Search NASA⌕ Search

SEARCH · Search NASA

Results for “Microspheres”

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.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 55 records · Page 3
All sourcesNASA NTRSDOE OSTI
DOE OSTI2015

MO-A-BRD-00: Current Trends in Y90-Microsphere Therapy: Delivery and Dosimetry

Yttrium-90 (Y90) microsphere therapy, a form of radiation therapy, is an increasingly popular option for care of patients with liver metastases or unresectable hepatocellular carcinoma. The therapy directly delivers Y90 microspheres via the hepatic artery to disease sites. Following delivery, a vast majority of microspheres preferentially lodge in the capillary vessels due to their embolic size and targeted trans-arterial delivery – depositing up to 90% of its energy in the first 5 mm of tissue. There have been a number of advances in tomographic imaging within both interventional radiology and nuclear medicine that has advanced therapy planning techniques. Quantitative imaging of Y90 microsphere distribution post-therapy has also seen innovations that have led to improvements in tumor dosimetry and characterization of tumor response. A review of current trends and recent innovation in Y90 microsphere therapies will be presented. Learning Objectives: To present the imaging requirements for Y90 microsphere therapy planning To explain the standard dosimetry models used in Y90 microsphere therapy planning To report on advances in imaging for therapy planning and posttherapy assessment of tumor dosimetry and response.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2023

Synthesis and characterization of polylactic acid microspheres via emulsion-based processing

Polylactic acid (PLA) microspheres are primarily used in drug delivery applications and rarely manufactured commercially. In encapsulation, the drug encapsulation and microsphere synthesis process happen simultaneously. Simultaneous synthesis necessitates conditions that ensure the drugs to be encapsulated remain viable in the synthesis process. Here, in the present work, solid pure PLA microspheres are prepared using a repeatable centrifugal mixing method to create a single emulsion system. A planetary thinky mixer is used to achieve centrifugal mixing. PLA acts as the dispersed phase of the emulsion, whereas Polyvinyl alcohol (emulsifier) dissolved in deionized water serves as the bulk phase. The emulsions are stirred for about 4 min at 2000 rpm. Microspheres prepared by mechanical mixing are compared with microspheres prepared by centrifugal mixing. The microspheres prepared by centrifugal mixing proved to be narrower and closer to a normal distribution with a mean size (D x 50) of 30 microns. The size distribution of planetary mixed microspheres did not change from one batch to another.

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

POROUS WALL, HOLLOW GLASS MICROSPHERES

Hollow Glass Microspheres (HGM) is not a new technology. All one has to do is go to the internet and Google{trademark} HGM. Anyone can buy HGM and they have a wide variety of uses. HGM are usually between 1 to 100 microns in diameter, although their size can range from 100 nanometers to 5 millimeters in diameter. HGM are used as lightweight filler in composite materials such as syntactic foam and lightweight concrete. In 1968 a patent was issued to W. Beck of the 3M{trademark} Company for 'Glass Bubbles Prepared by Reheating Solid Glass Particles'. In 1983 P. Howell was issued a patent for 'Glass Bubbles of Increased Collapse Strength' and in 1988 H. Marshall was issued a patent for 'Glass Microbubbles'. Now Google{trademark}, Porous Wall, Hollow Glass Microspheres (PW-HGMs), the key words here are Porous Wall. Almost every article has its beginning with the research done at the Savannah River National Laboratory (SRNL). The Savannah River Site (SRS) where SRNL is located has a long and successful history of working with hydrogen and its isotopes for national security, energy, waste management and environmental remediation applications. This includes more than 30 years of experience developing, processing, and implementing special ceramics, including glasses for a variety of Department of Energy (DOE) missions. In the case of glasses, SRS and SRNL have been involved in both the science and engineering of vitreous or glass based systems. As a part of this glass experience and expertise, SRNL has developed a number of niches in the glass arena, one of which is the development of porous glass systems for a variety of applications. These porous glass systems include sol gel glasses, which include both xerogels and aerogels, as well as phase separated glass compositions, that can be subsequently treated to produce another unique type of porosity within the glass forms. The porous glasses can increase the surface area compared to 'normal glasses of a 1 to 2 order of magnitude, which can result in unique properties in areas such as hydrogen storage, gas transport, gas separations and purifications, sensors, global warming applications, new drug delivery systems and so on. One of the most interesting porous glass products that SRNL has developed and patented is Porous Wall, Hollow Glass Microspheres (PW-HGMs) that are being studied for many different applications. The European Patent Office (EPO) just recently notified SRS that the continuation-in-part patent application for the PW-HGMs has been accepted. The original patent, which was granted by the EPO on June 2, 2010, was validated in France, Germany and the United Kingdom. The microspheres produced are generally in the range of 2 to 100 microns, with a 1 to 2 micron wall. What makes the SRNL microspheres unique from all others is that the team in Figure 1 has found a way to induce and control porosity through the thin walls on a scale of 100 to 3000 {angstrom}. This is what makes the SRNL HW-HGMs one-of-a-kind, and is responsible for many of their unique properties and potential for various applications, including those in tritium storage, gas separations, H-storage for vehicles, and even a variety of new medical applications in the areas of drug delivery and MRI contrast agents. SRNL Hollow Glass Microspheres, and subsequent, Porous Wall, Hollow Glass Microspheres are fabricated using a flame former apparatus. Figure 2 is a schematic of the apparatus.

