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

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At least 307 records · Page 17
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Vacuum-assisted extrusion to reduce internal porosity in large-format additive manufacturing

Large-scale 3D printing of polymer composite structures has gained popularity and seen extensive use over the last decade. Much of the research related to improving the mechanical properties of 3D-printed parts has focused on exploring new materials and optimizing print parameters to improve geometric control and minimize voids between printed beads. However, porosity at the microstructural level (within the printed bead) has been much less studied although it is almost universally observed at levels of 4 %-10 % when using fiber reinforced materials. This study introduces a vacuum-assist approach that minimizes internal porosity by removing ambient air from the interstitial space between pellets in the hopper and acts as a negative pressure vent for gases that evolve during the initial stages of single-screw extrusion. Vacuum-assisted extrusion was able to reduce porosity below 2 % across a wide range of processing parameters, moisture content, fiber reinforcements, and printing platforms. Specifically, when printing on a large-format extruder (Strangpresse Model-30), the vacuum-assisted extrusion reduced internal porosity by 35–75 % compared to conventional non-vacuum extrusion, and only pores with length scale > 2 microns are affected. The success of this approach prompted the design of a patent-pending continuous vacuum hopper relevant for large-scale 3D printing on commercial systems.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Performance assessment of radiant cooling system integrated with desiccant assisted DOAS with solar regeneration

The Radiant cooling system integrated with Dedicated Outdoor Air System (DOAS) is a viable substitution for conventional all air system in order to reduce primary energy consumption, as it decouples the cooling and ventilation task. In DOAS major portion of energy is consumed in cooling coil where it dehumidifies the process supply air. This study describes an alternate solution for dehumidification, with the substitution of the desiccant wheel with solar regeneration in place of a chilled water coil based dehumidifier. In this paper, simulations were carried out using EnergyPlus on a reference medium office building to investigate the contribution of solar energy towards the total energy consumption of desiccant assisted DOAS with radiant cooling system. To evaluate the system performance and energy saving potential, desiccant based DOAS is compared with cooling coil assisted DOAS integrated with Radiant cooling system. Simulations were carried out for different solar collector area to evaluate primary energy savings. Results indicate that from 7.4 % to 28.6 % energy saving (according to different collector area) can be achieved due to the solar regeneration in desiccant assisted DOAS, the impact of different solar collector area on potential of energy savings is also described.

42 ENGINEERING↗
DOE OSTI2022

Effect of surfactant assisted ultrasonic pretreatment on production of volatile fatty acids from mixed food waste

In this study, the potential effect of surfactant assisted ultrasonic pretreatment on mixed food waste was investigated. Surfactants, such as Rhamnolipid, Sodium dodecyl sulfate; Glucopon and Triton X 100 were evaluated in this work. Among them, the maximum solubilization of chemical oxygen demand of 45.5 % and the highest release of soluble COD of 31 g/L were observed for ultrasonication assisted by Triton X 100 at a dose of 0.01 g/g TS in 30 min. The presence of a surfactant also reduced 27.5 % of energy demand when compared to ultrasonic pretreatment alone. Compared to the non-pretreated samples after anaerobic digestion, ultrasonication assisted by Triton X 100 led to 95 % increase of volatile fatty acid titers and 83 % increase of carbon conversion efficiency. Furthermore, sonication with the addition of Triton X 100 was proven to be highly effective toward increasing digestibility of and yield of volatile fatty acid from mixed food waste.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2025

SAXS Assistant: Automated SAXS analysis for structural discovery in biologics and polymeric nanoparticles

