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DOE OSTI2015

Thermal conductivity of nitride films of Ti, Cr, and W deposited by reactive magnetron sputtering

Nitride films of Ti, Cr, and W were deposited using reactive magnetron sputtering from metal targets in argon and nitrogen plasma. TiN films with (200) orientation were achieved on silicon (100) at the substrate temperature of 500 and 600 °C. The films were polycrystalline at lower temperature. An amorphous interface layer was observed between the TiN film and Si wafer deposited at 600 °C. TiN film deposited at 600 °C showed the nitrogen to Ti ratio to be near unity, but films deposited at lower temperature were nitrogen deficient. CrN film with (200) orientation and good stoichiometry was achieved at 600 °C on Si(111) wafer but the film deposited at 500 °C showed cubic CrN and hexagonal Cr{sub 2}N phases with smaller grain size and amorphous back ground in the x-ray diffraction pattern. An amorphous interface layer was not observed in the cubic CrN film on Si(111) deposited at 600 °C. Nitride film of tungsten deposited at 600 °C on Si(100) wafer was nitrogen deficient, contained both cubic W{sub 2}N and hexagonal WN phases with smaller grain size. Nitride films of tungsten deposited at 500 °C were nonstoichiometric and contained cubic W{sub 2}N and unreacted W phases. There was no amorphous phase formed along the interface for the tungsten nitride film deposited at 600 °C on the Si wafer. Thermal conductivity and interface thermal conductance of all the nitride films of Ti, Cr, and W were determined by transient thermoreflectance technique. The thermal conductivity of the films as function of deposition temperature, microstructure, nitrogen stoichiometry and amorphous interaction layer at the interface was determined. Tungsten nitride film containing both cubic and hexagonal phases was found to exhibit much higher thermal conductivity and interface thermal conductance. The amorphous interface layer was found to reduce effective thermal conductivity of TiN and CrN films.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Characterization of XR-RV3 GafChromic{sup ®} films in standard laboratory and in clinical conditions and means to evaluate uncertainties and reduce errors

Purpose: To investigate the optimal use of XR-RV3 GafChromic{sup ®} films to assess patient skin dose in interventional radiology while addressing the means to reduce uncertainties in dose assessment. Methods: XR-Type R GafChromic films have been shown to represent the most efficient and suitable solution to determine patient skin dose in interventional procedures. As film dosimetry can be associated with high uncertainty, this paper presents the EURADOS WG 12 initiative to carry out a comprehensive study of film characteristics with a multisite approach. The considered sources of uncertainties include scanner, film, and fitting-related errors. The work focused on studying film behavior with clinical high-dose-rate pulsed beams (previously unavailable in the literature) together with reference standard laboratory beams. Results: First, the performance analysis of six different scanner models has shown that scan uniformity perpendicular to the lamp motion axis and that long term stability are the main sources of scanner-related uncertainties. These could induce errors of up to 7% on the film readings unless regularly checked and corrected. Typically, scan uniformity correction matrices and reading normalization to the scanner-specific and daily background reading should be done. In addition, the analysis on multiple film batches has shown that XR-RV3 films have generally good uniformity within one batch (<1.5%), require 24 h to stabilize after the irradiation and their response is roughly independent of dose rate (<5%). However, XR-RV3 films showed large variations (up to 15%) with radiation quality both in standard laboratory and in clinical conditions. As such, and prior to conducting patient skin dose measurements, it is mandatory to choose the appropriate calibration beam quality depending on the characteristics of the x-ray systems that will be used clinically. In addition, yellow side film irradiations should be preferentially used since they showed a lower dependence on beam parameters compared to white side film irradiations. Finally, among the six different fit equations tested in this work, typically used third order polynomials and more rational and simplistic equations, of the form dose inversely proportional to pixel value, were both found to provide satisfactory results. Fitting-related uncertainty was clearly identified as a major contributor to the overall film dosimetry uncertainty with up to 40% error on the dose estimate. Conclusions: The overall uncertainty associated with the use of XR-RV3 films to determine skin dose in the interventional environment can realistically be estimated to be around 20% (k = 1). This uncertainty can be reduced to within 5% if carefully monitoring scanner, film, and fitting-related errors or it can easily increase to over 40% if minimal care is not taken. This work demonstrates the importance of appropriate calibration, reading, fitting, and other film-related and scan-related processes, which will help improve the accuracy of skin dose measurements in interventional procedures.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2016

Pore orientation effects on the kinetics of mesostructure loss in surfactant templated titania thin films

