Carbon Coated α-Fe2O3 Photoanode Synthesized by a Facile Anodic Electrodeposition for Highly Efficient Water Oxidation

NASA Astrophysics Data System (ADS)

Zhang, Honglei; Li, Longzhu; Liu, Changhai; Wang, Wenchang; Liang, Penghua; Mitsuzak, Naotoshi; Chen, Zhidong

2018-05-01

This work provides a facile anodic electrodeposition method for synthesizing carbon coated α-Fe2O3 photoanode followed by annealing treatment with argon atmosphere. Compared with bare hematite photoanode, the carbon coated α-Fe2O3 photoanodes annealed at lower temperature (Fe2O3/C-L) and higher temperature (Fe2O3/C-H) have higher photocurrent density as 0.3 and 0.5 mA cm-2 (at 1.23 V vs. RHE), respectively. The excellent PEC performance is attributed to the synergistic reaction of carbon and vacancy oxygen. The morphology and properties of the sample were characterized with scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy, UV-Vis spectra, X-ray diffractometry, X-ray photoelectron spectra, and photoelectrical measurements.

Enhancing the bioavailability of magnolol in rabbits using melting solid dispersion with polyvinylpyrrolidone.

PubMed

Lin, Shiuan-Pey; Hou, Yu-Chi; Liao, Tzu-Yun; Tsai, Shang-Yuan

2014-03-01

Preparation of magnolol-loaded amorphous solid dispersion was investigated for improving the bioavailability. A solid dispersion of magnolol was prepared with polyvinylpyrrolidone K-30 (PVP) by melting method, and the physical properties were characterized by using differential scanning calorimetry, powder X-ray diffractometry, Fourier transformation-infrared spectroscopy and scanning electron microscope. In addition, dissolution test was also performed. Subsequently, the bioavailability of magnolol pure compound, its physical mixture and solid dispersion were compared in rabbits. The blood samples withdrawn via marginal ear vein at specific time points were assayed by HPLC method. Oral administration of the solid dispersion of magnolol with PVP significantly increased the systemic exposures of magnolol and magnolol sulfates/glucuronides by 80.1% and 142.8%, respectively, compared to those given with magnolol pure compound. Magnolol-loaded amorphous solid dispersion with PVP has demonstrated enhanced bioavailability of magnolol in rabbits.

Different preparation methods and characterization of magnetic maghemite coated with chitosan

NASA Astrophysics Data System (ADS)

Hojnik Podrepšek, Gordana; Knez, Željko; Leitgeb, Maja

2013-06-01

The preparation of maghemite (γ-Fe2O3) micro- and nanoparticles coated with chitosan, used as carriers for immobilized enzymes, was investigated. γ-Fe2O3 nanoparticles were synthesized by coprecipitation of Fe2+ and Fe3+ ions in the presence of ammonium. They were coated with chitosan by the microemulsion process, suspension cross-linking technique, and covalent binding of chitosan on the γ-Fe2O3 surface. The methods distinguished the concentration of chitosan, concentration of acetic acid solution, concentration of a cross-linking agent, temperature of synthesis, pH of the medium, and time of synthesis. γ-Fe2O3 micro- and nanoparticles coated with chitosan prepared after three preparation methods were evaluated by scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy analysis, energy dispersive spectrometry, thermogravimetric analysis, differential scanning calorimetry analysis, vibrating sample magnetometry, dynamic light scattering, laser diffraction granulometry, and X-ray diffractometry. These positive attributes demonstrated that these magnetic micro- and nanoparticles coated with chitosan may be used as a promising carrier for further diverse biomedical applications.

Modified extrusion-spheronization as a technique of microencapsulation for stabilization of choline bitartrate using hydrogenated soya bean oil

PubMed Central

Gangurde, Avinash Bhaskar; Sav, Ajay Kumar; Javeer, Sharadchandra Dagadu; Moravkar, Kailas K; Pawar, Jaywant N; Amin, Purnima D

2015-01-01

Introduction: Choline bitartrate (CBT) is a vital nutrient for fetal brain development and memory function. It is hygroscopic in nature which is associated with stability related problem during storage such as development of fishy odor and discoloration. Aim: Microencapsulation method was adopted to resolve the stability problem and for this hydrogenated soya bean oil (HSO) was used as encapsulating agent. Materials and Methods: Industrially feasible modified extrusion-spheronization technique was selected for microencapsulation. HSO was used as encapsulating agent, hydroxypropyl methyl cellulose E5/E15 as binder and microcrystalline cellulose as spheronization aid. Formulated pellets were evaluated for parameters such as flow property, morphological characteristics, hardness-friability index (HFI), drug content, encapsulation efficiency, and in vitro drug release. The optimized formulations were also characterized for particle size (by laser diffractometry), differential scanning calorimetry, powder X-ray diffractometry (PXRD), Fourier transform infrared spectroscopy, and scanning electron microscopy. Results and Discussions: The results from the study showed that coating of 90% and 60% CBT was successful with respect to all desired evaluation parameters. Optimized formulation was kept for 6 months stability study as per ICH guidelines, and there was no change in color, moisture content, drug content, and no fishy odor was observed. Conclusion: Microencapsulated pellets of CBT using HSO as encapsulating agent were developed using modified extrusion spheronization technique. Optimized formulations, CBT 90% (F5), and CBT 60% (F10), were found to be stable for 4M and 6M, respectively, at accelerated conditions. PMID:26682198

Low Temperature Synthesis of Cobalt-Chromium Carbide Nanoparticles-Doped Carbon Nanofibers.

PubMed

Yousef, Ayman; Brooks, Robert M; Abutaleb, Ahmed; Al-Deyab, Salem S; El-Newehy, Mohamed H

2018-04-01

Electrospinning has been used to synthesize cobalt-chromium carbide nanoparticles (NPs)-doped carbon nanofibers (CNFs) (Composite). Electrospun mat comprising of cobalt acetate, chromium acetate and poly(vinyl alcohol) (PVA) has been carbonized at low temperature (850 °C) for 3 h under argon atmosphere to produce the introduced composite. The process was achieved at low temperature due to the presence of cobalt as an activator. Field emission scanning electron microscope (FE-SEM), X-ray diffractometry (XRD), and transmission electron microscopy (TEM) equipped with EDX techniques were used to determine the products characteristics. The results indicated the formation of pure cobalt (Co), Cr7C3 NPs and crystalline CNFs. The Co and Cr7C3 NPs were covered with CNFs. Overall, the proposed NFs open new avenue to prepare different metals-metal carbides-carbon NFs at low temperature and short reaction time.

Self-assembled biomimetic superhydrophobic CaCO3 coating inspired from fouling mineralization in geothermal water.

PubMed

Wang, Gong G; Zhu, Li Q; Liu, Hui C; Li, Wei P

2011-10-18

Inspired from fouling self-mineralization in geothermal water, a novel biomimetic cactuslike CaCO(3) coating with superhydrophobic features is reported in this letter. The structure, morphologies, and phases of the CaCO(3) coating were characterized by X-ray diffractometry, scanning electron microscopy, transmission electron microscopy, and infrared spectrophotometry. After prenucleation treatment, a continuous cactuslike CaCO(3) coating with hierarchical nano- and microstructures was self-assembled on stainless steel surfaces after immersion in simulated geothermal water at 50 °C for 48 h. After being modified with a low-surface-energy monolayer of sodium stearate, the as-prepared coating exhibited superhydrophobic properties with a water contact angle of 158.9° and a sliding angle of 2°. Therefore, this work might open up a new application field of geothermal resources and provide insight into designing multidimensional structures with functional applications, including superhydrophobic surfaces. © 2011 American Chemical Society

Manganese porphyrin immobilized on magnetic MCM-41 nanoparticles as an efficient and reusable catalyst for alkene oxidations with sodium periodate

NASA Astrophysics Data System (ADS)

Hajian, Robabeh; Ehsanikhah, Amin

2018-01-01

This study describes the immobilization of tetraphenylporphyrinatomanganese(III) chloride, (MnPor), onto imidazole functionalized MCM-41 with magnetite nanoparticle core (Fe3O4@MCM-41-Im). The resultant material (Fe3O4@MCM-41-Im@MnPor) was characterized by X-ray diffractometry (XRD), Fourier transform infra-red (FT-IR), diffuse reflectance UV-Vis spectrophotometry (DR UV-Vis), field emission scanning electron microscopy (FESEM), Inductively coupled plasma (ICP), analyzer transmission electron microscopy (TEM) and Brunauer-Emmett-Teller (BET) surface area. This new heterogenized catalyst was applied as an efficient catalyst for the epoxidation of a variety of cyclic and linear olefins with NaIO4 under mild conditions. The prepared catalyst can be easily recovered through the application of an external magnet, and reused several times without any significant decrease in activity and magnetic properties.

Hydrothermal epitaxy and resultant properties of EuTiO3 films on SrTiO3(001) substrate

PubMed Central

2014-01-01

We report a novel epitaxial growth of EuTiO3 films on SrTiO3(001) substrate by hydrothermal method. The morphological, structural, chemical, and magnetic properties of these epitaxial EuTiO3 films were examined by scanning electron microscopy, transmission electron microscopy, high-resolution X-ray diffractometry, X-ray photoelectron spectroscopy, and superconducting quantum interference device magnetometry, respectively. As-grown EuTiO3 films with a perovskite structure were found to show an out-of-plane lattice shrinkage and room-temperature ferromagnetism, possibly resulting from an existence of Eu3+. Postannealing at 1,000°C could reduce the amount of Eu3+, relax the out-of-plane lattice shrinkage, and impact the magnetic properties of the films. PACS 81.10.Aj; 81.15.-z; 61.05.-a PMID:24948889

Silica nanoparticles produced by DC arc plasma from a solid raw materials

NASA Astrophysics Data System (ADS)

Kosmachev, P. V.; Vlasov, V. A.; Skripnikova, N. K.

2017-05-01

Plasma synthesis of SiO2 nanoparticles in experimental atmospheric pressure plasma reactor on the basis of DC arc plasma generator was presented in this paper. Solid high-silica raw materials such as diatomite from Kamyshlovskoye deposit in Russia, quartzite from Chupinskoye deposit in Russia and milled window glass were used. The obtained nanoparticles were characterized based on their morphology, chemical composition and size distribution. Scanning electron microscopy, laser diffractometry, nitrogen absorption (Brunauer-Emmett-Teller method), X-ray photoelectron spectroscopy and energy-dispersive X-ray spectroscopy were used to characterize the synthesized products. The obtained silica nanoparticles are agglomerated, have spherical shape and primary diameters between 10-300 nm. All samples of synthesized nanopowders were compared with commercial nanopowders.

Selective laser sintering of single-phase powder Cr-V tool steel

NASA Astrophysics Data System (ADS)

Kovalev, A. I.; Mishina, V. P.; Wainstein, D. L.; Titov, V. I.; Moiseev, V. F.; Tolochko, N. K.

2002-10-01

Presented is positive experience from selective laser sintering (SLS) of cylindrical steel specimens (3.0% C, 3.0% Cr, 1.0% Si, 12.0% V, Fe balance) 30 mm long and 5 mm in diameter by rapid prototyping. It was demonstrated that monolithic steel material could be successfully fabricated by this technology. Differential thermal analysis (DTA), scanning electron microscopy (SEM), and x-ray diffractometry (XRD) were used to study the microstructure, phase, and chemical composition of the source material and obtained specimens. Low-melting cementite-based eutectic was found to provide the liquid phase sintering of powder tool steel. The porosity of the green sintered specimens did not exceed 5%. The mean hardness value of sintered specimens was 825 HV.

Clay-mineraloid weathering products in Antarctic meteorites

NASA Technical Reports Server (NTRS)

Gooding, James L.

1986-01-01

The production of clay mineraloids (CMs) in the weathering of stony meteorites recovered in the Allan Hills and Elephant Moraine areas of Antarctica is investigated, applying electron microbeam analysis, pyrolysis/mass spectroscopy, X-ray diffractometry, and differential scanning calorimetry to whole-rock chips from two eucrites, two diogenites, and an H5 chondrite. The data are presented in tables, graphs, and photomicrographs and characterized in detail. Massive to incipient-vermicular CM formations with smectitelike or micalike compositions and indications of poor crystallization are observed and attributed to hydrocryogenic diagenesis (with little or no liquid water) on time scales of 10-1000 kyr. The need to take the compositional effects of weathering into account before attempting to reconstruct the preterrestrial histories of meteorites is stressed.

Chitosan microparticles: influence of the gelation process on the release profile and oral bioavailability of albendazole, a class II compound.

PubMed

Piccirilli, Gisela N; García, Agustina; Leonardi, Darío; Mamprin, María E; Bolmaro, Raúl E; Salomón, Claudio J; Lamas, María C

2014-11-01

Encapsulation of albendazole, a class II compound, into polymeric microparticles based on chitosan-sodium lauryl sulfate was investigated as a strategy to improve drug dissolution and oral bioavailability. The microparticles were prepared by spray drying technique and further characterized by means of X-ray powder diffractometry, infrared spectroscopy and scanning electron microscopy. The formation of a novel polymeric structure between chitosan and sodium lauryl sulfate, after the internal or external gelation process, was observed by infrared spectroscopy. The efficiency of encapsulation was found to be between 60 and 85% depending on the internal or external gelation process. Almost spherically spray dried microparticles were observed using scanning electron microscopy. In vitro dissolution results indicated that the microparticles prepared by internal gelation released 8% of the drug within 30 min, while the microparticles prepared by external gelation released 67% within 30 min. It was observed that the AUC and Cmax values of ABZ from microparticles were greatly improved, in comparison with the non-encapsulated drug. In conclusion, the release properties and oral bioavailability of albendazole were greatly improved by using spraydried chitosan-sodium lauryl sulphate microparticles.

Effect of Laser Powder Bed Fusion Parameters on the Microstructure and Texture Development in Superelastic Ti-18Zr-14Nb Alloy

NASA Astrophysics Data System (ADS)

Kreitcberg, A.; Brailovski, V.; Sheremetyev, V.; Prokoshkin, S.

2017-12-01

The effect of different laser powder bed fusion (L-PBF) parameters on the phase composition, microstructure, and crystallographic texture of Ti-18Zr-14Nb alloy was studied. Two levels of laser power, scanning speed, and hatching space were used, while the layer thickness was kept constant. The resulting volume energy density was ranged from 20 to 60 J/mm3, and the build rate, from 12 to 36 cm3/h. The manufactured coupons were analyzed by X-ray diffractometry, transmission, and scanning electron microscopy. It was found that the greater influence observed on the microstructure and texture development was caused by the value of laser power, while the lowest, by that of hatching space. Based on the results obtained, the processing optimization strategy aimed at improving the density, superelastic, and fatigue properties of the L-PBF manufactured Ti-18Zr-14Nb alloy was proposed.

Preparation of CMC-modified melamine resin spherical nano-phase change energy storage materials.

PubMed

Hu, Xiaofeng; Huang, Zhanhua; Zhang, Yanhua

2014-01-30

A novel carboxymethyl cellulose (CMC)-modified melamine-formaldehyde (MF) phase change capsule with excellent encapsulation was prepared by in situ polymerization. Effects of CMC on the properties of the capsules were studied by Fourier transformation infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), scanning electronic microscopy (SEM), X-ray diffractometry (XRD), and thermogravimetric analysis (TGA). The results showed that the CMC-modified capsules had an average diameter of about 50nm and good uniformity. The phase change enthalpy of the capsules was increased and the cracking ratio decreased by incorporating a suitable amount of CMC. The optimum phase change enthalpy of the nanocapsules was 83.46J/g, and their paraffin content was 63.1%. The heat resistance of the capsule shells decreased after CMC modification. In addition, the nanocapsule cracking ratio of the nanocapsules was 11.0%, which is highly attractive for their application as nano phase change materials. Copyright © 2013 Elsevier Ltd. All rights reserved.

Marble protection: An inorganic electrokinetic approach

NASA Astrophysics Data System (ADS)

Meloni, Paola; Manca, Francesco; Carcangiu, Gianfranco

2013-05-01

The influence of an electric potential difference in an aqueous solution was studied as a method for depositing a calcium oxalate coating over a weathered carbonatic stone. Samples of weathered Carrara white marble were treated at 15 and 50 °C for 5 h in an electrokinetic cell, specifically conceived for this study, containing a solution of ammonium oxalate (4% by weight), and were subsequently characterised by scanning electron microscopy, X-ray diffractometry, thermogravimetric analysis and mercury intrusion porosimetry. The electrokinetic treatment proved to be a cost effective and time saving process, able to produce a thick and homogeneous calcium oxalate coating over the stone surface that improves its chemical and physical resistance in low pH environments, and is able to protect the stone from the by-products of urban pollution.

A facile and efficient strategy for the fabrication of porous linseed gum/cellulose superabsorbent hydrogels for water conservation.

PubMed

Zhang, Hao; Luan, Qian; Huang, Qingde; Tang, Hu; Huang, Fenghong; Li, Wenlin; Wan, Chuyun; Liu, Changsheng; Xu, Jiqu; Guo, Pingmei; Zhou, Qi

2017-02-10

The linseed gum/cellulose composite hydrogels were successfully fabricated by mixing cellulose and linseed gum solutions dissolved in the NaOH/urea aqueous system and cross-linked with epichlorohydrin. The morphology and structure of the composite hydrogels were investigated by scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy, X-ray diffractometry (XRD) and thermogravimetric analysis (TGA). The swelling ratio and water retention properties were investigated. The results revealed that linseed gum mainly contributed to water adsorption, whereas the cellulose acted as a backbone to strengthen the porous structure. This work provided a simple way to prepare cellulose-based superabsorbent hydrogels, which could be potentially applied as an effective water conservation material in agriculture. Copyright © 2016 Elsevier Ltd. All rights reserved.

Characterization of calcium phosphate coatings deposited by Nd:YAG laser ablation at 355 nm: influence of thickness.

PubMed

Fernández-Pradas, J M; Clèries, L; Sardin, G; Morenza, J L

2002-05-01

Calcium phosphate coatings were deposited by pulsed laser ablation with a radiation of 355 nm from a Nd:YAG laser. All the coatings were obtained at the same conditions, but deposition was stopped after different number of pulses to get coatings with different thickness. The influence of thickness in the structural and mechanical properties of the coatings was investigated. Coatings structure was characterised by scanning electron microscopy, grazing incidence X-ray diffractometry and Raman spectroscopy. The mechanical properties were evaluated by scratch test. The morphology of the coatings is dominated by the presence of droplets. The coatings are composed mainly of hydroxyapatite, alpha tricalcium phosphate and amorphous calcium phosphate. Thinner coatings withstand higher loads of failure in the scratch test.

Ultrastructure of selected struvite-containing urinary calculi from dogs.

PubMed

Domingo-Neumann, R A; Ruby, A L; Ling, G V; Schiffman, P S; Johnson, D L

1996-09-01

To elucidate the ultrastructural details of struvite-containing urinary calculi from dogs. 38 specimens were selected from a collection of approximately 13,000 canine urinary calculi: 18 of these were composed entirely of struvite, and 20 consisted of struvite and calcium phosphate (apatite). Qualitative and quantitative analyses of specimens included use of plain and polarized light microscopy, x-ray diffractometry, scanning electron microscopy with backscattered electron imagery, x-ray fluorescence scans, and electron microprobe analysis. 4 textural types were recognized among struvite calculi, and 4 textural types of struvite-apatite calculi were described. Evidences of calculus dissolution were described from 4 calculi studied. The presence of small, well interconnected primary pores in struvite-containing urinary calculi from dogs appears to be a significant factor in determining the possible interaction of calculi with changes in the urine composition. The progress of dissolution from the calculus surface to the calculus interior appears to be largely affected by the primary porosity originally present between crystals forming the calculus framework. Apatite was observed to be more resistant to dissolution than struvite. The prevalence of fine concentric laminations having low porosity, and the common occurrence of apatite among struvite-containing urinary calculi from dogs may be 2 reasons why the efficacy of dietary and medicinal manipulations in dissolving urinary calculi is greater among cats than it is among dogs.

Heteroepitaxial growth of Ge films on (100) GaAs by pyrolysis of digermane

NASA Astrophysics Data System (ADS)

Eres, Djula; Lowndes, Douglas H.; Tischler, J. Z.; Sharp, J. W.; Geohegan, D. B.; Pennycook, S. J.

1989-08-01

Pyrolysis of high-purity digermane (Ge2 H6 ) has been used to grow epitaxial Ge films of high crystalline quality on (100) GaAs substrates in a low-pressure environment. X-ray double-crystal diffractometry shows that fully commensurate, coherently strained epitaxial Ge films can be grown on (100) GaAs at digermane partial pressures of 0.05-40 mTorr for substrate temperatures of 380-600 °C. Amorphous films also were deposited. Information about the crystalline films surface morphology, growth mode, and microstructure was obtained from scanning electron microscopy, cross-section transmission electron microscopy, and in situ reflectivity measurements. The amorphous-to-crystalline transition temperature and the morphology of the crystalline films were both found to depend on deposition conditions (primarily the incidence rate of Ge-bearing species and the substrate temperature). Epitaxial growth rates using digermane were found to be about two orders of magnitude higher than rates using germane (GeH4 ) under similar experimental conditions.

Fine Structure Study of the Plasma Coatings B4C-Ni-P

NASA Astrophysics Data System (ADS)

Kornienko, E. E.; Bezrukova, V. A.; Kuz'min, V. I.; Lozhkin, V. S.; Tutunkova, M. K.

2017-12-01

The article considers structure of coatings formed of the B4C-Ni-P powder. The coatings were deposited using air-plasma spraying with the unit for annular injection of powder. The pipes from steel 20 (0.2 % C) were used as a substrate. The structure and phase composition of the coatings were studied by optical microscopy, scanning electron microscopy, transmission electron microscopy and X-ray diffractometry. It is shown that high-density composite coatings consisting of boron carbide particles distributed in the nickel boride metal matrix are formed using air-plasma spraying. The areas with round inclusions characterized by the increased amount of nickel, phosphorus and boron are located around the boron carbide particles. Boron oxides and nickel oxides are also present in the coatings. Thin interlayers with amorphous-crystalline structure are formed around the boron carbide particles. The thickness of these interlayers does not exceed 1 μm. The metal matrix material represents areas with nanocrystalline structure and columnar crystals.

Purification Procedures for Single-Wall Carbon Nanotubes

NASA Technical Reports Server (NTRS)

Gorelik, Olga P.; Nikolaev, Pavel; Arepalli, Sivaram

2001-01-01

This report summarizes the comparison of a variety of procedures used to purify carbon nanotubes. Carbon nanotube material is produced by the arc process and laser oven process. Most of the procedures are tested using laser-grown, single-wall nanotube (SWNT) material. The material is characterized at each step of the purification procedures by using different techniques including scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM), Raman, X-ray diffractometry (XRD), thermogravimetric analysis (TGA), nuclear magnetic resonance (NMR), and high-performance liquid chromatography (HPLC). The identified impurities are amorphous and graphitic carbon, catalyst particle aggregates, fullerenes, and hydrocarbons. Solvent extraction and low-temperature annealing are used to reduce the amount of volatile hydrocarbons and dissolve fullerenes. Metal catalysts and amorphous as well as graphitic carbon are oxidized by reflux in acids including HCl, HNO3 and HF and other oxidizers such as H2O2. High-temperature annealing in vacuum and in inert atmosphere helps to improve the quality of SWNTs by increasing crystallinity and reducing intercalation.

RF sputtered silicon and hafnium nitrides as applied to 440C steel

NASA Technical Reports Server (NTRS)

Grill, A.; Aron, P. R.

1984-01-01

Silicon nitride and hafnium nitride coatings were deposited on oxidized and unoxidized 440C stainless steel substrates. Sputtering was done in mixtures of argon and nitrogen gases from pressed powder silicon nitride and from hafnium metal targets. The coatings and the interface between the coating and substrate were investigated by X-ray diffractometry, scanning electron microscopy, energy dispersive X-ray analysis and Auger electron spectroscopy. Oxide was found at all interfaces with an interface width of at least 600 A for the oxidized substrates and at least 300 A for the unoxidized substrates. Scratch test results demonstrate that the adhesion of hafnium nitride to both oxidized and unoxidized 440C is superior to that of silicon nitride. Oxidized 440C is found to have increased adhesion, to both nitrides, over that of unoxidized 440C. Coatings of both nitrides deposited at 8 mtorr were found to have increased adhesion to both oxidized and unoxidized 440C over those deposited at 20 mtorr.

Enhancement of valve metal osteoconductivity by one-step hydrothermal treatment.

PubMed

Zuldesmi, Mansjur; Waki, Atsushi; Kuroda, Kensuke; Okido, Masazumi

2014-09-01

In this study, we produced super-hydrophilic surfaces of valve metals (Ti, Nb, Ta and Zr) by one-step hydrothermal treatment. Their surface characteristics and osteoconductivity using an in vivo test were then assessed. These data were compared with that of as-polished, as-anodized and both anodized+hydrothermally treated samples. Changes in surface chemistry, surface morphology and structure were investigated by X-ray photoelectron spectroscopy, scanning electron microscopy, and X-ray diffractometry. The results revealed that the water contact angles of valve metals were decreased by hydrothermal treatment and continued to reduce dramatically until lower than 10° after being immersed in phosphate buffered solution. By producing super-hydrophilic surfaces, the osteoconductivity of these hydrothermally treated valve metals was enhanced by up to 55%. Copyright © 2014 Elsevier B.V. All rights reserved.

Gold leaf counter electrodes for dye-sensitized solar cells

NASA Astrophysics Data System (ADS)

Shimada, Kazuhiro; Toyoda, Takeshi

2018-03-01

In this study, a gold leaf 100 nm thin film is used as the counter electrode in dye-sensitized solar cells. The traditional method of hammering gold foil to obtain a thin gold leaf, which requires only small amounts of gold, was employed. The gold leaf was then attached to the substrate using an adhesive to produce the gold electrode. The proposed approach for fabricating counter electrodes is demonstrated to be facile and cost-effective, as opposed to existing techniques. Compared with electrodes prepared with gold foil and sputtered gold, the gold leaf counter electrode demonstrates higher catalytic activity with a cobalt-complex electrolyte and higher cell efficiency. The origin of the improved performance was investigated by surface morphology examination (scanning electron microscopy), various electrochemical analyses (cyclic voltammetry, linear sweep voltammetry, and electrochemical impedance spectroscopy), and crystalline analysis (X-ray diffractometry).

Delaminating and restacking MgAl-layered double hydroxide monitored and characterized by a range of instrumental methods

NASA Astrophysics Data System (ADS)

Muráth, Szabolcs; Somosi, Zoltán; Tóth, Ildikó Y.; Tombácz, Etelka; Sipos, Pál; Pálinkó, István

2017-07-01

The delamination-restacking properties of MgAl-layered double hydroxide (MgAl-LDH) were studied in various solvents. The LDH samples were successfully delaminated in polar amides (formamide, N-methylformamide, N-methylacetamide). Usually, delamination was finalized by ultrasonic treatment. As rehydrating solutions, numerous Na-salts with single-, double- and triple-charged anions were used. Reconstruction was accomplished with anions of one or two negative charges, but triple-charged ones generally disrupted the rebuilding process, likely, because their salts with the metals of the LDH are very stable, and the thin layers can more readily transform to salts than the ordered materials. Samples and delamination-restacking processes were characterized by X-ray diffractometry (XRD), infrared spectroscopy (IR), dynamic light scattering (DLS), scanning electron microscopy (SEM) and energy-dispersive X-ray analysis (EDX).

[Study on the traditional lime mortar from the memorial archway in the southern Anhui province].

PubMed

Wei, Guo-Feng; Sun, Sheng; Wang, Cheng-Xing; Zhang, Bing-Jian; Chen, Xi-Min

2013-07-01

The traditional lime mortar was investigated by means of scanning electron microscope (SEM), X-ray diffractometry and Fourier transform infrared spectrometry (FTIR). The results show that the mortar from the memorial archway in the southern Anhui province was the organic-inorganic composite materials composed of lime with tung oil or sticky rice. It was found that the excellent performance of the tung oil-lime mortar can be explained by the compact lamellar organic-inorganic composite structure that was produced by carbonization reaction of lime, cross-linking reactions of tung oil and oxygen and complexing reaction of Ca2+ and -COO-. The compact micro-structure of sticky rice-lime mortar, which was produced due to carbonation process of lime controlled by amylopectin, should be the cause of the good performance of this kind of organic-inorganic mortar.

Electrochemical properties of monolithic nickel sulfide electrodes for use in sodium batteries

DOE Office of Scientific and Technical Information (OSTI.GOV)

Go, Dae-Yeon; Park, Jinsoo, E-mail: jsp@ikw.ac.kr; Noh, Pan-Jin

2014-10-15

Highlights: • We succeeded in preparing monolithic Ni{sub 3}S{sub 2} integrated electrode through the sulfuration. • The sulfuration is a facile and useful method to synthesize metal sulfides with nanostructure. • As-prepared monolithic Ni{sub 3}S{sub 2} electrodes showed very stable and cycle performance over charge/discharge cycling. - Abstract: Monolithic nickel sulfide electrodes were prepared using a facile synthesis method, sulfuration and annealing. As-prepared Ni{sub 3}S{sub 2} electrodes were characterized by X-ray diffractometry and field emission scanning electron microscopy. Thermal stability was determined by thermal gravimetric analysis and differential scanning calorimetry. Electrochemical properties were measured by galvanostatic charge and discharge cyclingmore » for Na-ion batteries. Three kinds of Ni{sub 3}S{sub 2} electrodes were prepared by varying the sulfuration time (5, 15 and 25 min). The electrochemical results indicated that the capacities increased with an increase in sulfuration time and the cycle performance was stable as a result of monolithic integration of nanostructured Ni{sub 3}S{sub 2} on Ni plates, leading to low interfacial resistance.« less

Preparation and characterization of non-crystalline granular starch and corresponding carboxymethyl starch.

PubMed

Zhang, Bao; Li, Xiaomin; Xie, Qiutao; Tao, Han; Wang, Wu; Chen, Han-Qing

2017-10-01

Native corn starch slurried in 50% ethanol solution was treated at 60°C, 70°C, 80°C, and 85°C, respectively. The resultant starches were investigated by polarized microscopy, scanning electron microscopy (SEM), differential scanning calorimetry (DSC), and X-ray diffractometry (XRD). The Maltese cross of ethanol-heating treated starch gradually weaken with increasing temperature and completely disappeared at 85°C. SEM data indicated the treated granular exhibited a rougher surface with more pores and grooves than native starch granular, but the shape of the treated starch was still intact. DSC and XRD data confirmed ethanol-heating treated starch changed from crystalline to non-crystalline structure at 85°C. The highest degree of substitution (DS) and corresponding reaction efficiency (RE) for the carboxymethylation of native starch were 0.66 and 36.7%, respectively, while the corresponding DS and RE for non-crystalline granular starches increased by 0.29 and 16.1% at the same reaction condition, respectively. Copyright © 2017 Elsevier B.V. All rights reserved.

Preparation, characterization and in vitro evaluation of solid dispersions containing docetaxel.

PubMed

Chen, Jie; Qiu, Liyan; Hu, Minxin; Jin, Yi; Han, Jieru

2008-06-01

Solid dispersions using water-soluble carriers were studied for improving the dissolution of docetaxel, a poorly soluble compound. In order to obtain the most optimized formulation, we prepared many solid dispersions with different carriers, different solvents, or at a series of drug-to-carrier ratios, and compared their dissolution. The accumulative dissolution of docetaxel from poloxamer 188 was more excellent than that from PVP(k30) and glyceryl monostearate, and the dissolution of docetaxel from solid dispersion was markedly higher than that of pure docetaxel; meanwhile the increased dissolution was partly dependent on the ratios of docetaxel and poloxamer 188. The ethanol used to prepare solid dispersion is of more significant effect on the dissolution of docetaxel than that of acetone. The docetaxel/poloxamer 188 system was characterized by differential scanning calorimetry (DSC), X-ray diffractometry (XRD), and environmental scanning electron microscope (ESEM). The results of DSC, XRD, and ESEM analyses of docetaxel/poloxamer 188 system showed that there are intermolecular interactions between docetaxel and poloxamer, and the crystallinity of docetaxel disappeared. These results show that solid dispersion is a promising approach of developing docetaxel drug formulates.

