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At least 973 records · Page 54
All sourcesNASA NTRSDOE OSTI
DOE OSTI2012

Variations in dose distribution and optical properties of Gafchromic{sup TM} EBT2 film according to scanning mode

Purpose: The authors aim was to investigate the effects of using transmission and reflection scanning modes, the film orientation during scanning, and ambient room light on a dosimetry system based on the Gafchromic{sup TM} EBT2 film model. Methods: For calibration, the films were cut to 3 x 3 cm{sup 2} and irradiated from 20 to 700 cGy at the depth of maximum dose using 6 and 10 MV photon beams in a 10 x 10 cm{sup 2} field size. Absolute dose calibration of the linear accelerator was done according to the TRS398 protocol. An FG65-G ionization chamber was used to monitor the dose while irradiating the films in solid water. The film pieces were scanned with an EPSON Expression 1680 Pro flatbed scanner in transmission and reflection modes. Authors investigated the effect of orientation on films and examined the optical properties of EBT2 film using an ellipsometer and an ultraviolet (UV)/visible spectrometer to explain the dosimetric dependence of the film on orientation during the scanning process. To investigate the effect of ambient room light, films were preirradiated in 6 and 10 MV photon beams with intensity-modulated radiotherapy (IMRT) quality assurance (QA) plans, and then exposed to room light, either directly for 2 days in a workroom or for 2 months in a film box. Gamma index pass criteria of (3%, 3 mm) were used. Results: The dose response curves based on net optical density (NOD) indicated that the reflection scanning mode can provide a better dose sensitivity than the transmission scanning mode, whereas the standard deviation of the dose is greater in reflection mode than in transmission mode. When the film was rotated 90 deg. from the portrait orientation, the average dose of the EBT2 film decreased by 11.5-19.6% in transmission mode and by 1.5-2.3% in reflection mode. Using an ellipsometer, variation of the refractive index of EBT2 film--the birefringence property--was found to be the largest between 45 deg. (1.72 and 1.71) and 135 deg. (1.8 and 1.77) for 300 and 800 cGy. Absorption spectra of EBT2 films measured with spectrometer were the function of film orientation. The readings in reflection scanning mode were more stable against room light than those in transmission scanning mode, although dose readings increased in both modes after the films were exposed to room light. Conclusions: The transmission scanning mode exhibited a strong dependence on film orientation during scanning and a change in optical density resulting from room light exposure, so a constant scanning orientation and minimal exposure to light can reduce uncertainty in the measured dose (23 {+-} 3%). The angular dependence was analyzed using Jones matrices and optical properties of EBT2 film were obtained using an ellipsometer and an UV/visible spectrometer. The reflection scanning mode has relatively good stability with respect to room light and film orientation on a scanner, although the large standard deviation of dose is a disadvantage in measurements of absolute dose. Reflection scanning mode can offer a potential advantage for film dosimetry in radiotherapy, although transmission scanning mode is still recommended for dosimetry as it provides better uncertainty results.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2014

Development and characterization of a three-dimensional radiochromic film stack dosimeter for megavoltage photon beam dosimetry

Purpose: Three-dimensional (3D) dosimeters are particularly useful for verifying the commissioning of treatment planning and delivery systems, especially with the ever-increasing implementation of complex and conformal radiotherapy techniques such as volumetric modulated arc therapy. However, currently available 3D dosimeters require extensive experience to prepare and analyze, and are subject to large measurement uncertainties. This work aims to provide a more readily implementable 3D dosimeter with the development and characterization of a radiochromic film stack dosimeter for megavoltage photon beam dosimetry. Methods: A film stack dosimeter was developed using Gafchromic{sup ®} EBT2 films. The dosimeter consists of 22 films separated by 1 mm-thick spacers. A Virtual Water™ phantom was created that maintains the radial film alignment within a maximum uncertainty of 0.3 mm. The film stack dosimeter was characterized using simulations and measurements of 6 MV fields. The absorbed-dose energy dependence and orientation dependence of the film stack dosimeter were investigated using Monte Carlo simulations. The water equivalence of the dosimeter was determined by comparing percentage-depth-dose (PDD) profiles measured with the film stack dosimeter and simulated using Monte Carlo methods. Film stack dosimeter measurements were verified with thermoluminescent dosimeter (TLD) microcube measurements. The film stack dosimeter was also used to verify the delivery of an intensity-modulated radiation therapy (IMRT) procedure. Results: The absorbed-dose energy response of EBT2 film differs less than 1.5% between the calibration and film stack dosimeter geometries for a 6 MV spectrum. Over a series of beam angles ranging from normal incidence to parallel incidence, the overall variation in the response of the film stack dosimeter is within a range of 2.5%. Relative to the response to a normally incident beam, the film stack dosimeter exhibits a 1% under-response when the beam axis is parallel to the film planes. Measured and simulated PDD profiles agree within a root-mean-square difference of 1.3%. In-field film stack dosimeter and TLD measurements agree within 5%, and measurements in the field penumbra agree within 0.5 mm. Film stack dosimeter and TLD measurements have expanded (k = 2) overall measurement uncertainties of 6.2% and 5.8%, respectively. Film stack dosimeter measurements of an IMRT dose distribution have 98% agreement with the treatment planning system dose calculation, using gamma criteria of 3% and 2 mm. Conclusions: The film stack dosimeter is capable of high-resolution, low-uncertainty 3D dose measurements, and can be readily incorporated into an existing film dosimetry program.