The mesostructure loss kinetics are measured as a function of the orientation of micelles in 2D hexagonal close packed (HCP) columnar mesostructured titania thin films using in situ grazing incidence small angle x-ray scattering (GISAXS). Complementary supporting information is provided by ex situ scanning electron microscopy. Pluronic surfactant P123 acts as the template to synthesize HCP structured titania thin films. When the glass substrates are modified with crosslinked P123, the micelles of the HCP mesophase align orthogonal to the films, whereas a mix of parallel and orthogonal alignment is found on unmodified glass. The rate of mesostructure loss of orthogonally oriented (o-HCP) thin films (~60 nm thickness) prepared on modified substrate is consistently found to be less by a factor of 2.5 ± 0.35 than that measured for mixed orientation HCP films on unmodified substrates. The activation energy for mesostructure loss is only slightly greater for films on modified glass (155 ± 25 kJ/mol -1 ) than on unmodified (128 kJ/mol -1 ), which implies that the rate difference stems a greater activation entropy for mesostructure loss in o-HCP titania films. Nearly perfect orthogonal orientation of micelles on modified surfaces contributes to the lower rate of mesostructure loss by supporting the anisotropic stresses that develop within the films during annealing due to continuous curing, sintering and crystallization into the anatase phase during high temperature calcination (>450 °C). Because the film thickness dictates the propagation of orientation throughout the films and the degree of confinement, thicker (~250 nm) films cast onto P123-modified substrates have a much lower activation energy for mesostructure loss (89 ± 27 kJ/mol -1 ) due to the mix of orientations found in the films. Thus, in conclusion, this kinetic study shows that thin P123- templated o-HCP titania films are not only better able to achieve good orthogonal alignment of 3 the mesophase relative to thicker films or films on unmodified substrates, but that alignment of the mesophase in the films stabilizes the mesophase against thermally-induced mesostructure loss.

36 MATERIALS SCIENCE↗

NASA NTRS1975

Skylab program payload integration. Skylab film environmental effects

The effects of the Skylab environments on the 22 types of film used for data recording on Skylab were evaluated. Environmental histories and sensitometric curves for 114 rolls of film used for this evaluation are presented. Photographic parameters evaluated in detail were film fogging of black and white films, changes in maximum density of color film, latent image fading, and changes in film sensitivity. Other photographic and film physical anomalies such as electrostatic exposure, emulsion cracking, and reciprocity failure were also documented. Results based upon comparison of film sensitometric data for flight film with ground control film and ground test film are presented independently for each film type. The study showed that photographic film fulfilled the requirements of the Skylab applications in which it was used. Environmental film degradation, although present on almost every roll, did not preclude recording sufficient data to meet experiment requirements for all film, except film type SC-5. Specific conclusions are provided in the areas of further analyses, tests, and developments.

Source record↗

NASA NTRS2002

Stability and Heat Transfer Characteristics of Condensing Films

The overall objective of this research is to investigate the fundamental physics of film condensation in reduced gravity. The condensation of vapor on a cool surface is important in many engineering problems,including spacecraft thermal control and also the behavior of condensate films that may form on the interior surfaces of spacecraft. To examine the effects of body force on condensing films, two different geometries have been tested in the laboratory: (1) a stabilizing gravitational body force (+1g, or condensing surface facing 'upwards') and (2) de-stabilizing gravitational body force (-1g, or 'downwards'). For each geometry, different fluid configurations are employed to help isolate the fluid mechanical and thermal mechanisms operative in condensing films. The fluid configurations are (a) a condensing film, and (b) a non-condensing film with film growth by mass addition by through the plate surface. Condensation experiments are conducted in a test cell containing a cooled copper or brass plate with an exposed diameter of 12.7 cm. The metal surface is polished to allow for double-pass shadowgraph imaging, and the test surface is instrumented with imbedded heat transfer gauges and thermocouples. Representative shadowgraph images of a condensing, unstable (-1g) n-pentane film are shown. The interfacial disturbances associated with the de-stabilizing body force leading to droplet formation and break-off can be clearly seen. The heat transfer coefficient associated with the condensing film is shown. The heat transfer coefficient is seen to initially decrease, consistent with the increased thermal resistance due to layer growth. For sufficiently long time, a steady value of heat transfer is observed, accompanied by continuous droplet formation and break-off. The non-condensing cell consists of a stack of thin stainless steel disks 10 cm in diameter mounted in a brass enclosure. The disks are perforated with a regular pattern of 361 holes each 0.25 mm in diameter. Non-condensing experiments in -1g have employed 50 cSt and 125 cSt silicone oil pumped through the perforated disks at a specified rate by a syringe micropump. The time to droplet break-off and the disturbance wavelengths appear to decrease with increasing pumping rate. The ability to reliably perform multi-point, ultrasonic measurements of the film thickness has been demonstrated. A linear array of eight transducers of 6 mm diameter (with a beam footprint of comparable size) are pulsed with a square-wave signal at a frequency of 5 MHz and a pulse duration of approximately 0.3 s. For thin films (60 m to 2-3 mm in thickness) the layer thickness is determined by frequency analysis, where the received ultrasound pulse is Fourier transformed and the spacing between the peaks in the frequency spectrum is analyzed. For thicker layers (up to at least 1 cm in thickness), time-domain analysis is performed of the received ultrasound pulses to generate directly the layer thickness. A time-trace of the film thickness at a point using a single transducer in the linear array is shown for the case of an unstable (-1g) n-pentane film. The oscillations in film thickness are evidently due to the passage and/or shedding of droplets from the cooled plate surface. The entire transducer array was used to measure the changes in film thickness resulting from the passage of gravity waves generated either by an oscillating wall or the impact of a single droplet on the free surface of a film. The enclosure in both cases was 14 cm square and the transducer spacing was 12 mm. Best results were obtained using as test fluid a mixture of 50% glycerol and 50% water with a fluid layer thickness of 3-5 mm. In both cases the measured wavelengths and wave propagation speeds using the ultrasound technique compared reasonably well with those observed by optical imaging. Additional information can be found in the original extended abstract.