Preparation and Optimization of Amorphous Ursodeoxycholic Acid Nano-suspensions by Nanoprecipitation based on Acid-base Neutralization for Enhanced Dissolution.

PubMed

Xie, Yike; Chen, Zhongjian; Su, Rui; Li, Ye; Qi, Jianping; Wu, Wei; Lu, Yi

2017-01-01

Ursodeoxycholic acid, usually used to dissolve cholesterol gallstones in clinic, is a typical hydrophobic drug with poor oral bioavailability due to dissolution rate-limited performance. The objective of this study was to increase the dissolution of ursodeoxycholic acid by amorphous nanosuspensions. Nanoprecipitation based on acid-base neutralization was used to prepare the nanosuspensions with central composite design to optimize the formula. The nanosuspensions were characterized by particle size, morphology, crystallology and dissolution. The ursodeoxycholic acid nanosuspensions showed mean particle size around 380 nm with polydispersion index value about 0.25. Scanning electron microscope observed high coverage of HPMC-E50 onto the surface of the nanosuspensions. Differential scanning calorimetry and powder X-ray diffractometry revealed amorphous structure of the ursodeoxycholic acid nanosuspensions. A significant increase of dissolution in acidic media was achieved by the amorphous nanosuspensions compared with the physical mixture. It can be predicted that the amorphous nanosuspensions show great potential in improving the oral bioavailability of ursodeoxycholic acid. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

Physical and structural changes induced by high pressure on corn starch, rice flour and waxy rice flour.

PubMed

Cappa, Carola; Lucisano, Mara; Barbosa-Cánovas, Gustavo V; Mariotti, Manuela

2016-07-01

The impact of high pressure (HP) processing on corn starch, rice flour and waxy rice flour was investigated as a function of pressure level (400MPa; 600MPa), pressure holding time (5min; 10min), and temperature (20°C; 40°C). Samples were pre-conditioned (final moisture level: 40g/100g) before HP treatments. Both the HP treated and the untreated raw materials were evaluated for pasting properties and solvent retention capacity, and investigated by differential scanning calorimetry, X-ray diffractometry and environmental scanning electron microscopy. Different pasting behaviors and solvent retention capacities were evidenced according to the applied pressure. Corn starch presented a slower gelatinization trend when treated at 600MPa. Corn starch and rice flour treated at 600MPa showed a higher retention capacity of carbonate and lactic acid solvents, respectively. Differential scanning calorimetry and environmental scanning electron microscopy investigations highlighted that HP affected the starch structure of rice flour and corn starch. Few variations were evidenced in waxy rice flour. These results can assist in advancing the HP processing knowledge, as the possibility to successfully process raw samples in a very high sample-to-water concentration level was evidenced. This work investigates the effect of high pressure as a potential technique to modify the processing characteristics of starchy materials without using high temperature. In this case the starches were processed in the powder form - and not as a slurry as in previously reported studies - showing the flexibility of the HP treatment. The relevance for industrial application is the possibility to change the structure of flour starches, and thus modifying the processability of the mentioned products. Copyright © 2016 Elsevier Ltd. All rights reserved.

Effect of heavy tempering on microstructure and yield strength of 28CrMo48VTiB martensitic steel

NASA Astrophysics Data System (ADS)

Sun, Yu; Gu, Shunjie; Wang, Qian; Wang, Huibin; Wang, Qingfeng; Zhang, Fucheng

2018-02-01

The 28CrMo48VTiB martensitic steel for sulfide stress cracking (SSC) resistance oil country tubular goods (OCTG) of C110 grade was thermally processed through quenching at 890 °C and tempering at 600 °C-720 °C for 30-90 min. The microstructures of all samples were characterized using field emission scanning electron microscopy (FESEM), electron backscattering diffraction (EBSD), transmission electron microscopy (TEM) and x-ray diffractometry (XRD). Also, the tensile properties were measured. The results indicated that the yield strength (YS) decreased as both the tempering temperature and duration increased, due to the coarsening of martensitic packet/block/lath structures, the reduction of dislocation density, as well as the increase of both the volume fraction and average diameter of the precipitates. The martensitic lath width was the key microstructural parameter controlling the YS of this heavily-tempered martensitic steel, whereas the corresponding relationship was in accordance with the Langford-Cohen model. Furthermore, the martensitic structure boundary and the solid solution strengthening were the two most significant factors dominating the YS, in comparison with the dislocation and precipitation strengthening.

Observation of defect-induced Photoresponse and charge carrier transport in single GeSe2 nanobelt devices

NASA Astrophysics Data System (ADS)

Mukherjee, Bablu; Tok, Eng Soon; Haur Sow, Chorng

2013-03-01

Single crystal GeSe2 nanobelts were grown using chemical vapor deposition techniques. Morphology of the nanostructures was characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffractometry (XRD) and Raman spectroscopy. Electronic transport properties, impedance spectroscopy, photoconductive characteristics and temperature-dependent electrical resistivity measurements were carried out on individual GeSe2 nanobelt devices. The photosensitivity of single GeSe2 nanobelt (NB) devices was examined with two different excitation wavelengths of laser beams with photon energies above band gap and at sub-band gap of the NB. A maximum photoconductive gain 106 % was achieved at a wavelength of 808 nm. The magnitude of the photocurrent and response time of the individual GeSe2 NB device indicate that the photoresponse could be attributed to the presence of isolated mid band gap defect levels. Temperature dependent photocurrent measurements indicate the rough estimation of the energy levels for the defect states. Localized photostudy shows that the large photoresponse of the device primarily occurs at the metal-NB contact regions. Department of Physics, 2 Science Drive 3, National University of Singapore (NUS), Singapore 117542

Effects of fines content on hydraulic conductivity and morphology of laterite soil as hydraulic barrier

NASA Astrophysics Data System (ADS)

Bello Yamusa, Yamusa; Yunus, Nor Zurairahetty Mohd; Ahmad, Kamarudin; Rahman, Norhan Abd; Sa'ari, Radzuan

2018-03-01

Laterite soil was investigated to find out the effects of fines content and to identify the micro-structural and molecular characteristics to evaluate its potentiality as a compacted soil landfill liner material. Tests were carried out on natural soil and reconstituted soil by dry weight of soil samples to determine the physical and engineering properties of the soil. All tests were carried out on the samples by adopting the British Standard 1377:1990. The possible mechanisms that contributed to the clay mineralogy were analyzed using spectroscopic and microscopic techniques such as field emission scanning electron microscopy (FESEM), energy-dispersive X-ray (EDX) and X-ray diffractometry (XRD). The laterite soil was found to contain kaolinite as the major clay minerals. A minimum of 50% fines content of laterite soil met the required result for hydraulic barriers in waste containment facilities.

Observing Graphene Grow: Catalyst–Graphene Interactions during Scalable Graphene Growth on Polycrystalline Copper

PubMed Central

2013-01-01

Complementary in situ X-ray photoelectron spectroscopy (XPS), X-ray diffractometry, and environmental scanning electron microscopy are used to fingerprint the entire graphene chemical vapor deposition process on technologically important polycrystalline Cu catalysts to address the current lack of understanding of the underlying fundamental growth mechanisms and catalyst interactions. Graphene forms directly on metallic Cu during the high-temperature hydrocarbon exposure, whereby an upshift in the binding energies of the corresponding C1s XPS core level signatures is indicative of coupling between the Cu catalyst and the growing graphene. Minor carbon uptake into Cu can under certain conditions manifest itself as carbon precipitation upon cooling. Postgrowth, ambient air exposure even at room temperature decouples the graphene from Cu by (reversible) oxygen intercalation. The importance of these dynamic interactions is discussed for graphene growth, processing, and device integration. PMID:24041311

Nacre-like calcium carbonate controlled by ionic liquid/graphene oxide composite template.

PubMed

Yao, Chengli; Xie, Anjian; Shen, Yuhua; Zhu, Jinmiao; Li, Hongying

2015-06-01

Nacre-like calcium carbonate nanostructures have been mediated by an ionic liquid (IL)-graphene oxide (GO) composite template. The resultant crystals were characterized by scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) spectroscopy, and X-ray powder diffractometry (XRD). The results showed that either 1-butyl-3-methylimidazolium tetrafluoroborate ([BMIM]BF4) or graphene oxide can act as a soft template for calcium carbonate formation with unusual morphologies. Based on the time-dependent morphology changes of calcium carbonate particles, it is concluded that nacre-like calcium carbonate nanostructures can be formed gradually utilizing [BMIM]BF4/GO composite template. During the process of calcium carbonate formation, [BMIM]BF4 acted not only as solvents but also as morphology templates for the fabrication of calcium carbonate materials with nacre-like morphology. Based on the observations, the possible mechanisms were also discussed. Copyright © 2015 Elsevier B.V. All rights reserved.

Different decay patterns observed in a nineteenth-century building (Palma, Spain).

PubMed

Genestar, Catalina; Pons, Carmen; Cerro, José Carlos; Cerdà, Víctor

2014-01-01

The effects of atmospheric pollutants and climatic conditions were studied in a decayed column in the Seminary of Sant Pere. This nineteenth-century building is situated in the historic centre of Palma (Mallorca, Spain), less than 0.5 km from the sea. Samples were collected from the internal and external part of the crusts formed in the four sides of the column. The samples were analysed by means of thermal analysis, X-ray diffractometry, scanning electron microscopy, Fourier transform infrared spectroscopy and ion chromatography. Results show significant differences in the four sides of the column. A high degree of carbonate stone sulfation is observed in all of the samples analysed. A synergistic effect between atmospheric factors and micropollutants on the deterioration of stone is observed. A high uptake of atmospheric particulate matter is found in the external part of the black crusts.

Synthesis of vaterite and aragonite crystals using biomolecules of tomato and capsicum

NASA Astrophysics Data System (ADS)

Chen, Long; Xu, Wang-Hua; Zhao, Ying-Guo; Kang, Yan; Liu, Shao-Hua; Zhang, Zai-Yong

2012-12-01

In this paper, biomimetic synthesis of calcium carbonate (CaCO3) in the presence of biomolecules of two vegetables-tomato and capsicum is investigated. Scanning electron microscopy and X-ray powder diffractometry were used to characterize the CaCO3 obtained. The biomolecules in the extracts of two vegetables are determined by UV-vis or FTIR. The results indicate that a mixture of calcite and vaterite spheres constructed from small particles is produced with the extract of tomato, while aragonite rods or ellipsoids are formed in the presence of extract of capsicum. The possible formation mechanism of the CaCO3 crystals with tomato biomolecules can be interpreted by particle-aggregation based non-classical crystallization laws. The proteins and/or other biomolecules in tomato and capsicum may control the formation of vaterite and aragonite crystals by adsorbing onto facets of them.

Improvement in the Shape Memory Response of Ti50.5Ni24.5Pd25 High-Temperature Shape Memory Alloy with Scandium Microalloying

NASA Technical Reports Server (NTRS)

Atli, K. C.; Karaman, I; Noebe, R. D.; Garg, A.; Chumlyakov, Y. I.; Kireeva, I. V.

2010-01-01

A Ti(50.5)Ni(24.5)Pd25 high-temperature shape memory alloy (HTSMA) is microalloyed with 0.5 at. pct scandium (Sc) to enhance its shape-memory characteristics, in particular, dimensional stability under repeated thermomechanical cycles. For both Ti(50.5)Ni(24.5)Pd25 and the Sc-alloyed material, differential scanning calorimetry is conducted for multiple cycles to characterize cyclic stability of the transformation temperatures. The microstructure is evaluated using electron microscopy, X-ray diffractometry, and wavelength dispersive spectroscopy. Isobaric thermal cycling experiments are used to determine transformation temperatures, dimensional stability, and work output as a function of stress. The Sc-doped alloy displays more stable shape memory response with smaller irrecoverable strain and narrower thermal hysteresis than the baseline ternary alloy. This improvement in performance is attributed to the solid solution hardening effect of Sc.

Inorganic fullerene-like tungsten disulfide nanocoating for friction reduction of nickel-titanium alloys.

PubMed

Samorodnitzky-Naveh, Gili R; Redlich, Meir; Rapoport, Lev; Feldman, Yishay; Tenne, Reshef

2009-12-01

To fabricate a friction-reducing coating onto different nickel-titanium (NiTi) substrates using inorganic fullerene-like tungsten disulfide (IF-WS(2)) nanoparticles and to estimate in vitro friction reducing extent of the coating. Different NiTi substrates were coated with cobalt and IF-WS(2) nanoparticles film by the electrodeposition procedure. Coating composition analyses was made by scanning-electron microscopy, energy dispersive x-ray spectroscopy, x-ray powder diffractometry and x-ray photoelectron spectroscopy. Friction evaluation was carried out using standard tribological tests and an Instron system. Stable and well-adhered cobalt + IF-WS(2) coating of the NiTi substrates was obtained. Friction tests presented up to 66% reduction of the friction coefficient. NiTi alloy is widely used for many medical appliances; hence, this unique friction-reducing coating could be implemented to provide better manipulation and lower piercing rates.

The ceramics of Malpaís of Zacapu, Michoacán, Mexico, during the Early and Middle Postclassic periods (900-1450 AD): Micro-chemical characterization of surface paintings

NASA Astrophysics Data System (ADS)

Jadot, E.; Schiavon, N.; Manso, M.

2016-05-01

Tarascan ceramic sherds from two Postclassical archaeological sites (900-1450 AD) at the Malpaís of Zacapu, Michoacán, Mexico, were investigated by combining Back-Scattered Scanning Electron Microscopy and Energy Dispersive Spectroscopy (BSEM-EDS), μ-X-Ray Diffractometry (μ-XRD), μ-X-ray Fluorescence Spectroscopy (μ-XRF) and μ-Raman Spectroscopy. These sherds are famous for their forms and decorations although the composition of its raw materials remains so far unknown and focused only on the composition of the ceramic paste. For the purpose of surface decoration characterization, the pigments used in slips and paintings were identified as hematite, magnetite, amorphous carbon, graphite and lignite. Furthermore chemical and molecular structure determination allowed the identification of technological aspects such as the firing temperatures and atmospheres used in ceramics production.

Petro-mineralogical Studies of the Paleoproterozoic Phosphorites in the Sonrai basin, Lalitpur District, Uttar Pradesh, India

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dar, Shamim A., E-mail: sjshamim@gmail.com; Khan, K. F.; Khan, Saif A.

2015-09-15

The Paleoproterozoic phosphorites constitute an economically significant component of the Sonrai basin of Lalitpur district. These are associated with ferruginous shale, ironstone, limestone and quartz breccia. Petro-mineralogical studies of samples of the phosphorites, using X-ray diffractometry and scanning electron microscopy, reveal that the collophane (carbonate-fluorapatite) is the dominant phosphate mineral. Calcite, dolomite, quartz, mica and haematite are the dominant gangue constituents. The phosphate minerals occur as oolites mutually replaced by carbonate and silica. The presence of iron oxides has been found in most of the thin sections. There is meagre evidence of organic matter in the form of filaments ofmore » microbial phosphate laminae in the samples of phosphorite. The mineral assemblages, their texture and various forms in these phosphorites may be due to some environmental vicissitudes followed by replacement processes and biogenic activities.« less

Fabrication of Ti-0.48Al Alloy by Centrifugal Casting.

PubMed

Park, Jong Bum; Lee, Jung-Il; Ryu, Jeong Ho

2018-09-01

Many of the unique properties of TiAl alloys that make are attractive for use in high-temperature structural applications also make it challenging to process them into useful products. Cast TiAl is rapidly nearing commercialization, particularly in the vehicle industry, owing to its low production cost. In this study, the centrifugal casting of a TiAl (Ti-48%Al, mole fraction) turbocharger was simulated and an experimental casting was created in vacuum using an induction melting furnace coupled to a ceramic composite mold. Numerical simulation results agreed with the experiment. The crystal structure, microstructure, and chemical composition of the TiAl prepared by centrifugal casting were studied by X-ray diffractometry, optical microscopy, field emission scanning electron microscopy (FE-SEM) and energy dispersive spectroscopy (EDS). FE-SEM and EDS examinations of the TiAl casting revealed that the thickness of the oxide layer (α-case) was typically less than 35 μm.

Archaeometallurgy in Messina: Iron Slug From A Dig at Blog P, Laboratory Analyses and Interpretation.

NASA Astrophysics Data System (ADS)

Caterina, Ingoglia; Maurizio, Triscari; Giuseppe, Sabatino

The archaeological site in Via La Farina, Block P, in Messina, is unique in many ways, due also to the high quantity of samples of iron slag. The slag was examined to identify the production centres of such materials, and, after characterization, was compared to similar material, exclusively for product typology, from different archaeological sites in the province of Messina, situated in the Peloritani Mountains (Messina city, S. Marco d'Alunzio, Milazzo, Francavilla di Sicilia, Novara di Sicilia as well as the archaeological site of Halaesa, near Tusa). Mineralogical characterization of the phases carried out by X-ray diffractometry (XRD) and Rietveld data elaboration, morphological study of slag findings and a semi-quantitative analysis by scanning electronic microscope (SEM+EDX) were performed. A chemical investigation was carried out by electron probe micro analysis (EPMA), to determine major element,. Minor and trace elements were determined by LA-ICP-MS. All the examined slag is related to iron metallurgy, and, in the case of Via La Farina, there is firm archaeological evidence pinpointing to smelting activity.

Dissolution enhancement of tadalafil by liquisolid technique.

PubMed

Lu, Mei; Xing, Haonan; Yang, Tianzhi; Yu, Jiankun; Yang, Zhen; Sun, Yanping; Ding, Pingtian

2017-02-01

This study aimed to enhance the dissolution of tadalafil, a poorly water-soluble drug by applying liquisolid technique. The effects of two critical formulation variables, namely drug concentration (17.5% and 35%, w/w) and excipients ratio (10, 15 and 20) on dissolution rates were investigated. Pre-compression tests, including particle size distribution, flowability determination, Fourier transform infrared (FT-IR), differential scanning calorimetry (DSC), X-ray diffractometry (XRD) and scanning electron microscopy (SEM), were carried out to investigate the mechanism of dissolution enhancement. Tadalafil liquisolid tablets were prepared and their quality control tests, dissolution study, contact angle measurement, Raman mapping, and storage stability test were performed. The results suggested that all the liquisolid tablets exhibited significantly higher dissolution rates than the conventional tablets and pure tadalafil. FT-IR spectrum reflected no drug-excipient interactions. DSC and XRD studies indicated reduction in crystallinity of tadalafil, which was further confirmed by SEM and Raman mapping outcomes. The contact angle measurement demonstrated obvious increase in wetting property. Taken together, the reduction of particle size and crystallinity, and the improvement of wettability were the main mechanisms for the enhanced dissolution rate. No significant changes were observed in drug crystallinity and dissolution behavior after storage based on XRD, SEM and dissolution results.

Piroxicam/2-hydroxypropyl-beta-cyclodextrin inclusion complex prepared by a new fluid-bed coating technique.

PubMed

Zhang, Xingwang; Wu, Danni; Lai, Jie; Lu, Yi; Yin, Zongning; Wu, Wei

2009-02-01

This work was aimed at investigating the feasibility of fluid-bed coating as a new method to prepare cyclodextrin inclusion complex. The inclusion complex of the model drug piroxicam (PIX) and 2-hydroxypropyl-beta-cyclodextrin (HPCD) in aqueous ethanol solution was sprayed and deposited onto the surface of the pellet substrate upon removal of the solvent. The coating process was fluent with high coating efficiency. Scanning electron microscopy revealed a coarse pellet surface, and a loosely packed coating structure. Significantly enhanced dissolution, over 90% at 5 min, was observed at stoichiometric PIX/HPCD molar ratio (1/1) and at a ratio with excessive HPCD (1/2). Differential scanning calorimetry and powder X-ray diffractometry confirmed absence of crystallinity of PIX at PIX/HPCD molar ratio of 1/1 and 1/2. Fourier transform-infrared spectrometry and Raman spectrometry revealed interaction between PIX and HPCD adding evidence on inclusion of PIX moieties into HPCD cavities. Solid-state (13)C NMR spectrometry indicated possible inclusion of PIX through the pyridine ring. It is concluded that fluid-bed coating has potential to be used as a new technique to prepare cyclodextrin inclusion complex.

Formation and morphology of Zn(2)Ti(3)O(8) powders using hydrothermal process without dispersant agent or mineralizer.

PubMed

Wang, Cheng-Li; Hwang, Weng-Sing; Chang, Kuo-Ming; Ko, Horng-Huey; Hsi, Chi-Shiung; Huang, Hong-Hsin; Wang, Moo-Chin

2011-01-28

Synthesis of Zn(2)Ti(3)O(8) powders for attenuating UVA using TiCl(4), Zn(NO(3))(2)·6H(2)O and NH(4)OH as precursor materials by hydrothermal process has been investigated. The X-ray diffractometry (XRD) results show the phases of ZnO, anatase TiO(2) and Zn(2)Ti(3)O(8) coexisted when the zinc titanate powders were calcined at 600 °C for 1 h. When calcined at 900 °C for 1 h, the XRD results reveal the existence of ZnO, Zn(2)TiO(4), rutile TiO(2) and ZnTiO(3). Scanning electron microscope (SEM) observations show extensive large agglomeration in the samples. Transmission electron microscope (TEM) and electron diffraction (ED) examination results indicate that ZnTiO(3) crystallites formed with a size of about 5 nm on the matrix of plate-like ZnO when calcined at 700 °C for 1 h. The calcination samples have acceptable absorbance at a wavelength of 400 nm, indicating that the zinc titanate precursor powders calcined at 700 °C for 1 h can be used as an UVA-attenuating agent.

Formation and Morphology of Zn2Ti3O8 Powders Using Hydrothermal Process without Dispersant Agent or Mineralizer

PubMed Central

Wang, Cheng-Li; Hwang, Weng-Sing; Chang, Kuo-Ming; Ko, Horng-Huey; Hsi, Chi-Shiung; Huang, Hong-Hsin; Wang, Moo-Chin

2011-01-01

Synthesis of Zn2Ti3O8 powders for attenuating UVA using TiCl4, Zn(NO3)2·6H2O and NH4OH as precursor materials by hydrothermal process has been investigated. The X-ray diffractometry (XRD) results show the phases of ZnO, anatase TiO2 and Zn2Ti3O8 coexisted when the zinc titanate powders were calcined at 600 °C for 1 h. When calcined at 900 °C for 1 h, the XRD results reveal the existence of ZnO, Zn2TiO4, rutile TiO2 and ZnTiO3. Scanning electron microscope (SEM) observations show extensive large agglomeration in the samples. Transmission electron microscope (TEM) and electron diffraction (ED) examination results indicate that ZnTiO3 crystallites formed with a size of about 5 nm on the matrix of plate-like ZnO when calcined at 700 °C for 1 h. The calcination samples have acceptable absorbance at a wavelength of 400 nm, indicating that the zinc titanate precursor powders calcined at 700 °C for 1 h can be used as an UVA-attenuating agent. PMID:21541035

Microstructure and properties of Fe-based composite coating by laser cladding Fe-Ti-V-Cr-C-CeO2 powder

NASA Astrophysics Data System (ADS)

Zhang, Hui; Zou, Yong; Zou, Zengda; Wu, Dongting

2015-01-01

In situ TiC-VC reinforced Fe-based cladding layer was obtained on low carbon steel surface by laser cladding with Fe-Ti-V-Cr-C-CeO2 alloy powder. The microstructure, phases and properties of the cladding layer were investigated by X-ray diffractometry (XRD), scanning electron microscopy (SEM), energy dispersive spectrometry (EDS), transmission electron microscopy (TEM), potentio-dynamic polarization and electro-chemical impedance spectroscopy (EIS). Results showed Fe-Ti-V-Cr-C-CeO2 alloy powder formed a good cladding layer without defects such as cracks and pores. The phases of the cladding layer were α-Fe, γ-Fe, TiC, VC and TiVC2. The microstructures of the cladding layer matrix were lath martensite and retained austenite. The carbides were polygonal blocks with a size of 0.5-2 μm and distributed uniformly in the cladding layer. High resolution transmission electron microscopy showed the carbide was a complex matter composed of nano TiC, VC and TiVC2. The cladding layer with a hardness of 1030 HV0.2 possessed good wear and corrosion resistance, which was about 16.85 and 9.06 times than that of the substrate respectively.

Passivation of hematite nanorod photoanodes with a phosphorus overlayer for enhanced photoelectrochemical water oxidation

NASA Astrophysics Data System (ADS)

Xiong, Dehua; Li, Wei; Wang, Xiaoguang; Liu, Lifeng

2016-09-01

Hematite (i.e., α-Fe2O3) nanorod photoanodes passivated with a phosphorus overlayer have been fabricated by decomposing sodium hypophosphite (NaH2PO2) at a low temperature over the hematite nanorod surface. Extensive scanning electron microscopy, transmission electron microscopy, x-ray diffractometry and UV-vis spectroscopy characterizations confirm that conformal deposition of an amorphous phosphorus overlayer does not change the crystal structure, morphology, and optical absorption properties of hematite photoanodes. X-ray photoelectron spectroscopy reveals that phosphorus in the deposited overlayer exists in an oxidized state. Comprehensive steady-state polarization, transient photocurrent response, and impedance spectroscopy measurements as well as Mott-Schottky analysis manifest that the phosphorus overlayer is able to effectively passivate surface states and suppress electron-hole recombination, substantially enhancing the photocurrent for water oxidation. Combining the phosphorization treatment with two-step thermal activation, a photocurrent density of 1.1 mA cm-2 is achieved at 1.23 V versus reversible hydrogen electrode under illumination of 100 mW cm-2, ca 55 times higher than that of the non-activated pristine hematite photoanode measured under the same conditions. The simple and fast phosphorization strategy we present here can be readily applied to passivate surfaces of other semiconductor photoelectrodes to improve their photoelectrochemical performance.

Morphological characterization and in vitro biocompatibility of a porous nickel-titanium alloy.

PubMed

Prymak, Oleg; Bogdanski, Denise; Köller, Manfred; Esenwein, Stefan A; Muhr, Gert; Beckmann, Felix; Donath, Tilmann; Assad, Michel; Epple, Matthias

2005-10-01

Disks consisting of macroporous nickel-titanium alloy (NiTi, Nitinol, Actipore) are used as implants in clinical surgery, e.g. for fixation of spinal dysfunctions. The morphological properties were studied by scanning electron microscopy (SEM) and by synchrotron radiation-based microtomography (SRmuCT). The composition was studied by X-ray diffractometry (XRD), differential scanning calorimetry (DSC), and energy-dispersive X-ray spectroscopy (EDX). The mechanical properties were studied with temperature-dependent dynamical mechanical analysis (DMA). Studies on the biocompatibility were performed by co-incubation of porous NiTi samples with isolated peripheral blood leukocyte fractions (polymorphonuclear neutrophil granulocytes, PMN; peripheral blood mononuclear leukocytes, PBMC) in comparison with control cultures without NiTi samples. The cell adherence to the NiTi surface was analyzed by fluorescence microscopy and scanning electron microscopy. The activation of adherent leukocytes was analyzed by measurement of the released cytokines using enzyme-linked immunosorbent assay (ELISA). The cytokine response of PMN (analyzed by the release of IL-1ra and IL-8) was not significantly different between cell cultures with or without NiTi. There was a significant increase in the release of IL-1ra (p<0.001), IL-6 (p<0.05), and IL-8 (p<0.05) from PBMC in the presence of NiTi samples. In contrast, the release of TNF-alpha by PBMC was not significantly elevated in the presence of NiTi. IL-2 was released from PBMC only in the range of the lower detection limit in all cell cultures. The material, clearly macroporous with an interconnecting porosity, consists of NiTi (martensite; monoclinic, and austenite; cubic) with small impurities of NiTi2 and possibly NiC(x). The material is not superelastic upon manual compression and shows a good biocompatibility.

Ferric ion-assisted in situ synthesis of silver nanoplates on polydopamine-coated silk.

PubMed

Xiao, Jing; Zhang, Huihui; Mao, Cuiping; Wang, Ying; Wang, Ling; Lu, Zhisong

2016-10-01

In the present study, a ferric ion (Fe(3+))-assisted in situ synthesis approach was developed to grow silver (Ag) nanoplates on the polydopamine (PDA)-coated silk without the use of additional reductants. The essential role of Fe(3+) in the formation of Ag nanoplates is revealed by comparing the morphologies of Ag nanostructures prepared on the silk-coated PDA film with/without Fe(3+) doping. Scanning electron micrographs show that high-density Ag nanoplates could be synthesized in the reaction system containing 50μg/mL FeCl3 and 50mM AgNO3. The size of the Ag nanoplate could be tuned by adjusting the reaction duration. Based on the data, a mechanism involving the Fe(3+)-selected growth of Ag atoms along the certain crystal faces was proposed to explain the fabrication process. Transmission electron microscopy and X-ray diffractometry indicate that the Ag nanoplates possess good crystalline structures. Raman spectra demonstrate that the nanoplates could strongly enhance the Raman scattering of the PDA molecules. The Ag nanoplate-coated silk could be utilized as a flexible substrate for the development of surface-enhanced Raman scattering biosensors. Copyright © 2016 Elsevier Inc. All rights reserved.

Synthesis of high generation thermo-sensitive dendrimers for extraction of rivaroxaban from human fluid and pharmaceutic samples.

PubMed

Parham, Negin; Panahi, Homayon Ahmad; Feizbakhsh, Alireza; Moniri, Elham

2018-04-13

In this present study, poly (N-isopropylacrylamide) as a thermo-sensitive agent was grafted onto magnetic nanoparticles, then ethylenediamine and methylmethacrylate were used to synthesize the first generation of poly amidoamine (PAMAM) dendrimers successively and the process continued alternatively until the ten generations of dendrimers. The synthesized nanocomposite was investigated using Fourier transform infrared spectrometry, thermalgravimetry analysis, X-ray diffractometry, elemental analysis and vibrating-sample magnetometer. The particle size and morphology were characterized using dynamic light scattering, field emission scanning electron microscopy and transmission electron microscopy. Batch experiments were conducted to investigate the parameters affecting adsorption and desorption of rivaroxaban by synthesized nanocomposite. The maximum sorption of rivaroxaban by the synthesized nanocomposite was obtained at pH of 8. The resulting grafted magnetic nanoparticle dendrimers were applied for extraction of rivaroxaban from biologic human liquids and medicinal samples. The specifications of rivaroxaban sorbed by a magnetic nanoparticle dendrimer showed good accessibility and high capacity of the active sites within the dendrimers. Urine and drug matrix extraction recoveries of more than 92.5 and 99.8 were obtained, respectively. Copyright © 2018 Elsevier B.V. All rights reserved.

Use of an integrated approach to characterize the physicochemical properties of foundry green sands

USDA-ARS?s Scientific Manuscript database

A fresh green sand, spent green sand, and a weathered spent green sand from a landfill were analyzed using diffractometry, electron microscopy, granulometry, spectrometry, and thermogravimetry. Our objective was to understand how the physicochemical properties of the green sands change from their o...

The Synergistic Effect of Iodide and Sodium Nitrite on the Corrosion Inhibition of Mild Steel in Bicarbonate-Chloride Solution.