62 RADIOLOGY AND NUCLEAR MEDICINE↗
DOE OSTI2015

Using Radiochromic Films to Characterize the Dispersion of ZrO{sub 2} Nano-sized Grain Clusters in Protective Polymer Composites

Radiation dosimetry is commonly used to prevent deterministic radiation effects in high dose medical procedures. Radiochromic films find nowadays widely application in radiotherapy, interventional procedures and CT exams for isodose and maximum skin dose measurements. Moreover the size of the irradiated area and its distribution can be performed through the reading of the individual components in the RGB-spectrum. Particularly, radiochromic film has multiple advantages over alternative dosimeters for low-kV X-rays dosimetry. Concerned to spatial resolution it is far superior to that of ionization chambers and thermoluminescent dosimeters. For high energy photon fields (keV to MeV) the most used radiochromic film commercially available belongs to the EBT Gafchromic{sup R} series. On the other hand, for low energy photon fields in the x-ray range (20 kVp to 200 kVp) the best choice belongs to the XR-QA Gafchromic{sup R} film series. In this work we demonstrate the possibility of generating 2D images of thin polymeric composites films using EBT3 and XR-QA2 Gafchromic{sup R} films exposed to 6 MeV and 40 keV x-ray photons, respectively, using the digital filtering tools of the ImageJ{sup R} free software. In this context, EBT3 films were placed on the surface of a rigid anthropomorphic phantom. Then, they were covered with a thermoplastic mask made of PCL polymer. This setup was then exposed to 2.0 Gy absorbed dose in the Linear Accelerator beam. The EBT3 films were then scanned in the high resolution mode in a commercial scanner and the images subsequently treated with digital filters. It is somehow possible to see the image of the thermoplastic mask in the scanned image. However, in the treated image it is easy to observe the mask arrangement. The unexpected phenomenon here is the EB3 film ability to detect the attenuation of high energy photons by a plastic material, which in turn has a very low mass-energy attenuation coefficient, producing a very clear 2D image. This result is discussed in terms of the high Z halides added to the sensitive layer of EB3 film, once the main components are C (42.3%), H (39.7%) and O (16.0%)1-2. Based on the above results, we have speculated about the abilities of XR-AQ films in the detection of the distribution of nano-sized particles that has high mass-energy attenuation coefficients for low energy x-rays, in polymer composites. In another investigation we tested the ability of XR-QA2 Gafchromic{sup R} films to evaluate the dispersion of ZrO{sub 2} nano-sized grain clusters in protective composites. The P(VDFTrFE)/ ZrO{sub 2} film was sandwiched between two XR-QA2 radiochromic films. In this setup, one radiochromic film is directly exposed to 100 mGy of the x-rays beam and another one measures the attenuated beam. After storage for 24 hours at room temperature under no light conditions, the irradiated radiochromic films were scanned under the same conditions in order to obtain a more reliable result. All films were scanned using the same size ROI in high resolution mode and saved as tagged image file format (TIFF). The untreated scanned image of the XR-AQ2 film directed exposed to the X-ray beam and the correspondent treated image with digital filters are shown. The untreated and treated image of the XR-AQ2 film that was exposed to the attenuated x-ray beam is shown. The image treated with digital filters seems to reproduce the dispersion of ZrO{sub 2} nano-sized grain clusters in the P(VDF-TrFE) copolymer matrix. This result is also discussed in terms of the high Z halides added to the sensitive layer of XR-AQ2 film and compared to the MEV images obtained from the P(VDF-TrFE)/ZrO{sub 2} composites. The results indicate a clear correlation between the 2D radiochromic image and the MEV photography.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
NASA NTRS2002

The Effects of Ultra Thin Films on Dynamic Wetting

Dynamic wetting, the displacement of one fluid by another immiscible fluid on a surface, controls many natural and technological phenomena, such as coating, printing, spray painting and lubricating. Particularly in coating and spraying applications, contact lines advance across pre-existing fluid films. Most previous work has focused on contact lines advancing across films sufficiently thick that they behave as simple Newtonian fluids. Ultrathin films, where the film thickness may impinge on fundamental length scales in the fluid, have received less attention. In this talk, we will discuss the effects of ultrathin polymer films on dynamic wetting. We measure the interface shape within microns of moving contact lines advancing across preexisting films and compare the measurements to existing models of viscous bending for interfaces advancing across dry surfaces and 'thick' (in the sense that they behave as liquids) films. In the experiments, we advance a contact line of 10-poise and 1-poise polydimethylsiloxane (silicone oil) across pre-coated films of the same fluid with thickness from a single chain thickness (approx. 10 A) through a couple of radii of gyration (100-200 A) to films so thick they are likely bulk in behavior (10(exp 3) A). All films are physisorbed, i.e. they readily rinse from the surface. Thus, molecules in the film are not anchored to the surface and can move within the film if the hydrodynamics dictate such motion. For films of the thickness of a single chain (approx. 10 A), our experiments indicate that the advancing fluid behaves just as it would if it advanced over a dry surface. For the thicker films (10(exp 3) A), we find behavior indicating that the molecules in the film are acting as a fluid with the bulk properties. In this regime, results for the two different fluids are identical when the experiments are performed at the same pre-existing film thickness and advancing capillary number, Ca. For film of thickness of a few radii of gyration (approx. 100-200 A), the behavior depends on Ca of the advancing meniscus. At low Ca, the viscous bending of the interface near the contact line does not behave as it would on a dry surface. It has a lower curvature than expected. However, at higher Ca, the viscous bending is described by the model for spreading over a dry surface. These results show that the fluid flow in the film does behave differently than bulk as the film thickness becomes comparable to molecular length scale. But even more intriguing is the unusual velocity dependence of that behavior where the film behaves more solid-like at higher contact line speeds. We will discuss these results in terms of the properties of confined polymer melts.