Hermanson, J. C.↗

DOE OSTI2013

Evaporation-driven instability of the precorneal tear film

Tear-film instability is widely believed to be a signature of eye health. When an interblink is prolonged, randomly distributed ruptures occur in the tear film. "Black spots" and/or "black streaks" appear in 15 to 40 s for normal individuals. For people who suffer from dry eye, tear-film breakup time (BUT) is typically less than a few seconds. To date, however, there is no satisfactory quantitative explanation for the origin of tear rupture. It was proposed recently that tear-film breakup is related to locally high evaporative thinning. A spatial variation in the thickness of the tear-film lipid layer (TFLL) may lead to locally elevated evaporation and subsequent tear-film breakup. We examine the local-evaporation-driven tear-film-rupture hypothesis in a one-dimensional (1-D) model for the evolution of a thin aqueous tear film overriding the cornea subject to locally elevated evaporation at its anterior surface and osmotic water influx at its posterior surface. Evaporation rate depends on mass transfer both through the coating lipid layer and through ambient air. We establish that evaporation-driven tear-film breakup can occur under normal conditions but only for higher aqueous evaporation rates. Predicted roles of environmental conditions, such as wind speed and relative humidity, on tear-film stability agree with clinical observations. More importantly, locally elevated evaporation leads to hyperosmolar spots in the tear film and, hence, vulnerability to epithelial irritation. In addition to evaporation rate, tear-film instability depends on the strength of healing flow from the neighboring region outside the breakup region, which is determined by the surface tension at the tear-film surface and by the repulsive thin-film disjoining pressure. This study provides a physically consistent and quantitative explanation for the formation of black streaks and spots in the human tear film during an interblink.

dry eye↗

DOE OSTI2015

SU-E-T-206: Comparison of EBT and EBT3 RadioChromic Films in Radiation Field of Parotid Cancer Radiotherapy

Purpose: The aim of the current study is to compare EBT and EBT3 RadioChromic films in dosimetry of radiotherapy fields for treatment of parotid cancer. Methods: The calibrations of EBT and EBT3 films were performed with the same setups for doses ranging from 0.2 Gy to 5 Gy using 6 MV photon beam of a Siemens Primus linac. These films were scanned in color mode (RGB) by a Microtek (1000XL) scanner and the red color channel data was extracted. Treatment planning for parotid cancer radiation therapy was performed on a RANDO phantom. Skin dose was measured at different points in the right anterior oblique (RAO) and right posterior oblique (RPO) fields by EBT and EBT3 films. Results: Dosimetry was performed with the same conditions for the two film types for calibration and in-phantom in parotid cancer radiotherapy. The measured net optical density (NOD) in EBT film was in some extent higher than that from EBT3 film. The minimum difference between these two films under calibration conditions was about 2.9% (for 0.2 Gy). However, the maximum difference was 35.5% (for 0.5 Gy). In the therapeutic fields of parotid cancer radiotherapy at different points, the measured dose from EBT film was higher than the EBT3 film. In these fields the minimum and maximum measured dose differences were 16.0% and 25.5%, respectively. Conclusion: With the same irradiation and reading conditions, EBT film demonstrates higher NOD than the EBT3 film. This effect may be related to the higher sensitivity of EBT film over EBT3 film. However, the obtained dose differences between these two films in low dose range can be due to the differences in fitting functions applied following the calibration process.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2012

