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At least 253 records · Page 14
All sourcesNASA NTRSDOE OSTI
DOE OSTI2013

Atomic layer deposition of Al-doped ZnO thin films

Atomic layer deposition has been used to fabricate thin films of aluminum-doped ZnO by depositing interspersed layers of ZnO and Al{sub 2}O{sub 3} on borosilicate glass substrates. The growth characteristics of the films have been investigated through x-ray diffraction, x-ray reflection, and x-ray fluorescence measurements, and the efficacy of the Al doping has been evaluated through optical reflectivity and Seebeck coefficient measurements. The Al doping is found to affect the carrier density of ZnO up to a nominal Al dopant content of 5 at. %. At nominal Al doping levels of 10 at. % and higher, the structure of the films is found to be strongly affected by the Al{sub 2}O{sub 3} phase and no further carrier doping of ZnO is observed.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Design, Development and Operational Experience of Demonstration Facility for Cs-137 Source Pencil Production at Trombay - 13283

Radioactive waste management is a vital aspect of any nuclear program. The commercial feasibility of the nuclear program largely depends on the efficiency of the waste management techniques. One of such techniques is the separation of high yield radio-nuclides from the waste and making it suitable for medical and industrial applications. This will give societal benefit in addition to revenue generation. Co-60, the isotope presently being used for medical applications, needs frequent replacement because of its short half life. Cs-137, the major constituent of the nuclear waste, is a suitable substitute for Co-60 as a radioactive source because of its longer half life (28 years). Indian nuclear waste management program has given special emphasis on utilization of Cs-137 for such applications. In view of this a demonstration facility has been designed for vitrification of Cs-137 in borosilicate glass, cast in stainless steel pencils, to be used as source pencils of 300 Ci strength for blood irradiation. An induction heated metallic melter of suitable capacity has been custom designed for the application and employed for the Cs-137 pencil fabrication facility. This article describes various systems, design features, experiments and resulting modifications, observations and remote handling features necessary for the actual operation of such facility. The layout of the facility has been planned in such a way that the same can be adopted in a hot cell for commercial production of source pencils. (authors)

07 ISOTOPE AND RADIATION SOURCES↗
DOE OSTI2016

Coherent interface structures and intergrain Josephson coupling in dense MgO/Mg{sub 2}Si/MgB{sub 2} nanocomposites

Many efforts are under way to control the structure of heterointerfaces in nanostructured composite materials for designing functionality and engineering application. However, the fabrication of high-quality heterointerfaces is challenging because the crystal/crystal interface is usually the most defective part of the nanocomposite materials. In this work, we show that fully dense insulator (MgO)/semiconductor(Mg{sub 2}Si)/superconductor(MgB{sub 2}) nanocomposites with atomically smooth and continuous interfaces, including epitaxial-like MgO/Mg{sub 2}Si interfaces, are obtained by solid phase reaction between metallic magnesium and a borosilicate glass. The resulting nanocomposites exhibit a semiconductor-superconducting transition at 36 K owing to the MgB{sub 2} nanograins surrounded by the MgO/Mg{sub 2}Si matrix. This transition is followed by the intergrain phase-lock transition at ∼24 K due to the construction of Josephson-coupled network, eventually leading to a near-zero resistance state at 17 K. The method not only provides a simple process to fabricate dense nanocomposites with high-quality interfaces, but also enables to investigate the electric and magnetic properties of embedded superconducting nanograins with good intergrain coupling.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2015

Electronic transport in highly conducting Si-doped ZnO thin films prepared by pulsed laser deposition

Highly conducting (ρ = 3.9 × 10{sup −4} Ωcm) and transparent (83%) polycrystalline Si-doped ZnO (SiZO) thin films have been deposited onto borosilicate glass substrates by pulsed laser deposition from (ZnO){sub 1−x}(SiO{sub 2}){sub x} (0 ≤ x ≤ 0.05) ceramic targets prepared using a sol-gel technique. Along with their structural, chemical, and optical properties, the electronic transport within these SiZO samples has been investigated as a function of silicon doping level and temperature. Measurements made between 80 and 350 K reveal an almost temperature-independent carrier concentration consistent with degenerate metallic conduction in all of these samples. The temperature-dependent Hall mobility has been modeled by considering the varying contribution of grain boundary and electron-phonon scattering in samples with different nominal silicon concentrations.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2018

Improved Miniaturized Linear Ion Trap Mass Spectrometer Using Lithographically Patterned Plates and Tapered Ejection Slit