Chen, Xia↗
NASA NTRS2011

Real-Time Deposition Monitor for Ultrathin Conductive Films

A device has been developed that can be used for the real-time monitoring of ultrathin (2 or more) conductive films. The device responds in less than two microseconds, and can be used to monitor film depositions up to about 60 thick. Actual thickness monitoring capability will vary based on properties of the film being deposited. This is a single-use device, which, due to the very low device cost, can be disposable. Conventional quartz/crystal microbalance devices have proven inadequate to monitor the thickness of Pd films during deposition of ultrathin films for hydrogen sensor devices. When the deposited film is less than 100 , the QCM measurements are inadequate to allow monitoring of the ultrathin films being developed. Thus, an improved, high-sensitivity, real-time deposition monitor was needed to continue Pd film deposition development. The new deposition monitor utilizes a surface acoustic wave (SAW) device in a differential delay-line configuration to produce both a reference response and a response for the portion of the device on which the film is being deposited. Both responses are monitored simultaneously during deposition. The reference response remains unchanged, while the attenuation of the sensing path (where the film is being deposited) varies as the film thickness increases. This device utilizes the fact that on high-coupling piezoelectric substrates, the attenuation of an SAW undergoes a transition from low to very high, and back to low as the conductivity of a film on the device surface goes from nonconductive to highly conductive. Thus, the sensing path response starts with a low insertion loss, and as a conductive film is deposited, the film conductivity increases, causing the device insertion loss to increase dramatically (by up to 80 dB or more), and then with continued film thickness increases (and the corresponding conductivity increases), the device insertion loss goes back down to the low level at which it started. This provides a continuous, real-time monitoring of film deposition. For use with different films, the device would need to be calibrated to provide an understanding of how film thickness is related to film conductivity, as the device is responding primarily to conductivity effects (and not to mass loading effects) in this ultrathin film regime.

Hines, Jacqueline↗
DOE OSTI2011

Calibration of GafChromic XR-RV3 radiochromic film for skin dose measurement using standardized x-ray spectra and a commercial flatbed scanner

Purpose: In this study, newly formulated XR-RV3 GafChromic film was calibrated with National Institute of Standards and Technology (NIST) traceability for measurement of patient skin dose during fluoroscopically guided interventional procedures. Methods: The film was calibrated free-in-air to air kerma levels between 15 and 1100 cGy using four moderately filtered x-ray beam qualities (60, 80, 100, and 120 kVp). The calibration films were scanned with a commercial flatbed document scanner. Film reflective density-to-air kerma calibration curves were constructed for each beam quality, with both the orange and white sides facing the x-ray source. A method to correct for nonuniformity in scanner response (up to 25% depending on position) was developed to enable dose measurement with large films. The response of XR-RV3 film under patient backscattering conditions was examined using on-phantom film exposures and Monte Carlo simulations. Results: The response of XR-RV3 film to a given air kerma depended on kVp and film orientation. For a 200 cGy air kerma exposure with the orange side of the film facing the source, the film response increased by 20% from 60 to 120 kVp. At 500 cGy, the increase was 12%. When 500 cGy exposures were performed with the white side facing the x-ray source, the film response increased by 4.0% (60 kVp) to 9.9% (120 kVp) compared to the orange-facing orientation. On-phantom film measurements and Monte Carlo simulations show that using a NIST-traceable free-in-air calibration curve to determine air kerma in the presence of backscatter results in an error from 2% up to 8% depending on beam quality. The combined uncertainty in the air kerma measurement from the calibration curves and scanner nonuniformity correction was {+-}7.1% (95% C.I.). The film showed notable stability. Calibrations of film and scanner separated by 1 yr differed by 1.0%. Conclusions: XR-RV3 radiochromic film response to a given air kerma shows dependence on beam quality and film orientation. The presence of backscatter slightly modifies the x-ray energy spectrum; however, the increase in film response can be attributed primarily to the increase in total photon fluence at the sensitive layer. Film calibration curves created under free-in-air conditions may be used to measure dose from fluoroscopic quality x-ray beams, including patient backscatter with an error less than the uncertainty of the calibration in most cases.

07 ISOTOPE AND RADIATION SOURCES↗
DOE OSTI2013

Calibrating page sized Gafchromic EBT3 films

Purpose: The purpose is the development of a novel calibration method for dosimetry with Gafchromic EBT3 films. The method should be applicable for pretreatment verification of volumetric modulated arc, and intensity modulated radiotherapy. Because the exposed area on film can be large for such treatments, lateral scan errors must be taken into account. The correction for the lateral scan effect is obtained from the calibration data itself. Methods: In this work, the film measurements were modeled using their relative scan values (Transmittance, T). Inside the transmittance domain a linear combination and a parabolic lateral scan correction described the observed transmittance values. The linear combination model, combined a monomer transmittance state (T{sub 0}) and a polymer transmittance state (T{sub {infinity}}) of the film. The dose domain was associated with the observed effects in the transmittance domain through a rational calibration function. On the calibration film only simple static fields were applied and page sized films were used for calibration and measurements (treatment verification). Four different calibration setups were considered and compared with respect to dose estimation accuracy. The first (I) used a calibration table from 32 regions of interest (ROIs) spread on 4 calibration films, the second (II) used 16 ROIs spread on 2 calibration films, the third (III), and fourth (IV) used 8 ROIs spread on a single calibration film. The calibration tables of the setups I, II, and IV contained eight dose levels delivered to different positions on the films, while for setup III only four dose levels were applied. Validation was performed by irradiating film strips with known doses at two different time points over the course of a week. Accuracy of the dose response and the lateral effect correction was estimated using the dose difference and the root mean squared error (RMSE), respectively. Results: A calibration based on two films was the optimal balance between cost effectiveness and dosimetric accuracy. The validation resulted in dose errors of 1%-2% for the two different time points, with a maximal absolute dose error around 0.05 Gy. The lateral correction reduced the RMSE values on the sides of the film to the RMSE values at the center of the film. Conclusions: EBT3 Gafchromic films were calibrated for large field dosimetry with a limited number of page sized films and simple static calibration fields. The transmittance was modeled as a linear combination of two transmittance states, and associated with dose using a rational calibration function. Additionally, the lateral scan effect was resolved in the calibration function itself. This allows the use of page sized films. Only two calibration films were required to estimate both the dose and the lateral response. The calibration films were used over the course of a week, with residual dose errors Less-Than-Or-Slanted-Equal-To 2% or Less-Than-Or-Slanted-Equal-To 0.05 Gy.