Charge Compensated (Al, N) Co-Doped Zinc Oxide (ZnO) Films for Photlelectrochemical Application

ZnO thin films with significantly reduced bandgaps were synthesized by doping N and co-doping Al and N at 100oC. All the films were synthesized by radio-frequency magnetron sputtering on F-doped tin-oxide-coated glass. We found that co-doped ZnO:(Al,N) thin films exhibited significantly enhanced crystallinity as compared to ZnO doped solely with N, ZnO:N, at the same growth conditions. Furthermore, annealed ZnO:(Al,N) thin films exhibited enhanced N incorporation over ZnO:N films. As a result, ZnO:(Al,N) films exhibited improved photocurrents than ZnO:N films grown with pure N doping, suggesting that charge-compensated donor-acceptor co-doping could be a potential method for bandgap reduction of wide-bandgap oxide materials to improve their photoelectrochemical performance.

14 SOLAR ENERGY↗

DOE OSTI2015

Effects of different annealing atmospheres on the properties of cadmium sulfide thin films

Graphical abstract: The effects of different annealing atmospheres (air and sulfur) on the structural, morphological and optical properties of CdS thin films were studied at three different pH values. - Highlights: • Compactness and smoothness of the films were enhanced after sulfur annealing. • Micro-strain values of some films were improved after sulfur annealing. • Dislocation density values of some films were improved after sulfur annealing. • Band gap values of the films were improved after sulfur annealing. - Abstract: Cadmium sulfide (CdS) thin films were prepared on glass substrates by using chemical bath deposition (CBD) technique. The effects of different annealing atmospheres (air and sulfur) on the structural, morphological and optical properties of CdS thin films were studied at three different pH values. Compactness and smoothness of the films (especially for pH 10.5 and 11) enhanced after sulfur annealing. pH value of the precursor solution remarkably affected the roughness, uniformity and particle sizes of the films. Based on the analysis of X-ray diffraction (XRD) patterns of the films, micro-strain and dislocation density values of the sulfur-annealed films (pH 10.5 and 11) were found to be lower than those of air-annealed films. Air-annealed films (pH 10.5, 11 and 11.5) exhibited higher transmittance than sulfur-annealed films in the wavelength region of 550–800 nm. Optical band gap values of the films were found between 2.31 eV and 2.36 eV.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Preliminary study of CdTe and CdTe:Cu thin films nanostructures deposited by using DC magnetron sputtering

Growth and properties of CdTe and CdTe:Cu thin films nanostrucures deposited by using dc magnetron sputtering are reported. Scanning electron microscope (SEM) was used to observe the surface morphologies of the thin films. At growth conditions of 250 °C and 14 W, CdTe films did not yet evenly deposited. However, at growth temperature and plasma power of 325 °C and 43 W, both CdTe and CdTe:Cu(2%) have deposited on the substrates. In this condition, the morphology of the films indicate that the films have a grain-like nanostructures. Grain size diameter of about 200 nm begin to appear on top of the films. Energy Dispersive X-rays spectroscopy (EDX) was used to investigate chemical elements of the Cu doped CdTe film deposited. It was found that the film deposited consist of Cd, Te and Cu elements. XRD was used to investigate the full width at half maximum (FWHM) values of the thin films deposited. The results show that CdTe:Cu(2%) thin film has better crystallographic properties than CdTe thin film. The UV-Vis spectrometer was used to investigate the optical properties of thin films deposited. The transmittance spectra showed that transmittance of CdTe:Cu(2%) film is lower than CdTe film. It was found that the bandgap energy of CdTe and CdTe:Cu(2%) thin films of about 1.48 eV.

36 MATERIALS SCIENCE↗

DOE OSTI2011

Optical transparency and electrical conductivity of nonstoichiometric ultrathin In{sub x}O{sub y} films