08 HYDROGEN↗
NASA NTRS2000

High-Q Microsphere Cavity for Laser Stabilization and Optoelectronic Microwave Oscillator

With submillimeter size and optical Q up to approximately 10 (exp 10), microspheres with whispering-gallery (WG) modes are attractive new component for fiber-optics/photonics applications and a potential core in ultra-compact high-spectral-purity optical and microwave oscillators. In addition to earlier demonstrated optical locking of diode laser to WG mode in a microsphere, we report on microsphere application in the microwave optoelectronic oscillator, OEO. In OEO, a steady-state microwave modulation of optical carrier is obtained in a closed loop including electro-optical modulator, fiber-optic delay, detector and microwave amplifier. OEO demonstrates exceptionally low phase noise (-140 dBc/Hz at l0kHz from approximately 10GHz carrier) with a fiber length approximately 2km. Current technology allows to put all parts of the OEO, except the fiber, on the same chip. Microspheres, with their demonstrated Q equivalent to a kilometer fiber storage, can replace fiber delays in a truly integrated device. We have obtained microwave oscillation in microsphere-based OEO at 5 to 18 GHz, with 1310nm and 1550nm optical carrier, in two configurations: 1) with external DFB pump laser, and 2) with a ring laser including microsphere and a fiber optic amplifier. Also reported is a simple and efficient fiber coupler for microspheres facilitating their integration with existing fiber optics devices.

Ilchenko, Vladimir S.↗
DOE OSTI2017

Production of cerium dioxide microspheres by an internal gelation sol–gel method

An internal gelation sol-gel technique was used to prepare cerium dioxide microspheres with uniform diameters near 100 µm. In this process, chilled aqueous solutions containing cerium, hexamethylenetetramine (HMTA), and urea are transformed into a solid gel by heat addition and are subsequently washed, dried, and sintered to produce pure cerium dioxide. Cerous nitrate and ceric ammonium nitrate solutions were compared for their usefulness in microsphere production. Gelation experiments were performed with both cerous nitrate and ceric ammonium nitrate to determine desirable concentrations of cerium, HMTA, and urea in feed solutions as well as the necessary quantity of ammonium hydroxide added to cerium solutions. Analysis of the pH before and after sample gelation was found to provide a quantitative metric for optimal parameter selection along with subjective evaluations of gel qualities. The time necessary for chilled solutions to gel upon inserting into a hot water bath was determined for samples with a variety of parameters and also used to determine desirable formulations for microsphere production. A technique for choosing the optimal mixture of ceric ammonium nitrate, HMTA, and urea was determined using gelation experiments and used to produce microspheres by dispersion of the feed solution into heated silicone oil. Gelled spheres were washed to remove excess reactants and reaction products before being dried and sintered. X-ray diffraction of air-dried microspheres, sintered microspheres, and commercial CeO 2 powders indicated that air-dried and sintered spheres were pure CeO 2 .