07 ISOTOPE AND RADIATION SOURCES↗
NASA NTRS1999

Gravitational Effects on the Morphology and Kinetics of Photodeposition of Polydiacetylene Thin Films From Monomer Solutions

The goal of this proposed work is to study gravitational effects on the photodeposition of polydiacetylene thin films from monomer solutions onto transparent substrates. Polydiacetylenes have been an extensively studied class of organic polymers because they exhibit many unusual and interesting properties, including electrical conductivity and optical nonlinearity. Their long polymeric chains render polydiacetylenes readily conducive to thin film formation, which is necessary for many applications. These applications require thin polydiacetylene films possessing uniform thicknesses, high purity, minimal inhomogeneities and defects (such as scattering centers), etc. Also, understanding and controlling the microstructure and morphology of the films is important for optimizing their electronic and optical properties. The lack of techniques for processing polydiacetylenes into such films has been the primary limitation to their commercial use. We have recently discovered a novel method for the formation of polydiacetylene thin films using photo-deposition from monomer solutions onto transparent substrates with UV light. This technique is very simple to carry out, and can yield films with superior quality to those produced by conventional methods. Furthermore, these films exhibit good third-order properties and are capable of waveguiding. We have been actively studying the chemistry of diacetylene polymerization in solution and the photo-deposition of polydiacetylene thin films from solution. It is well-known that gravitational factors such as buoyancy-driven convection and sedimentation can affect chemical and mass transport processes in solution. One important aspect of polydiacetylene thin film photodeposition in solution, relevant to microgravity science, is that heat generated by absorption of UV radiation induces thermal density gradients that under the influence of gravity, can cause fluid flows (buoyancy-driven convection). Additionally, changes in the chemical composition of the solution during polymerization may cause solutal convection. These fluid flows affect transport of material to and from the film surface and thereby affect the kinetics of the growth process. This manifests itself in the morphology of the resulting films; films grown under the influence of convection tend to have less uniform thicknesses, and can possess greater inhomogeneities and defects. Specifically, polydiacetylene films photodeposited from solution, when viewed under a microscope, exhibit very small particles of solid polymer which get transported by convection from the bulk solution to the surface of the growing film and become embedded. Even when carried out under conditions designed to minimize unstable density gradients (i.e., irradiating the solution from the top), some fluid flow still takes place (particles remain present in the films). It is also possible that defect nucleation may be occurring within the films or on the surface of the substrate; this, too, can be affected by convection (as is the case with crystal growth). Hence films grown in 1-g will, at best, still possess some defects. The objective of this proposal is to investigate, both in 1-g and in low-g, the effects of gravitational factors (primarily convection) on the dynamics of these processes, and on the quality, morphology, and properties of the films obtained.

Paley, Mark S.↗
DOE OSTI2021

Thermal Conductivity of β-Phase Ga 2 O 3 and (Al x Ga 1– x ) 2 O 3 Heteroepitaxial Thin Films

Heteroepitaxy of β-phase gallium oxide (β-Ga 2 O 3 ) thin films on foreign substrates shows promise for the development of next-generation deep ultraviolet solar blind photodetectors and power electronic devices. In this work, the influences of the film thickness and crystallinity on the thermal conductivity of ($\bar{2}01$)-oriented β-Ga 2 O 3 heteroepitaxial thin films were investigated. Unintentionally doped β-Ga 2 O 3 thin films were grown on c-plane sapphire substrates with off-axis angles of 0° and 6° toward $\langle$$11\bar{2}0$$\rangle$ via metal–organic vapor phase epitaxy (MOVPE) and low-pressure chemical vapor deposition. The surface morphology and crystal quality of the β-Ga 2 O 3 thin films were characterized using scanning electron microscopy, X-ray diffraction, and Raman spectroscopy. The thermal conductivities of the β-Ga 2 O 3 films were measured via time-domain thermoreflectance. The interface quality was studied using scanning transmission electron microscopy. The measured thermal conductivities of the submicron-thick β-Ga 2 O 3 thin films were relatively low as compared to the intrinsic bulk value. The measured thin film thermal conductivities were compared with the Debye–Callaway model incorporating phononic parameters derived from first-principles calculations. The comparison suggests that the reduction in the thin film thermal conductivity can be partially attributed to the enhanced phonon-boundary scattering when the film thickness decreases. They were found to be a strong function of not only the layer thickness but also the film quality, resulting from growth on substrates with different offcut angles. Growth of β-Ga 2 O 3 films on 6° offcut sapphire substrates was found to result in higher crystallinity and thermal conductivity than films grown on on-axis c-plane sapphire. However, the β-Ga 2 O 3 films grown on 6° offcut sapphire exhibit a lower thermal boundary conductance at the β-Ga 2 O 3 /sapphire heterointerface. In addition, the thermal conductivity of MOVPE-grown ($\bar{2}01$)-oriented β-(Al x Ga 1–x ) 2 O 3 thin films with Al compositions ranging from 2% to 43% was characterized. Because of phonon-alloy disorder scattering, the β-(Al x Ga 1–x ) 2 O 3 films exhibit lower thermal conductivities (2.8–4.7 W/m∙K) than the β-Ga 2 O 3 thin films. The dominance of the alloy disorder scattering in β-(Al x Ga 1–x ) 2 O 3 is further evidenced by the weak temperature dependence of the thermal conductivity. This work provides fundamental insight into the physical interactions that govern phonon transport within heteroepitaxially grown β-phase Ga 2 O 3 and (Al x Ga 1–x ) 2 O 3 thin films and lays the groundwork for the thermal modeling and design of β-Ga 2 O 3 electronic and optoelectronic devices.