The effect of thickness and composition on the electrical conductivity and optical transparency, mainly in the infrared, of ultrathin In{sub x}O{sub y} films was studied. In{sub x}O{sub y} films 35-470 A thick with oxygen atomic fractions of {approx}0.3 and {approx}0.5 were prepared via dc magnetron sputtering. All films were polycrystalline, consisting of only the cubic bixbiyte phase of In{sub 2}O{sub 3}. The average grain size of the films increased from 30 to 95 nm as the film thickness increased. The weak dependence of the electrical conductivity on the frequency and the low activation energies for conduction, a few hundredths of an eV, provided an indication that free band conduction was the primary electrical conduction mechanism in the case of all ultrathin In{sub x}O{sub y} films. It was found that introducing a high degree of nonstoichiometry in the form of oxygen deficiency did not help improve the electrical conductivity, since not all vacancies contributed two free electrons for conduction and due to impurity scattering. The optical nature of these films, studied mainly by ellipsometry, was found to be dependent on the film's composition and thickness. In the infrared, the dielectric function of all In{sub x}O{sub y} films was consistent with the Drude model, inferring that the transparency loss in this region was a result of free charge carriers. In the visible however, In{sub x}O{sub y} films under 170 A, which had an oxygen atomic fraction of {approx}0.5, were modeled by extending the Drude model to the shorter wavelengths. Films over 170 A, with the same composition, were modeled using the Cauchy dispersion model, meaning that no absorption was measured. These results indicate that, optically, under specific compositions, ultrathin In{sub x}O{sub y} films undergo a transition from metalliclike behavior to dielectric behavior with increasing film thickness. Using a figure of merit approach, it was determined that a nonstoichiometric 230 A thick In{sub x}O{sub y} film, with an oxygen atomic fraction of {approx}0.3, had the best combination of conductivity and transparency, namely, absorption of less than 20% in the infrared, about 10% in the visible, and electrical resistance of only 230 {Omega} at 20 kHz. Such a film may be classified as a highly conductive transparent oxide even in the infrared.

36 MATERIALS SCIENCE↗

DOE OSTI2012

Effect of O{sub 2} gas partial pressure on mechanical properties of Al{sub 2}O{sub 3} films deposited by inductively coupled plasma-assisted radio frequency magnetron sputtering

The effect of O{sub 2} partial pressure on the mechanical properties of Al{sub 2}O{sub 3} films is studied. Using films prepared by inductively coupled plasma-assisted radio frequency magnetron sputtering, the deposition rate of Al{sub 2}O{sub 3} decreases rapidly when oxygen is added to the argon sputtering gas. The internal stresses in the films are compressive, with magnitude decreasing steeply from 1.6 GPa for films sputtered in pure argon gas to 0.5 GPa for films sputtered in argon gas at an O{sub 2} partial pressure of 0.89 Multiplication-Sign 10{sup -2} Pa. Stress increases gradually with increasing O{sub 2} partial pressure. Using a nanoindentation tester with a Berkovich indenter, film hardness was measured to be about 14 GPa for films sputtered in pure argon gas. Hardness decreases rapidly on the addition of O{sub 2} gas, but increases when the O{sub 2} partial pressure is increased. Adhesion, measured using a Vickers microhardness tester, increases with increasing O{sub 2} partial pressure. Electron probe microanalyzer measurements reveal that the argon content of films decreases with increasing O{sub 2} partial pressure, whereas the O to Al composition ratio increases from 1.15 for films sputtered in pure argon gas to 1.5 for films sputtered in argon gas at O{sub 2} partial pressures over 2.4 Multiplication-Sign 10{sup -2} Pa. X-ray diffraction measurements reveal that films sputtered in pure argon gas have an amorphous crystal structure, whereas {gamma}-Al{sub 2}O{sub 3} is produced for films sputtered in argon gas with added O{sub 2} gas. Atomic force microscopy observations reveal that the surface topography of sputtered Al{sub 2}O{sub 3} films changes from spherical to needlelike as O{sub 2} partial pressure is increased. Fracture cross sections of the films observed by scanning electron microscopy reveal that the film morphology exhibits no discernible features at all O{sub 2} partial pressures.

36 MATERIALS SCIENCE↗

DOE OSTI2012

Comparison of Gafchromic EBT2 and EBT3 films for clinical photon and proton beams

Purpose: Dose verification in highly conformal radiation therapy such as IMRT or proton therapy can benefit from the high spatial resolution offered by radio-chromic films such as Gafchromic EBT or EBT2. Recently, a new generation of these films, EBT3, has become available. The composition and thickness of the sensitive layer are the same as for the previous EBT2 films. The most important change is the symmetric layer configuration to eliminate side orientation dependence, which is reported for EBT2 films. Methods: The general film characteristics such as sensitivity to read-out orientation and postexposure darkening evolution of the new EBT3 film are evaluated. Film response has been investigated in clinical photon and proton beams and compared to former EBT2 films. Quenching effects in the proton Bragg peak region have been studied for both, EBT2 and EBT3 films. Results: The general performance of EBT3 is comparable to EBT2, and the orientation dependence with respect to film side is completely eliminated in EBT3 films. Response differences of EBT2 and EBT3 films are of the same order of magnitude as batch-to-batch variations observed for EBT2 films. No significant difference has been found for both generations of EBT films between photon and proton exposure. Depth dose measurements of EBT2 and EBT3 show an excellent agreement, though underestimating dose by up to 20% in the Bragg peak region. Conclusions: The symmetric configuration of EBT3 presents a major improvement for film handling. EBT3 has similar dosimetric performance as its precursor EBT2 and can, thus, be applied to dose verification in IMRT in the same way. For dose verification in proton therapy the underresponse in the Bragg peak region has to be taken into account.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2015