We present a new two-plate linear ion trap mass spectrometer that overcomes both performance-based and miniaturization-related issues with prior designs. Borosilicate glass substrates are patterned with aluminum electrodes on one side and wire-bonded to printed circuit boards. Ions are trapped in the space between two such plates. Tapered ejection slits in each glass plate eliminate issues with charge build-up within the ejection slit and with blocking of ions that are ejected at off-nominal angles. The tapered slit allows miniaturization of the trap features (electrode size, slit width) needed for further reduction of trap size while allowing the use of substrates that are still thick enough to provide ruggedness during handling, assembly, and in-field applications. Plate spacing was optimized during operation using a motorized translation stage. A scan rate of 2300 Th/s with a sample mixture of toluene and deuterated toluene (D8) and xylenes (a mixture of o-, m-, p-) showed narrowest peak widths of 0.33 Th (FWHM). .

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2013

Investigation of processing advanced waste forms in Cold Crucible Induction Melter systems

The Cold Crucible Induction Melter (CCIM) technology has been identified in several independent reviews and studies as a potential alternative or supplemental vitrification technology for specific U.S. Department of Energy (DOE) high level radioactive waste (HLW) streams. These inventories have unique chemistries, such as high alumina, high iron, high chromium, etc., that are not amenable to efficient immobilization in conventional borosilicate glass (BSG) matrices. Advanced waste forms, such as iron phosphate glass (FePG), high crystalline BSG (HC-BSG), and alumino-silicate glass-ceramic (GC) have been shown to provide significantly improved immobilization matrices for these challenging waste streams, including dramatically improved waste loadings; however, they are difficult to efficiently process in the baseline joule-heated ceramic melters (JHCMs). The CCIM technology can effectively process these advanced waste forms at the desired high waste loadings. This paper describes the most recent collaborative activities between the DOE Office of Environmental Management (DOE EM) and various Russian institutions in modeling, development and testing of advanced waste forms in CCIMs, including FePG and HC-BSG formulations. Additionally, past interactions with other international partners, including France and Korea, are described. Finally, recent enhancements to CCIM processing related to modeling, draining techniques and automated control, which were collaboratively developed, will be discussed. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2013

Progress of the High Level Waste Program at the Defense Waste Processing Facility - 13178

The Defense Waste Processing Facility at the Savannah River Site treats and immobilizes High Level Waste into a durable borosilicate glass for safe, permanent storage. The High Level Waste program significantly reduces environmental risks associated with the storage of radioactive waste from legacy efforts to separate fissionable nuclear material from irradiated targets and fuels. In an effort to support the disposition of radioactive waste and accelerate tank closure at the Savannah River Site, the Defense Waste Processing Facility recently implemented facility and flowsheet modifications to improve production by 25%. These improvements, while low in cost, translated to record facility production in fiscal years 2011 and 2012. In addition, significant progress has been accomplished on longer term projects aimed at simplifying and expanding the flexibility of the existing flowsheet in order to accommodate future processing needs and goals. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2013

Reevaluation of Vitrified High-Level Waste Form Criteria for Potential Cost Savings at the Defense Waste Processing Facility - 13598

At the Savannah River Site (SRS) the Defense Waste Processing Facility (DWPF) has been immobilizing SRS's radioactive high level waste (HLW) sludge into a durable borosilicate glass since 1996. Currently the DWPF has poured over 3,500 canisters, all of which are compliant with the U. S. Department of Energy's (DOE) Waste Acceptance Product Specifications for Vitrified High-Level Waste Forms (WAPS) and therefore ready to be shipped to a federal geologic repository for permanent disposal. Due to DOE petitioning to withdraw the Yucca Mountain License Application (LA) from the Nuclear Regulatory Commission (NRC) in 2010 and thus no clear disposal path for SRS canistered waste forms, there are opportunities for cost savings with future canister production at DWPF and other DOE producer sites by reevaluating high-level waste form requirements and compliance strategies and reducing/eliminating those that will not negatively impact the quality of the canistered waste form. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2013

Hanford Low-Activity Waste Processing: Demonstration of the Off-Gas Recycle Flowsheet - 13443