Small-angle x-ray scattering (SAXS) is a powerful technique for assessing macromolecular structure. High-throughput SAXS is limited by the time-consuming and, at times, subjective nature of SAXS data interpretation. Here, we present SAXS Assistant, a Python-based script that streamlines SAXS data analysis to extract features for machine learning (ML) and key structural parameters, including the Guinier radius of gyration (R g ), pair distance distribution function (PDDF)-derived R g , maximum particle dimension (D max ), and Kratky plots. The script builds upon BioXTAS RAW and validates reliability via Guinier/PDDF R g agreement, an important indicator of well-measured data sets. For assistance in D max estimation, a multilayer perceptron regressor was trained with 1940 data files from the Small Angle Scattering Biological Data Bank. The model achieved a test set performance R 2 = 0.90 and mean absolute error = 11.7 Å. Training exclusively with experimental data translates analyses from researchers, including experts in the field, to the ML model, which helps assess D max estimations from PDDF. Gaussian mixture model clustering was implemented to classify profiles into structural classes based on entries in the Small Angle Scattering Biological Data Bank. Users may therefore assess the similarity between experimental samples and known biomolecular shapes within the mapped repository entries. This probabilistic clustering aids in quantifying information from Kratky and generating shape-descriptive features. SAXS Assistant accelerates SAXS data analysis through enforced quality control, ML-ready outputs, and flags for low-confidence results. In addition to providing the ability to analyze large data sets at high throughput, this tool is versatile and may serve researchers in both biological and synthetic polymer research fields.

36 MATERIALS SCIENCE↗
DOE OSTI2022

DINGO: Digital assistant to grid operators for resilience management of power distribution system

With increasing adverse weather events and disasters, enabling resiliency of the power distribution system (PDS) is becoming increasingly important. Here in this work, resiliency is defined as the systems ability to keep supplying critical loads even with multiple contingencies. Resiliency may depend on: (a) advanced tools to assist operators in situational awareness and decision making with the increasing volume of data generated by the PDS, (b) visualization and ease of interaction with system resources and information, especially during extreme events and resulting human operator stress, and (c) flexible resources and autonomous control. Operators and support engineers need to interact with the system for key information and take action under stress, given the requirement for decisions in a short time. Integrated technological solutions are prevailing steps to support the most appropriate decision during critical times to serve essential loads. In order to meet the required goals, a Real-time Resiliency Monitoring and Operational Decision Support (RT-RMOD) tool have been developed. It supports various functionalities, including real-time monitoring, resilience assessment, and proactive decision support. However, this work makes advanced feature additions to the tool by developing data-enabled resilience management algorithms for (i) outage detection and localization, (ii) Resiliency-metric driven restoration and reconfiguration, and (iii) NLP based digital assistant for operators called DINGO (DIgital assistaNt to Grid Operators) to interact with Advanced Distribution Management System (ADMS) and RT-RMOD. The developed algorithm was validated for multiple cases of weather events using a real-world, off-grid microgrid system modeled in a real-time simulator, sensor data, and software tools.

24 POWER TRANSMISSION AND DISTRIBUTION↗
DOE OSTI2011

A practical grinding-assisted dry synthesis of nanocrystalline NiMoO{sub 4} polymorphs for oxidative dehydrogenation of propane

A practical two-stage reactive grinding-assisted pathway waste-free and cost-effective for the synthesis of NiMoO{sub 4} has been successfully developed. It was demonstrated that proper design in synthetic strategy for grinding plays a crucial role in determining the ultimate polymorph of NiMoO{sub 4}. Specifically, direct grinding (DG) of MoO{sub 3} and NiO rendered {alpha}-NiMoO{sub 4} after annealing, whereas sequential grinding (SG) of the two independently pre-ground oxides followed by annealing generated {beta}-NiMoO{sub 4} solid solution. Characterizations in terms of Raman and X-ray diffraction suggest the creation of {beta}-NiMoO{sub 4} precursor in the latter alternative is the key aspect for the formation of {beta}-NiMoO{sub 4}. The DG-derived {alpha}-NiMoO{sub 4} tested by oxidative dehydrogenation of propane exhibited superior activity in contrast to its analog synthesized via conventional coprecipitation. It is suggested that the favorable chemical composition facilely obtained via grinding in contrast to that by coprecipitation was essential for achieving a more selective production of propylene. - Graphical Abstract: Grinding-assisted synthesis of NiMoO{sub 4} offers higher and more reproducible activities in contrast to coprecipitation for oxidative dehydrogenation of propane, and both {alpha}- and {beta}-NiMoO{sub 4} can be synthesized. Highlights: Black-Right-Pointing-Pointer NiMoO{sub 4} was prepared through grinding-assisted pathway. Black-Right-Pointing-Pointer Direct/sequential grinding rendered {alpha}-, {beta}-NiMoO{sub 4}, respectively. Black-Right-Pointing-Pointer Grinding-derived {alpha}-NiMoO{sub 4} showed high and reproducible activity for oxidative dehydrogenation of propane.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2012