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2020

Impurity Levels in Cerium Oxide Microspheres Prepared by Internal Gelation Sol-Gel Methods

Impurity levels were measured in cerium oxide microspheres fabricated by modified internal gelation sol-gel methods. A combination of glow discharge mass spectrometry, electron impact mass spectrometry, combustion gas analysis and instrumental gas analysis were used to assess a wide range of potential elemental impurities. Low concentrations of carbon, nitrogen, and hydrogen impurities in microspheres showed a dependence on how microspheres were washed. Silicon impurities are believed to derive from silicone oil used during sol-gel processing. Spheres washed by the preferred approach had impurity levels below 100 ppm for all elements tested. For applications such as nuclear fuels, sol-gel methods could meet purity specifications as long as metal nitrate feed solutions of sufficient purity are used and microspheres are washed appropriately. In this study, cerium was used as a surrogate for plutonium-238, which is used in radioisotope power systems as a heat source, to determine whether carbon or other impurities were concentrated during internal gelation processing and remained after heat treatments. Analyses indicated low concentrations of impurities in cerium oxide microspheres after sintering steps that were well below documented limits for plutonium-238 oxide fuels. Modified washing methods, combined with a pressurized water treatment, resulted in sintered cerium oxide sol-gel microspheres with low impurity levels.

cerium oxide, sol-gel, internal gelation, microsph↗
DOE OSTI2012

Patient Selection and Activity Planning Guide for Selective Internal Radiotherapy With Yttrium-90 Resin Microspheres

Purpose: Selective internal radiotherapy (SIRT) with yttrium-90 ({sup 90}Y) resin microspheres can improve the clinical outcomes for selected patients with inoperable liver cancer. This technique involves intra-arterial delivery of {beta}-emitting microspheres into hepatocellular carcinomas or liver metastases while sparing uninvolved structures. Its unique mode of action, including both {sup 90}Y brachytherapy and embolization of neoplastic microvasculature, necessitates activity planning methods specific to SIRT. Methods and Materials: A panel of clinicians experienced in {sup 90}Y resin microsphere SIRT was convened to integrate clinical experience with the published data to propose an activity planning pathway for radioembolization. Results: Accurate planning is essential to minimize potentially fatal sequelae such as radiation-induced liver disease while delivering tumoricidal {sup 90}Y activity. Planning methods have included empiric dosing according to degree of tumor involvement, empiric dosing adjusted for the body surface area, and partition model calculations using Medical Internal Radiation Dose principles. It has been recommended that at least two of these methods be compared when calculating the microsphere activity for each patient. Conclusions: Many factors inform {sup 90}Y resin microsphere SIRT activity planning, including the therapeutic intent, tissue and vasculature imaging, tumor and uninvolved liver characteristics, previous therapies, and localization of the microsphere infusion. The influence of each of these factors has been discussed.

62 RADIOLOGY AND NUCLEAR MEDICINE↗
DOE OSTI2012

Controlled synthesis of three-dimensional hierarchical Bi{sub 2}WO{sub 6} microspheres with optimum photocatalytic activity

Highlights: Black-Right-Pointing-Pointer The synthesized method is very simple. It can be widely used in the production. Black-Right-Pointing-Pointer The morphology is novel and the property is fine. Black-Right-Pointing-Pointer The formation of 3D hierarchical microsphere can be induced by changing the concentration of KNO{sub 3}. -- Abstract: Three-dimensional (3D) hierarchical Bi{sub 2}WO{sub 6} microsphere and octahedral Bi{sub 2}WO{sub 6} have been synthesized by a facile hydrothermal method using KNO{sub 3} solution and distilled water as solvent, respectively. The obtained products were characterized by X-ray diffraction, scanning electron microscopy, N{sub 2} adsorption/desorption, and UV-vis diffuse reflectance spectroscopy in detail. The concentration of KNO{sub 3} played a key role in the formation of 3D hierarchical Bi{sub 2}WO{sub 6} microspheres. A possible formation mechanism of Bi{sub 2}WO{sub 6} microsphere was proposed. The photocatalytic activity of the as-synthesized products was evaluated by monitoring the degradation of MB solution under sunlight irradiation. It was found that the photocatalytic activity of the 3D hierarchical Bi{sub 2}WO{sub 6} microsphere was superior to the octahedral Bi{sub 2}WO{sub 6}, which was attributed to the larger surface area and special hierarchical structure of Bi{sub 2}WO{sub 6} microsphere.