36 MATERIALS SCIENCE↗
DOE OSTI2016

SU-F-T-581: The Effect of Scanning Orientation On New EBT-XD Film Using Vidar and Epson Scanners

Purpose: To study the effect of film scanning orientation for new EBT-XD film using Vidar and Epson scanners, compared with EBT3 films. Methods: The EBT-XD (lot#01081501) and EBT3 films (lot#11031501) were cut into 4cm×7cm pieces and each film piece was uniformly exposed to a 6MV photon beam (15×15cm{sup 2}) at 5 cm depth and 100cm SAD in polystyrene phantom, one at a time. The doses delivered were 0,2.5,5,10,20,30,40 and 50 Gy for EBT-XD films, and 0,0.5,1,2,4,8,12 and 16 Gy for EBT3 films, respectively. All films were scanned at least 16 hours after irradiation, one at a time, in portrait or landscape orientation, using a Vidar DosimetryPro Advantage Red and an Epson 10000XL scanner (red channel). Each film piece was positioned at the center of a frame (36cm×36cm) with a cutout slightly larger than the film size for scanning. The scanned data (71 dpi), were analyzed using ImageJ and the average in the ROI (3cm×3cm) of each film at the center was obtained. Results: Dose response curves (netOD vs. dose) were established and compared with EBT-XD and EBT3 film in portrait or landscape orientation using these two scanners. The portrait to landscape (P/L) ratio for each film/scanner combination was determined. The EBT-XD film is about three times less sensitive than EBT3 film. The netOD is higher for portrait than landscape orientation for all the film/scanner combinations. For EBT-XD and EBT3, the average P/L ratios are 1.02 and 1.03 using Vidar scanner, and 1.03 and 1.05 using Epson scanner (red channel), respectively. Conclusion: The effect of film scanning orientation for new EBT-XD film using Vidar Advantage Red and Epson 10000XL scanners has been studied, in comparison with EBT3 film. The portrait/landscape ratios are the lowest for EBT-XD film using Vidar Advantage Red scanner among the four film/scanner combinations.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2017

Enhancement of spin-lattice coupling in nanoengineered oxide films and heterostructures by laser MBE

The objective of the proposed research is to investigate nanoengineered oxide films and multilayer structures that are predicted to show desirable properties. The main focus of the project is an atomic layer-by-layer laser MBE (ALL-Laser MBE ) technique that is superior to the conventional laser MBE in broadening the conditions for the synthesis of high quality nanoscale oxides and new designer materials. In ALL-Laser MBE, separate oxide targets are used instead of one compound target in the conventional laser MBE. The targets are switched back and forth in front of a UV laser beam as they are alternately ablated. The oxide film is thus constructed one atomic layer at a time. The growth of each atomic layer is monitored and controlled by the reflection high energy electron diffraction (RHEED). The intensity of the diffraction spots increases or decreases depending on the chemistry of each atomic layer as well as the surface roughness. This allows us to determine whether the chemical ratio of the different elements in the films meets the desired value and whether each atomic layer is complete. ALL-Laser MBE is versatile: it works for non-polar film on non-polar substrate, polar film on polar substrate, and polar film on non-polar substrate. (In a polar material, each atomic layer is charged whereas in a non-polar material the atomic layers are charge neutral.) It allows one to push the thermodynamic boundary further in stabilizing new phases than reactive MBE and PLD, two of the most successful techniques for oxide thin films. For example, La 5 Ni 4 O 13 , the Ruddlesden-Popper phase with n = 4, has never been reported in the literature because it needs atomic layer-by-layer growth at high oxygen pressures, not possible with other growth techniques. ALL-Laser MBE makes it possible. We have studied the interfacial 2-dimensional electron gas in the LaAlO 3 /SrTiO 3 system, whose mechanism has been a subject of controversy. According to the most prevailing electronic reconstruction mechanism, a positive diverging electric potential is built up in the polar LaAlO 3 film when it is grown on a TiO 2 -terminated SrTiO 3 substrate, which is non-polar. This leads to the transfer of half of an electron from the LaAlO 3 film surface to SrTiO 3 when the LaAlO 3 layer is thicker than 4 unit cells, creating a 2D electron gas at the interface with a sheet carrier density of 3.3×10 14 /cm 2 for sufficiently thick LaAlO 3 . A serious inconsistency with this mechanism is that the carrier densities reported experimentally are invariably lower than the expected value. The most likely reason is that the SrTiO 3 substrate is oxygen difficient due to the low oxygen pressures (< 10 mTorr) during growth, and post-growth annealing in oxygen is often used to remove the oxygen vacancies. People cannot grow the LaAlO 3 film in higher oxygen pressures - it results in insulating samples or 3D island growth. Because we grow the LaAlO 3 film one atomic layer at a time, we were able to grow conducting LaAlO 3 /SrTiO 3 interfaces at a high oxygen pressure with ALL-Laser MBE, as high as 37 mTorr. The high oxygen pressure helps to prevent the possible oxygen reduction in SrTiO 3 , ensure that the LaAlO 3 films are sufficiently oxygenated. Measurements of x-ray linear dichroism (XLD) and x-ray magnetic circular dichroism (XMCD) both show that the spectra of our films are similar to those of well oxygenated samples. In the LaAlO 3 /SrTiO 3 interfaces grown by ALL-Laser MBE at 37 mTorr oxygen pressure, a quantitative agreement between our experimental result and the theoretical prediction was observed, which provides a strong support to the electronic reconstruction mechanism. The key differences between our result and the previous reports are the high oxygen pressure during the film growth and the high film crystallinity. The high oxygen pressure suppresses the likelihood of oxygen vacancies in SrTiO 3 . Well oxygenated samples produced during film growth can avoid possible defects when sufficient oxygen is provided only after the growth by annealing. Using ALL-Laser MBE, we also synthesized high-quality singlec-rystalline CaMnO 3 films. The systematic increase of the oxygen vacancy content in CaMnO 3 as a function of applied in-plane strain is observed and confirmed experimentally using high-resolution soft x-ray XAS and hard x-ray photoemission spectroscopy (HAXPES). The relevant defect states in the densities of states are identified and the vacancy content in the films quantified using the combination of first-principles theory and core-hole multiplet calculations with holistic fitting. The strain-induced oxygen-vacancy formation and ordering are a promising avenue for designing and controlling new functionalities in complex transition-metal oxides.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Use of aluminum oxide as a permeation barrier for producing thin films on aluminum substrates