Vitrification of Hanford Low-Activity Waste (LAW) is nominally the thermal conversion and incorporation of sodium salts and radionuclides into borosilicate glass. One key radionuclide present in LAW is technetium-99. Technetium-99 is a low energy, long-lived beta emitting radionuclide present in the waste feed in concentrations on the order of 1-10 ppm. The long half-life combined with a high solubility in groundwater results in technetium-99 having considerable impact on performance modeling (as potential release to the environment) of both the waste glass and associated secondary waste products. The current Hanford Tank Waste Treatment and Immobilization Plant (WTP) process flowsheet calls for the recycle of vitrification process off-gas condensates to maximize the portion of technetium ultimately immobilized in the waste glass. This is required as technetium acts as a semi-volatile specie, i.e. considerable loss of the radionuclide to the process off-gas stream can occur during the vitrification process. To test the process flowsheet assumptions, a prototypic off-gas system with recycle capability was added to a laboratory melter (on the order of 1/200 scale) and testing performed. Key test goals included determination of the process mass balance for technetium, a non-radioactive surrogate (rhenium), and other soluble species (sulfate, halides, etc.) which are concentrated by recycling off-gas condensates. The studies performed are the initial demonstrations of process recycle for this type of liquid-fed melter system. This paper describes the process recycle system, the waste feeds processed, and experimental results. Comparisons between data gathered using process recycle and previous single pass melter testing as well as mathematical modeling simulations are also provided. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2015

Plasma nitriding monitoring reactor: A model reactor for studying plasma nitriding processes using an active screen

A laboratory scale plasma nitriding monitoring reactor (PLANIMOR) has been designed to study the basics of active screen plasma nitriding (ASPN) processes. PLANIMOR consists of a tube reactor vessel, made of borosilicate glass, enabling optical emission spectroscopy (OES) and infrared absorption spectroscopy. The linear setup of the electrode system of the reactor has the advantages to apply the diagnostic approaches on each part of the plasma process, separately. Furthermore, possible changes of the electrical field and of the heat generation, as they could appear in down-scaled cylindrical ASPN reactors, are avoided. PLANIMOR has been used for the nitriding of steel samples, achieving similar results as in an industrial scale ASPN reactor. A compact spectrometer using an external cavity quantum cascade laser combined with an optical multi-pass cell has been applied for the detection of molecular reaction products. This allowed the determination of the concentrations of four stable molecular species (CH{sub 4}, C{sub 2}H{sub 2}, HCN, and NH{sub 3}). With the help of OES, the rotational temperature of the screen plasma could be determined.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2016

Obtaining a Special Administrative License Exemption to Ship the West Valley Melter Box - 16327

In order to ship the West Valley Melter Package (WVMP) package to support its disposal, the U.S. Department of Energy (DOE) requested a one-time shipment license exemption from the U.S. Nuclear Regulatory Commission (NRC). Based on content, the previously constructed WVMP, containing residual borosilicate glass and Low Density Cellular Concrete was shown to require a Type B Package. Therefore, Title 10 of the United States Code of Federal Regulations, Part 71 (10 CFR 71) required that radioactive releases under Normal Conditions of Transport (NCT) and Hypothetical Accident Conditions (HAC) would remain less than 1 E-7 A{sub 2}/hour and 1 E-1 A{sub 2}/week, respectively. Although the NRC normal method for demonstrating conformance to the 10CFR71 requirement is through performance of leak rate testing per American National Standards Institute (ANSI) standard N14.5, the WVMP does not contain a pressure vessel; therefore, performance of leak rate testing was not applicable/possible. Instead, an alternate method, adapted from DOE Handbook 3010 was used to show that the maximum allowed 10 CFR 71 radionuclide release rates for NCT and HAC would not be exceeded. Summarizing the effort, this paper provides the technical synopsis for requesting the exemption. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2020

Investigation into Reductive Separation of Tc-99 from Low Activity Waste Off-Gas Condensate by Zero Valent Iron Materials - 20311

