that the additive CN is beneficial to regulate the crystallization transformation kinetics of perovskite to form high quality crystal films. The steady-state PL measurement suggested that the films with additive contained less charge traps and defects. The planar heterojunction perovskite solar cells fabricated from perovskite precursor solution containing CN additive demonstrated 30% enhancement in performance compared to the devices with pristine films. The improvement in device efficiency is mainly attributed to the good crystal structures, more homogenous film morphology, and also fewer trap centers and defects in the films with the additive.

36 MATERIALS SCIENCE↗