Aluminum has desirable characteristics of good thermal properties, good electrical characteristics, good optical properties, and the characteristic of being nonmagnetic and having a low atomic weight (26.98 g atoms), but because of its low melting point (660 °C) and ability as a reactive metal to alloy with most common metals in use, it has been ignored as a substrate material for use in processing thin films. The author developed a simple solution to this problem, by putting a permeation barrier of alumina (Al{sub 2}O{sub 3}) onto the surface of pure Al substrates by using a standard chemical oxidation process of the surface (i.e., anodization), before additional film deposition of reactive metals at temperatures up to 500 °C for 1-h, without the formation of alloys or intermetallic compounds to affect the good properties of Al substrates. The chromic acid anodization process used (MIL-A-8625) produced a film barrier of ∼(500–1000) nm of alumina. The fact that refractory Al{sub 2}O{sub 3} can inhibit the reaction of metals with Al at temperatures below 500 °C suggests that Al is a satisfactory substrate if properly oxidized prior to film deposition. To prove this concept, thin film samples of Cr, Mo, Er, Sc, Ti, and Zr were prepared on anodized Al substrates and studied by x-ray diffraction, Rutherford ion back scattering, and Auger/argon sputter surface profile analysis to determine any film substrate interactions. In addition, a major purpose of our study was to determine if ErD{sub 2} thin films could be produced on Al substrates with fully hydrided Er films. Thus, a thin film of ErD{sub 2} on an anodized Al substrate was prepared and studied, with and without the alumina permeation barrier. Films for study were prepared on 1.27 cm diameter Al substrates with ∼500 nm of the metals studied after anodization. Substrates were weighed, cleaned, and vacuum fired at 500 °C prior to use. The Al substrates were deposited using standard electron beam cold crucible evaporation techniques, and after deposition the Er film was hydrided with D{sub 2} gas using a standard nonair exposure hydriding technique. All processing was conducted in an all metal ion pumped ultrahigh vacuum system. Results showed that e-beam deposition of films studied onto Al substrates could be successfully performed, if a permeation barrier of Al{sub 2}O{sub 3} from 500 to 1000 nm was made prior to thin film deposition up to temperatures of 500 °C for 1-h. Hydrides also, could be produced with full gas/metal atomic ratios of ∼2.0 as evidenced by the ErD{sub 2} films produced. Thus, the use of a simple permeation barrier of Al{sub 2}O{sub 3} on Al substrates prior to additional metal film deposition was proven to be a successful method of producing both thin metal films and hydride films of various types for many applications.

36 MATERIALS SCIENCE↗
NASA NTRS2004

ITO-MgF2 Film Development for PowerSphere Polymer Surface Protection

Multi-kilogram class microsatellites with a PowerSphere electric power system are attractive for fulfilling a variety of potential NASA missions. However, PowerSphere polymer surfaces must be coated with a film that has suitable electrical sheet resistivity for electrostatic discharge control, be resistant to atomic oxygen attack, be transparent to ultraviolet light for composite structure curing and resist ultraviolet light induced darkening for efficient photovoltaic cell operation. In addition, the film must be tolerant of polymer layer folding associated with launch stowage of PowerSphere inflatable structures. An excellent film material candidate to meet these requirements is co-sputtered, indium oxide (In2O3) - tin oxide (SnO2), known as 'ITO', and magnesium fluoride (MgF2). While basic ITO-MgF2 film properties have been the subject of research over the last decade, further research is required in the areas of film durability for space-inflatable applications and precise film property control for large scale commercial production. In this paper, the authors present film durability results for a folded polymer substrate and film resistance to vacuum UV darkening. The authors discuss methods and results in the area of film sheet resistivity measurement and active control, particularly dual-channel, plasma emission line measurement of ITO and MgF2 plasma sources. ITO-MgF2 film polymer coupon preparation is described as well as film deposition equipment, procedures and film characterization. Durability testing methods are also described. The pre- and post-test condition of the films is assessed microscopically and electrically. Results show that an approx. 500A ITO-18vol% MgF2 film is a promising candidate to protect PowerSphere polymer surfaces for Earth orbit missions. Preliminary data also indicate that in situ film measurement methods are promising for active film resistivity control in future large scale production. Future film research plans are also discussed.