Microwave-assisted hydrothermally grown epitaxial ZnO films on Left-Pointing-Angle-Bracket 1 1 1 Right-Pointing-Angle-Bracket MgAl{sub 2}O{sub 4} substrate

In this report, epitaxial ZnO films were grown on Left-Pointing-Angle-Bracket 1 1 1 Right-Pointing-Angle-Bracket MgAl{sub 2}O{sub 4} single crystal substrates using Microwave Assisted Hydrothermal (MAH) method with microwave radiation heating (2.45 GHz) at 90 Degree-Sign C in a short time (within 15 min). Scanning electron microscopy confirms that these films possess smooth surface morphology with fully coalesced grains. In addition, photoluminescence (PL) measurements exhibit strong ultraviolet emission at room temperature, indicating potential applications for short-wave light-emitting photonic devices. The PL properties were improved by a thermal annealing process without generating structural defects. Hall measurements after thermal treatment show the carrier concentration to be of the order of 10{sup 19} cm{sup -3} which is comparable to those grown by conventional solution methods. The MAH method will offer a rapid route to synthesize epitaxial ZnO films with good optical and electrical properties for various applications. - Graphical abstract: FESEM images showing the morphology and cross sectional view of ZnO films grown using microwave assisted hydrothermal method at 90 Degree-Sign C for 30 min. Highlights: Black-Right-Pointing-Pointer Microwave Assisted Hydrothermal (MAH) method was introduced to synthesize epitaxial ZnO films. Black-Right-Pointing-Pointer The films possess smooth surface morphology, fully coalesced grains with high optical properties. Black-Right-Pointing-Pointer It exhibit good electrical properties (carrier concentration 10{sup 19} cm{sup -3}, mobility 19 cm{sup 2}/Vs).

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2012

Microwave-assisted hydrothermal synthesis of porous SnO{sub 2} nanotubes and their lithium ion storage properties

Porous SnO{sub 2} nanotubes have been synthesized by a rapid microwave-assisted hydrothermal process followed by annealing in air. The detailed morphological and structural studies indicate that the SnO{sub 2} tubes typically have diameters from 200 to 400 nm, lengths from 0.5 to 1.5 {mu}m and wall thicknesses from 50 to 100 nm. The SnO{sub 2} nanotubes are self-assembled by interconnected nanocrystals with sizes {approx}8 nm resulting in a specific surface area of {approx}54 m{sup 2} g{sup -1}. The pristine SnO{sub 2} nanotubes are used to fabricate lithium half cells to evaluate their lithium ion storage properties. The porous SnO{sub 2} nanotubes are characteristic with high lithium ion storage capacity, that is found to be 1258, 951, 757, 603, 458, and 288 mAh g{sup -1}, at 0.1, 0.2, 0.5, 1, 2, and 4C, respectively. The enhanced electrochemical properties of the SnO{sub 2} nanotubes can be ascribed to their unique geometry and porous structures. - Graphical abstract: Porous SnO{sub 2} nanotubes are synthesized by a fast microwave-assisted hydrothermal process and exhibit high lithium ion storage properties due to their unique geometry and porous characteristics. Highlights: Black-Right-Pointing-Pointer A microwave-assisted hydrothermal method was used to prepare porous SnO{sub 2} nanotubes. Black-Right-Pointing-Pointer The porous SnO{sub 2} nanotubes have abundant mesopores on their tube walls. Black-Right-Pointing-Pointer The porous SnO{sub 2} nanotubes possess high lithium ion storage properties. Black-Right-Pointing-Pointer Our results may promote the development of high-performance anode materials.