PubMed

Eyu, Gaius Debi; Will, Geoffrey; Dekkers, Willem; MacLeod, Jennifer

2016-10-26

The effect of potassium iodide (KI) and sodium nitrite (NaNO₂ inhibitor on the corrosion inhibition of mild steel in chloride bicarbonate solution has been studied using electrochemical techniques. Potentiodynamic polarisation data suggest that, when used in combination, KI and NaNO₂ function together to inhibit reactions at both the anode and the cathode, but predominantly anodic. KI/NO₂ - concentration ratios varied from 2:1 to 2:5; inhibition efficiency was optimized for a ratio of 1:1. The surface morphology and corrosion products were analysed using scanning electron microscopy (SEM) and X-ray diffractometry (XRD). The latter shows that the addition of I - to NO₂ facilitates the formation of a passivating oxide (γ-Fe₂O₃) as compared to NO₂ - alone, decreasing the rate of metal dissolution observed in electrochemical testing. The synergistic effect of KI/NO₂ - inhibition was enhanced under the dynamic conditions associated with testing in a rotating disc electrode.

Structural investigation of chitosan-based microspheres with some anti-inflammatory drugs

NASA Astrophysics Data System (ADS)

Dreve, Simina; Kacso, Iren; Popa, Adriana; Raita, Oana; Dragan, Felicia; Bende, A.; Borodi, Gh.; Bratu, I.

2011-06-01

The use of chitosan as an excipient in oral formulations, as a drug delivery vehicle for ulcerogenic anti-inflammatory drugs and as base in polyelectrolyte complex systems, to prepare solid release systems as sponges was investigated. The preparation by double emulsification of chitosan hydrogels carrying diclofenac, acetyl-salycilic acid and hydrocortisone acetate as anti-inflammatory drugs is reported. The concentration of anti-inflammatory drug in the chitosan hydrogel generating the sponges was 0.08 mmol. Chitosan-drug loaded sponges with anti-inflammatory drugs were prepared by freeze-drying at -60 °C and 0.009 atm. Structural investigations of the solid formulations were done by Fourier-transformed infrared and ultraviolet-visible spectroscopy, spectrofluorimetry, differential scanning calorimetry and X-ray diffractometry. The results indicated that the drug molecules are forming temporary chelates in chitosan hydrogels and sponges. Electron paramagnetic resonance demonstrates the presence of free radicals in a wide range and the antioxidant activity for chitosan-drug supramolecular cross-linked assemblies.

Photoluminescent properties of complex metal oxide nanopowders for gas sensing

NASA Astrophysics Data System (ADS)

Bovhyra, R. V.; Mudry, S. I.; Popovych, D. I.; Savka, S. S.; Serednytski, A. S.; Venhryn, Yu. I.

2018-03-01

This work carried out research on the features of photoluminescence of the mixed and complex metal oxide nanopowders (ZnO/TiO2, ZnO/SnO2, Zn2SiO4) in vacuum and gaseous ambient. The nanopowders were obtained using pulsed laser reactive technology. The synthesized nanoparticles were characterized by X-ray diffractometry, energy-dispersive X-ray analysis, and scanning and transmission electron microscopy analysis for their sizes, shapes and collocation. The influence of gas environment on the photoluminescence intensity was investigated. A change of ambient gas composition leads to a rather significant change in the intensity of the photoluminescence spectrum and its deformation. The most significant changes in the photoluminescent spectrum were observed for mixed ZnO/TiO2 nanopowders. This obviously is the result of a redistribution of existing centers of luminescence and the appearance of new adsorption centers of luminescence on the surface of nanopowders. The investigated nanopowders can be effectively used as sensing materials for the construction of the multi-component photoluminescent sensing matrix.

Mortar radiocarbon dating: preliminary accuracy evaluation of a novel methodology.

PubMed

Marzaioli, Fabio; Lubritto, Carmine; Nonni, Sara; Passariello, Isabella; Capano, Manuela; Terrasi, Filippo

2011-03-15

Mortars represent a class of building and art materials that are widespread at archeological sites from the Neolithic period on. After about 50 years of experimentation, the possibility to evaluate their absolute chronology by means of radiocarbon ((14)C) remains still uncertain. With the use of a simplified mortar production process in the laboratory environment, this study shows the overall feasibility of a novel physical pretreatment for the isolation of the atmospheric (14)CO(2) (i.e., binder) signal absorbed by the mortars during their setting. This methodology is based on the assumption that an ultrasonic attack in liquid phase isolates a suspension of binder carbonates from bulk mortars. Isotopic ((13)C and (14)C), % C, X-ray diffractometry (XRD), and scanning electron microscopy (SEM) analyses were performed to characterize the proposed methodology. The applied protocol allows suppression of the fossil carbon (C) contamination originating from the incomplete burning of the limestone during the quick lime production, providing unbiased dating for "laboratory" mortars produced operating at historically adopted burning temperatures.

Phase purity of NiCo2O4, a catalyst candidate for electrolysis of water

NASA Technical Reports Server (NTRS)

Singer, J.; Fielder, W. L.; Garlick, R. G.; Negas, T.

1987-01-01

NiCo2O4 is shown to be difficult to obtain as a pure phase, and may never have been so obtained. High resolution x-ray diffractometry is required for its precise characterization. Film XRD is not likely to show the asymmetry in the spinel diffraction lines, caused by poorly crystallized NiO, as seen in diffractometer traces. The Co3O4 which is expected to accompany NiO as an impurity in NiCo2O4 syntheses has the same diffraction pattern as the binary oxide. Firings of the co-precipitated hydroxides at 300, 350, and 400 C, including one in pure O2, failed to produce single phase cobaltate. Scanning electron microscopy showed all the sintered products to range over several orders of magnitude in agglomerate/particle size. Surface areas by BET were all in the range 40 to 110 m sq/g, equivalent to particles of 200 to 100 Angstrom diameter. The spinel diffraction line breadths were compatible with those approximate dimensions.

Hydrothermal synthesis of nanostructured Y2O3 and (Y0.75Gd0.25)2O3 based phosphors

NASA Astrophysics Data System (ADS)

Mančić, Lidija; Lojpur, Vesna; Marinković, Bojan A.; Dramićanin, Miroslav D.; Milošević, Olivera

2013-08-01

Examples of (Y2O3-Gd2O3):Eu3+ and Y2O3:(Yb3+/Er3+) rare earth oxide-based phosphors are presented to highlight the controlled synthesis of 1D and 2D nanostructures through simple hydrothermal method. Conversion of the starting nitrates mixture into carbonate hydrate phase is performed with the help of ammonium hydrogen carbonate solution during hydrothermal treatment at 200 °C/3 h. Morphological architectures of rare earth oxides obtained after subsequent powders thermal treatment at 600 and 1100 °C for 3 and 12 h and their correlation with the optical characteristics are discussed based on X-ray powder diffractometry, field emission scanning electron microscopy, infrared spectroscopy and photoluminescence measurements. Strong red and green emission followed by the superior decay times are attributed to the high powders purity and homogeneous dopants distribution over the host lattice matrix.

Magnetic force microscopy study of domain walls in Co{sub 2}Z ferrite

DOE Office of Scientific and Technical Information (OSTI.GOV)

Qin, Lang; Verweij, Henk, E-mail: verweij.1@osu.edu

2014-03-01

Graphical abstract: - Highlights: • Hexaferrite Co{sub 2}Z is synthesized through the modified Pechini method. • Magnetic domains are observed in anisotropic Co{sub 2}Z single grain using MFM. • Observed single grain domain thickness is in good agreement with Dotsh model. - Abstract: Hexaferrite Co{sub 2}Z was synthesized through the modified Pechini method. Partially oriented samples were obtained after consolidation with uniaxial pressing and calcination/sintering at 1300 °C/1330 °C. The sample composition and morphology was identified with X-ray diffractometry (XRD) and scanning electron microscopy (SEM) with energy-dispersive X-ray spectrometry (EDS). MFM studies of the single grains revealed a domain structuremore » with 0.7 μm wide. The Co{sub 2}Z static magnetization was measured with a vibrating sample magnetometer (VSM), and was used to calculate a single grain domain with a thickness of 4.8 μm. This result is in good agreement with SEM observations of the single grain thickness.« less

Synthesis of barium and strontium carbonate crystals with unusual morphologies using an organic additive

NASA Astrophysics Data System (ADS)

Chen, Long; Jiang, Jizhong; Bao, Zuben; Pan, Jian; Xu, Weibing; Zhou, Lili; Wu, Zhigang; Chen, Xu

2013-12-01

In this paper, strontium carbonate (SrCO3) and barium carbonate (BaCO3) crystals were synthesized in the presence of an organic additive-hexamethylenetetramine (HMT) using two CO2 sources. Scanning electron microscopy and X-ray powder diffractometry were used to characterize the products. The results showed that the morphologies of orthorhombic strontianite SrCO3 transformed from branch-like to flower-like, and to capsicum-like at last, while the morphologies of BaCO3 change from fiber-like to branchlike, and to rod-like finally with an increase of the molar ratio HMT/Sr2+ and HMT/Ba2+ from 0.2 to 10 using ammonium carbonate as CO2 source. When using diethyl carbonate instead of ammonium carbonate as CO2 source, SrCO3 flowers aggregated by rods and BaCO3 shuttles were formed. The possible formation mechanisms of SrCO3 and BaCO3 crystals obtained in different conditions were also discussed.

Hierarchical macro-mesoporous structures in the system TiO{sub 2}-Al{sub 2}O{sub 3}, obtained by hydrothermal synthesis using Tween-20 as a directing agent

DOE Office of Scientific and Technical Information (OSTI.GOV)

Garcia-Benjume, M.L.; Espitia-Cabrera, M.I.; Contreras-Garcia, M.E., E-mail: eucontre@zeus.umich.mx

2009-12-15

Macro-mesoporous powders of titania, alumina, and mixed titania-20%alumina systems were obtained by hydrothermal synthesis employing surfactant Tween-20 as structural directing agent in order to promote the textural properties of titania. The effect of the alumina in the titania phase and on textural properties was analyzed. The obtained powders presented a macroporous channel structure that was characterized by X-ray diffractometry, scanning and transmission electron microscopy, N{sub 2} adsorption-desorption analysis, pore size distribution, Fourier transform infrared spectrometry, and thermogravimetric analysis. It was found that alumina content retarded the anatase phase crystallization and increased the Brunauer-Emmet-Teller surface area from 136 to 210 m{supmore » 2}/g. The powders calcined at 400 deg. C are thermally stable and possess an interconnected macro-mesoporous hierarchical structure; the results indicate that this synthesis can be employed to prepare mixed titania-alumina with good textural properties.« less

Mechanochemical synthesis and intercalation of Ca(II)Fe(III)-layered double hydroxides

NASA Astrophysics Data System (ADS)

Ferencz, Zs.; Szabados, M.; Varga, G.; Csendes, Z.; Kukovecz, Á.; Kónya, Z.; Carlson, S.; Sipos, P.; Pálinkó, I.

2016-01-01

A mechanochemical method (grinding the components without added water - dry grinding, followed by further grinding in the presence of minute amount of water or NaOH solution - wet grinding) was used in this work for the preparation and intercalation of CaFe-layered double hydroxides (LDHs). Both the pristine LDHs and the amino acid anion (cystinate and tyrosinate) intercalated varieties were prepared by the two-step grinding procedure in a mixer mill. By systematically changing the conditions of the preparation method, a set of parameters could be determined, which led to the formation of close to phase-pure LDH. The optimisation procedure was also applied for the intercalation processes of the amino acid anions. The resulting materials were structurally characterised by a range of methods (X-ray diffractometry, scanning electron microscopy, energy dispersive analysis, thermogravimetry, X-ray absorption and infra-red spectroscopies). It was proven that this simple mechanochemical procedure was able to produce complex organic-inorganic nanocomposites: LDHs intercalated with amino acid anions.

Chitosan-based nanocarriers for antimalarials

NASA Astrophysics Data System (ADS)

Dreve, Simina; Kacso, Iren; Popa, Adriana; Raita, Oana; Bende, A.; Borodi, Gh.; Bratu, I.

2012-02-01

The objective of this research was to synthesize and characterize chitosan-based liquid and solid materials with unique absorptive and mechanical properties as carriers for quinine - one of the most used antimalarial drug. The use of chitosan (CTS) as base in polyelectrolyte complex systems, to prepare solid release systems as sponges is presented. The preparation by double emulsification of CTS hydrogels carrying quinine as anti-malarial drug is reported. The concentration of quinine in the CTS hydrogel was 0.08 mmol. Chitosan - drug loaded hydrogel was used to generate solid sponges by freeze-drying at -610°C and 0.09 atm. Structural investigations of the solid formulations were done by Fourier-transformed infrared spectroscopy (FTIR), ultraviolet-visible spectroscopy (UV-VIS), spectrofluorimetry, differential scanning calorimetry (DSC) and X-ray diffractometry. The results indicated that the drug molecule is forming temporary chelates in CTS hydrogels and sponges. Electron paramagnetic resonance (EPR) demonstrates the presence of free radicals in a wide range and the antioxidant activity for chitosan - drug supramolecular cross-linked assemblies.

Enhanced photocatalytic activity of Fe-doped TiO2 coated on N-doped activated carbon composites for photocatalytic degradation of dyeing wastewater

NASA Astrophysics Data System (ADS)

Zhou, Jie; Zhu, Beibei; Wang, Lu; Li, Ya; Qiao, Qichen

2017-10-01

Fe-doped TiO2 coated on N-doped activated carbon (Fe-TiO2/N-AC, FTNA) composites were synthesized simply by a straightforward two-step procedure. The obtained materials were characterized by X-ray diffractometry (XRD), N2 adsorption-desorption, scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and FT-IR spectroscopies. Through the degradation of dyeing wastewater, the photocatalytic activity of FTNA was investigated under ultraviolet light irradiation. The results showed that containing N functional groups were successfully introduced onto the surface of the activated carbon. Compared with Fe-TiO2/AC (FTA), FTNA with average particle size of TiO2 13.6 nm and surface area 1007.89 m2/g showed a higher photoactivity. Additionally, for the photocatalytic degradation of dyeing wastewater, the optimum N content and catalyst content were 0.8% and 5g/L, respectively. Moreover, the photoactivity and photo stability of the catalyst after many runs was also evaluated.

Encapsulation of Ethylene Gas into Granular Cold-Water-Soluble Starch: Structure and Release Kinetics.

PubMed

Shi, Linfan; Fu, Xiong; Tan, Chin Ping; Huang, Qiang; Zhang, Bin

2017-03-15

Ethylene gas was introduced into granular cold-water-soluble (GCWS) starches using a solid encapsulation method. The morphological and structural properties of the novel inclusion complexes (ICs) were characterized using scanning electron microscopy, X-ray diffractometry, and Raman spectroscopy. The V-type single helix of GCWS starches was formed through controlled gelatinization and ethanol precipitation and was approved to host ethylene gas. The controlled release characteristics of ICs were also investigated at various temperature and relative humidity conditions. Avrami's equation was fitted to understand the release kinetics and showed that the release of ethylene from the ICs was accelerated by increasing temperature or RH and was decelerated by increased degree of amylose polymerization. The IC of Hylon-7 had the highest ethylene concentration (31.8%, w/w) among the five starches, and the IC of normal potato starch showed the best controlled release characteristics. As a renewable and inexpensive material, GCWS starch is a desirable solid encapsulation matrix with potential in agricultural and food applications.

Synthesization, Characterization, and in Vitro Evaluation of Cytotoxicity of Biomaterials Based on Halloysite Nanotubes.

PubMed

Sánchez-Fernández, Antonio; Peña-Parás, Laura; Vidaltamayo, Román; Cué-Sampedro, Rodrigo; Mendoza-Martínez, Ana; Zomosa-Signoret, Viviana C; Rivas-Estilla, Ana M; Riojas, Paulina

2014-12-04

Halloysite is an aluminosilicate clay that has been widely used for controlled drug delivery, immobilization of enzymes, and for the capture of circulating tumor cells (CTCs). Surface modification of halloysite by organosilanes has been explored to improve their properties. In this study halloysite clay nanotubes (HNTs) were functionalized by two different organosilanes: Trimethoxy(propyl)silane (TMPS), and Triethoxy(octyl)silane (EOS). Untreated and modified samples were characterized by scanning electron microscopy (SEM), X-ray diffractometry (XRD), thermogravimetrical analysis (TGA), and Fourier transform infrared spectroscopy (FTIR). Results showed a strong interaction of organosilanes with the chemical groups present in HNTs. Biocompatibility and cytotoxicity of these nanomaterials were determined using C6 rat glioblastoma cells. Our results indicate that prior to functionalization, HNTs show a high biocompatibility and low cytotoxicity. However, HNTs functionalized with EOS and TMPS showed high cytotoxicity by inducing apoptosis. These results allow the identification of potential applications in biomedical areas for HNTs.

Synthesization, Characterization, and in Vitro Evaluation of Cytotoxicity of Biomaterials Based on Halloysite Nanotubes

PubMed Central

Sánchez-Fernández, Antonio; Peña-Parás, Laura; Vidaltamayo, Román; Cué-Sampedro, Rodrigo; Mendoza-Martínez, Ana; Zomosa-Signoret, Viviana C.; Rivas-Estilla, Ana M.; Riojas, Paulina

2014-01-01

Halloysite is an aluminosilicate clay that has been widely used for controlled drug delivery, immobilization of enzymes, and for the capture of circulating tumor cells (CTCs). Surface modification of halloysite by organosilanes has been explored to improve their properties. In this study halloysite clay nanotubes (HNTs) were functionalized by two different organosilanes: Trimethoxy(propyl)silane (TMPS), and Triethoxy(octyl)silane (EOS). Untreated and modified samples were characterized by scanning electron microscopy (SEM), X-ray diffractometry (XRD), thermogravimetrical analysis (TGA), and Fourier transform infrared spectroscopy (FTIR). Results showed a strong interaction of organosilanes with the chemical groups present in HNTs. Biocompatibility and cytotoxicity of these nanomaterials were determined using C6 rat glioblastoma cells. Our results indicate that prior to functionalization, HNTs show a high biocompatibility and low cytotoxicity. However, HNTs functionalized with EOS and TMPS showed high cytotoxicity by inducing apoptosis. These results allow the identification of potential applications in biomedical areas for HNTs. PMID:28788274

In situ removal of arsenic from groundwater by using permeable reactive barriers of organic matter/limestone/zero-valent iron mixtures.

PubMed

Gibert, O; de Pablo, J; Cortina, J-L; Ayora, C

2010-08-01

In this study, two mixtures of municipal compost, limestone and, optionally, zero-valent iron were assessed in two column experiments on acid mine treatment. The effluent solution was systematically analysed throughout the experiment and precipitates from both columns were withdrawn for scanning electron microscopy, energy-dispersive X-ray spectroscopy, X-ray diffractometry analysis and, from the column containing zero-valent iron, solid digestion and sequential extraction analysis. The results showed that waters were cleaned of arsenic, metals and acidity, but chemical and morphological analysis suggested that metal removal was not due predominantly to biogenic sulphide generation but to pH increase, i.e. metal (oxy)hydroxide and carbonate precipitation. Retained arsenic and metal removal were clearly associated to co-precipitation with and/or sorption on iron and aluminum (oxy)hydroxides. An improvement on the arsenic removal efficiency was achieved when the filling mixture contained zero-valent iron. Values of arsenic concentrations were then always below 10 microg/L.

Characterization of the bioactive and mechanical behavior of dental ceramic/sol-gel derived bioactive glass mixtures.

PubMed

Abbasi, Zahra; Bahrololoum, Mohammad E; Bagheri, Rafat; Shariat, Mohammad H

2016-02-01

Dental ceramics can be modified by bioactive glasses in order to develop apatite layer on their surface. One of the benefits of such modification is to prolong the lifetime of the fixed dental prosthesis by preventing the formation of secondary caries. Dental ceramic/sol-gel derived bioactive glass mixture is one of the options for this modification. In the current study, mixtures of dental ceramic/bioactive glass with different compositions were successfully produced. To evaluate their bioactive behavior, prepared samples were immersed in a simulated body fluid at various time intervals. The prepared and soaked specimens were characterized using Fourier transform infrared spectroscopy, X-ray diffractometry and scanning electron microscopy. Since bioactive glasses have deleterious effects on the mechanical properties of dental ceramics, 3-point bending tests were used to evaluate the flexural strength, flexural strain, tangent modulus of elasticity and Weibull modulus of the specimens in order to find the optimal relationship between mechanical and bioactive properties. Copyright © 2015 Elsevier Ltd. All rights reserved.

Composite HPMC and sodium alginate based buccal formulations for nicotine replacement therapy.

PubMed

Okeke, Obinna C; Boateng, Joshua S

2016-10-01

Smoking cessation is of current topical interest due to the significant negative health and economic impact in many countries. This study aimed to develop buccal films and wafers comprising HPMC and sodium alginate (SA) for potential use in nicotine replacement therapy via the buccal mucosa, as a cheap but effective alternative to currently used nicotine patch and chewing gum. The formulations were characterised using texture analyser (tensile and hardness, mucoadhesion), scanning electron microscopy, X-ray diffractometry, attenuated total reflection-Fourier transform infrared (ATR-FTIR), differential scanning calorimetry (DSC) and swelling capacity. Drug loaded films and wafers were characterised for content uniformity (HPLC) whilst the drug loaded wafers only were further characterised for in vitro drug dissolution. SA modified and improved the functional properties of HPMC at optimum ratio of HPMC: SA of 1.25: 0.75. Generally, both films and wafers (blank and drug loaded) were amorphous in nature which impacted on swelling and mucoadhesive performance. HPMC-SA composite wafers showed a porous internal morphology with higher mucoadhesion, swelling index and drug loading capacity compared to the HPMC-SA composite films which were non-porous. The study demonstrates the potential use of composite HPMC-SA wafers in the buccal delivery nicotine. Copyright © 2016 Elsevier B.V. All rights reserved.

Comparative evaluation of ibuprofen/beta-cyclodextrin complexes obtained by supercritical carbon dioxide and other conventional methods.

PubMed

Hussein, Khaled; Türk, Michael; Wahl, Martin A

2007-03-01

The preparation of drug/cyclodextrin complexes is a suitable method to improve the dissolution of poor soluble drugs. The efficacy of the Controlled Particle Deposition (CPD) as a new developed method to prepare these complexes in a single stage process using supercritical carbon dioxide is therefore compared with other conventional methods. Ibuprofen/beta-cyclodextrin complexes were prepared with different techniques and characterized using FTIR-ATR spectroscopy, powder X-ray diffractometry (PXRD), differential scanning calorimetry (DSC) and scanning electron microscopy (SEM). In addition, the influences of the processing technique on the drug content (HPLC) and the dissolution behavior were studied. Employing the CPD-process resulted in a drug content of 2.8+/-0.22 wt.% in the carrier. The material obtained by CPD showed an improved dissolution rate of ibuprofen at pH 5 compared with the pure drug and its physical mixture with beta-cyclodextrin. In addition CPD material displays the highest dissolution (93.5+/- 2.89% after 75 min) compared to material obtained by co-precipitation (61.3 +/-0.52%) or freeze-drying (90.6 +/-2.54%). This study presents the CPD-technique as a well suitable method to prepare a drug/beta-cyclodextrin complex with improved drug dissolution compared to the pure drug and materials obtained by other methods.

Formation of Al3Ti/Mg composite by powder metallurgy of Mg-Al-Ti system.

PubMed

Yang, Zi R; Qi Wang, Shu; Cui, Xiang H; Zhao, Yu T; Gao, Ming J; Wei, Min X

2008-07-01

An in situ titanium trialuminide (Al 3 Ti)-particle-reinforced magnesium matrix composite has been successfully fabricated by the powder metallurgy of a Mg-Al-Ti system. The reaction processes and formation mechanism for synthesizing the composite were studied by differential scanning calorimetry (DSC), x-ray diffractometry (XRD), scanning electron microscopy (SEM) and energy-dispersive x-ray spectroscopy (EDS). Al 3 Ti particles are found to be synthesized in situ in the Mg alloy matrix. During the reaction sintering of the Mg-Al-Ti system, Al 3 Ti particles are formed through the reaction of liquid Al with as-dissolved Ti around the Ti particles. The formed intermetallic particles accumulate at the original sites of the Ti particles. As sintering time increases, the accumulated intermetallic particles disperse and reach a relatively homogeneous distribution in the matrix. It is found that the reaction process of the Mg-Al-Ti system is almost the same as that of the Al-Ti system. Mg also acts as a catalytic agent and a diluent in the reactions and shifts the reactions of Al and Ti to lower temperatures. An additional amount of Al is required for eliminating residual Ti and solid-solution strengthening of the Mg matrix.

Enhanced Photocatalytic Activity toward Organic Pollutants Degradation and Mechanism Insight of Novel CQDs/Bi₂O₂CO₃ Composite.

PubMed

Zhang, Zisheng; Lin, Shuanglong; Li, Xingang; Li, Hong; Zhang, Tong; Cui, Wenquan

2018-05-15

Novel carbon quantum dots (CQDs) modified with Bi₂O₂CO₃ (CQDs/Bi₂O₂CO₃) were prepared using a simple dynamic-adsorption precipitation method. X-ray diffractometry (XRD), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDX), and scanning electron microscopy (SEM) were used to test the material composition, structure, and band structures of the as-prepared samples. Methylene blue (MB) and colorless phenol, as target organic pollutants, were used to evaluate the photocatalytic performance of the CQDs/Bi₂O₂CO₃ hybrid materials under visible light irradiation. Experimental investigation shows that 2⁻5 nm CQDs were uniformly decorated on the surface of Bi₂O₂CO₃; CQDs/Bi₂O₂CO₃ possess an efficient photocatalytic performance, and the organic matter removal rate of methylene blue and phenol can reach up to 94.45% and 61.46% respectively, within 2 h. In addition, the degradation analysis of phenol by high performance liquid chromatography (HPLC) proved that there are no other impurities in the degradation process. Photoelectrochemical testing proved that the introduction of CQDs (electron acceptor) effectively suppresses the recombination of e - -h⁺, and promotes charge transfer. Quenching experiments and electron spin resonance (ESR) suggested that ·OH, h⁺, and ·O₂ - were involved in the photocatalytic degradation process. These results suggested that the up-conversion function of CQDs could improve the electron transfer and light absorption ability of photocatalysts and ·O₂ - formation. Furthermore, the up-conversion function of CQDs would help maintain photocatalytic stability. Finally, the photocatalytic degradation mechanism was proposed according to the above experimental result.

Green synthesis palladium nanoparticles mediated by white tea (Camellia sinensis) extract with antioxidant, antibacterial, and antiproliferative activities toward the human leukemia (MOLT-4) cell line.

PubMed

Azizi, Susan; Mahdavi Shahri, Mahnaz; Rahman, Heshu Sulaiman; Rahim, Raha Abdul; Rasedee, Abdullah; Mohamad, Rosfarizan

2017-01-01

Among nanoparticles used for medical applications, palladium nanoparticles (PdNPs) are among the least investigated. This study was undertaken to develop PdNPs by green synthesis using white tea (W.tea; Camellia sinensis ) extract to produce the Pd@W.tea NPs. The Pd@W.tea NPs were characterized by UV-vis spectroscopy and X-ray diffractometry, and evaluated with transmission electron microscopy (TEM) and scanning electron microscopy (SEM). The Pd@W.tea NPs were spherical (size 6-18 nm) and contained phenols and flavonoids acquired from the W.tea extract. Pd@W.tea NPs has good 1-diphenyl-2-picrylhydrazyl (DPPH), OH, and NO-scavenging properties as well as antibacterial effects toward Staphylococcus epidermidis and Escherichia coli . MTT assay showed that Pd@W.tea NPs (IC 50 =0.006 μM) were more antiproliferative toward the human leukemia (MOLT-4) cells than the W.tea extract (IC 50 =0.894 μM), doxorubicin (IC 50 =2.133 μM), or cisplatin (IC 50 =0.013 μM), whereas they were relatively innocuous for normal human fibroblast (HDF-a) cells. The anticancer cell effects of Pd@W.tea NPs are mediated through the induction of apoptosis and G2/M cell-cycle arrest.

Atomic Layer Deposition of Rhenium Disulfide.

PubMed

Hämäläinen, Jani; Mattinen, Miika; Mizohata, Kenichiro; Meinander, Kristoffer; Vehkamäki, Marko; Räisänen, Jyrki; Ritala, Mikko; Leskelä, Markku

2018-06-01

2D materials research is advancing rapidly as various new "beyond graphene" materials are fabricated, their properties studied, and materials tested in various applications. Rhenium disulfide is one of the 2D transition metal dichalcogenides that has recently shown to possess extraordinary properties such as that it is not limited by the strict monolayer thickness requirements. The unique inherent decoupling of monolayers in ReS 2 combined with a direct bandgap and highly anisotropic properties makes ReS 2 one of the most interesting 2D materials for a plethora of applications. Here, a highly controllable and precise atomic layer deposition (ALD) technique is applied to deposit ReS 2 thin films. Film growth is demonstrated on large area (5 cm × 5 cm) substrates at moderate deposition temperatures between 120 and 500 °C, and the films are extensively characterized using field emission scanning electron microscopy/energy-dispersive X-ray spectroscopy, X-ray diffractometry using grazing incidence, atomic force microscopy, focused ion beam/transmission electron microscopy, X-ray photoelectron spectroscopy, and time-of-flight elastic recoil detection analysis techniques. The developed ReS 2 ALD process highlights the potential of the material for applications beyond planar structure architectures. The ALD process also offers a route to an upgrade to an industrial scale. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A Novel Microcharacterization Technique in the Measurement of Strain and Orientation Gradient in Advanced Materials

NASA Technical Reports Server (NTRS)

Garmestai, H.; Harris, K.; Lourenco, L.

1997-01-01

Representation of morphology and evolution of the microstructure during processing and their relation to properties requires proper experimental techniques. Residual strains, lattice distortion, and texture (micro-texture) at the interface and the matrix of a layered structure or a functionally gradient material and their variation are among parameters important in materials characterization but hard to measure with present experimental techniques. Current techniques available to measure changes in interred material parameters (residual stress, micro-texture, microplasticity) produce results which are either qualitative or unreliable. This problem becomes even more complicated in the case of a temperature variation. These parameters affect many of the mechanical properties of advanced materials including stress-strain relation, ductility, creep, and fatigue. A review of some novel experimental techniques using recent advances in electron microscopy is presented here to measure internal stress, (micro)texture, interracial strength and (sub)grain formation and realignment. Two of these techniques are combined in the chamber of an Environmental Scanning Electron Microscope to measure strain and orientation gradients in advanced materials. These techniques which include Backscattered Kikuchi Diffractometry (BKD) and Microscopic Strain Field Analysis are used to characterize metallic and intermetallic matrix composites and superplastic materials. These techniques are compared with the more conventional x-ray diffraction and indentation techniques.

Enhanced UV-visible response of bismuth subcarbonate nanowires for degradation of xanthate and photocatalytic reaction mechanism.

PubMed

Cui, Kuixin; He, Yuehui; Jin, Shengming

2016-04-01

(BiO)2CO3 nanowires were prepared by simple hydrothermal treatment of commercial Bi2O3 powders and characterized by X-ray diffractometry, scanning electron microscopy, transmission electron microscopy (TEM), high-resolution TEM, and X-ray photoelectron spectroscopy (XPS). The photocatalytic activity of (BiO)2CO3 nanowires was studied through degradation of sodium isopropyl xanthate. Photocatalytic experimental results indicated that the as-prepared (BiO)2CO3 nanowires show high photocatalytic efficiency. Photocatalytic activity increased after two cycles. Time-dependent UV-vis spectra demonstrated that the final degradation products included isopropyl alcohol and carbon disulfide. UV-vis diffuse reflection spectra showed that the band gap of the as-prepared (BiO)2CO3 nanowires and recycled (BiO)2CO3 nanowires were 2.75 eV and 1.15 eV, respectively. XPS results indicated that formation of Bi2S3@(BiO)2CO3 core-shell nanowires occurred after recycled photodegradation of isopropyl xanthate owing to existence of two types of Bi configurations in the recycled (BiO)2CO3 nanowires. A probable degradation mechanism of isopropyl xanthate was also proposed. Copyright © 2016 Elsevier Ltd. All rights reserved.