This study is investigating the potential for reductive separation of technetium-99 (Tc) from off-gas condensate generated from vitrification of legacy tank waste at the Hanford Tank Waste Treatment and Immobilization Plant. Management of Tc is a high-priority activity for the U.S. Department of Energy (DOE) Office of Environmental Management (EM) complex, which must be addressed based on knowledge gaps and technology development needs outlined in the DOE-EM Technetium Management Program Plan [1]. Technetium is one of the main risk drivers in the permanent disposal of low activity waste (LAW) by vitrification at the Hanford Site due to its high volatility and only fractional incorporation into borosilicate glass. Volatilized Tc will be captured by an off-gas treatment system, and the current plan is to continuously recycle generated condensate back to the LAW glass melter feed. Off-gas recycling is effective at increasing Tc loading in the LAW glass, but it also disproportionately increases concentrations of sulfate, halides, and other volatile compounds impeding overall LAW processing leading to significantly greater waste glass volume requirements. Removal of Tc from secondary liquid waste offers an alternative disposal route to continuous off-gas recycling which may result in significant reduction of the volumes of LAW waste glass and substantial cost savings. The objective of this research funded by the DOE-EM Minority Serving Institutions Partnership Program (MSIPP) is to determine the suitability of zero valent iron (ZVI) as a separation technology to remove Tc from the off-gas condensate stream to minimize its recycle. While ZVI has been proposed for various remediation applications with Tc, it has not been studied for its suitability for removing Tc from the LAW off-gas condensate. The goal is to identify the optimal conditions for which Tc{sup (VII)} will be reduced to Tc{sup (IV)} species and incorporated into an iron matrix. This paper presents a programmatic overview of our evaluation of commercial ZVI materials for their efficiency towards Tc{sup (VII)} reductive removal from simplified off-gas simulant solutions under aerobic conditions. Tc concentrations in solutions were monitored for up to 30 days to determine efficiency and kinetics of reductive removal of Tc. The best performing candidate materials were selected for further experiments evaluating the effects of (1) variable ionic strength, (2) the presence of chromium and corrosive anions, and (3) ZVI aging on Tc{sup (VII)} reductive removal in batch experiments. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2015

Microstructure evolution of Al-doped zinc oxide and Sn-doped indium oxide deposited by radio-frequency magnetron sputtering: A comparison

The microstructure and morphology evolution of Al-doped zinc oxide (AZO) and Sn-doped indium oxide (ITO) thin films on borosilicate glass substrates deposited by radio-frequency magnetron sputtering at room temperature (RT) and 300 °C were investigated by X-ray diffraction and atomic force microscopy (AFM). One-dimensional power spectral density (1DPSD) functions derived from the AFM profiles, which can be used to distinguish different growth mechanisms, were used to compare the microstructure scaling behavior of the thin films. The rms roughness R{sub q} evolves with film thickness as a power law, R{sub q} ∼ d{sub f}{sup β}, and different growth exponents β were found for AZO and ITO films. For AZO films, β of 1.47 and 0.56 are obtained for RT and 300 °C depositions, respectively, which are caused by the high compressive stress in the film at RT and relaxation of the stress at 300 °C. While for ITO films, β{sub 1} = 0.14 and β{sub 2} = 0.64 for RT, and β{sub 1} = 0.89 and β{sub 2} = 0.3 for 300 °C deposition are obtained, respectively, which is related to the strong competition between the surface diffusion and shadowing effect and/or grain growth. Electrical properties of both materials as a function of film thickness were also compared. By the modified Fuchs-Sondheimer model fitting of the electrical transport in both materials, different nucleation states are pointed out for both types of films.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Modular Caustic-Side Solvent Extraction Unit (MCU) Improved Solvent Quality and Processing Results - 17496

The Modular Caustic-Side Solvent Extraction (CSSX) Unit (MCU) is a process for Cs-137 removal from legacy nuclear waste. MCU began hot operations in 2008 with an initial planned operating life of three years and a design life of five years. After eight years of operation, MCU has processed more than 23.8 million liters (6.3 million gallons) of waste. The MCU process uses a solvent developed by Oak Ridge National Laboratory (ORNL) to extract the fission product Cs-137 from liquid salt waste, or salt solution (SS), stored in the Tank Farms at Savannah River Site (SRS) after the material has been treated through the Actinide Removal Process (ARP). Batches of SS are prepared and first fed to the ARP, where it is treated to become clarified SS (CSS), then fed to MCU. Once the Cs-137 has been extracted by the solvent, the CSS becomes decontaminated SS (DSS), which is ultimately processed into a cementitious grout at the Saltstone Production Facility (SPF) and subsequently disposed of at the Saltstone Disposal Facility (SDF). The Cs-137 is then stripped from the solvent into an aqueous strip effluent (SE) stream for incorporation into borosilicate glass at the Defense Waste Processing Facility (DWPF). The solvent used in the MCU process is made of four components: the extractant (extracts Cs-137 from CSS), the modifier (increases solubility of extractant and suppressor in the diluent), the suppressor (suppresses the effects of anions and improves stripping), and the diluent (controls density and viscosity). There have been two solvents utilized during the lifetime of MCU. The first solvent was developed by ORNL and was used to design the plant based on its cesium removal capability. Due to the extended life of MCU, in order to continue to minimize the curies disposed at SDF, a new solvent capable of removing more cesium from the CSS was developed by ORNL and implemented at MCU. The second MCU solvent, Next-Generation Solvent (NGS), uses the same modifier and diluent as the original solvent, but a different extractant and suppressor. Subsequent changes to the overall MCU flowsheet were made for the use of NGS. The success of cesium removal from the CSS is often presented as the cesium decontamination factor (DF) achieved for each batch processed. The DF is the ratio of the concentration of cesium in the CSS to the cesium concentration in the DSS. The BOBCalixC6 based solvent was capable of achieving DFs between 100 and 400 for each DSS batch. The NGS solvent is capable of achieving DFs greater than 40,000 for each DSS batch. The NGS blend solvent is currently meeting the goals of the pure NGS solvent. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2016