Hambourger, Paul D.↗
DOE OSTI2011

Spectroscopic evidence of the formation of (V,Ti)O{sub 2} solid solution in VO{sub 2} thinner films grown on TiO{sub 2}(001) substrates

We have prepared VO{sub 2} thin films epitaxially grown on TiO{sub 2}(001) substrates with thickness systematically varied from 2.5 to 13 nm using a pulsed laser deposition method, and studied the transport property and electronic states of the films by means of resistivity and in situ synchrotron photoemission spectroscopy (SRPES). In resistivity measurements, the 13-nm-thick film exhibits a metal-insulator transition at around 290 K on cooling with change of three orders of magnitudes in resistivity. As the film thickness decreases, the metal-insulator transition broadens and the transition temperature increases. Below 4 nm, the films do not show the transition and become insulators. In situ SRPES measurements of near the Fermi level valence band find that the electronic state of the 2.5-nm-thick film is different than that of the temperature-induced insulator phase of VO{sub 2} itself although these two states are insulating. Ti 2p core-level photoemission measurements reveal that Ti ions exist near the interface between the films and TiO{sub 2} substrates, with a chemical state similar to that in (V,Ti)O{sub 2} solid solution. These results indicate that insulating (V,Ti)O{sub 2} solid solution is formed in the thinner films. We propose a simple growth model of a VO{sub 2} thin film on a TiO{sub 2}(001) substrate. Near the interface, insulating (V,Ti)O{sub 2} solid solution is formed due to the diffusion of Ti ions from the TiO{sub 2} substrate into the VO{sub 2} film. The concentration of Ti in (V,Ti)O{sub 2} is relatively high near the interface and decreases toward the surface of the film. Beyond a certain film thickness (about 7 nm in the case of the present 13-nm-thick film), the VO{sub 2} thin film without any Ti ions starts to grow. Our work suggests that developing a technique for preparing the sharp interface between the VO{sub 2} thin films and TiO{sub 2} substrates is a key issue to study the physical property of an ultrathin film of ''pure'' VO{sub 2}, especially to examine the presence of the novel electronic state called a semi-Dirac point phase predicted by calculations.

36 MATERIALS SCIENCE↗
DOE OSTI2012

An efficient protocol for radiochromic film dosimetry combining calibration and measurement in a single scan

Purpose: Radiochromic film provides dose measurement at high spatial resolution, but often is not preferred for routine evaluation of patient-specific intensity modulated radiation therapy (IMRT) plans owing to ease-of-use factors. The authors have established an efficient protocol that combines calibration and measurement in a single scan and enables measurement results to be obtained in less than 30 min. This avoids complications due to postexposure changes in radiochromic film that delay the completion of a measurement, often for up to 24 h, in commonly used methods. In addition, the protocol addresses the accuracy and integrity of the measurement by eliminating environmental and interscan variability issues. Methods: The authors collected dose-response data from six production lots of Gafchromic EBT3 film and three production lots of EBT2 film at doses up to 480 cGy. In this work, the authors used seven different scanners of two different models-Epson 10000XL and V700; postexposure times before scanning from 30 min to 9 days; ambient temperatures for scanning spanning 11 Degree-Sign C; and two film orientations. Scanning was in 48-bit RGB format at 72 dpi resolution. Dose evaluation was conducted using a triple-channel dosimetry method. To evaluate the measurement protocol, patient specific IMRT and volumetric modulated arc therapy (VMAT) plans were exposed onto EBT3 films on a Varian Trilogy Linac. Film scanning was done following the protocol under a number of different conditions and the dose maps were analyzed to demonstrate the equivalence of results. Results: The results indicated that the dose-response data could be fit by a set of related rational functions leading to the description of a generic calibration curve. A simplified dosimetry protocol was established where dose-response data for a specific film lot, scanner, and scanning conditions could be derived from two films exposed to known doses. In most cases only one calibrated exposure was required since the dose for one of the films could be zero. Using the Gamma test criterion of 2%/2 mm to evaluate the measurements, similar passing rates ranging between about 95% and 99% for the fields studied were obtained from application films digitized under a variety of conditions all of them different than the conditions under which the calibration films were scanned. Conclusions: The authors have developed a simplified and efficient protocol to measure doses delivered by an IMRT or VMAT plan using only the patient film, one calibration film, one unexposed film, and applying a single scan to acquire a digital image for calculation and analysis. The simplification and timesaving offer a potential practical solution for using radiochromic film for routine treatment plan quality assurance without sacrificing spatial resolution for convenience.