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

Synthesis of flower-like Boehmite (γ-AlOOH) via a one-step ionic liquid-assisted hydrothermal route

A simple and novel synthesis process, one-step ionic liquid-assisted hydrothermal synthesis route, has been developed in the work to synthesize Bohemithe (γ-AlOOH) with flower-like structure. The samples were characterized by X-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FT-IR) and Scanning Electron Microscope (SEM). Ionic liquid [Omim]{sup +}Cl{sup −}, as a template, plays an important role in the morphology and pore structure of the products due to its strong interactions with reaction particles. With the increase in the dosage of ionic liquid [Omim]{sup +}Cl{sup −}, the morphology of the γ-AlOOH was changed from initial bundles of nanosheets (without ionic liquid) into final well-developed monodispersed 3D flower-like architectures ([Omim]{sup +}Cl{sup −}=72 mmol). The pore structure was also altered gradually from initial disordered slit-like pore into final relatively ordered ink-bottle pore. Furthermore, the proposed formation mechanism and other influencing factors such as reaction temperature and urea on formation and morphology of the γ-AlOOH have also been investigated. - Graphical abstract: The flower-like γ-AlOOH architectures composed by nanosheets with narrow size distribution (1.6–2.2 μm) and uniform pore size (6.92 nm) have been synthesized via a one-step ionic liquid-assisted hydrothermal route. - Highlights: • The γ-AlOOH microflowers were synthesized via an ionic liquid-assisted hydrothermal route. • Ionic liquid plays an important role on the morphology and porous structure of the products. • Ionic liquid can be easily removed from the products and reused in recycling experiments. • A “aggregation–recrystallization–Ostwald Ripening“formation mechanism may occur.

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

Microwave assisted synthesis of sheet-like Cu/BiVO{sub 4} and its activities of various photocatalytic conditions

The Cu/BiVO{sub 4} photocatalyst with visible-light responsivity was prepared by the microwave-assisted hydrothermal method. The phase structures, chemical composition and surface physicochemical properties were well-characterized via X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), UV–vis diffuse reflectance absorption (UV–vis/DRS), scanning electron microscopy (SEM), and N{sub 2} adsorption–desorption tests. Results indicate that the crystal structure of synthetic composite materials is mainly monoclinic scheelite BiVO{sub 4}, which is not changed with the increasing doping amount of Cu. In addition, the presence of Cu not only enlarges the range of the composite materials under the visible-light response, but also increases the BET value significantly. Compared to pure BiVO{sub 4}, 1% Cu/BiVO{sub 4}-160 performs the highest photocatalytic activity to degrade methylene blue under the irradiation of ultraviolet, visible and simulated sunlight. In addition, the capture experiments prove that the main active species was superoxide radicals during photocatalytic reaction. Moreover, the 1% Cu/BiVO{sub 4}-160 composite shows good photocatalytic stability after three times of recycling. - Graphical abstract: A series of BiVO{sub 4} with different amounts of Cu doping were prepared by the microwave-assisted method, moreover, which performed the high photocatalytic activities to degrade methylene blue under multi-mode. - Highlights: • A series of Cu/BiVO{sub 4} with different amounts of Cu doping were prepared by microwave-assisted synthesis. • The morphologies of as-samples were different with the amount of Cu doping increased. • Compared with pure BiVO{sub 4}, as-Cu/BiVO{sub 4} showed stronger absorption in the visible light region obviously. • 1% Cu/BiVO{sub 4}-160 performed the high photocatalytic activities to degrade methylene blue under multi-mode. • OH{sup •} and h{sup +} both play important roles in the photocatalytic reaction.