36 MATERIALS SCIENCE↗
DOE OSTI2013

One-pot synthesis and visible light photocatalytic activity of monodispersed AgIn{sub 5}S{sub 8} microspheres

Graphical abstract: Display Omitted Highlights: ► Monodispersed AgIn{sub 5}S{sub 8} microspheres were prepared in a one-pot process. ► The process is environmental friendly. ► The AgIn{sub 5}S{sub 8} microspheres display high photocatalytic activity. -- Abstract: Monodispersed AgIn{sub 5}S{sub 8} microspheres were synthesized using a one-pot solution method and characterized with X-ray diffraction, UV–vis diffuse reflectance spectroscopy, scanning electron microscope, energy dispersive X-ray spectroscopy and N{sub 2} adsorption–desorption isotherm. The results indicated that the AgIn{sub 5}S{sub 8} microspheres were of cubic spinel structure and the mean diameter of about 0.5 μm. In addition, the visible light photocatalytic activity of AgIn{sub 5}S{sub 8} microspheres was also investigated at room temperature. The AgIn{sub 5}S{sub 8} microspheres showed very high photocatalytic activity for the degradation of methyl orange with a degradation efficiency of about 98% under visible light irradiation for 20 min.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Uniform hierarchical SnS microspheres: Solvothermal synthesis and lithium ion storage performance

Graphical abstract: - Highlights: • Uniform hierarchical SnS microspheres via solvothermal reaction. • The formation process was investigated in detail. • The obtained hierarchical SnS microspheres exhibit superior capacity (1650 mAh g{sup −1}) when used as lithium battery for the hierarchical microsphere structure. - Abstract: Hierarchical SnS microspheres have been successfully synthesized by a mild solvothermal process using poly(vinylpyrrolidone) as surfactant in this work. The morphology and composition of the microspheres were investigated by X-ray diffraction, scanning electron microscopy and transmission electron microscopy. The influence of reaction parameters, such as sulfur sources, reaction temperature and the concentration of PVP, on the final morphology of the products are investigated. On the basis of time-dependent experiments, the growth mechanism has also been proposed. The specific surface area of the 3D hierarchitectured SnS microspheres were investigated by using nitrogen adsorption and desorption isotherms. Lithium ion storage performances of the synthesized materials as anodes for Lithium-ion battery were investigated in detail and it exhibits excellent electrochemical properties.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Mo-N-co-doped mesoporous TiO{sub 2} microspheres with enhanced visible light photocatalytic activity

Highlights: • The Mo-N-co-doped mesoporous TiO{sub 2} microspheres were synthesized via a solvothermal method and further nitriding treatment. • The properties of TiO{sub 2} microspheres can be tuned by Mo-N-co-doping. • Photocatalytic rate is much higher than Pure TiO{sub 2} catalyst powder and Mo doped TiO{sub 2} microspheres. • The higher activity is attributed to the large BET surface area, narrow band gap and intense light absorbance in visible region. - Abstract: Mo-N-co-doped mesoporous TiO{sub 2} microspheres were synthesized via a solvothermal method, followed by nitriding treatment under ammonia gas flow. The efficiency of the samples was investigated by monitoring the degradation of Rhodamine-B under visible light irradiation. The experimental results revealed that Mo-N-co-doped mesoporous TiO{sub 2} microspheres showed better performances than Mo-TiO{sub 2} microspheres. It was observed that; 0.1% molar quantity of Mo doped on TiO{sub 2} at 500 °C for 2 h under nitriding conditions gave highest photocatalytic activities. The nitridation under ammonia gas of Mo-TiO{sub 2} samples created oxygen vacant sites and led to incorporation of substitutional and interstitial Nitrogen. The enhanced visible light photocatalytic activities of Mo-N-co-doped TiO{sub 2} photocatalyst was attributed to the large surface areas, narrow band gap and intense light absorbance in visible region. This study may create a promising and eco-friendly method towards synthesis of metal and non-metals co-doped on semiconductor materials to improve their photocatalytic activities and applications.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Near-field focused photoemission from polystyrene microspheres studied with photoemission electron microscopy