Microstructures and Mechanical Properties of Co-Cr Dental Alloys Fabricated by Three CAD/CAM-Based Processing Techniques

PubMed Central

Kim, Hae Ri; Jang, Seong-Ho; Kim, Young Kyung; Son, Jun Sik; Min, Bong Ki; Kim, Kyo-Han; Kwon, Tae-Yub

2016-01-01

The microstructures and mechanical properties of cobalt-chromium (Co-Cr) alloys produced by three CAD/CAM-based processing techniques were investigated in comparison with those produced by the traditional casting technique. Four groups of disc- (microstructures) or dumbbell- (mechanical properties) specimens made of Co-Cr alloys were prepared using casting (CS), milling (ML), selective laser melting (SLM), and milling/post-sintering (ML/PS). For each technique, the corresponding commercial alloy material was used. The microstructures of the specimens were evaluated via X-ray diffractometry, optical and scanning electron microscopy with energy-dispersive X-ray spectroscopy, and electron backscattered diffraction pattern analysis. The mechanical properties were evaluated using a tensile test according to ISO 22674 (n = 6). The microstructure of the alloys was strongly influenced by the manufacturing processes. Overall, the SLM group showed superior mechanical properties, the ML/PS group being nearly comparable. The mechanical properties of the ML group were inferior to those of the CS group. The microstructures and mechanical properties of Co-Cr alloys were greatly dependent on the manufacturing technique as well as the chemical composition. The SLM and ML/PS techniques may be considered promising alternatives to the Co-Cr alloy casting process. PMID:28773718

Direct observation of the ferroelectric polarization in the layered perovskite Bi{sub 4}Ti{sub 3}O{sub 12}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Urushihara, Daisuke; Asaka, Toru, E-mail: asaka.toru@nitech.ac.jp; Frontier Research Institute for Materials Science, Nagoya Institute of Technology, Nagoya 466-8555

We investigated the crystal structure and ferroelectric domains of Bi{sub 4}Ti{sub 3}O{sub 12} (BTO) by means of transmission electron microscopy (TEM) and single-crystal X-ray diffractometry. From the extinction rule, we determined that the space group in the ferroelectric phase of BTO is P1a1 rather than B2cb and B1a1 which have been proposed previously. We successfully refined the crystal structure based on the space group P1a1. The 180° and 90° ferroelectric domain structures were observed by the [001]-zone dark-field TEM imaging. In the 180° domain structure, we determined that one component of the polarization vector is parallel to the a-axis. Anmore » annular bright-field scanning transmission electron microscopy (ABF-STEM) was performed for the direct observation of the crystal structures. The ABF-STEM images displayed the contrasts with respect to every atomic position in spite of the highly distorted structure of BTO. We could evaluate the tilting and distortion of the [TiO{sub 6}] octahedra relatively. Therefore, we directly observed the ferroelectric displacements of Bi and Ti ions.« less

Organic-Inorganic Hydrophobic Nanocomposite Film with a Core-Shell Structure

PubMed Central

Liu, Peng; Chen, Ying; Yu, Zhiwu

2016-01-01

A method to prepare novel organic-inorganic hydrophobic nanocomposite films was proposed by a site-specific polymerization process. The inorganic part, the core of the nanocomposite, is a ternary SiO2–Al2O3–TiO2 nanoparticles, which is grafted with methacryloxy propyl trimethoxyl silane (KH570), and wrapped by fluoride and siloxane polymers. The synthesized samples are characterized by transmission electron microscopy (TEM), Fourier transform infrared (FTIR) spectrscopy, X-ray diffractometry (XRD), contact angle meter (CA), and scanning electron microscope (SEM). The results indicate that the novel organic-inorganic hydrophobic nanocomposite with a core-shell structure was synthesized successfully. XRD analysis reveals the nanocomposite film has an amorphous structure, and FTIR analysis indicates the nanoparticles react with a silane coupling agent (methacryloxy propyl trimethoxyl silane KH570). Interestingly, the morphology of the nanoparticle film is influenced by the composition of the core. Further, comparing with the film synthesized by silica nanoparticles, the film formed from SiO2–Al2O3–TiO2 nanoparticles has higher hydrophobic performance, i.e., the contact angle is greater than 101.7°. In addition, the TEM analysis reveals that the crystal structure of the particles can be changed at high temperatures. PMID:28774141

Ergonomic Synthesis Suitable for Industrial Production of Silver-Festooned Zinc Oxide Nanorods

NASA Astrophysics Data System (ADS)

Khan, G. R.; Khan, R. A.

2015-07-01

For maximizing productivity, minimizing cost, time-boxing process and optimizing human effort, a single-step, cost-effective, ultra-fast and environmentally benign synthesis suitable for industrial production of nanocrystalline ZnO, and Ag-doped ZnO has been reported in this paper. The synthesis based on microwave-supported aqueous solution method used zinc acetate dehydrate and silver nitrate as precursors for fabrication of nanorods. The synthesized products were characterized by X-ray diffractometry (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman spectroscopy and UV-Vis-NIR spectroscopy. The undoped and Ag-doped ZnO nanorods crystallized in a hexagonal wurtzite structure having spindle-like morphology. The blue shift occurred at absorption edge of Ag-doped ZnO around 260 nm compared to 365 nm of bulk ZnO. The red shift occurred at Raman peak site of 434 cm-1 compared to characteristic wurtzite phase peak of ZnO (437 cm-1). The bandgap energies were found to be 3.10 eV, 3.11 eV and 3.18 eV for undoped, 1% Ag-doped, and 3% Ag-doped ZnO samples, respectively. The TEM results provided average particle sizes of 17 nm, 15 nm and 13 nm for undoped, and 1% and 3% Ag-doped ZnO samples, respectively.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen Long; Department of Chemistry, Huangshan University, Huangshan 245041; Post-Doctoral Scientific Research Workstation, HuangShan NOVEL Co. Ltd, Huangshan 245061

In this paper, biomimetic synthesis of aragonite superstructures using a low molecular weight organic-hexamethylenetetramine (HMT) as an additive in the presence of CO{sub 2} supplied by an ammonium carbonate ((NH{sub 4}){sub 2}CO{sub 3}) diffusion method at room temperature was studied. The products were characterized by scanning or transmission electron microscopy, Fourier transform infrared (FT-IR) spectroscopy, X-ray powder diffractometry, and selected area electron diffraction. The results showed the aragonite superstructures especially dumbbell-flower-like ones were obtained. The formation process of calcium carbonate (CaCO{sub 3}) in HMT aqueous solution was investigated, suggesting that the products transformed from calcite to vaterite primarily, and thenmore » changed into a mixture of aragonite and calcite with an increase of reaction time. The formation mechanism of CaCO{sub 3} in HMT solution was also discussed, revealing that aragonite might be controlled by HMT molecules and NH{sub 4}{sup +} ions together. - Graphical abstract: The well-defined aragonite hierarchical superstructures are formed using hexamethylenetetramine in aqueous solution. Highlights: > Aragonite superstructures are formed with hexamethylenetetramine at about 25 deg. C. > Dumbbell-flower-like aragonite produces when hexamethylenetetramine/Ca{sup 2+}=10:1. > CaCO{sub 3} formation in hexamethylenetetramine solution violates the Ostwald ripening. > Hexamethylenetetramine and NH{sub 4}{sup +} might control the growth of aragonite together.« less

Structural, Optical and Electrical Properties of ITO Thin Films

NASA Astrophysics Data System (ADS)

Sofi, A. H.; Shah, M. A.; Asokan, K.

2018-02-01

Transparent and conductive thin films of indium tin oxide were fabricated on glass substrates by the thermal evaporation technique. Tin doped indium ingots with low tin content were evaporated in vacuum (1.33 × 10-7 kpa) followed by an oxidation for 15 min in the atmosphere in the temperature range of 600-700°C. The structure and phase purity, surface morphology, optical and electrical properties of thin films were studied by x-ray diffractometry and Raman spectroscopy, scanning electron microcopy and atomic force microscopy, UV-visible spectrometry and Hall measurements in the van der Pauw configuration. The x-ray diffraction study showed the formation of the cubical phase of polycrystalline thin films. The morphological analysis showed the formation of ginger like structures and the energy dispersive x-ray spectrum confirmed the presence of indium (In), tin (Sn) and oxygen (O) elements. Hall measurements confirmed n-type conductivity of films with low electrical resistivity ( ρ) ˜ 10-3 Ω cm and high carrier concentration ( n) ˜ 1020 cm-3. For prevalent scattering mechanisms in the films, experimental data was analyzed by calculating a mean free path ( L) using a highly degenerate electron gas model. Furthermore, to investigate the performance of the deposited films as a transparent conductive material, the optical figure of merit was obtained for all the samples.

Characterization and evaluation of miconazole salts and cocrystals for improved physicochemical properties.

PubMed

Tsutsumi, Shunichirou; Iida, Motoo; Tada, Norio; Kojima, Takashi; Ikeda, Yukihiro; Moriwaki, Toshiya; Higashi, Kenjirou; Moribe, Kunikazu; Yamamoto, Keiji

2011-12-15

Miconazole salts and cocrystals were studied to improve the physicochemical properties of miconazole. Maleate, hemifumarate, and hemisuccinate were prepared and characterized by powder X-ray diffractometry, differential scanning calorimetry, and single crystal X-ray diffractometry. The intrinsic dissolution rate and stability of each miconazole crystal form were compared to those of freebase and nitrate to evaluate the optimal crystal form. Crystal structure analysis indicated that maleate was a salt formed by proton transfer from the acid to the imidazole group of miconazole. Hemifumarate and hemisuccinate were determined to be cocrystals formed by hydrogen bonding between the acids and the base in their crystal lattices. Intrinsic dissolution tests showed that the formation of salts and cocrystals improved the dissolution rate of miconazole. Stability tests of preliminary formulations prepared with each crystal form indicated that maleate and hemifumarate were unstable at 80°C and generated a specific degraded product, i.e., a Michael adduct, between miconazole and the acids. Hemisuccinate had a superior intrinsic dissolution rate and stability, and is thus considered a promising crystal form of miconazole. Copyright © 2011 Elsevier B.V. All rights reserved.

Tri-functional Fe2O3-encased Ag-doped ZnO nanoframework: magnetically retrievable antimicrobial photocatalyst

NASA Astrophysics Data System (ADS)

Karunakaran, Chockalingam; Vinayagamoorthy, Pazhamalai

2016-11-01

Fe2O3-encased ZnO nanoframework was obtained by hydrothermal method and was doped with Ag through photoreduction process. Energy dispersive x-ray spectroscopy, transmission electron microscopy (TEM), high resolution TEM, selected area electron diffractometry, x-ray diffractometry and Raman spectroscopy were employed for the structural characterization of the synthesized material. While the charge transfer resistance of the prepared nanomaterial is larger than those of Fe2O3 and ZnO the coercivity of the nanocomposite is less than that of hydrothermally obtained Fe2O3 nanostructures. Although Fe2O3/Ag-ZnO exhibits weak visible light absorption its band gap energy does not differ from that of ZnO. The photoluminescence of the fabricated nanoframework is similar to that of ZnO. The radiative recombination of charge carriers is slightly slower in Fe2O3/Ag-ZnO than in ZnO. The synthesized Fe2O3-encased Ag-doped ZnO, under UV A light, exhibits sustainable photocatalytic activity to degrade dye and is magnetically recoverable. Also, the Fe2O3/Ag-ZnO nanocomposite disinfects bacteria effectively in absence of direct illumination.

Effect of hydrodynamics and surface roughness on the electrochemical behaviour of carbon steel in CSG produced water

NASA Astrophysics Data System (ADS)

Eyu, Gaius Debi; Will, Geoffrey; Dekkers, Willem; MacLeod, Jennifer

2015-12-01

The influence of fluid flow, surface roughness and immersion time on the electrochemical behaviour of carbon steel in coal seam gas produced water under static and hydrodynamic conditions has been studied. The disc electrode surface morphology before and after the corrosion test was characterized using scanning electron microscopy (SEM). The corrosion product was examined using X-ray photoelectron spectroscopy (XPS) and X-ray diffractometry (XRD).The results show that the anodic current density increased with increasing surface roughness and consequently a decrease in corrosion surface resistance. Under dynamic flow conditions, the corrosion rate increased with increasing rotating speed due to the high mass transfer coefficient and formation of non-protective akaganeite β-FeO(OH) and goethite α-FeO(OH) corrosion scale at the electrode surface. The corrosion rate was lowest at 0 rpm. The corrosion rate decreased in both static and dynamic conditions with increasing immersion time. The decrease in corrosion rate is attributed to the deposition of corrosion products on the electrode surface. SEM results revealed that the rougher surface exhibited a great tendency toward pitting corrosion.

Capacity fading of LiAlyNi1-x-yCoxO2 cathode for lithium-ion batteries during accelerated calendar and cycle life tests (effect of depth of discharge in charge-discharge cycling on the suppression of the micro-crack generation of LiAlyNi1-x-yCoxO2 particle)

NASA Astrophysics Data System (ADS)

Watanabe, Shoichiro; Kinoshita, Masahiro; Hosokawa, Takashi; Morigaki, Kenichi; Nakura, Kensuke

2014-08-01

Cycle performance of a LiAl0.10Ni0.76Co0.14O2 (NCA) cathode/graphite cell closely depended on the range of depth of discharge in charge-discharge processes (ΔDOD). When ΔDOD was 10-70%, cycle performance at 25 °C was maintained even at 60 °C. Deterioration phenomena were analyzed by electrochemical method, X-ray photoelectron spectroscopy (XPS), X-ray diffractometry (XRD), and micro-cracks in NCA particles were analyzed with cross-sectional views by scanning electron microscopy (SEM). Many micro-cracks were observed only after a 0-100% DOD region cycle test. Cycle tests in several restricted ΔDOD conditions showed that the deterioration was closely related to not the upper and lower limits of DOD or operation voltage but the width of ΔDOD.

Synthesis and Characterization of Cobalt Substituted Zinc Ferrite Nanoparticles by Microwave Combustion Method.

PubMed

Sundararajan, M; Kennedy, L John; Vijaya, J Judith

2015-09-01

Pure and cobalt doped zinc ferrites were prepared by microwave combustion method using L-arginine as a fuel. The prepared samples were characterized by various instrumental techniques such as X-ray powder diffractometry, high resolution scanning electron microscopy (HR-SEM), energy dispersive X-ray analysis, Fourier transformed infrared (FT-IR) spectroscopy, photoluminescence spectroscopy and UV-Visible diffuse reflectance spectroscopy. Vibrating sample magnetometry at room temperature was recorded to study the magnetic behavior of the samples. X-ray analysis confirmed the formation of zinc ferrites normal spinel-type structure with an average crystallite sizes in the range, 25.69 nm to 35.68 nm. The lattice parameters decreased as cobalt fraction was increased. The HR-SEM images showed nanoparticles are agglomerated. The estimated band gap energy value was found to decrease with an increase in cobalt content (1.87 to 1.62 eV). Broad visible emissions are observed in the photoluminescence spectra. A gradual increase in the coercivity and saturation magnetization (M(s)) were noted at relatively higher cobalt doping fractions.

From nicotinate-containing layered double hydroxides (LDHs) to NAD coenzyme-LDH nanocomposites - Syntheses and structural characterization by various spectroscopic methods

NASA Astrophysics Data System (ADS)

Muráth, Szabolcs; Dudás, Csilla; Kukovecz, Ákos; Kónya, Zoltán; Sipos, Pál; Pálinkó, István

2017-07-01

The syntheses of nicotinate anion- and NAD coenzyme-layered double hydroxide (LDH) composites were performed with the aim of having the organic component among the layers. In-house prepared CaAl-LDHs were the host materials. Intercalation was attempted by direct ion exchange or by the dehydration-rehydration method applying aqueous solvent mixtures (containing ethanol, propanol, acetone, N,N-dimethylformamide). For structural characterization, beside X-ray diffractometry, X-ray photoelectron and IR spectroscopies, transmission and scanning electron microscopies as well as energy-dispersive X-ray analysis were used. Molecular modelling served for the visualization of the arrangements of the intercalated ions among the layers of the LDH samples. Although not all the intercalation methods and solvent mixtures led to intercalated composite materials, successful ones could be identified. The combination of spectroscopic methods helped in proposing sensible spatial arrangements for the intercalated anions. The NAD-CaAl-LDH composite proved to be an active catalyst in the oxidation of hydroquinone to 1,4-bezoquinoe in the presence of H2O2.

Characterization and electrochemical properties of Ni(Si)/Ni5Si2 multiphase coatings prepared by HVOF spraying

NASA Astrophysics Data System (ADS)

Verdian, M. M.; Raeissi, K.; Salehi, M.

2012-11-01

Ni(Si)/Ni5Si2 powders were produced by mechanical alloying (MA) of Ni-25 at.% Si powder mixture. Then, the as-milled powders were sprayed onto copper substrate using high velocity oxy-fuel (HVOF) process. The phase composition and microstructure of the coatings were examined by X-ray diffractometry and scanning electron microscopy. Polarization tests and electrochemical impedance spectroscopy (EIS) measurements were also employed to study corrosion performance of the coatings in 3.5% NaCl solution. The results showed that although single phase Ni3Si was formed during annealing of Ni(Si)/Ni5Si2 powders, but, only Ni(Si) and Ni5Si2 are present in HVOF coatings and no new phase has been formed during spraying. The coatings had microhardness up to 746 HV0.05. Further investigations showed the corrosion performance of multiphase coatings in 3.5% NaCl solution was better than that of copper substrate. The phase transitions during MA, HVOF and annealing processes were discussed in association with Ni-Si phase diagram and nature of each process.

Review of Research Work on Ti-BASED Composite Coatings

NASA Astrophysics Data System (ADS)

Gabbitas, Brian; Salman, Asma; Zhang, Deliang; Cao, Peng

The service life of industrial components is limited predominantly by Chemical corrosion/mechanical wear. The project is concerned with the investigation of the capability of Ti(Al,O)/Al2O3 coatings to improve the service life of tool steel (H13) used for dies in aluminium high pressure die casting. This paper gives a general review on the research work conducted at the University of Waikato on producing and evaluating the titanium/alumina based composite coatings. The powder feedstocks for making the composite coatings were produced by high energy mechanical milling of a mixture of Al and TiO2 powders in two different molar ratios followed by a thermal reaction process. The feedstocks were then thermally sprayed using a high velocity air-fuel (HVAF) technique on H13 steel substrates to produce a Ti(Al,O)/Al2O3 composite coatings. The performance of the coating was assessed in terms of thermal shock resistance and reaction kinetics with molten aluminium. The composite powders and coatings were characterized using scanning electron microscopy (SEM), optical microscopy and X-ray diffractometry (XRD).

Novel Solid Encapsulation of Ethylene Gas Using Amorphous α-Cyclodextrin and the Release Characteristics.

PubMed

Ho, Binh T; Bhandari, Bhesh R

2016-05-04

This research investigated the encapsulation of ethylene gas into amorphous α-cyclodextrins (α-CDs) at low (LM) and high (HM) moisture contents at 1.0-1.5 MPa for 24-120 h and its controlled release characteristics at 11.2-52.9% relative humidity (RH) for 1-168 h. The inclusion complexes (ICs) were characterized using X-ray diffractometry (XRD), nuclear magnetic resonance spectroscopy (CP-MAS (13)C NMR), and scanning electron microscopy (SEM). Ethylene concentrations in the ICs were from 0.45 to 0.87 mol of ethylene/mol CD and from 0.42 to 0.54 mol of ethylene/mol CD for LM and HM α-CDs, respectively. Ethylene gas released from the encapsulated powder at higher rates with increasing RH. An analysis of release kinetics using Avrami's equation showed that the LM and HM amorphous α-CDs were not associated with significant differences in release constant k and parameter n for any given RH condition. NMR spectra showed the presence of the characteristic carbon-carbon double bond of ethylene gas in the encapsulated α-CD powder.

Photocatalytic degradation of an azo textile dye (C.I. Reactive Red 195 (3BF)) in aqueous solution over copper cobaltite nanocomposite coated on glass by Doctor Blade method

NASA Astrophysics Data System (ADS)

Habibi, Mohammad Hossein; Rezvani, Zoya

2015-08-01

The degradation of C.I. Reactive Red 195 (3BF) in aqueous solution using copper cobaltite nanocomposite coated on glass by Doctor Blade method was studied. Structural, optical and morphological properties of nanocomposite coatings were characterized by X-ray powder diffractometry (XRD), diffuse reflectance spectroscopy (DRS) and field emission scanning electron microscopy (FESEM). The nanoparticles exhibit a particle size of 31 nm, showing a good nanoscale crystalline morphology. The photocatalytic activity of copper cobaltite nanocomposite coated on glass was studied by performing the photocatalytic degradation of 3BF at different irradiation time. The effect of irradiation time on the degradation of 3BF was studied and the results showed that more than 85% of the 3BF was degraded in 45 min of irradiation. The pseudo-first-order kinetic models were used and the rate constants were evaluated with pseudo first order rate constants of 4.10 × 10-2 min-1. The main advantage of the photocatalyst coated on glass overcomes the difficulties in separation and recycle of photocatalyst suspensions.

Enhancement of the dissolution rate and bioavailability of fenofibrate by a melt-adsorption method using supercritical carbon dioxide

PubMed Central

Cha, Kwang-Ho; Cho, Kyung-Jin; Kim, Min-Soo; Kim, Jeong-Soo; Park, Hee Jun; Park, Junsung; Cho, Wonkyung; Park, Jeong-Sook; Hwang, Sung-Joo

2012-01-01

Background: The aim of this study was to enhance the bioavailability of fenofibrate, a poorly water-soluble drug, using a melt-adsorption method with supercritical CO2. Methods: Fenofibrate was loaded onto Neusilin® UFL2 at different weight ratios of fenofibrate to Neusilin UFL2 by melt-adsorption using supercritical CO2. For comparison, fenofibrate-loaded Neusilin UFL2 was prepared by solvent evaporation and hot melt-adsorption methods. The fenofibrate formulations prepared were characterized by differential scanning calorimetry, powder x-ray diffractometry, specific surface area, pore size distribution, scanning electron microscopy, and energy-dispersive x-ray spectrometry. In vitro dissolution and in vivo bioavailability were also investigated. Results: Fenofibrate was distributed into the pores of Neusilin UFL2 and showed reduced crystal formation following adsorption. Supercritical CO2 facilitated the introduction of fenofibrate into the pores of Neusilin UFL2. Compared with raw fenofibrate, fenofibrate from the prepared powders showed a significantly increased dissolution rate and better bioavailability. In particular, the area under the drug concentration-time curve and maximal serum concentration of the powders prepared using supercritical CO2 were 4.62-fold and 4.52-fold greater than the corresponding values for raw fenofibrate. Conclusion: The results of this study highlight the usefulness of the melt-adsorption method using supercritical CO2 for improving the bioavailability of fenofibrate. PMID:23118538

In vitro/in vivo evaluation of an optimized fast dissolving oral film containing olanzapine co-amorphous dispersion with selected carboxylic acids.

PubMed

Maher, Eman Magdy; Ali, Ahmed Mahmoud Abdelhaleem; Salem, Heba Farouk; Abdelrahman, Ahmed Abdelbary

2016-10-01

Improvement of water solubility, dissolution rate, oral bioavailability, and reduction of first pass metabolism of OL (OL), were the aims of this research. Co-amorphization of OL carboxylic acid dispersions at various molar ratios was carried out using rapid solvent evaporation. Characterization of the dispersions was performed using differential scanning calorimetry (DSC), Fourier transform infrared spectrometry (FTIR), X-ray diffractometry (XRD), and scanning electron microscopy (SEM). Dispersions with highest equilibrium solubility were formulated as fast dissolving oral films. Modeling and optimization of film formation were undertaken using artificial neural networks (ANNs). The results indicated co-amorphization of OL-ascorbic acid through H-bonding. The co-amorphous dispersions at 1:2 molar ratio showed more than 600-fold increase in solubility of OL. The model optimized fast dissolving film prepared from the dispersion was physically and chemically stable, demonstrated short disintegration time (8.5 s), fast dissolution (97% in 10 min) and optimum tensile strength (4.9 N/cm 2 ). The results of in vivo data indicated high bioavailability (144 ng h/mL) and maximum plasma concentration (14.2 ng/mL) compared with the marketed references. Therefore, the optimized co-amorphous OL-ascorbic acid fast dissolving film could be a valuable solution for enhancing the physicochemical and pharmacokinetic properties of OL.

Xylitol as a potential co-crystal co-former for enhancing dissolution rate of felodipine: preparation and evaluation of sublingual tablets.

PubMed

Arafa, Mona F; El-Gizawy, Sanaa A; Osman, Mohamed A; El Maghraby, Gamal M

2018-06-01

Dissolution enhancement is a promising strategy for improving drug bioavailability. Co-crystallization of drugs with inert material can help in this direction. The benefit will become even greater if the inert material can form co-crystal while maintaining its main function as excipient. Accordingly, the objective of the current study was to investigate xylitol as a potential co-crystal co-former for felodipine with the goal of preparing felodipine sublingual tablets. Co-crystallization was achieved by wet co-grinding of the crystals deposited from methanolic solutions containing felodipine with increasing molar ratios of xylitol (1:1, 1:2 and 1:3). The developed co-crystals were characterized using Fourier transform infrared spectroscopy (FTIR), X-ray diffractometry (XRD), differential scanning calorimetry (DSC) and scanning electron microscopy (SEM) before monitoring drug dissolution. These results reflected the development of new crystalline species depending on the relative proportions of felodipine and xylitol with complete co-crystallization of felodipine being achieved in the presence of double its molar concentration of xylitol. This co-crystal formulation was compressed into sublingual tablet with ultrashort disintegration time with subsequent fast dissolution. Co-crystal formation was associated with enhanced dissolution with the optimum formulation producing the fastest dissolution rate. In conclusion, xylitol can be considered as a co-crystal co-former for enhanced dissolution rate of drugs.

Spray-Freeze Drying: a Suitable Method for Aerosol Delivery of Antibodies in the Presence of Trehalose and Cyclodextrins.

PubMed

Pouya, Maryam Amini; Daneshmand, Behnaz; Aghababaie, Shabnam; Faghihi, Homa; Vatanara, Alireza

2018-05-08

We aimed to prepare spray-freeze-dried powder of IgG considering physicochemical stability and aerodynamic aspects. Spray-freeze drying (SFD) exposes proteins to various stresses which should be compensated by suitable stabilizers. The competence of cyclodextrins (CDs), namely beta-cyclodextrin (βCD) and hydroxypropyl βCD (HPβCD), at very low concentrations, was investigated in the presence of separate mannitol- and trehalose-based formulations. Spray-freeze-dried preparations were quantified in terms of monomer recovery and conformation by size exclusion chromatography (SEC-HPLC) and Fourier transform infrared (FTIR) spectroscopy, respectively. Differential scanning calorimetry (DSC) and X-ray diffractometry (XRD) were employed to identify the thermal characteristics of powders. Particle morphology was visualized by scanning electron microscopy (SEM). Aerodynamic behavior of powders was checked through an Anderson cascade impactor (ACI). Although all formulations protected antibody from aggregation during the SFD process (aggregation < 1%), mannitol-containing ones failed upon the storage (19.54% in the worst case). Trehalose-HPβCD incomparably preserved the formulation with fine particle fraction (FPF) of 51.29%. Crystallization of mannitol resulted in IgG destabilization upon storage. Although employed concentration of CDs is too low (less than 50:1 molar ratio to protein), they successfully served as stabilizing agents in SFD with perfect improvement in aerosol functionality. Graphical Abstract ᅟ.

A comparative study of the effect of spray drying and hot-melt extrusion on the properties of amorphous solid dispersions containing felodipine.

PubMed

Mahmah, Osama; Tabbakh, Rami; Kelly, Adrian; Paradkar, Anant

2014-02-01

To compare the properties of solid dispersions of felodipine for oral bioavailability enhancement using two different polymers, polyvinylpyrrolidone (PVP) and hydroxypropyl methylcellulose acetate succinate (HPMCAS), by hot-melt extrusion (HME) and spray drying. Felodipine solid dispersions were prepared by HME and spray drying techniques. PVP and HPMCAS were used as polymer matrices at different drug : polymer ratios (1 : 1, 1 : 2 and 1 : 3). Detailed characterization was performed using differential scanning calorimetry, powder X-ray diffractometry, scanning electron microscopy and in-vitro dissolution testing. Dissolution profiles were evaluated in the presence of sodium dodecyl sulphate. Stability of different solid dispersions was studied under accelerated conditions (40°C/75% RH) over 8 weeks. Spray-dried formulations were found to release felodipine faster than melt extruded formulations for both polymer matrices. Solid dispersions containing HMPCAS exhibited higher drug release rates and better wettability than those produced with a PVP matrix. No significant differences in stability were observed except with HPMCAS at a 1 : 1 ratio, where crystallization was detected in spray-dried formulations. Solid dispersions of felodipine produced by spray drying exhibited more rapid drug release than corresponding melt extruded formulations, although in some cases improved stability was observed for melt extruded formulations. © 2013 Royal Pharmaceutical Society.

Development and evaluation of paclitaxel nanoparticles using a quality-by-design approach.

PubMed

Yerlikaya, Firat; Ozgen, Aysegul; Vural, Imran; Guven, Olgun; Karaagaoglu, Ergun; Khan, Mansoor A; Capan, Yilmaz

2013-10-01

The aims of this study were to develop and characterize paclitaxel nanoparticles, to identify and control critical sources of variability in the process, and to understand the impact of formulation and process parameters on the critical quality attributes (CQAs) using a quality-by-design (QbD) approach. For this, a risk assessment study was performed with various formulation and process parameters to determine their impact on CQAs of nanoparticles, which were determined to be average particle size, zeta potential, and encapsulation efficiency. Potential risk factors were identified using an Ishikawa diagram and screened by Plackett-Burman design and finally nanoparticles were optimized using Box-Behnken design. The optimized formulation was further characterized by Fourier transform infrared spectroscopy, X-ray diffractometry, differential scanning calorimetry, scanning electron microscopy, atomic force microscopy, and gas chromatography. It was observed that paclitaxel transformed from crystalline state to amorphous state while totally encapsulating into the nanoparticles. The nanoparticles were spherical, smooth, and homogenous with no dichloromethane residue. In vitro cytotoxicity test showed that the developed nanoparticles are more efficient than free paclitaxel in terms of antitumor activity (more than 25%). In conclusion, this study demonstrated that understanding formulation and process parameters with the philosophy of QbD is useful for the optimization of complex drug delivery systems. © 2013 Wiley Periodicals, Inc. and the American Pharmacists Association.

Supercritical antisolvent precipitation of nimesulide: preliminary experiments.

PubMed

Moneghini, M; Perissutti, B; Vecchione, F; Kikic, I; Alessi, P; Cortesi, A; Princivalle, F

2007-07-01

The purpose of this preliminary study was to investigate the physico-chemical properties of nimesulide precipitated by continuous supercritical antisolvent (SAS) from different organic solvents like acetone, chloroform and dichloromethane at 40 degrees C and 80, 85 and 88 bar, respectively. Scanning electron microscopy, differential scanning calorimetry, X-Ray diffractometry and in vitro dissolution tests were employed to study how the technological process and the solvent nature would affect the final product. SAS-processed nimesulide particles showed dramatic morphological change in crystalline structure if compared to native nimesulide, resulting in needle and thin rods shaped crystals. The solid state analysis showed that using chloroform or dichloromethane as a solvent the drug solid state remained substantially unchanged, whilst if using acetone the applied method caused a transition from the starting form I to the meta-stable form II. So as to identify which process was responsible for this result, nimesulide was further precipitated from the same solvent by conventional evaporation method (RV-sample). On the basis of this comparison, the solvent was found to be responsible for the re-organization into the different polymorphic form and the potential of the SAS process to produce micronic needle shaped particles, with an enhanced dissolution rate if compared to the to the pure drug, was ascertained. Finally, the stability of the nimesulide form II, checked by DSC analysis, was ruled on over a period of 15 months.