Aging Infrastructure: Application of System Health Monitoring at the Defense Waste Processing Facility - 16069

The disposition of high level waste (HLW) into borosilicate glass canistered waste forms began at SRS in 1996. Since that time, the Defense Waste Processing Facility (DWPF) has produced nearly four thousand HLW canisters. The DWPF is now approaching 20 years of radioactive service and 25 years of operation since the commencement of nonradioactive testing in 1990. Many facility systems are challenged by equipment or component obsolescence, which places a premium on proper work planning, engineering, and maintenance resource allocation to ensure facility reliability. To this end, Savannah River Remediation (SRR) implements programs and procedures for performance monitoring of structures, systems, and components (SSCs) within all of its processing facilities. As these programs have matured, they have helped to identify vulnerabilities within facility systems and provided a framework for ranking system assets to ensure correct priority is established and maintained. This paper provides an overview of how SRR structures and implements system performance monitoring with specific focus on the recent replacement of the DWPF Safety Grade Purge Flowmeters. This case study will discuss: 1) How the performance monitoring process identified an availability risk due to the minimal vendor support for the in-use flow transmitters, 2) The design changes developed as part of the project to transition to a different measurement technology, which includes operational lessons learned from the original installation, 3) The execution of the replacement effort, which was complicated by the fact that the purge system is a Vital Safety System (VSS) and not easily taken out of service for extended maintenance, and 4) The need to consider future maintainability, particularly given that continued acceleration in technical innovation will likely increase the frequency of equipment obsolescence. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2018

Pseudo-dynamic Aspen Plus{sup R} Model of the Defense Waste Processing Facility - 18475

The Defense Waste Processing Facility (DWPF) at the Savannah River Site converts legacy high-level waste from the Cold War into borosilicate glass for permanent disposal in a geological repository. The waste sludge is chemically adjusted by the addition of acid, mixed with frit, and concentrated in the DWPF Chemical Process Cell (CPC) to ensure that the final glass has the desired properties. The resulting mixture is fed into the melter where the waste is melted and poured into stainless steel storage canisters. We present an Aspen Plus{sup R} model of the DWPF CPC, which is being developed to aid chemical processing decisions pertaining to the current flowsheet and to aid decisions regarding optimizing future processing. Given a waste feed composition with acid and frit additions, the model will predict the sludge and off-gas compositions throughout the processing, as well as the final melter feed composition. This allows different processing scenarios to be investigated easily, reducing the reliance on experimental testing, and hence saving time and money. The model has multiple potential applications, including calculating the acid and frit additions required to give acceptable glass properties, off-gas permitting, tracking mercury steam-stripped from the waste in the off-gas system, tracking flammable gases in the offgas system, investigating the effect of reducing air purges in the condensers, and general process optimization. The waste is processed in the CPC in batches, requiring dynamic simulation to track the time-dependent operations. Accurate modeling of the processing also requires calculations of phase and electrolyte chemical equilibria and parallel rate-dependent reactions. Due to existing technical limitations with dynamic simulation of the complex chemical system, we have adopted a pseudo-dynamic approach in which time intervals are treated as consecutive steady-state operations in Aspen Plus{sup R}. Thus, the model consists of ∼100 replicas of the processing vessel and its off-gas system, with the sludge output by one replica (representing one time interval) becoming the feed to the next (representing the next time interval). By examining the results from these replicas in sequence, one can see the time evolution of the model. This general approach can be used wherever simultaneous calculation of phase and electrolyte chemical equilibria in a dynamically evolving system is needed. In addition to describing the general structure and chemistry of the model, we present results from tests of the model against experimental data. These data are from laboratory-scale process simulations of the CPC with a nonradioactive waste sludge simulant. These tests include the model's predictions of the offgas composition, the sludge pH, and the final sludge composition. We will also discuss planned future developments of the model. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2014