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

Synthesis of hexagonal wurtzite Cu{sub 2}ZnSnS{sub 4} prisms by an ultrasound-assisted microwave solvothermal method

Wurtzite Cu{sub 2}ZnSnS{sub 4} (CZTS) hexagonal prisms were synthesized by a simple ultrasound-microwave solvothermal method. The product was characterized by XRD, FESEM, EDS, TEM, Raman and UV–vis spectrometer. The hexagonal prisms were 0.5–2 μm wide and 5–12 μm long. The PVP played an important role in the formation of the CZTS hexagonal prisms. In addition, the ultrasound-assisted microwave process was helpful for synthesis of wurtzite rather than kesterite phase CZTS. A nucleation–dissolution–recrystallization mechanism was also proposed to explain the growth of the CZTS hexagonal prisms. - Graphical abstract: Wurtzite Cu{sub 2}ZnSnS{sub 4} hexagonal prisms were synthesized by ultrasound-microwave solvothermal method. The ultrasound-assisted microwave process and PVP were useful to the growth of CZTS. A nucleation–dissolution–recrystallization growth mechanism was also proposed. - Highlights: • Wurtzite Cu{sub 2}ZnSnS{sub 4} was prepared by ultrasound-assisted microwave solvothermal method. • The wurtzite CZTS hexagonal prisms are demonstrated a band gap of 1.49 eV. • Synergistic effect of ultrasound and microwave is helpful to prepare Wurtzite CZTS. • PVP plays an important role in the formation of the CZTS hexagonal prisms. • Nucleation–dissolution–recrystallization growth mechanism of the CZTS was proposed.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2012

Synthesis, spectral character, electrochemical performance and in situ structure studies of Li{sub 1+x}V{sub 3}O{sub 8} cathode material prepared by tartaric acid assisted sol–gel process

Highlights: ► The adoption of tartaric acid lowers the crystallization temperature to 350 °C. ► No capacity decadence is observed in 50 cycles and a discharge capacity of 260 mAh g{sup −1} is obtained after 50 cycles. ► Two phases transition mechanism (Li{sub 4}V{sub 3}O{sub 8} and LiV{sub 3}O{sub 8}) while cycling revealed by in situ XRD. -- Abstract: Lithium-ion battery cathode material Li{sub 1+x}V{sub 3}O{sub 8} was synthesized by a tartaric acid assisted sol–gel method and thermally treated at 350 °C, 450 °C and 550 °C for 3 h for the formation of Li{sub 1+x}V{sub 3}O{sub 8} phase. The synthesized samples were fully characterized by FTIR, TG/DTA, XRD and charge–discharge tests. Li{sub 1+x}V{sub 3}O{sub 8} material synthesized by tartaric acid assisted route, followed by heat treatment at 450 °C for 3 h shows best electro-chemical performance. It shows a high initial capacity of 249 mAh g{sup −1} and still reserves a discharge capacity of 260 mAh g{sup −1} after 50 cycles. Moreover, for all tartaric assisted products, no capacity decadence is observed in 50 cycles. The in situ X-ray measurements reveal a two-phase transition mechanism in the lithium intercalation/deintercalation process. During lithium extraction, the structure of the delithiated compound changes from Li{sub 4}V{sub 3}O{sub 8} (x > 3.1) to the original LiV{sub 3}O{sub 8} phase (x < 1.4) via the coexistence state of these two phases (1.4 < x < 3.2). An obvious contraction, especially at Li(3)–Li(4) transition, along a axis and a slight expansion along b axis are also observed.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Microwave-assisted synthesis and characterization of hierarchically structured calcium fluoride

Graphical abstract: CaF{sub 2} with different morphologies and hierarchical structure such as dendrites, spherical and cube was prepared under microwave-assisted condition by a simple solvothermal synthesis route using CaCl{sub 2} and [BMIM]BF{sub 4} as initial reagents, respectively. It was found that the species of precursor was of vital importance for the formation of CaF{sub 2} crystals. That is, precursors itself also acted as structure directing agent. The outstanding features of the approach to obtain hierarchical structure CaF{sub 2} were its simplicity, effectiveness and ease of assembly. On the basis of the experimental results, a possible growth mechanism of the CaF{sub 2} crystals was proposed. Display Omitted Highlights: ► CaF{sub 2} with hierarchical structure was synthesized under microwave-assisted conditions. ► Characteristic morphologies with cube, dendrite, hierarchical sphere, etc. were observed. ► Thin cubes assembled into a spherical structure. ► Ionic liquid of [BMIM]BF{sub 4} was fluorine source. ► Possible growth mechanisms of CaF{sub 2} crystals were discussed. -- Abstract: CaF{sub 2} with different morphologies and hierarchical structures was prepared under microwave-assisted condition by a simple hydrothermal route using CaCl{sub 2} and ionic liquid [BMIM]BF{sub 4} as initial reagents, respectively. It was found that both the precursor and pH values played an important role in the formation of CaF{sub 2} crystals with different morphologies. The results suggested that the CaF{sub 2} with cube and spherical structures was obtained at different pH values (4, 8, 11), while the CaF{sub 2} with dendrite shape was formed through an oriented self-assembly growth using (NH{sub 4}){sub 2}HPO{sub 4} as a structure directing agent. Scanning electron microscope observation showed that the as-prepared CaF{sub 2} was of three-dimensional eight-horn-shaped dendritic structure. The influence of the pH values for the reaction solution and precursors has been discussed in detail. On the basis of the experimental results, possible growth mechanisms of the CaF{sub 2} microcrystals were proposed.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Preparation of silicon carbide SiC-based nanopowders by the aerosol-assisted synthesis and the DC thermal plasma synthesis methods