Multilayer encapsulated mesoporous silica nanospheres as an oral sustained drug delivery system for the poorly water-soluble drug felodipine.

PubMed

Hu, Liang; Sun, Hongrui; Zhao, Qinfu; Han, Ning; Bai, Ling; Wang, Ying; Jiang, Tongying; Wang, Siling

2015-02-01

We used a combination of mesoporous silica nanospheres (MSN) and layer-by-layer (LBL) self-assembly technology to establish a new oral sustained drug delivery system for the poorly water-soluble drug felodipine. Firstly, the model drug was loaded into MSN, and then the loaded MSN were repeatedly encapsulated by chitosan (CHI) and acacia (ACA) via LBL self-assembly method. The structural features of the samples were studied using scanning electron microscopy (SEM), transmission electron microscopy (TEM) and nitrogen adsorption. The encapsulating process was monitored by zeta-potential and surface tension measurements. The physical state of the drug in the samples was characterized by differential scanning calorimetry (DSC) and X-ray diffractometry (XRD). The influence of the multilayer with different number of layers on the drug release rate was studied using thermal gravimetric analysis (TGA) and surface tension measurement. The swelling effect and the structure changes of the multilayer were investigated to explore the relationship between the drug release behavior and the state of the multilayer under different pH conditions. The stability and mucosa adhesive ability of the prepared nanoparticles were also explored. After multilayer coating, the drug release rate was effectively controlled. The differences in drug release behavior under different pH conditions could be attributed to the different states of the multilayer. And the nanoparticles possessed good stability and strong mucosa adhesive ability. We believe that this combination offers a simple strategy for regulating the release rate of poorly water-soluble drugs and extends the pharmaceutical applications of inorganic materials and polymers. Copyright © 2014 Elsevier B.V. All rights reserved.

Synthesis of LiFePO4/C composites based on natural iron stone using a sol gel method

NASA Astrophysics Data System (ADS)

Angela, Riyan; Islam, Humaatul; Sari, Vamellia; Latif, Chaironi; Zainuri, Mochamad; Pratapa, Suminar

2017-01-01

Synthesis of LiFePO4/C composites has been carried out using a sol gel method. The Fe precursor was made from a natural iron stone of Tanah Laut, South Kalimantan, while the other raw materials were commercial Li2CO3 powder and NH4H2PO4 powder with HCl and water as solvents. Citric acid was used as the carbon source in the synthesis. This study used a molar ratio of 1:1:2 for Li:Fe:P with variation of added citric acid of 1.5 and 2.5 g. The solutions were dried in air at 100°C. The dried powders were characterized using DSC-TGA and then calcined at 600 and 700°C under argon environment for 10 hours. The calcined powders were characterized by X-ray diffractometry (XRD), scanning electron microscopy-energy dispersive x-ray (SEM-EDX), and LCR meter. It was found that the samples contained LiFePO4 as the dominant phase and LiFeP2O7 and Fe2O3 as secondary phases. The analysis showed that the addition of citric acid influenced the electronic conductivity of the composites. A Rietveld relative weight fraction of up to 94.7% was achieved in the synthesis at temperature 600°C. The LFP/C sample exhibited electronic conductivity of 4.56×10-3 Scm-1 which was six times of that of the pure LFP.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Zheng; Li, Zhilin; Institute of Carbon Fibers and Composites, Beijing University of Chemical Technology, Beijing 100029

Graphical abstract: The MWCNT/Ni-B catalyst has been successfully prepared by an electroless deposition process. The Ni-B nanoparticles on the supporter are amorphous and are well-distributed. The catalytic conversion towards hydrogenation of styrene shows excellent catalytic activity of the obtained materials. Highlights: Black-Right-Pointing-Pointer A two-step treatment of MWCNTs enabled the homogeneous growth of Ni-B nanoparticles. Black-Right-Pointing-Pointer Ni-B nanoparticles were amorphous with an average size of 60 nm. Black-Right-Pointing-Pointer There were electron transfer between Ni and B. Black-Right-Pointing-Pointer The catalyst had excellent catalytic activity towards hydrogenation of styrene. -- Abstract: Nickel-boron (Ni-B) nanoparticles supported on multi-walled carbon nanotubes (MWCNTs) were successfully synthesizedmore » through an electroless deposition process using the plating bath with sodium borohydride as a reducing agent. The structural and morphological analyses using field-emission scanning electron microscopy, X-ray diffractometry and high-resolution transmission electron microscopy have shown that the Ni-B nanoparticles deposited on the sidewalls of MWCNTs are fine spheres comprised of amorphous structure with the morphologically unique fine-structure like flowers, and homogenously dispersed with a narrow particle size distribution centered at around 60 nm diameter. The catalytic activity of MWCNT/Ni-B nanoparticles was evaluated with respect to hydrogenation of styrene. The hydrogenation catalyzed by MWCNT-supported Ni-B nanoparticles has been found to make styrene selectively converted into ethylbenzene. The highest conversion reaches 99.8% under proper reaction conditions, which demonstrates the high catalytic activity of MWCNT/Ni-B nanoparticles.« less

Use of glancing angle X-ray powder diffractometry to depth-profile phase transformations during dissolution of indomethacin and theophylline tablets.

PubMed

Debnath, Smita; Predecki, Paul; Suryanarayanan, Raj

2004-01-01

The purpose of this study was (i) to develop glancing angle x-ray powder diffractometry (XRD) as a method for profiling phase transformations as a function of tablet depth; and (ii) to apply this technique to (a) study indomethacin crystallization during dissolution of partially amorphous indomethacin tablets and to (b) profile anhydrate --> hydrate transformations during dissolution of theophylline tablets. The intrinsic dissolution rates of indomethacin and theophylline were determined after different pharmaceutical processing steps. Phase transformations during dissolution were evaluated by various techniques. Transformation in the bulk and on the tablet surface was characterized by conventional XRD and scanning electron microscopy, respectively. Glancing angle XRD enabled us to profile these transformations as a function of depth from the tablet surface. Pharmaceutical processing resulted in a decrease in crystallinity of both indomethacin and theophylline. When placed in contact with the dissolution medium, while indomethacin recrystallized, theophylline anhydrate rapidly converted to theophylline monohydrate. Due to intimate contact with the dissolution medium, drug transformation occurred to a greater extent at or near the tablet surface. Glancing angle XRD enabled us to depth profile the extent of phase transformations as a function of the distance from the tablet surface. The processed sample (both indomethacin and theophylline) transformed more rapidly than did the corresponding unprocessed drug. Several challenges associated with the glancing angle technique, that is, the effects of sorbed water, phase transformations during the experimental timescale, and the influence of phase transformation on penetration depth, were addressed. Increased solubility, and consequently dissolution rate, is one of the potential advantages of metastable phases. This advantage is negated if, during dissolution, the metastable to stable transformation rate > dissolution rate. Glancing angle XRD enabled us to quantify and thereby profile phase transformations as a function of compact depth. The technique has potential utility in monitoring surface reactions, both chemical decomposition and physical transformations, in pharmaceutical systems.

Synthesis and characterization of zeolites prepared from industrial fly ash.

PubMed

Franus, Wojciech; Wdowin, Magdalena; Franus, Małgorzata

2014-09-01

In this paper, we present the possibility of using fly ash to produce synthetic zeolites. The synthesis class F fly ash from the Stalowa Wola SA heat and power plant was subjected to 24 h hydrothermal reaction with sodium hydroxide. Depending on the reaction conditions, three types of synthetic zeolites were formed: Na-X (20 g fly ash, 0.5 dm(3) of 3 mol · dm(-3) NaOH, 75 °C), Na-P1 (20 g fly ash, 0.5 dm(3) of 3 mol · dm(-3) NaOH, 95 °C), and sodalite (20 g fly ash, 0.8 dm(3) of 5 mol · dm(-3) NaOH + 0.4 dm(3) of 3 mol · dm(-3) NaCl, 95 °C). As synthesized materials were characterized to obtain mineral composition (X-ray diffractometry, Scanning electron microscopy-energy dispersive spectrometry), adsorption properties (Brunauer-Emmett-Teller surface area, N2 isotherm adsorption/desorption), and ion exchange capacity. The most effective reaction for zeolite preparation was when sodalite was formed and the quantitative content of zeolite from X-ray diffractometry was 90 wt%, compared with 70 wt% for the Na-X and 75 wt% for the Na-P1. Residues from each synthesis reaction were the following: mullite, quartz, and the remains of amorphous aluminosilicate glass. The best zeolitic material as characterized by highest specific surface area was Na-X at almost 166 m(2) · g(-1), while for the Na-P1 and sodalite it was 71 and 33 m(2) · g(-1), respectively. The ion exchange capacity decreased in the following order: Na-X at 1.8 meq · g(-1), Na-P1 at 0.72 meq · g(-1), and sodalite at 0.56 meq · g(-1). The resulting zeolites are competitive for commercially available materials and are used as ion exchangers in industrial wastewater and soil decontamination.

Rapid disintegrating tablets of simvastatin dispersions in polyoxyethylene–polypropylene block copolymer for maximized disintegration and dissolution

PubMed Central

Balata, Gehan F; Zidan, Ahmad S; Abourehab, Mohamad AS; Essa, Ebtessam A

2016-01-01

The objective of this research was to improve the dissolution of simvastatin and to incorporate it in rapid disintegrating tablets (RDTs) with an optimized disintegration and dissolution characteristics. Polyoxyethylene–polypropylene block copolymer (poloxamer 188) was employed as a hydrophilic carrier to prepare simvastatin solid dispersions (SDs). Fourier transform infrared spectroscopy, differential scanning calorimetry (DSC) and X-ray diffractometry were employed to understand the interaction between the drug and the carrier in the solid state. The results obtained from Fourier transform infrared spectroscopy showed absence of any chemical interaction between the drug and poloxamer. The results of differential scanning calorimetry and X-ray diffractometry confirmed the conversion of simvastatin to distorted crystalline state. The SD of 1:2 w/w drug to carrier ratio showed the highest dissolution; hence, it was incorporated in RDT formulations using a 32 full factorial design and response surface methodology. The initial assessments of RDTs demonstrated an acceptable flow, hardness, and friability to indicate good mechanical strength. The interaction and Pareto charts indicated that percentage of croscarmellose sodium incorporated was the most important factor affecting the disintegration time and dissolution parameter followed by the hardness value and their interaction effect. Compression force showed a superior influence to increase RDT’s porosity and to fasten disintegration rather than swelling action by croscarmellose sodium. On the other hand, croscarmellose sodium was most important for the initial simvastatin release. The results suggest the potential use of poloxamer 188-based SD in RDT for the oral delivery of poor water-soluble antihyperlipidemic drug, simvastatin. PMID:27757012

Synthesis of core-shell structured FAU/SBA-15 composite molecular sieves and their performance in catalytic cracking of polystyrene

NASA Astrophysics Data System (ADS)

Du, Jinlong; Shi, Chunwei; Wu, Wenyuan; Bian, Xue; Chen, Ping; Cui, Qingzhu; Cui, Zhixuan

2017-12-01

Composite molecular sieves, FAU/SBA-15, having core-shell structure were synthesized. The synthesized composite sieves were characterized by X-ray diffractometry (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDS), pyrolysis fourier transform infrared (Py-FTIR) spectroscopy, temperature programmed desorption spectra (NH3-TPD), UV Raman spectroscopy, nuclear magnetic resonance (NMR) and other techniques. XRD, SEM, TEM, N2 adsorption-desorption, mass spectrometry, NMR and EDS results showed that the composite molecular sieve contained two pore channels. Py-FTIR results showed that the addition of HY molecular sieves improved the acidity of the composite zeolite. The crystallization mechanism during the growth of FAU/SBA-15 shell was deduced from the influence of crystallization time on the synthesis of FAU/SBA-15 core-shell structured composite molecular sieve. HY dissociated partially in H2SO4 solution, and consisted of secondary structural units. This framework structure was more stable than its presence in the isolated form on the same ring or in the absence of Al. Thus it played a guiding role and connected with SBA-15 closely through the Si-O bond. This resulted in the gradual covering of the exterior surface of FAU phase by SBA-15 molecular sieves. The presence of SBA-15 restricted the formation of the other high mass components and increased the selectivity towards ethylbenzene.

Soft chemistry routes for synthesis of rare earth oxide nanoparticles with well defined morphological and structural characteristics

NASA Astrophysics Data System (ADS)

Mancic, L.; Marinkovic, B. A.; Marinkovic, K.; Dramicanin, M.; Milosevic, O.

2011-11-01

Phosphors of (Y0.75Gd0.25)2O3:Eu3+ (5 at.%) have been prepared through soft chemistry routes. Conversion of the starting nitrates mixture into oxide is performed through two approaches: (a) hydrothermal treatment (HT) at 200 °C/3 h of an ammonium hydrogen carbonate precipitated mixture and (b) by thermally decomposition of pure nitrate precursor solution at 900 °C in dispersed phase (aerosol) within a tubular flow reactor by spray pyrolysis process (SP). The powders are additionally thermally treated at different temperatures: 600, 1000, and 1100 °C for either 3 or 12 h. HT—derived particles present exclusively one-dimensional morphology (nanorods) up to the temperatures of 600 °C, while the leaf-like particles start to grow afterward. SP—derived particles maintain their spherical shape up to the temperatures of 1100 °C. These submicron sized spheres were actually composed of randomly aggregated nanoparticles. All powders exhibits cubic Ia- 3 structure (Y0.75Gd0.25)2O3:Eu and have improved optical characteristics due to their nanocrystalline nature. The detailed study of the influence of structural and morphological powder characteristics on their emission properties is performed based on the results of X-ray powder diffractometry, scanning electron microscopy, X-ray energy dispersive spectroscopy, transmission electron microscopy, and photoluminescence measurements.

Sonochemical synthesis of highly crystalline photocatalyst for industrial applications.

PubMed

Noman, Muhammad Tayyab; Militky, Jiri; Wiener, Jakub; Saskova, Jana; Ashraf, Muhammad Azeem; Jamshaid, Hafsa; Azeem, Musaddaq

2018-02-01

Highly photo active pure anatase form of TiO 2 nanoparticles with average particle size 4nm have been successfully synthesized by ultrasonic acoustic method (UAM). The effects of process variables i.e. precursors concentration and sonication time were investigated based on central composite design and response surface methodology. The characteristics of the resulting nanoparticles (RNP) were analyzed by scanning electron microscopy, dynamic light scattering, transmission electron microscopy, X-ray diffractometry and Raman spectroscopy. Photocatalytic experiments were performed with methylene blue dye which is considered as model organic pollutant in textile industry. A comparative analysis between the RNP and commercially available Degussa P25 for photocatalytic performance against dye removal efficiency was performed. The rapid removal of methylene blue in case of RNP indicates their higher photocatalytic activity than P25. Maximum dye removal efficiency 98.45% was achieved with optimal conditions i.e. TTIP conc. 10mL, EG conc. 4mL and sonication time 1h. Interestingly, no significant difference was found in the photocatalytic performance of RNP after calcination. Moreover, self-cleaning efficiency of RNP deposited on cotton was evaluated in RGB color space. The obtained results indicate the significant impact of ultrasonic irradiations on the photocatalytic performance of pure anatase form than any other hybrid type of TiO 2 nanoparticles. Copyright © 2017 Elsevier B.V. All rights reserved.

Spectroellipsometric studies of sol-gel derived Sr0.6Ba0.4Nb2O6 films

NASA Astrophysics Data System (ADS)

Ho, Melanie M. T.; Tang, T. B.; Mak, C. L.; Pang, G. K. H.; Chan, K. Y.; Wong, K. H.

2006-10-01

Sr0.6Ba0.4Nb2O6 (SBN) films have been fabricated on (001)Si substrates by a sol-gel technique. The annealing process was carried out in air at various temperatures ranging from 200to700°C. Studies using x-ray diffractometry, high resolution transmission electron microscopy, and scanning electron microscopy showed that polycrystalline films, with a grain size of about 100nm, were obtained only for annealing temperatures ⩾600°C. The optical properties of these sol-gel derived SBN films were studied by spectroscopic ellipsometry (SE). In the analysis of the measured SE spectra, a triple-layer Lorentz model has been developed and used to deduce the optical properties of the SBN films. Our systematic SE measurements revealed that the refractive indices of the SBN films increase with the annealing temperature. This increase is more pronounced at around the crystallization temperature, i.e., between 500 and 600°C. The extinction coefficients of the films also exhibit a similar trend, showing a zero value for amorphous films and larger values for films annealed at above 600°C. Our results demonstrate that while crystallization helps to raise the refractive index of the film due to film densification, it also promotes scattering by grain boundary, resulting in a larger extinction coefficient.

Morphology and structure features of ZnAl{sub 2}O{sub 4} spinel nanoparticles prepared by matrix-isolation-assisted calcination

DOE Office of Scientific and Technical Information (OSTI.GOV)

Du, Xuelian, E-mail: xueliandu@126.com; Li, Liqiang; Zhang, Wenxing

2015-01-15

Graphical abstract: The substrate ZnO as the isolation medium is effective in preventing the sintering and agglomeration of ZnAl{sub 2}O{sub 4} nanoparticles, and it also prevents their contamination. High purity, well-dispersed, and single-crystal ZnAl{sub 2}O{sub 4} nanoparticles with 3.72 eV band gap were obtained. - Abstract: Well-dispersed ZnAl{sub 2}O{sub 4} spinel nanoparticles with an average crystalline size of 25.7 nm were synthesized successfully and easily by polymer-network and matrix-isolation-assisted calcination. The product microstructure and features were investigated by X-ray diffractometry, thermogravimetric and differential thermal analysis, Fourier transform-infrared spectroscopy, N{sub 2} adsorption–desorption isotherms, and energy dispersive X-ray spectra. The morphology andmore » optical performance of the as-prepared ZnAl{sub 2}O{sub 4} nanoparticles were characterized by scanning electron microscope, transmission electron microscopy, and photoluminescence spectrometer. Experimental results indicate that excess ZnO acted as the isolation medium is effective in preventing the sintering and agglomeration of ZnAl{sub 2}O{sub 4} nanoparticles, and it also prevents their contamination. Then, high purity and well-dispersed ZnAl{sub 2}O{sub 4} nanoparticles with single-crystal structure were obtained.« less

Water treatment with exceptional virus inactivation using activated carbon modified with silver (Ag) and copper oxide (CuO) nanoparticles.

PubMed

Shimabuku, Quelen Letícia; Arakawa, Flávia Sayuri; Fernandes Silva, Marcela; Ferri Coldebella, Priscila; Ueda-Nakamura, Tânia; Fagundes-Klen, Márcia Regina; Bergamasco, Rosangela

2017-08-01

Continuous flow experiments (450 mL min -1 ) were performed in household filter in order to investigate the removal and/or inactivation of T4 bacteriophage, using granular activated carbon (GAC) modified with silver and/or copper oxide nanoparticles at different concentrations. GAC and modified GAC were characterized by X-ray diffractometry, specific surface area, pore size and volume, pore average diameter, scanning electron microscopy, transmission electron microscopy, zeta potential and atomic absorption spectroscopy. The antiviral activity of the produced porous media was evaluated by passing suspensions of T4 bacteriophage (∼10 5  UFP/mL) through filters. The filtered water was analyzed for the presence of the bacteriophage and the release of silver and copper oxide. The porous media containing silver and copper oxide nanoparticles showed high inactivation capacity, even reaching reductions higher than 3 log. GAC6 (GAC/Ag0.5%Cu1.0%) was effective in the bacteriophage inactivation, reaching 5.53 log reduction. The levels of silver and copper released in filtered water were below the recommended limits (100 ppb for silver and 1000 ppb for copper) in drinking water. From this study, it is possible to conclude that activated carbon modified with silver and copper oxide nanoparticles can be used as a filter for virus removal in the treatment of drinking water.

Development and characterization of lecithin stabilized glibenclamide nanocrystals for enhanced solubility and drug delivery.

PubMed

Kumar, B Sajeev; Saraswathi, R; Kumar, K Venkates; Jha, S K; Venkates, D P; Dhanaraj, S A

2014-05-01

Novel LNCs (lipid nanocrystals) were developed with an aim to improve the solubility, stability and targeting efficiency of the model drug glibenclamide (GLB). PEG 20000, Tween 80 and soybean lecithin were used as polymer, surfactant and complexing agent, respectively. GLB nanocrystals (NCs) were prepared by precipitation process and complexed using hot and cold melt technique. The LNCs were evaluated by drug loading, saturation solubility (SL), optical clarity, in vitro dissolution, solid state characterization, in vivo and stability analysis. LNCs exhibited a threefold increase in SL and a higher dissolution rate than GLB. The percentage dissolution efficiency was found to decrease with increase in PEG 20000. The average particle size was in the range of 155-842 nm and zeta potential values tend to increase after complexation. X-ray powder diffractometry and differential scanning calorimetry results proved the crystallinity prevailed in the samples. Spherical shaped particles (<1000 nm) with a lipid coat on the surface were observed in scanning electron microscopy analysis. Fourier transform infrared results proved the absence of interaction between drug and polymer and stability study findings proved that LNCs were stable. In vivo study findings showed a decrease in drug concentration to pancreas in male Wistar rats. It can be concluded that LNCs are could offer enhanced solubility, dissolution rate and stability for poorly water soluble drugs. The targeting efficiency of LNCs was decreased and further membrane permeability studies ought to be carried out.

Fabrication, characterization and in vitro evaluation of silibinin nanoparticles: an attempt to enhance its oral bioavailability

PubMed Central

Sahibzada, Muhammad Umar Khayam; Sadiq, Abdul; Khan, Shahzeb; Faidah, Hani S; Naseemullah; Khurram, Muhammad; Amin, Muhammad Usman; Haseeb, Abdul

2017-01-01

Background Silibinin has gained in importance in the past few decades as a hepatoprotector and is used widely as oral therapy for toxic liver damage, liver cirrhosis, and chronic inflammatory liver diseases, as well as for the treatment of different types of cancers. Unfortunately, it has low aqueous solubility and inadequate dissolution, which results in low oral bioavailability. Materials and methods In this study, nanoparticles (NPs) of silibinin, which is a hydrophobic drug, were manufactured using two cost-effective methods. Antisolvent precipitation with a syringe pump (APSP) and evaporative precipitation of nanosuspension (EPN) were used. The prepared NPs were characterized using different analytical techniques such as scanning electron microscopy (SEM), fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), and X-ray powder diffractometry (XRD) and were sifted for their bioavailability through in vitro dissolution and solubility studies. Moreover, the prepared NPs were evaluated for antimicrobial activity against a battery of bacteria and yeast. Results DSC and XRD studies indicated that the prepared NPs were amorphous in nature, with more solubility and dissolution compared to the crystalline form of this drug. NPs prepared through the EPN method had better results than those prepared using the APSP method. Antimicrobial activities of the NPs were improved compared to the unprocessed drugs, while having comparable activities to standard antimicrobial drugs. Conclusion Results indicate that the NPs have significantly increased solubility, dissolution rate, and antimicrobial activities due to the conversion of crystalline structure into amorphous form. PMID:28553075

Naltrexone-loaded poly[La-(Glc-Leu)] polymeric microspheres for the treatment of alcohol dependence: in vitro characterization and in vivo biocompatibility assessment.

PubMed

Pagar, Kunal P; Vavia, Pradeep R

2014-06-01

The poly[La-(Glc-Leu)] copolymer was applied in the present investigation as polymeric carrier to fabricate naltrexone (NTX)-loaded poly[La-(Glc-Leu)] microspheres in the single emulsion solvent evaporation technique for the long-term treatment of alcohol dependence. Newly synthesized poly[La-(Glc-Leu)] copolymer exhibited diminished crystallanity, good biocompatibility and favorable biodegradability to be explored for drug delivery application. Scanning Electron Microscopy study revealed smooth and spherical-shaped NTX-loaded polymeric microspheres with a mean size of 10-90 µm. Influence of various decisive formulation variables such as amount of polymer, stabilizer concentration, homogenization speed, homogenization time, drug loading and organic-to-aqueous phase ratio on particle size, and entrapment efficiency was studied. Differential scanning calorimeter and X-ray diffractometry study confirmed the drug entrapment within polymer matrix into the microsphere environment. In vitro drug release showed the sustained drug release of formulation for the period of 28 d giving biphasic release pattern. Histological examination of NTX-loaded poly[La-(Glc-Leu)] microspheres injected intramuscularly into the thigh muscle of Wistar rats showed minimal inflammatory reaction, demonstrating that NTX-loaded microspheres were biocompatible. Insignificant increase in the serum creatine phosphokinase level (p < 0.05) as compared with the normal value revealed good muscle compatibility of the poly[La-(Glc-Leu)] microsphere system. Biocompatible nature and sustained drug-release action of poly[La-(Glc-Leu)] microspheres may have potential application in depot therapy.

Amorphous Sulfadoxine: A Physical Stability and Crystallization Kinetics Study.

PubMed

Aucamp, Marique; Milne, Marnus; Liebenberg, Wilna

2016-10-01

Poor aqueous solubility of drugs and the improvement thereof has always been a challenge for the pharmaceutical industry. With this, one of the focuses of the pharmaceutical research scientist involves investigating possible metastable forms of a given drug to be incorporated into solid dosage forms. The rationale being, the improved solubility offered by the metastable solid-state forms of drugs. Solubility remains a major challenge for formulation scientists, especially with antimicrobial agents where the emergence of resistance is directly dependent on the concentration and duration of the parasite exposed to the drug. Sulfadoxine-pyrimethamine combination therapies are still the recommended treatments for uncomplicated Plasmodium falciparum malaria. The aim of this study was to prepare an amorphous form of sulfadoxine and to investigate the stability and recrystallization behavior thereof. The amorphous form was prepared by the well-known quench cooling of the melt. The physico-chemical properties and stability of amorphous sulfadoxine were studied using hot-stage microscopy (HSM), scanning electron microscopy (SEM), x-ray powder diffractometry (XRPD), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), as well as microcalorimetry. The recrystallization kinetics were studied isothermally by applying the Johnson-Mehl-Avrami model and non-isothermally by applying the Kissinger model. The physical stabilization of the amorphous form was investigated using physical mixtures of amorphous sulfadoxine with polyvinylpyrrolidone-25 (PVP-25). It was proved that sulfadoxine is a good glass former with relative high physical stability; however, water acts as a strong plasticizer for amorphous sulfadoxine, detrimentally affecting the stability during exposure to high moisture conditions.

Solid-state characterization of mefenamic acid.

PubMed

Panchagnula, Ramesh; Sundaramurthy, Prakash; Pillai, Omathanu; Agrawal, Shrutidevi; Raj, Yasvanth Ashok

2004-04-01

The purpose of this study was to characterize mefenamic acid (MA) from commercial samples and samples crystallized from different solvents. Various techniques used for characterization included microscopy (hot stage microscopy, scanning electron microscopy), intrinsic dissolution rate, differential scanning calorimetry (DSC), Fourier transform infrared (FTIR) spectroscopy and powder X-ray diffractometry (pXRD). The commercial samples varied in their crystal habit, thermal behavior, and intrinsic dissolution rate. It was found that the commercial samples were polymorphic Form I, which converted to Form II on heating in a DSC pan. Similarly, compression in an intrinsic dissolution rate (IDR) press resulted in the conversion of Form I to Form II. On the other hand, the samples recrystallized from different solvents under varying conditions yielded different crystal habits. Stirring and degree of supersaturation significantly influenced the crystal habit in all the solvents used in the study. Samples crystallized from ethanol and tetrahydrofuran yielded Form I, which behaved similarly to the commercial samples (M1 and M3). Recrystallization from ethyl acetate at a fast cooling rate yielded Form I, which on melting crystallized to Form II. The form I crystallized from ethyl acetate by fast cooling converted partially to form II on storing at ambient conditions. Forms I and II of MA were enantiotropically related. The results demonstrate the variable material characteristics of the commercial samples of MA and the influence of the crystallizing conditions on the formation of the polymorphs. Copyright 2004 Wiley-Liss, Inc. and the American Pharmacists Association.

Chitosan based atorvastatin nanocrystals: effect of cationic charge on particle size, formulation stability, and in-vivo efficacy

PubMed Central

Kurakula, Mallesh; El-Helw, AM; Sobahi, Tariq R; Abdelaal, Magdy Y

2015-01-01

Cationic charged chitosan as stabilizer was evaluated in preparation of nanocrystals using probe sonication method. The influence of cationic charge densities of chitosan (low CSL, medium CSM, high CSH molecular weights) and Labrasol® in solubility enhancement and modifying the release was investigated, using atorvastatin (ATR) as poorly soluble model drug. Compared to CSM and CSH; low cationic charge of CSL acted as both electrostatic and steric stabilizer by significant size reduction to 394 nm with charge of 21.5 meV. Solubility of ATR-CSL increased to 60-fold relative to pure ATR and ATR-L. Nanocrystals were characterized for physiochemical properties. Scanning electron microscopy revealed scaffold-like structures with high surface area. X-ray powder diffractometry and differential scanning calorimetry revealed crystalline to slight amorphous state changes after cationic charge size reduction. Fourier transform-infrared spectra indicated no potent drug-excipient interactions. The enhanced dissolution profile of ATR-CSL indicates that sustained release was achieved compared with ATR-L and Lipitor®. Anti-hyperlipidemic performance was pH dependent where ATR-CSL exhibited 2.5-fold higher efficacy at pH 5 compared to pH 6 and Lipitor®. Stability studies indicated marked changes in size and charge for ATR-L compared to ATR-CSL exemplifying importance of the stabilizer. Therefore, nanocrystals developed with CSL as a stabilizer is a promising choice to enhance dissolution, stability, and in-vivo efficacy of major Biopharmaceutical Classification System II/IV drugs. PMID:25609947

Surface microstructure and high temperature corrosion resistance of arc-sprayed FeCrAl coating irradiated by high current pulsed electron beam

NASA Astrophysics Data System (ADS)

Hao, Shengzhi; Zhao, Limin; He, Dongyun

2013-10-01

The surface microstructure of arc-sprayed FeCrAl coating irradiated by high current pulsed electron beam (HCPEB) with long pulse duration of 200 μs was characterized by using optical microscopy, scanning electron microscopy and X-ray diffractometry. The distribution of chemical composition in modified surface layer was measured with electron probe micro-analyzer. The high temperature corrosion resistance of FeCrAl coating was tested in a saturated Na2SO4 and K2SO4 solution at 650 °C. After HCPEB irradiation, the coarse surface of arc-sprayed coating was changed as discrete bulged nodules with smooth and compact appearance. When using low energy density of 20 J/cm2, the surface modified layer was continuous entirely with an average melting depth of ˜30 μm. In the surface remelted layer, Fe and Cr elements gave a uniform distribution, while Al and O elements agglomerated particularly at the concave part between nodule structures to form α-Al2O3 phase. After high temperature corrosion tests, the FeCrAl coating treated with HCPEB of 20 J/cm2 remained a glossy surface with weight increment of ˜51 mg/cm2, decreased by 20% as compared to the initial sample. With the increasing energy density of HCPEB irradiation, the integrity of surface modified layer got segmented due to the formation of larger bulged nodules and cracks at the concave parts. For the HCPEB irradiation of 40 J/cm2, the high temperature corrosion resistance of FeCrAl coating was deteriorated drastically.

Single Crystal Diffractometry

NASA Astrophysics Data System (ADS)

Arndt, U. W.; Willis, B. T. M.