We use photoemission electron microscopy(PEEM) to image 3 μm diameter polystyrene spheres supported on a metalthin film illuminated by 400 nm (~3.1 eV) and 800 nm (~1.5 eV) femtosecond (fs) laser pulses. Intense photoemission is generated by microspheres even though polystyrene is an insulator and its ionization threshold is well above the photon energies employed. We observe intense photoemission from the far side (the side opposite the incident light) of the illuminated microsphere that is attributed to light focusing within the microsphere. For the case of p-polarized, 800 nm fs laser pulses, we observe photoemission exclusively from the far side of the microsphere and additionally resolve sub-50 nm hot spots in the supporting Pt/Pd thin film that are located only within the focal region of the microsphere. We compare the PEEM images with finite difference time domain(FDTD) electrodynamic simulations to model our experimental results. Finally, the FDTD simulations predict light focusing in the microsphere and subsequent interaction with the supporting metal surface that is consistent with the experimental observations.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2015

Low threshold lasing of bubble-containing glass microspheres by non-whispering gallery mode excitation over a wide wavelength range

Bubble-containing Nd{sup 3+}-doped tellurite glass microspheres were fabricated by localized laser heating technique to investigate their optical properties for use as microresonators. Fluorescence and excitation spectra measurements were performed by pumping with a tunable CW-Ti:Sapphire laser. The excitation spectra manifested several sharp peaks due to the conventional whispering gallery mode (WGM) when the pumping laser was irradiated to the edge part of the microsphere. However, when the excitation light was irradiated on the bubble position inside the microsphere, “non-WGM excitation” was induced, giving rise to numerous peaks at a broad wavelength range in the excitation spectra. Thus, efficient excitation was achieved over a wide wavelength range. Lasing threshold excited at the bubble position was much lower than that for the excitation at the edges of the microsphere. The lowest value of the laser threshold was 34 μW for a 4 μm sphere containing a 0.5 μm bubble. Efficiency of the excitation at the bubble position with broadband light was calculated to be 5 times higher than that for the edge of the microsphere. The bubble-containing microsphere enables efficient utilization of broadband light excitation from light-emitting diodes and solar light.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2012

Determining the effects of microsphere and surrounding material composition on {sup 90}Y dose kernels using egsnrc and mcnp5