Correcting lateral response artifacts from flatbed scanners for radiochromic film dosimetry

Purpose: A known factor affecting the accuracy of radiochromic film dosimetry is the lateral response artifact (LRA) induced by nonuniform response of a flatbed scanner in the direction perpendicular to the scan direction. This work reports a practical solution to eliminate such artifacts for all forms of dose QA. Methods: EBT3 films from a single production lot (02181401) cut into rectangular 4 × 5 cm{sup 2} pieces, with the long dimension parallel to the long dimension of the original 20.3 × 25.4 cm{sup 2} sheets, were exposed at a depth of 5 cm on a Varian Trilogy at the center of a 20 × 20 cm{sup 2} open field at seven doses between 50 and 1600 cGy using 6 MV photons. These films together with an unexposed film from the same production lot were lined one next to the other on an Epson 10000XL or 11000XL scanner in portrait orientation with their long dimension parallel to the scan direction. Scanned images were then obtained with the line of films positioned at seven discrete lateral locations perpendicular to the scan direction. The process was repeated in landscape orientation and on three other Epson scanners. Data were also collected for three additional production lots of EBT3 film (11051302, 03031401, and 03171403). From measurements at the various lateral positions, the scanner response was determined as a function of the lateral position of the scanned film. For a given color channel X, the response at any lateral position L is related to the response at the center, C, of the scanner by Response(C, D, X) = A{sub L,X} + B{sub L,X}⋅Response(L, D, X), where D is dose and the coefficients A{sub L,X} and B{sub L,X} are determined from the film measurements at the center of the scanner and six other discrete lateral positions. The values at intermediate lateral positions were obtained by linear interpolation. The coefficients were determined for the red, green, and blue color channels, preserving the ability to apply triple-channel dosimetry once corrections were applied to compensate for the lateral position response artifact. To validate this method, corrections were applied to several films that were exposed to 15 × 15cm{sup 2} open fields and large IMRT and VMAT fields and scanned at the extreme edges of the scan window in addition to the central location. Calibration and response data were used to generate dose maps and perform gamma analysis using single- or triple-channel dosimetry with FilmQAPro 2014 software. Results: The authors’ study found that calibration curves at the different lateral positions could be correlated by a simple two-point rescaling using the response for unexposed film as well as the response of film exposed at high doses between 800 and 1600 cGy. The coefficients A{sub L,X} and B{sub L,X} for each color channel X were found to be independent of dose at each lateral location L. This made it possible to apply the relationship Response(C, D, X) = A{sub L,X} + B{sub L,X}⋅Response(L, D, X), to the raw film responses, permitting correction of the response values at any lateral position to an equivalent response, as if that part of the film was located at the center of the scanner. This correction method was validated for several films exposed to open as well as large IMRT and VMAT fields. Conclusions: The work reported elaborates on the process using the correction procedures to eliminate the lateral response artifact and demonstrates improvements in the accuracy of radiochromic film dosimetry for the radiation therapy quality assurance applications.

07 ISOTOPE AND RADIATION SOURCES↗

DOE OSTI2015

Micrometer-resolved film dosimetry using a microscope in microbeam radiation therapy

Purpose: Microbeam radiation therapy (MRT) is a still preclinical tumor therapy approach that uses arrays of a few tens of micrometer wide parallel beams separated by a few 100 μm. The production, measurement, and planning of such radiation fields are a challenge up to now. Here, the authors investigate the feasibility of radiochromic film dosimetry in combination with a microscopic readout as a tool to validate peak and valley doses in MRT, which is an important requirement for a future clinical application of the therapy. Methods: Gafchromic{sup ®} HD-810 and HD-V2 films are exposed to MRT fields at the biomedical beamline ID17 of the European Synchrotron Radiation Facility (ESRF) and are afterward scanned with a microscope. The measured dose is compared with Monte Carlo calculations. Image analysis tools and film handling protocols are developed that allow accurate and reproducible dosimetry. The performance of HD-810 and HD-V2 films is compared and a detailed analysis of the resolution, noise, and energy dependence is carried out. Measurement uncertainties are identified and analyzed. Results: The dose was measured with a resolution of 5 × 1000 μm{sup 2} and an accuracy of 5% in the peak and between 10% and 15% in the valley region. As main causes for dosimetry uncertainties, statistical noise, film inhomogeneities, and calibration errors were identified. Calibration errors strongly increase at low doses and exceeded 3% for doses below 50 and 70 Gy for HD-V2 and HD-810 films, respectively. While the grain size of both film types is approximately 2 μm, the statistical noise in HD-V2 is much higher than in HD-810 films. However, HD-810 films show a higher energy dependence at low photon energies. Conclusions: Both film types are appropriate for dosimetry in MRT and the microscope is superior to the microdensitometer used before at the ESRF with respect to resolution and reproducibility. However, a very careful analysis of the image data is required. Dosimetry at low photon energies should be performed with great caution due to the energy sensitivity of the films. In this respect, HD-V2 films showed to have an advantage over HD-810 films. However, HD-810 films have a lower statistical noise level. When a higher resolution is required, e.g., for the dosimetry of pencil beam irradiations, noise may render HD-V2 films inapplicable.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2019