2009-06-01

Preface; Acknowledgements; Part I. Introduction; Part II. Diffraction Geometry; Part III. The Design of Diffractometers; Part IV. Detectors; Part V. Electronic Circuits; Part VI. The Production of the Primary Beam (X-rays); Part VII. The Production of the Primary Beam (Neutrons); Part VIII. The Background; Part IX. Systematic Errors in Measuring Relative Integrated Intensities; Part X. Procedure for Measuring Integrated Intensities; Part XI. Derivation and Accuracy of Structure Factors; Part XII. Computer Programs and On-line Control; Appendix; References; Index.

Biocompatibility of the micro-patterned NiTi surface produced by femtosecond laser

NASA Astrophysics Data System (ADS)

Liang, Chunyong; Wang, Hongshui; Yang, Jianjun; Li, Baoe; Yang, Yang; Li, Haipeng

2012-11-01

Biocompatibility of the micro-patterned NiTi surface produced by femtosecond laser (FSL) was studied in this work. The surface characteristics of the laser treated NiTi alloys were investigated by scanning electron microscopy (SEM), atom force microscopy (AFM), X-ray diffractometry (XRD) and X-ray photoelectron spectrum (XPS). The biocompatibility was evaluated by in vitro cell culture test. The results showed that, grooves, ripples, which covered by nanoparticles were formed on the sample surfaces, and the Ni/Ti ratio on the alloy surface increased with increasing laser energy. The crystal structure was not changed by laser treatment. However, the cell culture test proved that the micro-patterns induced by FSL were beneficial to improve the biocompatibility of NiTi alloys: the growth of osteoblasts oriented along the grooves, a large amount of synapses and filopodias were formed due to the ripples, holes and nanoparticles on the alloy surface, and the proliferation rate and alkaline phosphatase (ALP) content of cells were increased after FSL treatment. However, due to the toxicity of Ni ions on cell growth, the NiTi alloy surface should not be treated by laser fluence of more than 3.82 J/cm2 to obtain the ideal biocompatibility.

One-Step Synthesis of Silver Nanoparticles on Polydopamine-Coated Sericin/Polyvinyl Alcohol Composite Films for Potential Antimicrobial Applications.

PubMed

Cai, Rui; Tao, Gang; He, Huawei; Song, Kai; Zuo, Hua; Jiang, Wenchao; Wang, Yejing

2017-04-30

Silk sericin has great potential as a biomaterial for biomedical applications due to its good hydrophilicity, reactivity, and biodegradability. To develop multifunctional sericin materials for potential antibacterial application, a one-step synthesis method for preparing silver nanoparticles (AgNPs) modified on polydopamine-coated sericin/polyvinyl alcohol (PVA) composite films was developed. Polydopamine (PDA) acted as both metal ion chelating and reducing agent to synthesize AgNPs in situ on the sericin/PVA composite film. Scanning electron microscopy and energy dispersive spectroscopy analysis revealed that polydopamine could effectively facilitate the high-density growth of AgNPs as a 3-D matrix. X-ray diffractometry studies suggested the synthesized AgNPs formed good face-centered cubic crystalline structures. Contact angle measurement and mechanical test indicated AgNPs modified PDA-sericin/PVA composite film had good hydrophilicity and mechanical property. The bacterial growth curve and inhibition zone assays showed the AgNPs modified PDA-sericin/PVA composite film had long-term antibacterial activities. This work develops a new method for the preparation of AgNPs modified PDA-sericin/PVA film with good hydrophilicity, mechanical performance and antibacterial activities for the potential antimicrobial application in biomedicine.

Molecular inclusion complex of curcumin-β-cyclodextrin nanoparticle to enhance curcumin skin permeability from hydrophilic matrix gel.

PubMed

Rachmawati, Heni; Edityaningrum, Citra Ariani; Mauludin, Rachmat

2013-12-01

Curcumin (CUR) has various pharmacological effects, but its extensive first-pass metabolism and short elimination half-life limit its bioavailability. Therefore, transdermal application has become a potential alternative to delivery CUR. To increase CUR solubility for the development of a transparent homogenous gel and also enhance the permeation rate of CUR into the skin, β-cyclodextrin-curcumin nanoparticle complex (BCD-CUR-N) was developed. CUR encapsulation efficiency was increased by raising the percentage of CUR to BCD up to 20%. The mean particle size of the best CUR loading formula was 156 nm. All evaluation data using infrared spectroscopy, Raman spectroscopy, powder X-ray diffractometry, differential thermal analysis and scanning electron microscopy confirmed the successful formation of the inclusion complex. BCD-CUR-N increased the CUR dissolution rate of 10-fold (p < 0.01). In addition, the improvement of CUR permeability acrossed skin model tissue was observed in gel containing the BCD-CUR-N and was about 1.8-fold when compared with the free CUR gel (p < 0.01). Overall, CUR in the form of the BCD-CUR-N improved the solubility further on the penetration of CUR.

Investigation on microstructure and mechanical properties of Mo2FeB2 based cermets with and without PVA

NASA Astrophysics Data System (ADS)

Shen, Yupeng; Huang, Zhifu; Jian, Yongxin; Yang, Ming; Li, Kemin

2018-03-01

Mo2FeB2 based cermets with and without PVA have been investigated by x-ray diffractometry (XRD), x-ray photoelectron spectroscope (XPS) and scanning electron microscopy (SEM). The density and transverse rupture strength (TRS) of green compact, relative density, hardness (HRA), fracture toughness (KIC) and TRS of Mo2FeB2 based cermets were also measured. The results indicate that, compared with the Mo2FeB2 based cermets without PVA, the density of green compact with PVA can be improved slightly at the same pressure. However, the much higher TRS is obtained for the green compact without PVA. Meanwhile, Mo2FeB2 particles exhibit the finer and less congruity feature for Mo2FeB2 based cermets without PVA. In addition, the higher relative density, hardness, fracture toughness and TRS can be acquired for the cermets without PVA. Obviously, considering the mechanical properties and preparation period of Mo2FeB2 based cermets, no adding PVA is the optimized process of powder molding in the manufacture of Mo2FeB2 based cermets.

Synthesis and surface properties of submicron barium sulfate particles

NASA Astrophysics Data System (ADS)

Zhang, Ming; Zhang, Bao; Li, Xinhai; Yin, Zhoulan; Guo, Xueyi

2011-10-01

Barium sulfate particles were synthesized in the presence of EDTA at room temperature. X-ray diffractometry (XRD), Fourier transform infrared resonance (FTIR) and scanning electron microscopy (SEM) were used to characterize the structure and morphology of BaSO 4 particles. The effect of the preparation parameters on the particle size distribution and morphology was investigated. The conditional formation constants of Ba-EDTA at different pH values were calculated. The results show that the size and morphology of BaSO 4 particles can be effectively controlled by adding EDTA in the precipitation process. Among all the operation conditions, the pH value has significant effect on the particle size. The obtained barium sulfate particles are spherical and well dispersed at pH = 9-10. Zeta potentials of BaSO 4 were measured at different pH. The isoelectric point (IEP) of barium sulfate colloid appears at pH 6.92. The model of the solid-solution interface at a particle of BaSO 4 was presented. The FTIR result indicates that the surface of the prepared BaSO 4 absorbs the functional groups of EDTA, which lower the IEP of the barium sulfate particles.

Effect of Ca addition on the damping capacity of Mg-Al-Zn casting alloys

NASA Astrophysics Data System (ADS)

Jun, Joong-Hwan; Moon, Jung-Hyun

2015-07-01

The influences of Ca addition on the microstructures and damping capacities of AZ91-(0˜2)%Ca casting alloys were investigated, on the basis of the results of X-ray diffractometry, optical microscopy, scanning electron microscopy and vibration tests in a single cantilever mode. The amount of intermetallic compounds decreased with increasing Ca content up to 0.5%, above which it increased; the average cell size showed the opposite tendency. All alloys exhibited similar damping levels in the strain-amplitude independent region. Considering the very low solubility of Ca in the matrix, and that most of the Ca elements are consumed by the formation of the Al2Ca phase and incorporation into the Mg17Al12 phase, this would be ascribed to the almost identical concentrations of Ca solutes distributed in the matrix. In the strain-amplitude dependent region, however, the AZ91-0.5%Ca alloy possessed the maximum damping capacity. From the viewpoint of microstructural evolution with Ca addition, the number density of compound particles is considered to be the principal factor affecting the damping behavior in the strain-amplitude dependent region.

Formation and characterization of calcium orthophosphates in the presence of two different acidic macromolecules

NASA Astrophysics Data System (ADS)

Pelin, Irina M.; Maier, Vasilica; Suflet, Dana M.; Popescu, Irina; Darie-Nita, Raluca N.; Aflori, Magdalena; Butnaru, Maria

2017-10-01

The synthetic nanocrystalline calcium orthophosphates have a notable bioactivity due to the chemical similarity with biological apatite from calcified tissues. In mineralized tissues, the highly ordered structures come from organized assemblies of biomacromolecules and inorganic nanoparticles. One of the purposes of this work was to study the effect of two types of acidic macromolecules: atelocollagen and phosphorylated curdlan onto calcium orthophosphates formation after 30 days of maturation at 2 ± 2 °C. The resulted samples after a long aging time, either calcium orthophosphates or composites, were first investigated by FT-IR spectroscopy and X-ray diffractometry and the results indicated that precipitated hydroxyapatite with low crystallinity was obtained when the synthesis was performed in the presence of phosphorylated curdlan. The macromolecules influenced the morphology of the particles as shown by scanning and transmission electron microscopy. The presence of macromolecules as demonstrated by thermal investigation also influenced the rheological properties of the samples. The second purpose of the work was to evaluate the cytotoxicity of the samples using the MTT assay, and the results revealed very good cells viability. The preliminary results are encouraging regarding the use of these materials for further tests in order to develop injectable bone substitutes.

Preparation of MWCNT-Fe3O4 Nanocomposites from Iron Sand Using Sonochemical Route

NASA Astrophysics Data System (ADS)

Rahmawati, R.; Melati, A.; Taufiq, A.; Sunaryono; Diantoro, M.; Yuliarto, B.; Suyatman, S.; Nugraha, N.; Kurniadi, D.

2017-05-01

The composites of multi-walled carbon nanotube (MWCNT) and magnetite (Fe3O4) nanoparticles from iron sand were successfully prepared via the sonochemical route. In this experiment, the MWCNT-Fe3O4 nanocomposites were prepared with different compositions of MWCNT (0.01%, 0.02%, and 0.04%) with the constant composition of Fe3O4 particles. The characterizations were performed by means of X-Ray Diffractometry (XRD), Fourier Transform Infra-Red (FTIR) Spectrometer and Scanning Electron Microscopy (SEM) integrated with Energy Dispersive X-Ray (EDX). The XRD data analysis showed that the Fe3O4 crystallize in spinel structure in nanometric size. Furthermore, the crystallinity of the samples tended to reduce by increasing the MWCNT compositions. The SEM images showed that Fe3O4 tend to agglomerate in nanometric size. The FTIR spectra detected the functional groups of Fe-O bonding that showed the existence of Fe2+ and Fe3+. In the composites, the Fe3O4 nanoparticles were physically mixed with the MWCNTs constructing a unique structure. The as prepared MWCNT-Fe3O4 nanocomposites have the potential for bio-applications.

Improving the tribocorrosion resistance of Ti6Al4V surface by laser surface cladding with TiNiZrO2 composite coating

NASA Astrophysics Data System (ADS)

Obadele, Babatunde Abiodun; Andrews, Anthony; Mathew, Mathew T.; Olubambi, Peter Apata; Pityana, Sisa

2015-08-01

Ti6Al4V alloy was laser cladded with titanium, nickel and zirconia powders in different ratio using a 2 kW CW ytterbium laser system (YLS). The microstructures of the cladded layers were examined using field emission scanning electron microscopy (FESEM) equipped with energy dispersive X-ray spectroscopy (EDS) and X-ray diffractometry (XRD). Corrosion and tribocorrosion tests were performed on the cladded surface in 1 M H2SO4 solution. The microstructure revealed the transformation from a dense dendritic structure in TiNi coating to a flower-like structure observed in TiNiZrO2 cladded layers. There was a significant increase in surface microindentation hardness values of the cladded layers due to the present of hard phase ZrO2 particles. The results obtained show that addition of ZrO2 improves the corrosion resistance property of TiNi coating but decrease the tribocorrosion resistance property. The surface hardening effect induced by ZrO2 addition, combination of high hardness of Ti2Ni phase could be responsible for the mechanical degradation and chemical wear under sliding conditions.

Microstructure and corrosion resistance of TC2 Ti alloy by laser cladding with Ti/TiC/TiB2 powders

NASA Astrophysics Data System (ADS)

Diao, Yunhua; Zhang, Kemin

2015-10-01

In the present work, a TiC/TiB2 composite coating was produced onto a TC2 Ti alloy by laser cladding with Ti/TiC/TiB2 powders. The surface microstructure, phase components and compositions were characterized with methods of optical microscopy (OM), scanning electron microscopy (SEM), X-ray diffractometry (XRD), and energy dispersive spectrometry (EDS). The cladding layer is consisted of Ti, TiC and TiB2. And the surface microhardness was measured. After laser cladding, a maximum hardness of 1100 HV is achieved in the laser cladding surface layer, which is more three times higher than that of the TC2 substrate (∼300 HV). Due to the formation of TiC and TiB2 intermetallic compounds in the alloyed region and grain refinement, the microhardness of coating is higher than TC2 Ti alloy. In this paper, the corrosion property of matrix material and treated samples were both measured in NaCl (3.5 wt%) aqueous solution. From the result we can see that the laser cladding specimens' corrosion property is clearly becoming better than that of the substrate.

Pulse electrodeposition of self-lubricating Ni-W/PTFE nanocomposite coatings on mild steel surface

NASA Astrophysics Data System (ADS)

Sangeetha, S.; Kalaignan, G. Paruthimal; Anthuvan, J. Tennis

2015-12-01

Ni-W/PTFE nanocomposite coatings with various contents of PTFE (polytetafluoroethylene) particles were prepared by pulse current (PC) electrodeposition from the Ni-W plating bath containing self lubricant PTFE particles to be co-deposited. Co-deposited PTFE particulates were uniformly distributed in the Ni-W alloy matrix. The coatings were characterized by Scanning Electron Microscopy (SEM), Energy Dispersive X-Ray Analysis (EDAX), X-ray Diffractometry (XRD) and Vicker's micro hardness tester. Tafel Polarization and electrochemical Impedance methods were used to evaluate the corrosion resistance behaviour of the nanocomposite coatings in 3.5% NaCl solution. It was found that, the Ni-W/PTFE nanocomposite coating has better corrosion resistance than the Ni-W alloy coating. Surface roughness and friction coefficient of the coated samples were assessed by Mitutoyo Surftest SJ-310 (ISO1997) and Scratch tester TR-101-M4 respectively. The contact angle (CA) of a water droplet on the surface of nanocomposite coating was measured by Optical Contact Goniometry (OCA 35). These results indicated that, the addition of PTFE in the Ni-W alloy matrix has resulted moderate microhardness, smooth surface, less friction coefficient, excellent water repellency and enhanced corrosion resistance of the nanocomposite coatings.

Structural characterization and bioavailability of ternary nanoparticles consisting of amylose, α-linoleic acid and β-lactoglobulin complexed with naringin.

PubMed

Feng, Tao; Wang, Ke; Liu, Fangfang; Ye, Ran; Zhu, Xiao; Zhuang, Haining; Xu, Zhimin

2017-06-01

Naringin is a bioflavonoid that is rich in citrus plants and possesses enormous health benefits. However, the use of naringin as a nutraceutical is significantly limited by its low bioavailability. In this study, a novel water-soluble ternary nanoparticle material consisting of amylose, α-linoleic acid and β-lactoglobulin was developed to encapsulate naringin to improve its bioavailability. The physicochemical characteristics of the ternary nanoparticle-naringin inclusion complex were analysed by ultraviolet-visible spectroscopy (UV), Fourier transform infrared spectroscopy (FT-IR), differential scanning calorimetry (DSC), high-resolution transmission electron microscopy (TEM), X-ray diffractometry (XRD) and particle size distribution. The results confirmed the formation of the ternary nanoparticle-naringin inclusion complex. The encapsulation efficiency (EE) and loading content (LC) of the ternary nanoparticle-naringin inclusion complex were 78.73±4.17% and 14.51±3.43%, respectively. In addition, the results of the ternary nanoparticle-naringin inclusion complex in simulated gastric fluid (SGF) and simulated intestinal fluid (SIF) demonstrated that naringin can be gradually released from the complex. In conclusion, ternary nanoparticles are considered promising carriers to effectively improve the bioavailability of naringin. Copyright © 2017 Elsevier B.V. All rights reserved.

Photocatalytic degradation of an azo textile dye (C.I. Reactive Red 195 (3BF)) in aqueous solution over copper cobaltite nanocomposite coated on glass by Doctor Blade method.

PubMed

Habibi, Mohammad Hossein; Rezvani, Zoya

2015-08-05

The degradation of C.I. Reactive Red 195 (3BF) in aqueous solution using copper cobaltite nanocomposite coated on glass by Doctor Blade method was studied. Structural, optical and morphological properties of nanocomposite coatings were characterized by X-ray powder diffractometry (XRD), diffuse reflectance spectroscopy (DRS) and field emission scanning electron microscopy (FESEM). The nanoparticles exhibit a particle size of 31 nm, showing a good nanoscale crystalline morphology. The photocatalytic activity of copper cobaltite nanocomposite coated on glass was studied by performing the photocatalytic degradation of 3BF at different irradiation time. The effect of irradiation time on the degradation of 3BF was studied and the results showed that more than 85% of the 3BF was degraded in 45 min of irradiation. The pseudo-first-order kinetic models were used and the rate constants were evaluated with pseudo first order rate constants of 4.10 × 10(-2) min(-1). The main advantage of the photocatalyst coated on glass overcomes the difficulties in separation and recycle of photocatalyst suspensions. Copyright © 2015 Elsevier B.V. All rights reserved.

The polymorphic and mesomorphic behavior of four esters of cholesterol.

NASA Technical Reports Server (NTRS)

Merritt, W. G.; Cole, G. D.; Walker, W. W.

1971-01-01

The techniques of differential scanning calorimetry, X-ray powder diffractometry, and positron annihilation have been used to study the polymorphic and mesomorphic behavior of the following esters of cholesterol: cholesteryl formate, cholesteryl butyrate, cholesteryl benzoate, and cholesteryl cinnamate. Each of these compounds exhibits a single mesophase of the cholesteric type. The solid phase formed from the melt for each ester was observed to be structurally different from the solid phase obtained from solution. Solvents from which the solution-grown samples were crystallized were as follows: cholesteryl formate and cholesteryl butyrate from acetone, cholesteryl benzoate from benzene, and cholesteryl cinnamate from 2-butanone.

Study the effect of mechanical alloying parameters on synthesis of Cr{sub 2}Nb–Al{sub 2}O{sub 3} nanocomposite

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shayesteh, Payam, E-mail: shayesteh.payam@gmail.com; Mirdamadi, Shamseddin; Razavi, Hossein

2014-01-01

Graphical abstract: - Highlights: • Cr{sub 2}Nb–Al{sub 2}O{sub 3} nanocomposite synthesized through MA. • Effect of BPR, rotating speed, milling time and PCA concentration investigated. • After annealing at 1100 °C crystalline phase were appeared. • Williamson–Hall analysis was used in order to study the grain size of nano composite. - Abstract: In this study, Cr{sub 2}Nb–20 vol.% Al{sub 2}O{sub 3} nanocomposite was prepared successfully by mechanochemical reaction between Al, Nb and Cr{sub 2}O{sub 3} powders. Amorphization of powder occurred during mechanical alloying because of high energy collisions between powders and steel balls in milling container which transfer high degreemore » of energy to powders. Therefore, annealing was needed to form crystalline phases. The influence of different mechanical alloying parameters such as BPR, rotating speed, milling time and PCA concentration on synthesis of composite material were investigated. After mechanical alloying, the powder was encapsulated in quartz and then annealed at 1100 °C for 3 h. After annealing, 3 different phases were appeared (Cr{sub 2}Nb (cubic), Cr{sub 2}Nb (hexagonal) and α-Al{sub 2}O{sub 3}). The structural changes of powder particles during mechanical alloying were studied by X-ray diffractometry (XRD), atomic force microscopy (AFM), scanning electron microscopy (SEM) and transmission electron microscopy (TEM)« less

He-irradiation effects on glass-ceramics for joining of SiC-based materials

NASA Astrophysics Data System (ADS)

Gozzelino, L.; Casalegno, V.; Ghigo, G.; Moskalewicz, T.; Czyrska-Filemonowicz, A.; Ferraris, M.

2016-04-01

CaO-Al2O3 (CA) and SiO2-Al2O3-Y2O3 (SAY) glass-ceramics are promising candidates for SiC/SiC indirect joints. In view of their use in locations where high radiation level is expected (i.e. fusion plants) it is important to investigate how radiation-induced damage can modify the material microstructure. To this aim, pellets of both types were irradiated with 5.5 MeV 4He+ ions at an average temperature of 75 °C up to a fluence of almost 2.3·1018 cm-2. This produces a displacement defect density that increases with depth and reaches a value of about 40 displacements per atom in the ion implantation region, where the He-gas reaches a concentration of several thousands of atomic parts per million. X-ray diffractometry and scanning electron microscopy showed no change in the microstructure and in the morphology of the pellet surface. Moreover, a transmission electron microscopy investigation on cross-section lamellas revealed the occurrence of structural defects and agglomerates of He-bubbles in the implantation region for the CA sample and a more homogeneous He-bubble distribution in the SAY pellet, even outside the implantation layer. In addition, no amorphization was found in both samples, even in correspondence to the He implantation zone. The radiation damage induced only occasional micro-cracks, mainly located at grain boundaries (CA) or within the grains (SAY).

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lan, Xiaodong; Wu, Hong, E-mail: wuhong927@126.com

Metallic glass composite coatings Ti{sub 45}Cu{sub 41}Ni{sub 9}Zr{sub 5} and Ti{sub 45}Cu{sub 41}Ni{sub 6}Zr{sub 5}Sn{sub 3} (at.%) on a Ti-30Nb-5Ta-7Zr (wt.%) (TNTZ) alloy were prepared by laser cladding. The microstructures of the coatings were characterized by means of X-ray diffractometry (XRD), scanning electron microscopy (SEM) equipped with energy dispersive X-ray analyzer (EDXA), and transmission electron microscopy (TEM). Results indicated that the coatings have an amorphous structure embedded with a few nanocrystalline phases and dendrites. A partial substitution of Ni by Sn can improve the glass forming ability of Ti-base metallic glass system, and induce the formation of nano-sized Ni{sub 2}SnTimore » phase during the cyclic laser heating. The tribological behavior of both the substrate and the coatings was investigated in detail. A significant improvement in both the hardness and the wear resistance of the coatings was achieved with the addition of Sn. The relationship between the wear resistance and the microstructures of the coatings was discussed. - Highlights: •Ti-based metallic glass composite coatings were prepared by laser cladding. •The wear resistance is greatly improved by laser cladding of composite coatings. •Substitution of Ni by Sn increases GFA and wear resistance of the coatings. •A good balance of crystalline/amorphous phases improves the wear resistance. •Adhesive wear serves as the dominant wear mechanism of the composite coatings.« less

Various types of semiconductor photocatalysts modified by CdTe QDs and Pt NPs for toluene photooxidation in the gas phase under visible light

NASA Astrophysics Data System (ADS)

Marchelek, M.; Grabowska, E.; Klimczuk, T.; Lisowski, W.; Zaleska-Medynska, A.

2017-01-01

A novel synthesis process was used to prepare TiO2 microspheres, TiO2 P-25, SrTiO3 and KTaO3 decorated by CdTe QDs and/or Pt NPs. The effect of semiconductor matrix, presence of CdTe QDs and/or Pt NPs on the semiconductor surface as well as deposition technique of Pt NPs (photodeposition or radiolysis) on the photocatalytic activity were investigated. The as-prepared samples were characterized by X-ray powder diffractometry (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM) with energy-dispersive X-ray (EDX) spectroscopy, scanning electron microscopy (SEM), photoluminescence spectrometry (PL), Fourier transform infrared (FT-IR) and Raman spectra, diffuse reflectance spectroscopy (DRS) and BET surface area analysis. The photocatalytic decomposition of toluene in gas phase, activated by light-emitting diodes (LEDs), with the CdTe/Pt nanoparticles-modified TiO2 microspheres, P25, SrTiO3 and KTaO3 semiconductors was investigated under UV-vis and visible irradiation.The results showed that the photoactivity depends on semiconductor matrix. The highest photoactivity under Vis light was observed for KTaO3/CdTe-Pt(R) sample (56% of toluene was decompose after 30 min of irradiation). The efficiency of the most active sample was 3 times higher than result for P25 and two times higher than for unmodified KTaO3.

Synthesis of core–shell structured FAU/SBA-15 composite molecular sieves and their performance in catalytic cracking of polystyrene

PubMed Central

Du, Jinlong; Shi, Chunwei; Wu, Wenyuan; Bian, Xue; Chen, Ping; Cui, Qingzhu; Cui, Zhixuan

2017-01-01

Abstract Composite molecular sieves, FAU/SBA-15, having core-shell structure were synthesized. The synthesized composite sieves were characterized by X-ray diffractometry (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDS), pyrolysis fourier transform infrared (Py-FTIR) spectroscopy, temperature programmed desorption spectra (NH3-TPD), UV Raman spectroscopy, nuclear magnetic resonance (NMR) and other techniques. XRD, SEM, TEM, N2 adsorption-desorption, mass spectrometry, NMR and EDS results showed that the composite molecular sieve contained two pore channels. Py-FTIR results showed that the addition of HY molecular sieves improved the acidity of the composite zeolite. The crystallization mechanism during the growth of FAU/SBA-15 shell was deduced from the influence of crystallization time on the synthesis of FAU/SBA-15 core-shell structured composite molecular sieve. HY dissociated partially in H2SO4 solution, and consisted of secondary structural units. This framework structure was more stable than its presence in the isolated form on the same ring or in the absence of Al. Thus it played a guiding role and connected with SBA-15 closely through the Si-O bond. This resulted in the gradual covering of the exterior surface of FAU phase by SBA-15 molecular sieves. The presence of SBA-15 restricted the formation of the other high mass components and increased the selectivity towards ethylbenzene. PMID:29383044

Effect of milling atmosphere on structural and magnetic properties of Ni-Zn ferrite nanocrystalline

NASA Astrophysics Data System (ADS)

Hajalilou, Abdollah; Hashim, Mansor; Ebrahimi-Kahrizsangi, Reza; Masoudi Mohamad, Taghi

2015-04-01

Powder mixtures of Zn, NiO, and Fe2O3 are mechanically alloyed by high energy ball milling to produce Ni-Zn ferrite with a nominal composition of Ni0.36Zn0.64Fe2O4. The effects of milling atmospheres (argon, air, and oxygen), milling time (from 0 to 30 h) and heat treatment are studied. The products are characterized using x-ray diffractometry, field emission scanning electron microscopy equipped with energy-dispersive x-ray spectroscopy, and transmitted electron microscopy. The results indicate that the desired ferrite is not produced during the milling in the samples milled under either air or oxygen atmospheres. In those samples milled under argon, however, Zn/NiO/Fe2O3 reacts with a solid-state diffusion mode to produce Ni-Zn ferrite nanocrystalline in a size of 8 nm after 30-h-milling. The average crystallite sizes decrease to 9 nm and 10 nm in 30-h-milling samples under air and oxygen atmospheres, respectively. Annealing the 30-h-milling samples at 600 °C for 2 h leads to the formation of a single phase of Ni-Zn ferrite, an increase of crystallite size, and a reduction of internal lattice strain. Finally, the effects of the milling atmosphere and heating temperature on the magnetic properties of the 30-h-milling samples are investigated. Project supported by the University Putra Malaysia Graduate Research Fellowship Section.

Molecular beam epitaxial growth and structural characterization of ZnS on (001) GaAs

NASA Technical Reports Server (NTRS)

Benz, R. G., II; Huang, P. C.; Stock, S. R.; Summers, C. J.

1988-01-01

The effect of surface nucleation processes on the quality of ZnS layers grown on (001) GaAs substrates by molecular beam epitaxy is reported. Reflection high energy electron diffraction indicated that nucleation at high temperatures produced more planar surfaces than nucleation at low temperatures, but the crystalline quality as assessed by X-ray double crystal diffractometry is relatively independent of nucleation temperature. A critical factor in layer quality was the initial roughness of the GaAs surfaces.

In Vitro and In Vivo Evaluation of Casein as a Drug Carrier for Enzymatically Triggered Dissolution Enhancement from Solid Dispersions.

PubMed

Bani-Jaber, Ahmad; Alshawabkeh, Iyad; Abdullah, Samaa; Hamdan, Imad; Ardakani, Adel; Habash, Maha

2017-07-01

Due to its unique properties, such as biodegradability, biocompatibility, high amphiphilic property, and micelle formation, casein (CS) has been increasingly studied for drug delivery. We used CS as a drug carrier in solid dispersions (SDs) and evaluated the effect of its degradation by trypsin on drug dissolution from the dispersions. SDs of CS and mefenamic acid (MA) were prepared by physical mixing, kneading, and coprecipitation methods. In comparison to pure MA, the dispersions were evaluated for drug-protein interaction, loss of drug crystalinity, and drug morphology by differential scanning calorimetry, X-ray diffractometry, Fourier transform infrared spectroscopy, and scanning electron microscopy. Drug dissolution from the dispersions was evaluated in simulated intestinal fluid as enzyme free and trypsin-enriched media. Furthermore, in vivo drug absorption of MA from CS-MA coprecipitate was evaluated in rats, in comparison with a reference SD of polyethylene glycol and MA (PEG-MA SD). Relative to other CS preparations, CS-MA coprecipitate showed the highest loss of drug crystallinity, drug micronization, and CS-MA interaction. CS remarkably enhanced the dissolution rate and extent of MA from the physical and kneaded mixtures. However, the highest dissolution enhancement was obtained when MA was coprecipitated with CS. Trypsin that can hydrolyze CS during dissolution resulted in further enhancement of MA dissolution from the physical and kneaded mixtures. However, a corresponding retardation effect was obtained for the coprecipitate. In correlation with in vitro drug release, CS-MA coprecipitate also showed significantly higher MA bioavailability in rats than PEG-MA SD.

In vitro investigation of anodization and CaP deposited titanium surface using MG63 osteoblast-like cells

NASA Astrophysics Data System (ADS)

Lee, J. M.; Lee, J. I.; Lim, Y. J.

2010-03-01

The aim of the present study was to investigate surface characteristics in four different titanium surfaces (AN: anodized at 270 V; AN-CaP: anodic oxidation and CaP deposited; SLA: sandblasted and acid etched; MA: machined) and to evaluate biological behaviors such as cell adhesion, cell proliferation, cytoskeletal organization, and osteogenic protein expression of MG63 osteoblast-like cells at the early stage. Surface analysis was performed using scanning electron microscopy, thin-film X-ray diffractometry, and a confocal laser scanning microscope. In order to evaluate cellular responses, MG63 osteoblast-like cells were used. The cell viability was evaluated by MTT assay. Immunofluorescent analyses of actin, type I collagen, osteonectin and osteocalcin were performed. The anodized and CaP deposited specimen showed homogeneously distributed CaP particles around micropores and exhibited anatase type oxides, titanium, and HA crystalline structures. This experiment suggests that CaP particles on the anodic oxidation surface affect cellular attachment and spreading. When designing an in vitro biological study for CaP coated titanium, it must be taken into account that preincubation in medium prior to cell seeding and the cell culture medium may affect the CaP coatings. All these observations illustrate the importance of the experimental conditions and the physicochemical parameters of the CaP coating. It is considered that further evaluations such as long-term in vitro cellular assays and in vivo experiments should be necessary to figure out the effect of CaP deposition to biological responses.