Microstructural, chemical and textural characterization of ZnO nanorods synthesized by aerosol assisted chemical vapor deposition

ZnO nanorods were synthesized by aerosol assisted chemical vapor deposition onto TiO{sub 2} covered borosilicate glass substrates. Deposition parameters were optimized and kept constant. Solely the effect of different nozzle velocities on the growth of ZnO nanorods was evaluated in order to develop a dense and uniform structure. The crystalline structure was characterized by conventional X-ray diffraction in grazing incidence and Bragg–Brentano configurations. In addition, two-dimensional grazing incidence synchrotron radiation diffraction was employed to determine the preferred growth direction of the nanorods. Morphology and growth characteristics analyzed by electron microscopy were correlated with diffraction outcomes. Chemical composition was established by X-ray photoelectron spectroscopy. X-ray diffraction results and X-ray photoelectron spectroscopy showed the presence of wurtzite ZnO and anatase TiO{sub 2} phases. Morphological changes noticed when the deposition velocity was lowered to the minimum, indicated the formation of relatively vertically oriented nanorods evenly distributed onto the TiO{sub 2} buffer film. By coupling two-dimensional X-ray diffraction and computational modeling with ANAELU it was proved that a successful texture determination was achieved and confirmed by scanning electron microscopy analysis. Texture analysis led to the conclusion of a preferred growth direction in [001] having a distribution width Ω = 20° ± 2°. - Highlights: • Uniform and pure single-crystal ZnO nanorods were obtained by AACVD technique. • Longitudinal and transversal axis parallel to the [001] and [110] directions, respectively. • Texture was determined by 2D synchrotron diffraction and electron microscopy analysis. • Nanorods have its [001] direction distributed close to the normal of the substrate. • Angular spread about the preferred orientation is 20° ± 2°.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Single and multi-layered core-shell structures based on ZnO nanorods obtained by aerosol assisted chemical vapor deposition

Core–shell nanorod structures were prepared by a sequential synthesis using an aerosol assisted chemical vapor deposition technique. Several samples consisting of ZnO nanorods were initially grown over TiO{sub 2} film-coated borosilicate glass substrates, following the synthesis conditions reported elsewhere. Later on, a uniform layer consisting of individual Al, Ni, Ti or Fe oxides was grown onto ZnO nanorod samples forming the so-called single MO{sub x}/ZnO nanorod core–shell structures, where MO{sub x} was the metal oxide shell. Additionally, a three-layer core–shell sample was developed by growing Fe, Ti and Fe oxides alternately, onto the ZnO nanorods. The microstructure of the core–shell materials was characterized by grazing incidence X-ray diffraction, scanning and transmission electron microscopy. Energy dispersive X-ray spectroscopy was employed to corroborate the formation of different metal oxides. X-ray diffraction outcomes for single core–shell structures showed solely the presence of ZnO as wurtzite and TiO{sub 2} as anatase. For the multi-layered shell sample, the existence of Fe{sub 2}O{sub 3} as hematite was also detected. Morphological observations suggested the existence of an outer material grown onto the nanorods and further microstructural analysis by HR-STEM confirmed the development of core–shell structures in all cases. These studies also showed that the individual Al, Fe, Ni and Ti oxide layers are amorphous; an observation that matched with X-ray diffraction analysis where no apparent extra oxides were detected. For the multi-layered sample, the development of a shell consisting of three different oxide layers onto the nanorods was found. Overall results showed that no alteration in the primary ZnO core was produced during the growth of the shells, indicating that the deposition technique used herein was and it is suitable for the synthesis of homogeneous and complex nanomaterials high in quality and purity. In addition, materials absorptance determined from the total transmittance and reflectance spectra revealed a broader absorption interval including visible light, indicating potential uses of these nanostructures on solar energy appliances. - Graphical abstract: Display Omitted - Highlights: • Uniform ZnO nanorods (core)–metal oxide (shell) were obtained sequentially by AACVD. • Shells were structured of homogeneous single or multi-layered non-mixed metal oxides. • ZnO nanorod core was preserved during the shell synthesis. • Optical absorptance revealed visible interval absorption for FeO{sub x} shell samples. • Materials can be suitable for photocatalytic or photovoltaic applications.

77 NANOSCIENCE AND NANOTECHNOLOGY↗