Purpose: Recent advances in the imaging of {sup 90}Y using positron emission tomography (PET) and improved uncertainty in the branching ratio for the internal pair production component of {sup 90}Y decay allow for a more accurate determination of the activity distribution of {sup 90}Y microspheres within a patient. This improved activity distribution can be convolved with the dose kernel of {sup 90}Y to calculate the dose distribution within a patient. This work investigates the effects of microsphere and surrounding material composition on {sup 90}Y dose kernels using egsnrc and mcnp5 and compares the results of these two transport codes. Methods: Monte Carlo simulations were performed with egsnrc and mcnp5 to calculate the dose rate at multiple radial distances around various {sup 90}Y sources. Point source simulations were completed with mcnp5 to determine the optimal electron transport settings for this work. After determining the optimal settings, point source simulations were completed using egsnrc (user code edknrc) and mcnp5 in water and liver [as defined by the International Commission on Radiation Units and Measurements (ICRU) Report 44]. The results were compared to ICRU Report 72 reference data. Point source simulations were also completed in water with a density of 1.06 g{center_dot}cm{sup -3} to evaluate the effect of the density of the surrounding material. Glass and resin microsphere simulations were performed with average and maximum diameter and density values (based on values given in the literature) in water and in liver. The results were compared to point source simulation results using the same transport code and in the same surrounding material. All simulations had statistical uncertainties less than 1%. Results: The optimal transport settings in mcnp5 for this work included using the energy-and step-specific algorithm (DBCN 17J 2) and ESTEP set to 10. These settings were used for all subsequent simulations with mcnp5. The point source simulations in water for both egsnrc and mcnp5 were found to agree within 2% of the ICRU 72 reference data over the investigated range. Point source simulations in liver had large differences relative to ICRU 72, approaching -60% near the maximum range of {sup 90}Y. These differences are mostly attributed to the difference in density between water (1.0 g{center_dot}cm{sup -3}) and liver (1.06 g{center_dot}cm{sup -3}). Glass and resin microsphere simulations showed a slight decrease in the dose rate near the maximum range of {sup 90}Y relative to the point source simulations. The largest relative differences were approximately -4.2% and -2.8% for the glass and resin microspheres, respectively. Agreement between the egsnrc and mcnp5 simulations results was generally good. Conclusions: The presence of the microsphere material causes slight differences in the {sup 90}Y dose kernel compared to those calculated with point sources. Large differences were seen between simulations in water and those in liver. For the most accurate calculation of the dose distribution, the density of the patient's liver should be accounted for in the calculation of the dose kernel. Lastly, due to the need to determine the optimal transport settings with mcnp5, electron transport with this code should be used with caution.

61 RADIATION PROTECTION AND DOSIMETRY↗
DOE OSTI2022

Development of Gelatin-Coated Hydrogel Microspheres for Novel Bioink Design: A Crosslinker Study

The development of vascularized tissue is a substantial challenge within the field of tissue engineering and regenerative medicine. Studies have shown that positively-charged microspheres exhibit dual-functions: (1) facilitation of vascularization and (2) controlled release of bioactive compounds. In this study, gelatin-coated microspheres were produced and processed with either EDC or transglutaminase, two crosslinkers. The results indicated that the processing stages did not significantly impact the size of the microspheres. EDC and transglutaminase had different effects on surface morphology and microsphere stability in a simulated colonic environment. Incorporation of EGM and TGM into bioink did not negatively impact bioprintability (as indicated by density and kinematic viscosity), and the microspheres had a uniform distribution within the scaffold. These microspheres show great potential for tissue engineering applications.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2023

Statistical 3D morphology characterization of vaterite microspheres produced by engineered Escherichia coli

Hollow vaterite microspheres are important materials for biomedical applications such as drug delivery and regenerative medicine owing to their biocompatibility, high specific surface area, and ability to encapsulate a large number of bioactive molecules and compounds. We demonstrated that hollow vaterite microspheres are produced by an Escherichia coli strain engineered with a urease gene cluster from the ureolytic bacteria Sporosarcina pasteurii in the presence of bovine serum albumin. We characterized the 3D nanoscale morphology of five biogenic hollow vaterite microspheres using 3D high-angle annular dark field scanning transmission electron microscopy (HAADF-STEM) tomography. Using automated high-throughput HAADF-STEM imaging across several sample tilt orientations, we show that the microspheres evolved from a smaller more ellipsoidal shape to a larger more spherical shape while the internal hollow core increased in size and remained relatively spherical, indicating that the microspheres produced by this engineered strain likely do not contain the bacteria. The statistical 3D morphology information demonstrates the potential for using biogenic calcium carbonate mineralization to produce hollow vaterite microspheres with controlled morphologies.