Self-assembled flower-like antimony trioxide microstructures with high infrared reflectance performance

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ge, Shengsong, E-mail: geshengsong@126.com; Yang, Xiaokun; Shao, Qian

A simple hydrothermal process was adopted to self-assembly prepare high infrared reflective antimony trioxide with three-dimensional flower-like microstructures. The morphologies of antimony trioxide microstructures were characterized by X-ray diffractometry (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and high resolution transmission electron microscopy (HRTEM) respectively. It is also found that experimental parameters, such as NaOH concentration, surfactant concentration and volume ratio of ethanol–water played crucial roles in controlling the morphologies of Sb{sub 2}O{sub 3} microstructures. A possible growth mechanism of flower-like Sb{sub 2}O{sub 3} microstructure was proposed based on the experimental data. UV–vis–NIR spectra verified that the near infraredmore » reflectivity of the obtained flower-like microstructures could averagely achieve as 92% with maximum reflectivity of 98%, obviously higher than that of other different morphologies of antimony trioxide microstructures. It is expected that the flower-like Sb{sub 2}O{sub 3} nanostructures have some applications in optical materials and heat insulation coatings. - Graphical abstract: Flower-like Sb{sub 2}O{sub 3} microstructures that composed of nanosheets with thickness of ca. 100 nm exhibit high reflectivity under UV–vis–NIR spectra. Highlights: ► Uniform flower-like microstructures were synthesized via simple hydrothermal reaction. ► The flower-like Sb{sub 2}O{sub 3} microstructures exhibited higher reflectivity than other morphologies under the UV–vis–NIR light. ► Influencing parameters on the Sb{sub 2}O{sub 3} morphologies have been discussed in detail. ► Possible mechanism leading to flower-like microstructures was proposed.« less

Electronic, optical and photocatalytic behavior of Mn, N doped and co-doped TiO{sub 2}: Experiment and simulation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhao, Ya Fei; Li, Can, E-mail: canli1983@gmail.com; Lu, Song

2016-03-15

The crystal phase structure, surface morphology, chemical states and optical properties of Mn, N mono-doped and co-doped TiO{sub 2} nanoparticles were investigated by X-ray powder diffractometry, Raman spectra, scanning electron microscopy, X-ray photoelectron spectroscopy and UV–vis diffuse reflectance spectroscopy. Meanwhile, geometry structures, formation energies, electronic and optical properties of all systems have been also analyzed by density functional theory. The results showed that the band gap values and the carrier mobility in the valence band, conduction band and impurity levels have a synergetic influence on the visible-light absorption and photocatalytic activity of the doped TiO{sub 2}. The number and themore » carrier mobility of impurity level jointly influence the photocatalytic activity of catalyst under visible-light. Especially, the photocatalytic activity of Mn-2N co-doped TiO{sub 2} beyond three-fold than that of pure TiO{sub 2} under visible-light. - Graphical abstract: The ILs formed by N-2p orbital in N single doped specimen lie above the VB, while the ILs formed by Mn-3d orbital in Mn single doped specimen appear below the CB. However, a large amount of ILs formed by N-2p orbital and Mn-3d orbital in N and Mn codoped specimens. The band gap values and the carrier mobility in the valence band, conduction band and impurity levels have a synergetic influence on the visible-light absorption and photocatalytic activity of the doped TiO{sub 2}. The number and the carrier mobility of impurity level jointly influence the photocatalytic activity of catalyst under visible-light.« less

Preparation and characterization of silk sericin/PVA blend film with silver nanoparticles for potential antimicrobial application.

PubMed

He, Huawei; Cai, Rui; Wang, Yejing; Tao, Gang; Guo, Pengchao; Zuo, Hua; Chen, Liqun; Liu, Xinyu; Zhao, Ping; Xia, Qingyou

2017-11-01

Sericin has great potentials in biomedical applications for its good reactive activity, biocompatibility and biodegradability. However, the undesirable mechanical performance limits its application. Here, we developed a green, facile and economic approach to prepare sericin/polyvinyl alcohol (PVA) blend film. Further, silver nanoparticles (AgNPs) were synthesized in situ on the surface of sericin/PVA film via UV-assisted green synthesis method. Mechanical performance, swelling, mass losing and water retention tests showed the blend film had good mechanical performance, hygroscopicity, water retention capacity and low mass losing ratio. Scanning electron microscopy, fourier transfer infrared spectroscopy, X-ray diffractometry diffraction and X-ray photoelectron spectroscopy indicated the blending of PVA and sericin promoted the formation of hydrogen bond network between sericin and PVA, thus enhanced the mechanical performance and the stability of sericin, as well as the hygroscopicity and water retention capacity. UV irradiation and AgNPs modification did not affect the inner crystalline structure of sericin/PVA blend film. The inhibition zone and bacteria growth curve assay suggested AgNPs-sericin/PVA film had good antibacterial activities against E. coli and S. aureus. This novel AgNPs-sericin/PVA film shows great potentials in biomedical materials such as wound dressing and skin tissue engineering. Copyright © 2017 Elsevier B.V. All rights reserved.

Synthesis of microsphere silicon carbide/nanoneedle manganese oxide composites and their electrochemical properties as supercapacitors

NASA Astrophysics Data System (ADS)

Kim, Myeongjin; Yoo, Youngjae; Kim, Jooheon

2014-11-01

Synthesis of microsphere silicon carbide/nanoneedle MnO2 (SiC/N-MnO2) composites for use as high-performance materials in supercapacitors is reported herein. The synthesis procedure involves the initial treatment of silicon carbide (SiC) with hydrogen peroxide to obtain oxygen-containing functional groups to provide anchoring sites for connection of SiC and the MnO2 nanoneedles (N-MnO2). MnO2 nanoneedles are subsequently formed on the SiC surface. The morphology and microstructure of the as-prepared composites are characterized via X-ray diffractometry, field-emission scanning electron microscopy, thermogravimetric analysis, and X-ray photoelectron spectroscopy. The characterizations indicate that MnO2 nanoneedles are homogeneously formed on the SiC surface in the composite. The capacitive properties of the as-prepared SiC/N-MnO2 electrodes are evaluated using cyclic voltammetry, galvanostatic charge/discharge testing, and electrochemical impedance spectroscopy in a three-electrode experimental setup using a 1-M Na2SO4 aqueous solution as the electrolyte. The SiC/N-MnO2(5) electrode, for which the MnO2/SiC feed ratio is 5:1, displays a specific capacitance as high as 273.2 F g-1 at 10 mV s-1.

Effect of Grinding on the Solid-State Stability and Particle Dissolution of Acyclovir Polymorphs.

PubMed

Magnoni, Federico; Gigliobianco, Maria Rosa; Vargas Peregrina, Dolores; Censi, Roberta; Di Martino, Piera

2017-10-01

The present work investigated the solid state change of 4 acyclovir polymorphs when ground at room temperature (Method A) and under cryo-grinding in the presence of liquid nitrogen (Method B). Modifications in particle size and shape (evaluated by scanning electron microscopy) and in the water content (evaluated by thermal analysis) were related to transitions at the solid state, as confirmed by X-ray powder diffractometry. Anhydrous Form I was stable under grinding by both Methods A and B. The anhydrous Form II was stable during grinding under Method A, whereas it was progressively converted to the hydrate Form V during grinding under Method B. The hydrate Form V was stable under Method A, whereas it was converted to the anhydrous Form I after 15 min and then to the hydrate Form VI after 45 min of grinding. The hydrate Form VI proved to be stable under grinding by both Methods A and B. Thus, Form I and VI were the only forms that yielded a sizeable decrease in particle size under grinding, with a consequent increase in particle dissolution rate, while maintaining solid state physicochemical stability. Form I treated under Method B grinding gave the best dissolution rate. Copyright © 2017 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

The Formation Mechanism and Corrosion Resistance of a Composite Phosphate Conversion Film on AM60 Alloy.

PubMed

Chen, Jun; Lan, Xiangna; Wang, Chao; Zhang, Qinyong

2018-03-08

Magnesium alloy AM60 has high duc and toughness, which is expected to increase in demand for automotive applications. However, it is too active, and coatings have been extensively studied to prevent corrosion. In this work, a Ba-containing composite phosphate film has been prepared on the surface of AM60. The composition and formation mechanism of the film have been investigated using a scanning electronic microscope equipped with energy dispersive X-ray spectroscopy, Fourier transform infrared, X-ray photoelectron spectroscopy, and X-ray diffractometry tests. The corrosion resistance of the film has been measured by electrochemical and immersion tests. The results show that the deposition film has fully covered the substrate but there are some micro-cracks. The structure of the film is complex, and consists of MgHPO₄·3H₂O, MnHPO₄·2.25H₂O, BaHPO₄·3H₂O, BaMg₂(PO₄)₂, Mg₃(PO₄)₂·22H₂O, Ca₃(PO₄)₂·xH₂O, and some amorphous phases. The composite phosphate film has better anticorrosion performance than the AM60 and can protect the bare alloy from corrosion for more than 12 h in 0.6 M NaCl.

Synthesis of Ti-6Al-4V alloy with nano-TiN microstructure via spark plasma sintering technique

NASA Astrophysics Data System (ADS)

E Falodun, O.; Obadele, B. A.; Oke, S. R.; E Maja, M.; Olubambi, P. A.

2017-12-01

The effect of nano-TiN dispersion strengthened Ti-6Al-4V via spark plasma sintering method has been investigated. Ti-6Al-4V with 4 vol. percent of nano-TiN were mixed in a Turbula shaker mixer for 8 h at a speed of 49 rpm and the admixed powders were sintered at sintering temperature range of 1000 - 1100 °C, holding time of 10-30 mins, heating rate of 100 °C/min under an applied pressure of 50 MPa. The morphology of the as-received and sintered compacts was examined by scanning electron microscopy (SEM) equipped with energy dispersive X-ray spectroscopy (EDS) and phase analysis was done by X-ray diffractometry (XRD). The sintered compacts without nano-TiN reveal lamellar structure while reinforced Ti-6Al-4V with nano-TiN shows a bimodal structure and titanium nitride has a great influence on a grain growth at high temperature. Furthermore, the microstructural formation mechanism was investigated. With the addition of the content of Ti-6Al-4V with 4 vol.% of nano-TiN, the micro-hardness also improved and this was due to homogenous distribution of TiN in Ti-6Al-4V matrix.

Fabrication of mineralized electrospun PLGA and PLGA/gelatin nanofibers and their potential in bone tissue engineering.

PubMed

Meng, Z X; Li, H F; Sun, Z Z; Zheng, W; Zheng, Y F

2013-03-01

Surface mineralization is an effective method to produce calcium phosphate apatite coating on the surface of bone tissue scaffold which could create an osteophilic environment similar to the natural extracellular matrix for bone cells. In this study, we prepared mineralized poly(D,L-lactide-co-glycolide) (PLGA) and PLGA/gelatin electrospun nanofibers via depositing calcium phosphate apatite coating on the surface of these nanofibers to fabricate bone tissue engineering scaffolds by concentrated simulated body fluid method, supersaturated calcification solution method and alternate soaking method. The apatite products were characterized by the scanning electron microscopy (SEM), Fourier transform-infrared spectroscopy (FT-IR), and X-ray diffractometry (XRD) methods. A large amount of calcium phosphate apatite composed of dicalcium phosphate dihydrate (DCPD), hydroxyapatite (HA) and octacalcium phosphate (OCP) was deposited on the surface of resulting nanofibers in short times via three mineralizing methods. A larger amount of calcium phosphate was deposited on the surface of PLGA/gelatin nanofibers rather than PLGA nanofibers because gelatin acted as nucleation center for the formation of calcium phosphate. The cell culture experiments revealed that the difference of morphology and components of calcium phosphate apatite did not show much influence on the cell adhesion, proliferation and activity. Copyright © 2012 Elsevier B.V. All rights reserved.

Cu-Doped ZnO Thin Films Deposited by a Sol-Gel Process Using Two Copper Precursors: Gas-Sensing Performance in a Propane Atmosphere.

PubMed

Gómez-Pozos, Heberto; Arredondo, Emma Julia Luna; Maldonado Álvarez, Arturo; Biswal, Rajesh; Kudriavtsev, Yuriy; Pérez, Jaime Vega; Casallas-Moreno, Yenny Lucero; Olvera Amador, María de la Luz

2016-01-29

A study on the propane gas-sensing properties of Cu-doped ZnO thin films is presented in this work. The films were deposited on glass substrates by sol-gel and dip coating methods, using zinc acetate as a zinc precursor, copper acetate and copper chloride as precursors for doping. For higher sensitivity values, two film thickness values are controlled by the six and eight dippings, whereas for doping, three dippings were used, irrespective of the Cu precursor. The film structure was analyzed by X-ray diffractometry, and the analysis of the surface morphology and film composition was made through scanning electron microscopy (SEM) and secondary ion mass spectroscopy (SIMS), respectively. The sensing properties of Cu-doped ZnO thin films were then characterized in a propane atmosphere, C₃H₈, at different concentration levels and different operation temperatures of 100, 200 and 300 °C. Cu-doped ZnO films doped with copper chloride presented the highest sensitivity of approximately 6 × 10⁴, confirming a strong dependence on the dopant precursor type. The results obtained in this work show that the use of Cu as a dopant in ZnO films processed by sol-gel produces excellent catalysts for sensing C₃H₈ gas.

Separation of Lead from Crude Antimony by Pyro-Refining Process with NaPO3 Addition

NASA Astrophysics Data System (ADS)

Ye, Longgang; Hu, Yuejie; Xia, Zhimei; Chen, Yongming

2016-06-01

The main purpose of this study was to separate lead from crude antimony through an oxidation pyro-refining process and by using sodium metaphosphate as a lead elimination reagent. The process parameters that will affect the refining results were optimized experimentally under controlled conditions, such as the sodium metaphosphate charging dosage, the refining temperature and duration, and the air flow rate, to determine their effect on the lead content in refined antimony and the lead removal rate. A minimum lead content of 0.0522 wt.% and a 98.6% lead removal rate were obtained under the following optimal conditions: W_{{{NaPO}_{{3}} }} = 15% W Sb (where W represents weight), a refining temperature of 800°C, a refining time of 30 min, and an air flow rate of 3 L/min. X-ray diffractometry and scanning electron microscopy showed that high-purity antimony was obtained. The smelting operation is free from smoke or ammonia pollution when using monobasic sodium phosphate or ammonium dihydrogen phosphate as the lead elimination reagent. However, this refining process can also remove a certain amount of sulfur, cobalt, and silicon simultaneously, and smelting results also suggest that sodium metaphosphate can be used as a potential lead elimination reagent for bismuth and copper refining.

In Situ Synthesis of Silver Nanoparticles on the Polyelectrolyte-Coated Sericin/PVA Film for Enhanced Antibacterial Application

PubMed Central

Cai, Rui; Tao, Gang; Guo, Pengchao; Yang, Meirong; Ding, Chaoxiang; Zuo, Hua; Wang, Lingyan; Zhao, Ping; Wang, Yejing

2017-01-01

To develop silk sericin (SS) as a potential antibacterial biomaterial, a novel composite of polyelectrolyte multilayers (PEMs) coated sericin/poly(vinyl alcohol) (SS/PVA) film modified with silver nanoparticles (AgNPs) has been developed using a layer-by-layer assembly technique and ultraviolet-assisted AgNPs synthesis method. Ag ions were enriched by PEMs via the electrostatic attraction between Ag ions and PEMs, and then reduced to AgNPs in situ with the assistance of ultraviolet irradiation. PEMs facilitated the high-density growth of AgNPs and protected the synthesized AgNPs due to the formation of a 3D matrix, and thus endowed SS/PVA film with highly effective and durable antibacterial activity. Scanning electron microscopy, energy dispersive spectroscopy, X-ray diffractometry, Fourier transfer infrared spectroscopy, water contact angle, mechanical property and thermogravimetric analysis were applied to characterize SS/PVA, PEMs-SS/PVA and AgNPs-PEMs-SS/PVA films, respectively. AgNPs-PEMs-SS/PVA film has exhibited good mechanical performance, hydrophilicity, water absorption capability as well as excellent and durable antibacterial activity against Escherichia coli, Staphylococcus aureus and Pseudomonas aeruginosa and good stability and degradability. This study has developed a simple method to design and prepare AgNPs-PEMs-SS/PVA film for potential antibacterial application. PMID:28820482

Effect of cooking temperature on the crystallinity of acid hydrolysed-oil palm cellulose

NASA Astrophysics Data System (ADS)

Kuthi, Fatin Afifah Binti Ahmad; Badri, Khairiah Haji

2014-09-01

In this research, we studied the effect of acid hydrolysis temperature on the crystallinity of cellulose produced from empty fruit bunch (EFB). The hydrolysis temperature was studied from 120 to 140 °C at a fixed time and sulfuric acid, H2SO4 concentration which were 1 h and 1% (v/v) respectively. X-ray diffractometry (XRD) was carried out to measure the crystallinity of cellulose produced at varying hydrolysis temperatures. During hydrolysis, the amorphous region of α-cellulose was removed and the crystalline region was obtained. Percentage of crystallinity (CrI) for acid hydrolysed cellulose at 120, 130 and 140 °C were 54.21, 50.59 and 50.55 % respectively. Morphological studies using scanning electron microscope (SEM) showed that acid hydrolysis defibrilised to microfibrils in α-cellulose. The extraction process to produce α-cellulose has also been successfully carried out as the impurities at the outer surface, lignin and hemicellulose were removed. These findings were supported by the disappearance of peaks at 1732, 1512 and 1243 cm-1 on Fourier Transform infrared (FTIR) spectrum of α-cellulose. Similar peaks were identified in both the commercial microcrystalline cellulose (C-MCC) and acid hydrolysed cellulose (H-EFB), indicating the effectiveness of heat-catalysed acid hydrolysis.

Influence of Sintering Temperature on Mechanical and Physical properties of Mill Scale based Bipolar Plates for PEMFC

NASA Astrophysics Data System (ADS)

Khaerudini, Deni S.; Berliana, Rina; Prakoso, Gatra B.; Insiyanda, Dita R.; Alva, Sagir

2018-03-01

This work concerns the utilization of mill scale, a by-product of iron and steel formed during the hot rolling of steel, as a potential material for use as bipolar plates in proton exchange membrane fuel cells (PEMFCs). On the other hand, mill scale is considered a very rich in iron source having characteristic required such as for current collector in bipolar plate and would significantly contribute to lower the overall cost of PEMFC based fuel cell systems. In this study, the iron reach source of mill scale powder, after sieving of 150 mesh, was mechanically alloyed with the aluminium source containing 30 wt.% using a shaker mill for 3 h. The mixed powders were then pressed at 300 MPa and sintered at various temperatures of 400, 450 and 500 °C for 1 h under inert gas atmosphere. The structural changes of powder particles during mechanical alloying and after sintering were studied by x-ray diffractometry, scanning electron microscopy (SEM) with energy dispersive X-ray spectroscopy (EDX), microhardness measurement, and density - porosity analysis. The details of the performance variation of three different sintering conditions can be preliminary explained by the metallographic and crystallographic structure and phase analysis as well as sufficient mechanical strength of the sintered materials was presented in this report.

Influence of the interface layer on the adhesion of pulsed laser deposited hydroxyapatite coatings on titanium alloy

NASA Astrophysics Data System (ADS)

Fernández-Pradas, J. M.; García-Cuenca, M. V.; Clèries, L.; Sardin, G.; Morenza, J. L.

2002-07-01

Hydroxyapatite (HA) coatings were deposited on Ti-6Al-4V substrates by laser ablation with a KrF excimer laser. Depositions were performed at 45 Pa of water vapour and at a substrate temperature of 575 °C. After 7 min of deposition, coatings were left at this temperature for different times before cooling down. The samples morphology and structure were characterised by scanning electron microscopy, X-ray diffractometry and Raman spectroscopy. The mechanical performance of the coatings was evaluated through the scratch-test technique. The coatings do not present important differences between them. However, there is an interface layer between the coating and the substrate that indeed presents an evolution with the heating time. This interface layer is constituted by two different species: titanium oxide and Ti-6Al-4V with oxygen diffused in its lattice. Its thickness increases during the first minutes of heating after deposition. An evolution of the titanium oxide phases with the time of heating has been detected by Raman spectroscopy. The samples fail at lower loads in the scratch-test as longer is the time that they remained at high temperature. The mode of failure of the samples suggests that failure occurs at the interface.

Devitrification studies of wollastonite-tricalcium phosphate eutectic glass.

PubMed

Magallanes-Perdomo, M; Pena, P; De Aza, P N; Carrodeguas, R G; Rodríguez, M A; Turrillas, X; De Aza, S; De Aza, A H

2009-10-01

The present paper describes and discusses the devitrification and crystallization process of wollastonite-tricalcium phosphate (W-TCP) eutectic glass. This process was studied in situ from room temperature up to 1375 degrees C, by neutron diffractometry in vacuum. The data obtained were combined and compared with those performed in ambient atmosphere by differential thermal analysis and with those of samples fired in air at selected temperatures, and then cooled down and subsequently studied by laboratory XRD and field emission scanning electron microscopy fitted with energy X-ray dispersive spectroscopy. The experimental evidence indicates that the devitrification of W-TCP eutectic glass begins at approximately 870 degrees C with the crystallization of a Ca-deficient apatite phase, followed by wollastonite-2M (CaSiO(3)) crystallization at approximately 1006 degrees C. At 1375 degrees C, the bio-glass-ceramic is composed of quasi-rounded colonies formed by a homogeneous mixture of pseudowollastonite (CaSiO(3)) and alpha-tricalcium phosphate (Ca(3)(PO(4))(2)). This microstructure corresponds to irregular eutectic structures. It was also found that it is possible to obtain from the eutectic composition of the wollastonite-tricalcium phosphate binary system a wide range of bio-glass-ceramics, with different crystalline phases present, through appropriate design of thermal treatments.

Effect of Temperature and Growth Time on Vertically Aligned ZnO Nanorods by Simplified Hydrothermal Technique for Photoelectrochemical Cells.

PubMed

Mohd Fudzi, Laimy; Zainal, Zulkarnain; Lim, Hong Ngee; Chang, Sook-Keng; Holi, Araa Mebdir; Sarif Mohd Ali, Mahanim

2018-04-29

Despite its large band gap, ZnO has wide applicability in many fields ranging from gas sensors to solar cells. ZnO was chosen over other materials because of its large exciton binding energy (60 meV) and its stability to high-energy radiation. In this study, ZnO nanorods were deposited on ITO glass via a simple dip coating followed by a hydrothermal growth. The morphological, structural and compositional characteristics of the prepared films were analyzed using X-ray diffractometry (XRD), field emission scanning electron microscopy (FESEM), and ultraviolet-visible spectroscopy (UV-Vis). Photoelectrochemical conversion efficiencies were evaluated via photocurrent measurements under calibrated halogen lamp illumination. Thin film prepared at 120 °C for 4 h of hydrothermal treatment possessed a hexagonal wurtzite structure with the crystallite size of 19.2 nm. The average diameter of the ZnO nanorods was 37.7 nm and the thickness was found to be 2680.2 nm. According to FESEM images, as the hydrothermal growth temperature increases, the nanorod diameter become smaller. Moreover, the thickness of the nanorods increase with the growth time. Therefore, the sample prepared at 120 °C for 4 h displayed an impressive photoresponse by achieving high current density of 0.1944 mA/cm².

Enhanced bioactivity, biocompatibility and mechanical behavior of strontium substituted bioactive glasses.

PubMed

Arepalli, Sampath Kumar; Tripathi, Himanshu; Hira, Sumit Kumar; Manna, Partha Pratim; Pyare, Ram; S P Singh

2016-12-01

Strontium contained biomaterials have been reported as a potential bioactive material for bone regeneration, as it reduces bone resorption and stimulates bone formation. In the present investigation, the bioactive glasses were designed to partially substitute SrO for SiO2 in Na2O-CaO-SrO-P2O5-SiO2 system. This work demonstrates that the substitution of SrO for SiO2 has got significant benefit than substitution for CaO in the bioactive glass. Bioactivity was assessed by the immersion of the samples in simulated body fluid for different intervals. The formation of hydroxy carbonate apatite layer was identified by X-ray diffractometry, scanning electron microscopy (SEM) and energy dispersive spectroscopy. The elastic modulus of the bioactive glasses was measured and found to increase with increasing SrO for SiO2. The blood compatibility of the samples was evaluated. In vitro cell culture studies of the samples were performed using human osteosarcoma U2-OS cell lines and found a significant improvement in cell viability and proliferation. The investigation showed enhancement in bioactivity, mechanical and biological properties of the strontia substituted for silica in glasses. Thus, these bioactive glasses would be highly potential for bone regeneration. Copyright © 2016 Elsevier B.V. All rights reserved.

Nanostructured lipid carriers as novel ophthalmic delivery system for mangiferin: improving in vivo ocular bioavailability.

PubMed

Liu, Rui; Liu, Zhidong; Zhang, Chengui; Zhang, Boli

2012-10-01

The aim of this study was to develop a novel nanostructured lipid carriers (NLCs) system to improve ocular bioavailability of mangiferin (MGN) for the potential treatment of cataract. The physicochemical properties of MGN-loaded NLC (MGN-NLC) formulation were characterized by particle size, polydispersity index, zeta potential, entrapment efficiency, drug loading, morphological property, and crystalline state. in vitro characteristics were investigated by drug release from NLC system, physical stability, and corneal permeation through excised rabbit cornea. Moreover, in vivo ocular tolerability was assessed by a modified Draize test and histological microscopy. Preocular retention capability was evaluated by slit-lamp observation. Pharmacokinetic study in the aqueous humor was performed by microdialysis technique. Transmission electron microscopy depicted spherical and uniform morphology. Differential scanning calorimetry and X-ray diffractometry displayed imperfect crystalline lattice. The optimized MGN-NLC formulation exhibited a sustained drug release with 3 months stability and 4.31-fold increase of in vitro corneal permeation. Furthermore, in vivo studies exhibited a high tolerance in the ocular tissues and prolonged drug retention capacity on the corneal surface. Finally, pharmacokinetic study suggested a 5.69-fold increase of ocular bioavailability compared with MGN solution (MGN-SOL). Therefore, NLC system is a promising approach for ocular delivery of MGN. Copyright © 2012 Wiley Periodicals, Inc.

Microstructure and Plastic Deformation of the As-Welded Invar Fusion Zones

NASA Astrophysics Data System (ADS)

Yao, D. J.; Zhou, D. R.; Xu, P. Q.; Lu, F. G.

2017-05-01

The as-welded Invar fusion zones were fabricated between cemented carbides and carbon steel using a Fe-Ni Invar interlayer and laser welding method. Three regions in the as-welded Invar fusion zones were defined to compare microstructures, and these were characterized and confirmed by scanning electron microscopy and X-ray diffractometry. The structure and plastic deformation mechanism for initial Invar Fe-Ni alloys and the as-welded Invar fusion zones are discussed. (1) After undergoing high-temperature thermal cycles, the microstructure of the as-welded Invar fusion zones contains γ-(Fe, Ni) solid solution (nickel dissolving in γ-Fe) with a face-centered cubic (fcc) crystal structure and mixed carbides (eutectic colonies, mixed carbides between two adjacent grains). The mixed carbides exhibited larger, coarser eutectic microstructures with a decrease in welding speed and an increase in heat input. (2) The structure of the initial Invar and the as-welded Invar is face-centered cubic γ-(Fe, Ni). (3) The as-welded Invar has a larger plastic deformation than initial Invar with an increase in local strain field and dislocation density. Slip deformation is propagated along the (111) plane. This finding helps us to understand microstructure and the formation of dislocation and plastic deformation when the Invar Fe-Ni alloy undergoes a high-temperature process.

Improving the Thermal Shock Resistance of Thermal Barrier Coatings Through Formation of an In Situ YSZ/Al2O3 Composite via Laser Cladding

NASA Astrophysics Data System (ADS)

Soleimanipour, Zohre; Baghshahi, Saeid; Shoja-razavi, Reza

2017-04-01

In the present study, laser cladding of alumina on the top surface of YSZ thermal barrier coatings (TBC) was conducted via Nd:YAG pulsed laser. The thermal shock behavior of the TBC before and after laser cladding was modified by heating at 1000 °C for 15 min and quenching in cold water. Phase analysis, microstructural evaluation and elemental analysis were performed using x-ray diffractometry, scanning electron microscopy (SEM), and energy-dispersive spectroscopy. The results of thermal shock tests indicated that the failure in the conventional YSZ (not laser clad) and the laser clad coatings happened after 200 and 270 cycles, respectively. The SEM images of the samples showed that delamination and spallation occurred in both coatings as the main mechanism of failure. Formation of TGO was also observed in the fractured cross section of the samples, which is also a main reason for degradation. Thermal shock resistance in the laser clad coatings improved about 35% after cladding. The improvement is due to the presence of continuous network cracks perpendicular to the surface in the clad layer and also the thermal stability and high melting point of alumina in Al2O3/ZrO2 composite.

Wood (Bagassa guianensis Aubl) and green coconut mesocarp (cocos nucifera) residues as textile dye removers (Remazol Red and Remazol Brilliant Violet).

PubMed

Monteiro, Mônica S; de Farias, Robson F; Chaves, José Alberto Pestana; Santana, Sirlane A; Silva, Hildo A S; Bezerra, Cícero W B

2017-12-15

In this work the efficiency of two lignocellulosic waste materials, wood residues and coconut mesocarp, were investigated as adsorbents towards two representative textile dyes (Remazol Red, RR and Remazol Brilliant Violet, RBV). The moisture, carbohydrate, protein, lipid, ash and fiber contents of both natural matrices were characterized. The materials were also characterized by infrared spectroscopy, X-ray diffractometry, scanning electron microscopy, specific surface area analysis and thermogravimetry. The adsorption of dyes was monitored by using UV-Vis spectrophotometry. It was verified that both, coconut mesocarp (CM) and wood residues can act as effective adsorbents towards the investigated dyes. It is verified that the maximum adsorption capacity Γ M (mg g -1 ) for RBV and RR are 7.28 and 3.97 towards CM and 0.64 and 0.71 towrads SD. Furthermore, it was verified that the adsorption is strongly pH dependent and, as a general behavior, an increase in the pH value is associated with a decrease of the total amount of adsorbed dye. The adsorption of violet dye onto coconut mesocarp is well described by the Langmuir model, while all the remazol red fitted better with the Freundlich equation. Copyright © 2017 Elsevier Ltd. All rights reserved.

p-type zinc-blende GaN on GaAs substrates

NASA Astrophysics Data System (ADS)

Lin, M. E.; Xue, G.; Zhou, G. L.; Greene, J. E.; Morkoç, H.

1993-08-01

We report p-type cubic GaN. The Mg-doped layers were grown on vicinal (100) GaAs substrates by plasma-enhanced molecular beam epitaxy. Thermally sublimed Mg was, with N2 carrier gas, fed into an electron-cyclotron resonance source. p-type zinc-blende-structure GaN films were achieved with hole mobilities as high as 39 cm2/V s at room temperature. The cubic nature of the films were confirmed by x-ray diffractometry. The depth profile of Mg was investigated by secondary ions mass spectroscopy.