Electrical and Optical Characteristics of Si-Nanoparticle Films Deposited onto Substrates by High-Voltage Electrospraying from Ethanol Sols

The optical and electrical characteristics of films consisting of nanocrystalline silicon (nc-Si) deposited onto substrates by the high-voltage electrospraying of nc-Si sols in ethanol are investigated. It is found that the interaction of ethanol droplets carrying Si nanoparticles with a corona-discharge electric field leads to the polymerization of ethanol and the formation of a polymer layer on the Si-nanoparticle surface. A high-voltage facility for depositing the films using an additional focusing electrode allows one to change the geometry of the electric field and intensity in the region of the ethanol droplet flow. As a result, nc-Si films with qualitatively different properties of the polymer on the nanoparticle surface are formed, specifically, nc-Si-A and nc-Si-B, obtained without a focusing electrode and with it, respectively. Upon annealing at temperatures of up to 400°С, the optical band gap E{sub g} of the nc-Si-A films increases from ~1.9 to ~2.2 eV, while the E{sub g} value of the nc-Si-B films remains constant and amounts to 1.85 eV. The constant E{sub g} value of the nc-Si-B films is explained by the properties of the polymer on the Si-nanoparticle surface and the more effective blocking of oxygen penetration from the surrounding environment upon annealing at temperatures of up to 400°C than in the case of a polymer in nc-Si-A films. The temperature dependences of the dark and photoinduced conductivity of nc-Si-A films are approximated with good accuracy by two activation-type exponential functions and the dark activation energies are ~0.75 and 0.1 eV, respectively. The conductivity of the nc-Si-A films noticeably decreases under irradiation of the samples at wavelengths of 460–470 nm. The temperature dependences of the conductivity of the nc-Si-B films are approximated with good accuracy by exponential functions with activation energies of 0.73 (in the dark) and 0.59 eV (under photoexcitation). In contrast to the case of nc-Si-A films, the photoconductivity of nc-Si-B films grows more than fourfold relative to the dark conductivity under analogous illumination. The nc-Si-B films are photoactive and sandwich-like Al/nc-Si-B/Al structures can generate a voltage. The dark conductivity and photoconductivity of the nc-Si-A films in the voltage range of V > 2 V are determined by the two-center Poole–Frenkel effect; the concentration of the centers affecting the Poole–Frenkel conductivity is ~3 × 10{sup 17} cm{sup –3}. In nc-Si-B films in the voltage range of 2–5 V, electron transport is determined by space-charge-limited currents and, at high voltages, by the two-center Poole–Frenkel effect. The concentration of traps contributing to the space-charge-limited currents is ~4 × 10{sup 16} cm{sup –3}. The concentration of Poole–Frenkel centers affecting the conductivity decreases according to the activation law with an activation energy of 0.7 eV from 3 × 10{sup 16} to 2 × 10{sup 14} cm{sup –3} with a decrease in temperature from 120°C to 40°C.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2020

Continuous polymer films deposited on top of porous substrates using plasma-enhanced atomic layer deposition and molecular layer deposition