Highlights: • Make-up of the SiC-based nanopowders is a function of the C:Si:O ratio in precursor. • Two-stage aerosol-assisted synthesis offers conditions close to equilibrium. • DC thermal plasma synthesis yields kinetically controlled SiC products. - Abstract: Nanosized SiC-based powders were prepared from selected liquid-phase organosilicon precursors by the aerosol-assisted synthesis, the DC thermal plasma synthesis, and a combination of the two methods. The two-stage aerosol-assisted synthesis method provides at the end conditions close to thermodynamic equilibrium. The single-stage thermal plasma method is characterized by short particle residence times in the reaction zone, which can lead to kinetically controlled products. The by-products and final nanopowders were characterized by powder XRD, infrared spectroscopy FT-IR, scanning electron microscopy SEM, and {sup 29}Si MAS NMR spectroscopy. BET specific surface areas of the products were determined by standard physical adsorption of nitrogen at 77 K. The major component in all synthesis routes was found to be cubic silicon carbide β-SiC with average crystallite sizes ranging from a few to tens of nanometers. In some cases, it was accompanied by free carbon, elemental silicon or silica nanoparticles. The final mesoporous β-SiC-based nanopowders have a potential as affordable catalyst supports.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Microwave-assisted synthesis of Mn{sub 3}O{sub 4} nanoparticles@reduced graphene oxide nanocomposites for high performance supercapacitors

Highlights: • Mn{sub 3}O{sub 4}@rGO nanocomposites were prepared by one-step microwave-assisted method. • The growth of Mn{sub 3}O{sub 4} and the reduction of graphene oxide occurred simultaneously. • Specific capacitance of the nanocomposite is higher than those of rGO and Mn{sub 3}O{sub 4}. • The nanocomposites have good rate capability and cycling stability. - ABSTRACT: One-step microwave-assisted synthetic route for the fabrication of Mn{sub 3}O{sub 4} nanoparticles@reduced graphene oxide (Mn{sub 3}O{sub 4}@rGO) nanocomposites has been demonstrated. The morphological structures of the nanocomposites are characterized by Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy, X-ray diffraction (XRD), thermogravimetric analyses (TGA), and scanning electron microscopy (SEM), respectively. All of the results indicate that the microwave-assisted synthesis results in the growth of Mn{sub 3}O{sub 4} and the reduction of graphene oxide simultaneously in ethylene glycol-water system. The specific capacitance of the as-prepared Mn{sub 3}O{sub 4}@rGO nanocomposite is higher than those of rGO and pure Mn{sub 3}O{sub 4}, which indicates the synergetic interaction between rGO and Mn{sub 3}O{sub 4}. The nanocomposites also have good rate capability and cycling stability in electrochemical experiments. This facile technique may be extended to the large scale and cost effective production of other composites based on graphene and metal oxide for many applications.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2015

A study of thermal properties of sodium titanate nanotubes synthesized by microwave-assisted hydrothermal method