3D morphology↗
DOE OSTI2012

Synthesis and characterization of flower-like CuIn{sub 1-x}Ga{sub x}S{sub 2} (x = 0.3) microspheres

Graphical abstract: In this paper, flower-like CuIn{sub 1-x}Ga{sub x}S{sub 2} (x = 0.3) microspheres were prepared via biomolecule-assisted solvothermal rate with CuCl{sub 2}{center_dot}2H{sub 2}O, GaCl{sub 3}, InCl{sub 3} and L-cystine as raw materials. UV-vis absorption spectrum showed that the band gap of CuIn{sub 0.7}Ga{sub 0.3}S{sub 2} microspheres was about 2.427 eV. Highlights: Black-Right-Pointing-Pointer We reported a small biomolecule-assisted route to synthesis CuIn{sub 0.3}Ga{sub 0.7}S{sub 2}. Black-Right-Pointing-Pointer The possible mechanisms of flower-like CuIn{sub 0.3}Ga{sub 0.7}S{sub 2} microspheres were proposed. Black-Right-Pointing-Pointer The as-prepared CuIn{sub 0.3}Ga{sub 0.7}S{sub 2} products were investigated by XRD, XPS, FESEM and TEM. Black-Right-Pointing-Pointer The optical properties were investigated by UV-vis spectroscopy and Raman spectrum. -- Abstract: We report the formation and characterization of the flower-like CuIn{sub 1-x}Ga{sub x}S{sub 2} (x = 0.3) microspheres using CuCl{sub 2}{center_dot}2H{sub 2}O, GaCl{sub 3}, InCl{sub 3} and L-cystine in the mixed solvent of ethylene glycol and distilled water (1:2, v/v) at 200 Degree-Sign C for 24 h. XRD results indicated that the CuIn{sub 0.7}Ga{sub 0.3}S{sub 2} nanostructures have a (1 1 2) preferred orientation. The EDS and XPS analyses of the sample revealed that Cu, In, Ga and S were present in an atomic ratio of approximately 1:0.7:0.3:2. FESEM and TEM images showed that the product was microspheres, consisting of nanoplates with the thickness of about 20 nm. The optical properties were investigated by ultraviolet-visible (UV-vis) absorption spectroscopy and Raman spectroscopy. UV-vis absorption spectrum indicated that the band gap of as-synthesized flower-like CuIn{sub 0.7}Ga{sub 0.3}S{sub 2} microspheres was about 2.427 eV. Raman spectrum of the obtained CuIn{sub 0.7}Ga{sub 0.3}S{sub 2} exhibited a high-intensity peak at 302 cm{sup -1} could be assigned as A1-mode.

36 MATERIALS SCIENCE↗
DOE OSTI2012

The simple preparation of birnessite-type manganese oxide with flower-like microsphere morphology and its remarkable capacity retention

Graphical abstract: Flower-like birnessite-type manganese oxide microspheres with large specific surface area and excellent electrochemical properties have been prepared by a facile hydrothermal method. Highlights: ► Birnessite-type manganese oxide with flower-like microsphere morphology and large specific surface area. ► A facile low-temperature hydrothermal method. ► Novel flower-like microsphere consists of the thin nano-platelets. ► Birnessite-type manganese oxide exhibits an ideal capacitive behavior and excellent cycling stability. -- Abstract: Birnessite-type manganese oxide with flower-like microsphere morphology and large specific surface area has been prepared by hydrothermal treating a mixture solution of KMnO{sub 4} and (NH{sub 4}){sub 2}SO{sub 4} at 90 °C for 24 h. The obtained material is characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and N{sub 2} adsorption–desorption. Results indicate that the birnessite-type manganese oxide shows novel flower-like microsphere morphology and a specific surface area of 280 m{sup 2} g{sup −1}, and the flower-like microsphere consists of the thin nano-platelets. Electrochemical characterization indicates that the prepared material exhibits an ideal capacitive behavior with a capacitance value of 278 F g{sup −1} in 1 mol L{sup −1} Na{sub 2}SO{sub 4} aqueous solution at a scan rate of 5 mV s{sup −1}. Moreover, the prepared manganese oxide electrode shows excellent cycle stability, and the specific capacitance can maintain 98.6% of the initial one after 5000 cycles.

36 MATERIALS SCIENCE↗