Molecular layer deposition (MLD) is able to produce ultrathin polymer films with control over thickness, cross-linking, and chemical composition. With these capabilities, MLD should be useful in the fabrication of novel polymer membranes on porous supports. However, confining a continuous MLD film to the surface of porous substrates is difficult because of MLD film growth in the pores. The deposition in the pores lowers the conductance of the porous support. This paper presents a method to deposit continuous polymer films on top of porous substrates. In this method, Al2O3 plasma-enhanced atomic layer deposition (PE-ALD) using trimethylaluminum and oxygen plasma as the reactants was first used to cap the pores of the substrate. Subsequently, a polyamide MLD film was deposited on the Al2O3 PE-ALD capping layer using m-phenylenediamine and trimesoyl chloride as the reactants. The Al2O3 pore caps were then removed from the porous substrate by etching from the backside using a timed exposure to a dilute sodium hydroxide solution. This method was demonstrated using anodic aluminum oxide (AAO) and polyethersulfone (PES) porous substrates. Al2O3 PE-ALD film growth was limited to the top of the porous substrate, resulting in rapid surface recombination or high sticking coefficients for the reactive plasma species within the pores. Gas permeance measurements confirmed the pore capping of the AAO substrates. The reopening of the pores by dissolving the Al2O3 pore caps with a sodium hydroxide solution was monitored using gas permeance versus etch time. The removal of the Al2O3 pore caps from the PES substrates could also dissolve the Al2O3 layer underneath the MLD film. The loss of this Al2O3 layer led to the detachment of the MLD film from the PES substrate. However, the MLD film could be anchored to the PES support at fractures located in the Al2O3 film prior to the MLD. The Al2O3 film fracture allowed the MLD film to anchor firmly to the PES substrate by MLD in the pores of the PES porous substrate. The distance between the anchor points was a function of fracture density. This distance could be controlled by applying a tensile stress to the Al2O3 PE-ALD film to fracture the film through sample bending. This method produced firmly anchored polymer MLD films on top of the PES porous substrates.

Welch, Brian C. (ORCID:000000029747045X)↗

DOE OSTI2020

Metalorganic chemical vapor deposition of ZnGeN 2 films on GaN: effects of cation stoichiometry on surface morphology and crystallinity

Novel optoelectronic device designs based on the heterostructures of III-N and II-IV-N 2 are promising to advance device performance significantly. For example, by utilizing InGaN-ZnGeN 2 quantum well (QW) structures instead of pure InGaN, the band structure engineering in the QW active region can lead to improved electron-hole wavefunction overlap, and thus enhance the radiative efficiency for photon generation. These novel heterostructures have great potential to address the current challenge of low quantum efficiency in InGaN QW based light emitting diodes emitting in green and beyond. The materials development of ZnGeN 2 is still at an early stage as compared to the much matured GaN material system. In an ideal octet rule preserving ordered structure of ZnGeN 2 , every N atom is coordinated by exactly two Zn and two Ge atoms. However, local violation of octet rule can be caused by non-ideal coordination of N by the cations. The disordered structure is thermodynamically less favorable but can still be achieved, for example, in kinetics-limited growth regime. The ordered ZnGeN 2 has a bandgap very close to that of GaN (~3.4 eV) and a lattice mismatch of <0.1% with GaN. Interestingly, the valence band of ZnGeN 2 has been predicted to be ~1 eV above that of GaN, which has inspired novel designs for high efficiency light emitters. In this work, we investigated the metalorganic chemical vapor deposition (MOCVD) of ZnGeN 2 films on GaN/c-sapphire templates. Diethylzinc (DEZn), germane (GeH4) and ammonia were used as the precursors for Zn, Ge and N, respectively. A systematic study was conducted to investigate the cation stoichiometry as a function of growth temperature (TG), total reactor pressure (P) and DEZn/GeH 4 molar flow rate ratio (RII/IV). Under the investigated growth window, the Zn/(Zn+Ge) composition in the films, determined from energy dispersive X-ray spectroscopy, decreased monotonically with increase in TG but increased with increase in P and RII/IV. Atom probe tomography data did not indicate the presence of any secondary phases such as Zn 3 N 2 or Ge 3 N 4 . The surface morphology and crystallinity of the grown films had strong correlation with the Zn/(Zn+Ge) composition. The scanning electron microscopy images showed that the near-stoichiometric films have planar surfaces whereas Zn-rich films had crystallites on their surface and the Zn-poor films had faceted surface. Scanning transmission electron microscopy (STEM) imaging revealed that the Zn-rich and Zn-poor films have columnar and filament-like morphology, respectively, whereas the near-stoichiometric films have continuous film-like cross-sectional morphology. TEM nano-diffraction patterns as well as X-ray diffraction 2θ-ω scan profiles indicate that the near stoichiometric films are single crystalline. Nano-diffraction pattern of the stoichiometric films resembled that of a disordered ZnGeN 2 structure. Room temperature Raman spectra of near-stoichiometric films showed only the phonon density of states like features of a cation disordered ZnGeN 2 . Cathodoluminescence and photoluminescence spectra measured at different temperatures had similar features with peak emission wavelength at ~ 2 eV. In conclusion, the stoichiometry of ZnGeN 2 films can be widely tuned by tuning the MOCVD growth parameters. The surface morphology and the crystallinity of the films were found to have strong correlation with the Zn/(Zn+Ge) composition. The stoichiometric ZnGeN 2 films grown on GaN were demonstrated with uniform surface morphology and high crystalline quality. The results from this work will provide pathway to implement ZnGeN 2 in device structures.

Karim, Md Rezaul↗