Highlights: • The microwave-assisted hydrothermal route was used for titanate nanotubes synthesis. • Conversion to single-phase nanotube morphology completes after 8 h reaction time. • The nanotube morphology is stable up to 600 °C, as determined by in-situ XRD and SEM. • Sodium ions migrate to the surface due to thermal motion and structure condensation. - Abstract: Sodium titanate nanotubes (NaTiNTs) were synthesized by microwave-assisted hydrothermal treatment of commercial TiO{sub 2}, at constant temperature (135 °C) and different irradiation times (15 min, 1, 4, 8 and 16 h). The products were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, differential scanning calorimetry and specific surface area measurements. The irradiation time turned out to be the key parameter for morphological control of the material. Nanotubes were observed already after 15 min of microwave irradiation. The analyses of the products irradiated for 8 and 16 h confirm the complete transformation of the starting TiO{sub 2} powder to NaTiNTs. The nanotubes are open ended with multi-wall structures, with the average outer diameter of 8 nm and specific surface area up to 210 m{sup 2}/g. The morphology, surface area and crystal structure of the sodium titanate nanotubes synthesized by microwave-assisted hydrothermal method were similar to those obtained by conventional hydrothermal method.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2017

Effect of Ar ion-beam-assistance and substrate temperature on physical properties of Al-doped ZnO thin films deposited by RF magnetron sputtering

Highlights: • AZO and IAZO (303–473 K) films were grown by RF magnetron sputtering technique. • Ar ion-beam converts its kinetic energy as diffusion energy to the deposited atoms. • Structural evolution relies on diffusion energy imparted to the deposited atoms. • Surface texture densify under the aid of ion-beam and substrate temperature. - Abstract: In this study, pronounced effects of ion-beam-assistance and substrate temperature were revealed by exploring the physical properties of Al-doped ZnO thin films deposited by the RF magnetron sputtering technique. Herein, two measurable parameters, ion-beam discharge current (0.1 A) and substrate temperature (303–473 K) were adopted to regulate the structural changes in Al-doped ZnO films. Specifically, progressive structural changes were achieved based on the addition of Ar ion-beam during the film growth. From XRD analysis, we observed significant structural changes that provided an improvement in the film growth towards c-axis (002) plane. In addition, FESEM and AFM analyses demonstrated excellent surface features with the assisted Ar ion-beam. As a result of this process, we effectively modulated the binding energy of Zn 2p level. Finally, the structural investigation accurately demonstrated that the dependence of assisted ion-beam and substrate temperature linearly related to the superior visible transmittance and reduced band gap.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Microwave-assistant hydrothermal synthesis of SnO2@ZnO hierarchical nanostructures enhanced photocatalytic performance under visible light irradiation

Highlights: • A photocatalyst of SnO{sub 2}@ZnO HNSs is prepared via a microwave-assistant hydrothermal method. • Enhanced photodegradation of methylene blue under the visible light irradiation has been observed. • The defect in photocatalyst is the main photocatalytic mechanism under the visible light irradiation. • The superoxide radical is the main photoactive species. - Abstract: In this paper, for the first time, SnO{sub 2}@ZnO hierarchical nanostructures (HNSs) were synthesized by a simple two-step microwave-assistant hydrothermal method. Systematical characterization of the SnO{sub 2}@ZnO HNSs revealed that the rutile SnO{sub 2} nanowires (NWs) were uniformly and tightly grown on the entire surface of each ZnO nanoflowers (NFs). The photocatalytic performance of the SnO{sub 2}@ZnO HNSs showed a remarkably enhanced photocatalytic performance under visible light irradiation (400 nm≤λ ≤ 800 nm). The photoluminescence (PL) spectrum results indicated that the defect related energy level is the main mechanism of the photocatalytic performance under the visible light irradiation. The unique morphology and heterojunction structures in SnO{sub 2}@ZnO HNSs were the core enhanced mechanism in photodegradation process. The advantage endowed with the microwave-assistant hydrothermal method can result in the efficient spatial charge separation between ZnO nanorods (NRs) and SnO{sub 2} NWs and reduce the charge recombination along the heterojunction, which makes SnO{sub 2}@ZnO HNSs a highly promising for photocatalytic applications.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