07 ISOTOPE AND RADIATION SOURCES↗
DOE OSTI2012

Room-temperature MBE deposition, thermoelectric properties, and advanced structural characterization of binary Bi[subscript 2]Te[subscript 3] and Sb[subscript 2]Te[subscript 3] thin films

Sb{sub 2}Te{sub 3} and Bi{sub 2}Te{sub 3} thin films were grown at room temperature on SiO{sub 2} and BaF{sub 2} substrates using molecular beam epitaxy. A layer-by-layer growth was achieved such that metallic layers of the elements with 0.2 nm thickness were deposited. The layer structure in the as-deposited films was confirmed by X-ray diffraction and was seen more clearly in Sb{sub 2}Te{sub 3} thin films. Subsequent annealing was done at 250 C for 2 h and produced the Sb{sub 2}Te{sub 3} and Bi{sub 2}Te{sub 3} crystal structure as confirmed by high-energy X-ray diffraction. This preparation process is referred to as nano-alloying and it was demonstrated to yield single-phase thin films of these compounds. In the thin films a significant texture could be identified with the crystal c axis being almost parallel to the growth direction for Sb{sub 2}Te{sub 3} and tilted by about 30{sup o} for Bi{sub 2}Te{sub 3} thin films. In-plane transport properties were measured for the annealed films at room temperature. Both films yielded a charge carrier density of about 2.6 x 10{sup 19} cm{sup -3}. The Sb{sub 2}Te{sub 3} films were p-type, had a thermopower of +130 {micro}V K{sup -1}, and surprisingly high mobilities of 402 cm{sup 2} V{sup -1} s{sup -1}. The Bi{sub 2}Te{sub 3} films were n-type, showed a thermopower of -153 {micro}V K{sup -1}, and yielded significantly smaller mobilities of 80 cm2 V{sup -1} s{sup -1}. The chemical composition and microstructure of the films were investigated by transmission electron microscopy (TEM) on cross sections of the thin films. The grain sizes were about 500 nm for the Sb{sub 2}Te{sub 3} and 250 nm for the Bi{sub 2}Te{sub 3} films. In the Bi{sub 2}Te{sub 3} thin film, energy-filtered TEM allowed to image a Bi-rich grain boundary phase, several nanometers thick. This secondary phase explains the poor mobilities of the Bi{sub 2}Te{sub 3} thin film. With these results the high potential of the nano-alloying deposition technique for growing films with a more complex layer architecture is demonstrated.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Influence of Fe doping on the structural, optical and acetone sensing properties of sprayed ZnO thin films

Graphical abstract: All the films are found to be polycrystalline ZnO possessing hexagonal wurtzite structure. The intensities of all the peaks are diminished strongly in the Fe-doped films, indicating their lower crystallinity as compared to the undoped ZnO film. The average crystallite size decreases from 35.21 nm (undoped sample) to 15.43 nm (1 at% Fe-doped sample). - Highlights: • Fe-doped ZnO films show smaller crystallinity with crystallite size: 15–26 nm. • Optical band gap in ZnO films decreases on Fe doping. • Fe-doped films exhibit the normal dispersion for the wavelength range 450–600 nm. • PL spectra of the Fe-doped films show quenching of the broad green-orange emission. • Acetone response of the Fe-doped films increases considerably at 300 °C. - Abstract: The ZnO thin films (undoped and Fe-doped) deposited by chemical spray pyrolysis technique have been analyzed by X-ray powder diffraction (XRD), atomic force microscopy (AFM) and scanning electron microscopy (SEM). Results show that all the films possess hexagonal wurtzite structure of zinc oxide having crystallite sizes in the range 15–36 nm. On 1 at% Fe doping, the surface roughness of the film increases which favors the adsorption of atmospheric oxygen on the film surface and thereby increase in the gas response. Optical studies reveal that the band gap decreases due to creation of some defect energy states below the conduction band edge, arising out of the lattice disorder in the doped films. The refractive index of the films decreases on Fe doping and follows the Cauchy relation of normal dispersion. Among all the films examined, the 1 at% Fe-doped film exhibits the maximum response (∼72%) at 300 °C for 100 ppm concentration of acetone in air.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Irreversible thermochromic response of RF sputtered nanocrystalline BaWO{sub 4} films for smart window applications

We report irreversible thermochromic behaviour of BaWO{sub 4} (BWO) films for the first time. BWO films have been deposited at different substrate temperatures (RT, 200, 400, 600 and 800 °C) using RF magnetron sputtering in pure argon plasma. BWO films deposited at 800 °C exhibit crystalline nature. Also, BWO films deposited in the temperature range of 400 - 600 °C exhibit WO{sub 3} as a secondary phase and its weight percentage decreases with an increase in deposition temperature, whereas the films deposited at 800 °C exhibited pure tetragonal phase. FESEM images revealed that as the average particle sizes of the films are higher as compared with the thickness of the films and is explained based on Avrami type nucleation and growth. The transmittance of the films decreases with an increase in deposition temperature up to 600 °C and increases thereafter. Films deposited at 600 °C show ≤ 20% transmittance, looking at the films deposited at room temperature and 800 °C exhibits 90 and 70%, respectively. The refractive index and extinction coefficient of the films show profound dependence on crystallinity and packing density. The optical bandgap of BWO films increases significantly with an increase in O{sub 2}% during the deposition. The optical bandgap of the BWO films deposited at different temperatures in pure argon plasma, are in the range of 3.7 to 3.94 eV whereas the films deposited at 600 °C under different O{sub 2} plasma are in the range of 3.6 - 4.5 eV. The formations of colour centres are associated with the oxygen vacancies, which are clearly seen from the optical bandgap studies. The observed irreversible thermochromic behaviour in BWO films is attributed to the presence of oxygen vacancies that arises due to the electrons trapped at oxygen vacancies causing an inter valence charge transfer of W{sup 5+} to W{sup 6+} and is confirmed through the change in the optical density (ΔOD). Further, the Raman spectra are being used to quantify the presence of oxygen vacancies and the formation of pure BWO phase. The obtained optical responses of BWO films are promising for solar cell and smart window applications.

36 MATERIALS SCIENCE↗