Mineralogical variation in the size fractions of a Ranong kaolin, southern Thailand

NASA Astrophysics Data System (ADS)

Pisutha-Arnond, Visut; Phuvichit, Suraphol; Leepowpanth, Quanchai

A representative crude Ranong kaolin from the Thungkla-Ranong mine was separated into > 2 mm (granule), 2-1 mm (very coarse sand), 1-0.5 mm (coarse sand), 0.5-0.25 mm (medium sand), 0.25-0.125 mm (fine sand), 0.125-0.062 mm (very fine sand) and 62-28, 28-14, 17-7, 7-4, 4-2, 2-1 and < 1 μ m size fractions. Those size fractions were analyzed by X-ray powder diffractometry (XRD), differential thermal analysis (DTA), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) with attached energy dispersive X-ray spectrometer (EDX). Kaolin group minerals were differentiated by using XRD in combination with various chemical and heat treatments together with TEM, SEM and DTA. The Ranong kaolin consists predominantly of tubular halloysite, poorly crystallized kaolinite and quartz with minor amounts of mica and K-feldspars. Other trace constituents include gibbsite, tourmaline, zircon and colored impurities (i.e. extractable iron hydroxide coating on clay mineral surface). The kaolin minerals are found in all size fractions by which their contents and halloysite/kaolinite ratios increase as the particle sizes become finer. Quartz and mica are also detected in almost all size fractions. They are, however, more abundant with coarsening particle size. Gibbsite, K-feldspar and tourmaline are mainly concentrated in the fine sand to silt size fractions. Crystallinity of kaolin minerals as measured by XRD varied moderately with size. Relatively pure kaolin minerals, predominantly halloysite and kaolinite, can be obtained in the particle size below 1 or 2 μm.

High-throughput multipesticides residue analysis in earthworms by the improvement of purification method: Development and application of magnetic Fe3 O4 -SiO2 nanoparticles based dispersive solid-phase extraction.

PubMed

Sun, Yuhan; Qi, Peipei; Cang, Tao; Wang, Zhiwei; Wang, Xiangyun; Yang, Xuewei; Wang, Lidong; Xu, Xiahong; Wang, Qiang; Wang, Xinquan; Zhao, Changshan

2018-06-01

As a key representative organism, earthworms can directly illustrate the influence of pesticides on environmental organisms in soil ecosystems. The present work aimed to develop a high-throughput multipesticides residue analytical method for earthworms using solid-liquid extraction with acetonitrile as the solvent and magnetic material-based dispersive solid-phase extraction for purification. Magnetic Fe 3 O 4 nanoparticles were modified with a thin silica layer to form Fe 3 O 4 -SiO 2 nanoparticles, which were fully characterized by field-emission scanning electron microscopy, transmission electron microscopy, Fourier-transform infrared spectroscopy, X-ray diffractometry, and vibrating sample magnetometry. The Fe 3 O 4 -SiO 2 nanoparticles were used as the separation media in dispersive solid-phase extraction with primary secondary amine and ZrO 2 as the cleanup adsorbents to eliminate matrix interferences. The amounts of nanoparticles and adsorbents were optimized for the simultaneous determination of 44 pesticides and six metabolites in earthworms by liquid chromatography with tandem mass spectrometry. The method performance was systematically validated with satisfactory results. The limits of quantification were 20 μg/kg for all analytes studied, while the recoveries of the target analytes ranged from 65.1 to 127% with relative standard deviation values lower than 15.0%. The developed method was subsequently utilized to explore the bioaccumulation of bitertanol in earthworms exposed to contaminated soil, verifying its feasibility for real sample analysis. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Analysis of physicochemical properties of ternary systems of oxaprozin with randomly methylated-ß-cyclodextrin and l-arginine aimed to improve the drug solubility.

PubMed

Mennini, Natascia; Maestrelli, Francesca; Cirri, Marzia; Mura, Paola

2016-09-10

The influence of l-arginine on the complexing and solubilizing power of randomly-methylated-β-cyclodextrin (RameβCD) towards oxaprozin, a very poorly soluble anti-inflammatory drug, was examined. The interactions between the components were investigated both in solution, by phase-solubility analysis, and in the solid state, by differential scanning calorimetry, FTIR and X-ray powder diffractometry. The morphology of the solid products was examined by Scanning Electron Microscopy. Results of phase-solubility studies indicated that addition of arginine enhanced the RameβCD complexing and solubilizing power of about 3.0 and 4.5 times, respectively, in comparison with the binary complex (both at pH≈6.8). The effect of arginine was not simply additive, but synergistic, being the ternary system solubility higher than the sum of those of the respective drug-CD and drug-arginine binary systems. Solid equimolar ternary systems were prepared by physical mixing, co-grinding, coevaporation and kneading techniques, to explore the effect of the preparation method on the physicochemical properties of the final products. The ternary co-ground product exhibited a dramatic increase in both drug dissolution efficiency and percent dissolved at 60min, whose values (83.6 and 97.1, respectively) were about 3 times higher than the sum of those given by the respective drug-CD and drug-aminoacid binary systems. Therefore, the ternary co-ground system with arginine and RameβCD appears as a very valuable product for the development of new more effective delivery systems of oxaprozin, with improved safety and bioavailability. Copyright © 2016 Elsevier B.V. All rights reserved.

Novel inclusion complex of ibuprofen tromethamine with cyclodextrins: physico-chemical characterization.

PubMed

Al Omari, Mahmoud M; Daraghmeh, Nidal H; El-Barghouthi, Musa I; Zughul, Mohammad B; Chowdhry, Babur Z; Leharne, Stephen A; Badwan, Adnan A

2009-10-15

Guest-host interactions of ibuprofen tromethamine salt (Ibu.T) with native and modified cyclodextrins (CyDs) have been investigated using several techniques, namely phase solubility diagrams (PSDs), proton nuclear magnetic resonance ((1)H NMR), differential scanning calorimetry (DSC), Fourier transform infrared spectroscopy (FT-IR), X-ray powder diffractometry (XRPD), scanning-electron microscopy (SEM) and molecular mechanics (MM). From the analysis of PSD data (A(L)-type) it is concluded that the anionic tromethamine salt of ibuprofen (pK(a)=4.55) forms 1:1 soluble complexes with all CyDs investigated in buffered water at pH 7.0, while the neutral form of Ibu forms an insoluble complex with beta-CyD (B(S)-type) in buffered water at pH 2.0. Ibu.T has a lower tendency to complex with beta-CyD (K(11)=58 M(-1) at pH 7.0) compared with the neutral Ibu (K(11)=4200 M(-1)) in water. Complex formation of Ibu.T with beta-CyD (DeltaG(o)=-20.4 kJ/mol) is enthalpy driven (DeltaH(o)=-22.9 kJ/mol) and is accompanied by a small unfavorable entropy (DeltaS(o)=-8.4 J/mol K) change. (1)H NMR studies and MM computations revealed that, on complexation, the hydrophobic central benzene ring of Ibu.T and part of the isobutyl group reside within the beta-CyD cavity leaving the peripheral groups (carboxylate, tromethamine and methyl groups) located near the hydroxyl group networks at either rim of beta-CyD. PSD, (1)H NMR, DSC, FT-IR, XRPD, SEM and MM studies confirmed the formation of Ibu.T/beta-CyD inclusion complex in solution and the solid state.

A new nanospray drying method for the preparation of nicergoline pure nanoparticles

NASA Astrophysics Data System (ADS)

Martena, Valentina; Censi, Roberta; Hoti, Ela; Malaj, Ledjan; Di Martino, Piera

2012-06-01

Three different batches of pure nanoparticles (NPs) of nicergoline (NIC) were prepared by spray drying a water:ethanol solution by a new Nano Spray Dryer Büchi B-90. Spherical pure NPs were obtained, and several analytical techniques such as differential scanning calorimetry and X-ray powder diffractometry permitted to assess their amorphous character. A comparison of the solubility, intrinsic dissolution, and drug release of original particles and pure amorphous NPs were determined, revealing an interesting improvement of biopharmaceutical properties of amorphous NPs, due to both amorphous properties and nanosize dimensions. Since in a previous work, the high-thermodynamic stability of amorphous NIC was demonstrated, this study is addressed toward the formulation of NIC as pure amorphous NPs.

Application of film-casting technique to investigate drug-polymer miscibility in solid dispersion and hot-melt extrudate.

PubMed

Parikh, Tapan; Gupta, Simerdeep Singh; Meena, Anuprabha K; Vitez, Imre; Mahajan, Nidhi; Serajuddin, Abu T M

2015-07-01

Determination of drug-polymer miscibility is critical for successful development of solid dispersions. This report details a practical method to predict miscibility and physical stability of drug with various polymers in solid dispersion and, especially, in melt extrudates by applying a film-casting technique. Mixtures of itraconazole (ITZ) with hydroxypropylmethylcellulose phthalate (HPMCP), Kollidon(®) VA 64, Eudragit(®) E PO, and Soluplus(®) were film-casted, exposed to 40°C/75% RH for 1 month and then analyzed using differential scanning calorimetry (DSC), powder X-ray diffractometry, and polarized light microscopy (PLM). ITZ had the highest miscibility with HPMCP, being miscible at drug to polymer ratio of 6:4 (w/w). There was a downward trend of lower miscibility with Soluplus(®) (miscible at 3:7, w/w, and a few microcrystals present at 4:6, w/w), Kollidon(®) VA 64 (2:8, w/w) and Eudragit(®) E PO (<1:9, w/w). PLM was found more sensitive to detect drug crystallization than DSC and powder X-ray diffractometry. There was general correlation between results of film casting and hot-melt extrusion (HME) using a twin screw extruder. For ITZ-Soluplus(®) mixtures, HME at 4:6 (w/w) resulted in a single phase, whereas drug crystallization was observed at higher drug load. HME of ITZ-Kollidon(®) VA 64 mixtures also correlated well with the miscibility predicted by film casting. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association.

Ultrafast electron diffraction and electron microscopy: present status and future prospects

NASA Astrophysics Data System (ADS)

Ishchenko, A. A.; Aseyev, S. A.; Bagratashvili, V. N.; Panchenko, V. Ya; Ryabov, E. A.

2014-07-01

Acting as complementary research tools, high time-resolved spectroscopy and diffractometry techniques proceeding from various physical principles open up new possibilities for studying matter with necessary integration of the 'structure-dynamics-function' triad in physics, chemistry, biology and materials science. Since the 1980s, a new field of research has started at the leading research laboratories, aimed at developing means of filming the coherent dynamics of nuclei in molecules and fast processes in biological objects ('atomic and molecular movies'). The utilization of ultrashort laser pulse sources has significantly modified traditional electron beam approaches to and provided high space-time resolution for the study of materials. Diffraction methods using frame-by-frame filming and the development of the main principles of the study of coherent dynamics of atoms have paved the way to observing wave packet dynamics, the intermediate states of reaction centers, and the dynamics of electrons in molecules, thus allowing a transition from the kinetics to the dynamics of the phase trajectories of molecules in the investigation of chemical reactions.

Functionalization of 2D macroporous silicon under the high-pressure oxidation

NASA Astrophysics Data System (ADS)

Karachevtseva, L.; Kartel, M.; Kladko, V.; Gudymenko, O.; Bo, Wang; Bratus, V.; Lytvynenko, O.; Onyshchenko, V.; Stronska, O.

2018-03-01

Addition functionalization after high-pressure oxidation of 2D macroporous silicon structures is evaluated. X-ray diffractometry indicates formation of orthorhombic SiO2 phase on macroporous silicon at oxide thickness of 800-1200 nm due to cylindrical symmetry of macropores and high thermal expansion coefficient of SiO2. Pb center concentration grows with the splitting energy of LO- and TO-phonons and SiO2 thickness in oxidized macroporous silicon structures. This increase EPR signal amplitude and GHz radiation absorption and is promising for development of high-frequency devices and electronically controlled elements.

In vitro biocompatibility of magnesium-incorporated submicro-porous titanium oxide surface produced by hydrothermal treatment

NASA Astrophysics Data System (ADS)

Park, Jin-Woo; Kim, Youn-Jeong; Jang, Je-Hee; An, Chang-Hyeon

2010-11-01

This study investigated the surface characteristics and in vitro biocompatibility of titanium (Ti) oxide surface incorporating magnesium ions (Mg), produced by hydrothermal treatment using an alkaline Mg-containing solution, for future biomedical applications. The surface characteristics were evaluated by scanning electron microscopy, thin-film X-ray diffractometry, X-ray photoelectron spectroscopy, inductively coupled plasma-atomic emission spectroscopy (ICP-AES) and optical profilometry. Mouse calvaria-derived osteoblastic cell (MC3T3-E1) attachment, spreading, proliferation, alkaline phosphatase (ALP) activity, and osteoblastic gene expression on Mg-containing surfaces were compared with untreated Ti surfaces. Hydrothermal treatment resulted in Mg-incorporated Ti oxide layer with submicro-porous surface structures approximately 2 μm in thickness. ICP-AES analysis revealed Mg ions release from treated surfaces into the solution. The Mg-incorporated surface displayed significantly increased cellular attachment and ALP activity compared with untreated surface ( p < 0.05), and supported better cell spreading. Real-time polymerase chain reaction analysis showed notably higher mRNA expression of the osteoblast transcription factor genes (Dlx5, Runx2) and the osteoblast phenotype genes (ALP, bone sialoprotein and osteocalcin) in cells grown on the Mg-incorporated surfaces than untreated surfaces. These results demonstrate that the Mg-incorporated submicro-porous Ti oxide surface produced by hydrothermal treatment may improve implant osseointegration by enhancing the attachment, spreading and differentiation of osteoblastic cells.

Structural characterization of silver nanoparticles phyto-mediated by a plant waste, seed hull of Vigna mungo and their biological applications

NASA Astrophysics Data System (ADS)

Varadavenkatesan, Thivaharan; Vinayagam, Ramesh; Selvaraj, Raja

2017-11-01

Nanobiotechnology has rapidly become a critical facet of nanotechnology. The green synthesis of silver nanoparticles, making use of the hull of black gram (Vigna mungo), paves the way for a simple and eco-friendly utilization of a domestic waste to a product with antioxidant and anticoagulant activities. The emergence of silver nanoparticles was characterized by a variety of methods UV-visible spectrophotometry, scanning electron microscopy added to energy dispersive spectroscopy, X-ray diffractometry, particle size distribution and FT-IR spectroscopy analyses. A discrete band at 421 nm was obtained from UV-visible spectroscopy of the silver nanoparticle suspension. The extract sourced from the hull of black gram showed evidence of the presence of a variety of functional moieties of phytochemicals using FTIR spectroscopy. These were also deemed responsible for maintaining the stability of silver nanoparticles. SEM and EDAX techniques combined, proved that the zero-valent silver nanoparticles were lesser than 100 nm in size. The crystallinity of the nanoparticles was confirmed, as deduced by the (1 1 1) plane, from XRD analysis. The potential of the phytochemicals in maintaining the steadiness of nanoparticles was implied by the zeta potential value that stood at -30.3 mV. In the current study, we have endeavored to comprehend the antioxidant and anticoagulant nature of the green-synthesized benign silver nanoparticles.

Energy dispersive X-ray fluorescence spectroscopy/Monte Carlo simulation approach for the non-destructive analysis of corrosion patina-bearing alloys in archaeological bronzes: The case of the bowl from the Fareleira 3 site (Vidigueira, South Portugal)

NASA Astrophysics Data System (ADS)

Bottaini, C.; Mirão, J.; Figuereido, M.; Candeias, A.; Brunetti, A.; Schiavon, N.

2015-01-01

Energy dispersive X-ray fluorescence (EDXRF) is a well-known technique for non-destructive and in situ analysis of archaeological artifacts both in terms of the qualitative and quantitative elemental composition because of its rapidity and non-destructiveness. In this study EDXRF and realistic Monte Carlo simulation using the X-ray Monte Carlo (XRMC) code package have been combined to characterize a Cu-based bowl from the Iron Age burial from Fareleira 3 (Southern Portugal). The artifact displays a multilayered structure made up of three distinct layers: a) alloy substrate; b) green oxidized corrosion patina; and c) brownish carbonate soil-derived crust. To assess the reliability of Monte Carlo simulation in reproducing the composition of the bulk metal of the objects without recurring to potentially damaging patina's and crust's removal, portable EDXRF analysis was performed on cleaned and patina/crust coated areas of the artifact. Patina has been characterized by micro X-ray Diffractometry (μXRD) and Back-Scattered Scanning Electron Microscopy + Energy Dispersive Spectroscopy (BSEM + EDS). Results indicate that the EDXRF/Monte Carlo protocol is well suited when a two-layered model is considered, whereas in areas where the patina + crust surface coating is too thick, X-rays from the alloy substrate are not able to exit the sample.

Modeling the formation of the quench product in municipal solid waste incineration (MSWI) bottom ash.

PubMed

Inkaew, Kanawut; Saffarzadeh, Amirhomayoun; Shimaoka, Takayuki

2016-06-01

This study investigated changes in bottom ash morphology and mineralogy under lab-scale quenching conditions. The main purpose was to clarify the mechanisms behind the formation of the quench product/layer around bottom ash particles. In the experiments, the unquenched bottom ashes were heated to 300°C for 1h, and were quenched by warm water (65°C) with different simulated conditions. After having filtered and dried, the ashes were analyzed by a combination of methodologies namely, particle size distribution analysis, intact particle and thin-section observation, X-ray diffractometry, and scanning electron microscope with energy dispersive X-ray spectroscopy. The results indicated that after quenching, the morphology and mineralogy of the bottom ash changed significantly. The freshly quenched bottom ash was dominated by a quench product that was characterized by amorphous and microcrystalline calcium-silicate-hydrate (CSH) phases. This product also enclosed tiny minerals, glasses, ceramics, metals, and organic materials. The dominant mineral phases produced by quenching process and detected by XRD were calcite, Friedel's salt, hydrocalumite and portlandite. The formation of quench product was controlled by the fine fraction of the bottom ash (particle size <0.425mm). From the observations, a conceptual model of the ash-water reactions and formation of the quench product in the bottom ash was proposed. Copyright © 2016 Elsevier Ltd. All rights reserved.

Mechanochemical synthesis and intercalation of Ca(II)Fe(III)-layered double hydroxides

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ferencz, Zs.; Szabados, M.; Varga, G.

2016-01-15

A mechanochemical method (grinding the components without added water – dry grinding, followed by further grinding in the presence of minute amount of water or NaOH solution – wet grinding) was used in this work for the preparation and intercalation of CaFe-layered double hydroxides (LDHs). Both the pristine LDHs and the amino acid anion (cystinate and tyrosinate) intercalated varieties were prepared by the two-step grinding procedure in a mixer mill. By systematically changing the conditions of the preparation method, a set of parameters could be determined, which led to the formation of close to phase-pure LDH. The optimisation procedure wasmore » also applied for the intercalation processes of the amino acid anions. The resulting materials were structurally characterised by a range of methods (X-ray diffractometry, scanning electron microscopy, energy dispersive analysis, thermogravimetry, X-ray absorption and infra-red spectroscopies). It was proven that this simple mechanochemical procedure was able to produce complex organic–inorganic nanocomposites: LDHs intercalated with amino acid anions. - Graphical abstract: Amino acid anion-Ca(II)Fe(III)-LDHs were successfully prepared by a two-step milling procedure. - Highlights: • Synthesis of pristine and amino acid intercalated CaFe-LDHs by two-step milling. • Identifying the optimum synthesis and intercalation parameters. • Characterisation of the samples with a range of instrumental methods.« less

Material Analysis of Coated Siliconized Silicon Carbide (SiSiC) Honeycomb Structures for Thermochemical Hydrogen Production

PubMed Central

Neises-von Puttkamer, Martina; Simon, Heike; Schmücker, Martin; Roeb, Martin; Sattler, Christian; Pitz-Paal, Robert

2013-01-01

In the present work, thermochemical water splitting with siliconized silicon carbide (SiSiC) honeycombs coated with a zinc ferrite redox material was investigated. The small scale coated monoliths were tested in a laboratory test-rig and characterized by X-ray diffractometry (XRD) and Scanning Electron Microscopy (SEM) with corresponding micro analysis after testing in order to characterize the changes in morphology and composition. Comparison of several treated monoliths revealed the formation of various reaction products such as SiO2, zircon (ZrSiO4), iron silicide (FeSi) and hercynite (FeAl2O4) indicating the occurrence of various side reactions between the different phases of the coating as well as between the coating and the SiSiC substrate. The investigations showed that the ferrite is mainly reduced through reaction with silicon (Si), which is present in the SiSiC matrix, and silicon carbide (SiC). These results led to the formulation of a new redox mechanism for this system in which Zn-ferrite is reduced through Si forming silicon dioxide (SiO2) and through SiC forming SiO2 and carbon monoxide. A decline of hydrogen production within the first 20 cycles is suggested to be due to the growth of a silicon dioxide and zircon layer which acts as a diffusion barrier for the reacting specie. PMID:28809316

Material Analysis of Coated Siliconized Silicon Carbide (SiSiC) Honeycomb Structures for Thermochemical Hydrogen Production.

PubMed

Neises-von Puttkamer, Martina; Simon, Heike; Schmücker, Martin; Roeb, Martin; Sattler, Christian; Pitz-Paal, Robert

2013-01-31

In the present work, thermochemical water splitting with siliconized silicon carbide (SiSiC) honeycombs coated with a zinc ferrite redox material was investigated. The small scale coated monoliths were tested in a laboratory test-rig and characterized by X-ray diffractometry (XRD) and Scanning Electron Microscopy (SEM) with corresponding micro analysis after testing in order to characterize the changes in morphology and composition. Comparison of several treated monoliths revealed the formation of various reaction products such as SiO₂, zircon (ZrSiO₄), iron silicide (FeSi) and hercynite (FeAl₂O₄) indicating the occurrence of various side reactions between the different phases of the coating as well as between the coating and the SiSiC substrate. The investigations showed that the ferrite is mainly reduced through reaction with silicon (Si), which is present in the SiSiC matrix, and silicon carbide (SiC). These results led to the formulation of a new redox mechanism for this system in which Zn-ferrite is reduced through Si forming silicon dioxide (SiO₂) and through SiC forming SiO₂ and carbon monoxide. A decline of hydrogen production within the first 20 cycles is suggested to be due to the growth of a silicon dioxide and zircon layer which acts as a diffusion barrier for the reacting specie.

Oxidation study of coated Crofer 22 APU steel in dry oxygen

NASA Astrophysics Data System (ADS)

Molin, Sebastian; Chen, Ming; Hendriksen, Peter Vang

2014-04-01

The effect of a dual layer coating composed of a layer of a Co3O4 and a layer of a La0.85Sr0.15MnO3/Co3O4 mixture on the high temperature corrosion of the Crofer 22 APU alloy is reported. Oxidation experiments were performed in dry oxygen at three temperatures: 800 °C, 850 °C and 900 °C for periods up to 1000 h. Additionally at 850 °C a 5000 h long oxidation test was performed to evaluate longer term suitability of the proposed coating. Corrosion kinetics were evaluated by measuring mass gain during oxidation. The corrosion kinetics for the coated samples are analyzed in terms of a parabolic rate law. Microstructural features were investigated by scanning electron microscopy, energy dispersive X-ray analysis and X-ray diffractometry. The coating is effective in reducing the corrosion rate and in ensuring long lifetime of coated alloys. The calculated activation energy for the corrosion process is around 1.8 eV. A complex Co-Mn-Cr spinel is formed caused by diffusion of Cr and Mn from the alloy into the Co3O4 coating and by additional diffusion of Mn from the LSM layer. Adding a layer of LSM/Co3O4, acting as an additional Mn source, on top of the cobalt spinel is beneficial for the improved corrosion resistance.

Microwave-driven asbestos treatment and its scale-up for use after natural disasters.

PubMed

Horikoshi, Satoshi; Sumi, Takuya; Ito, Shigeyuki; Dillert, Ralf; Kashimura, Keiichiro; Yoshikawa, Noboru; Sato, Motoyasu; Shinohara, Naoki

2014-06-17

Asbestos-containing debris generated by the tsunami after the Great East Japan Earthquake of March 11, 2011, was processed by microwave heating. The analysis of the treated samples employing thermo gravimetry, differential thermal analysis, X-ray diffractometry, scanning electron microscopy, and phase-contrast microscopy revealed the rapid detoxification of the waste by conversion of the asbestos fibers to a nonfibrous glassy material. The detoxification by the microwave method occurred at a significantly lower processing temperature than the thermal methods actually established for the treatment of asbestos-containing waste. The lower treatment temperature is considered to be a consequence of the microwave penetration depth into the waste material and the increased intensity of the microwave electric field in the gaps between the asbestos fibers resulting in a rapid heating of the fibers inside the debris. A continuous treatment plant having a capacity of 2000 kg day(-1) of asbestos-containing waste was built in the area affected by the earthquake disaster. This treatment plant consists of a rotary kiln to burn the combustible waste (wood) and a microwave rotary kiln to treat asbestos-containing inorganic materials. The hot flue gas produced by the combustion of wood is introduced into the connected microwave rotary kiln to increase the energy efficiency of the combined process. Successful operation of this combined device with regard to asbestos decomposition is demonstrated.

Pretreatment of eucalyptus wood chips for enzymatic saccharification using combined sulfuric acid-free ethanol cooking and ball milling.

PubMed

Teramoto, Yoshikuni; Tanaka, Noriko; Lee, Seung-Hwan; Endo, Takashi

2008-01-01

A combined sulfuric acid-free ethanol cooking and pulverization process was developed in order to achieve the complete saccharification of the cellulosic component of woody biomass, thereby avoiding the problems associated with the use of strong acid catalysts. Eucalyptus wood chips were used as a raw material and exposed to an ethanol/water/acetic acid mixed solvent in an autoclave. This process can cause the fibrillation of wood chips. During the process, the production of furfural due to an excessive degradation of polysaccharide components was extremely low and delignification was insignificant. Therefore, the cooking process is regarded not as a delignification but as an activation of the original wood. Subsequently, the activated solid products were pulverized by ball-milling in order to improve their enzymatic digestibility. Enzymatic hydrolysis experiments demonstrated that the conversion of the cellulosic components into glucose attained 100% under optimal conditions. Wide-angle X-ray diffractometry and particle size distribution analysis revealed that the scale affecting the improvement of enzymatic digestibility ranged from 10 nm to 1 microm. Field emission scanning electron microscopy depicted that the sulfuric acid-free ethanol cooking induced a pore formation by the removal of part of the lignin and hemicellulose fractions in the size range from a few of tens nanometers to several hundred nanometers. (c) 2007 Wiley Periodicals, Inc.

Development of highly porous scaffolds based on bioactive silicates for dental tissue engineering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Goudouri, O.M., E-mail: menti.goudouri@ww.uni-erlangen.de; Department of Physics, Aristotle University of Thessaloniki, 54124 Thessaloniki; Theodosoglou, E.

Graphical abstract: - Highlights: • Synthesis of an Mg-based glass-ceramic via the sol–gel technique. • The heat treatment of the glass-ceramic promoted the crystallization of akermanite. • Akermanite scaffolds coated with gelatin were successfully fabricated. • An HCAp layer was developed on the surface of all scaffolds after 9 days in SBF. - Abstract: Various scaffolding materials, ceramics and especially Mg-based ceramic materials, including akermanite (Ca{sub 2}MgSi{sub 2}O{sub 7}) and diopside (CaMgSi{sub 2}O{sub 6}), have attracted interest for dental tissue regeneration because of their improved mechanical properties and controllable biodegradation. The aim of the present work was the synthesis ofmore » an Mg-based glass-ceramic, which would be used for the construction of workable akermanite scaffolds. The characterization of the synthesized material was performed by Fourier Transform Infrared Spectroscopy (FTIR) X-Ray Diffractometry (XRD) and Scanning Electron Microscopy (SEM). Finally, the apatite forming ability of the scaffolds was assessed by immersion in simulated body fluid. The scaffolds were fabricated by the foam replica technique and were subsequently coated with gelatin to provide a functional surface for increased cell attachment. Finally, SEM microphotographs and FTIR spectra of the scaffolds after immersion in SBF solution indicated the inorganic bioactive character of the scaffolds suitable for the intended applications in dental tissue engineering.« less

The effect of nanoparticles size on photocatalytic and antimicrobial properties of Ag-Pt/TiO2 photocatalysts

NASA Astrophysics Data System (ADS)

Zielińska-Jurek, Anna; Wei, Zhishun; Wysocka, Izabela; Szweda, Piotr; Kowalska, Ewa

2015-10-01

Ag-Pt-modified TiO2 nanocomposites were synthesized using the sol-gel method. Bimetallic modified TiO2 nanoparticles exhibited improved photocatalytic activity under visible-light irradiation, better than monometallic Ag/TiO2 and Pt/TiO2 nanoparticles (NPs). All modified powders showed localized surface plasmon resonance (LSPR) in visible region. The photocatalysts' characteristics by X-ray diffractometry (XRD), scanning transmission electron microscopy (STEM), diffuse reflectance spectroscopy (DRS), X-ray photoelectron spectroscopy (XPS), nitrogen adsorption (BET method for specific surface area) showed that sample with the highest photocatalytic activity had anatase structure, about 93 m2/g specific surface area, maximum plasmon absorption at ca. 420 nm and contained small NPs of silver of 6 nm and very fine platinum NPs of 3 nm. The photocatalytic activity was estimated by measuring the decomposition rate of phenol in 0.2 mM aqueous solution under Vis and UV/vis light irradiation. It was found that size of platinum was decisive for the photocatalytic activity under visible light irradiation, i.e., the smaller Pt NPs were, the higher was photocatalytic activity. While, antimicrobial activities, estimated for bacteria Escherichia coli and Staphylococcus aureus, and pathogenic fungi belonging to Candida family, were only observed for photocatalysts containing silver, i.e., Ag/TiO2 and Ag-Pt/TiO2 nanocomposites.

Differentiations of Chitin Content and Surface Morphologies of Chitins Extracted from Male and Female Grasshopper Species

PubMed Central

Kaya, Murat; Lelešius, Evaldas; Nagrockaitė, Radvilė; Sargin, Idris; Arslan, Gulsin; Mol, Abbas; Baran, Talat; Can, Esra; Bitim, Betul

2015-01-01

In this study, we used Fourier transform infrared spectroscopy (FT-IR), elemental analysis (EA), thermogravimetric analysis (TGA), X-ray diffractometry (XRD), and scanning electron microscopy (SEM) to investigate chitin structure isolated from both sexes of four grasshopper species. FT-IR, EA, XRD, and TGA showed that the chitin was in the alpha form. With respect to gender, two main differences were observed. First, we observed that the quantity of chitin was greater in males than in females and the dry weight of chitin between species ranged from 4.71% to 11.84%. Second, using SEM, we observed that the male chitin surface structure contained 25 – 90nm wide nanofibers and 90 – 250 nm nanopores, while no pores or nanofibers were observed in the chitin surface structure of the majority of females (nanofibers were observed only in M. desertus females). In contrast, the elemental analysis, thermal properties, and crystalline index values for chitin were similar in males and females. Also, we carried out enzymatic digestion of the isolated chitins using commercial chitinase from Streptomyces griseus. We observed that there were no big differences in digestion rate of the chitins from both sexes and commercial chitin. The digestion rates were for grasshoppers’ chitins; 88.45–95.48% and for commercial chitin; 94.95%. PMID:25635814

Cu-Doped ZnO Thin Films Deposited by a Sol-Gel Process Using Two Copper Precursors: Gas-Sensing Performance in a Propane Atmosphere

PubMed Central

Gómez-Pozos, Heberto; Arredondo, Emma Julia Luna; Maldonado Álvarez, Arturo; Biswal, Rajesh; Kudriavtsev, Yuriy; Pérez, Jaime Vega; Casallas-Moreno, Yenny Lucero; Olvera Amador, María de la Luz

2016-01-01

A study on the propane gas-sensing properties of Cu-doped ZnO thin films is presented in this work. The films were deposited on glass substrates by sol-gel and dip coating methods, using zinc acetate as a zinc precursor, copper acetate and copper chloride as precursors for doping. For higher sensitivity values, two film thickness values are controlled by the six and eight dippings, whereas for doping, three dippings were used, irrespective of the Cu precursor. The film structure was analyzed by X-ray diffractometry, and the analysis of the surface morphology and film composition was made through scanning electron microscopy (SEM) and secondary ion mass spectroscopy (SIMS), respectively. The sensing properties of Cu-doped ZnO thin films were then characterized in a propane atmosphere, C3H8, at different concentration levels and different operation temperatures of 100, 200 and 300 °C. Cu-doped ZnO films doped with copper chloride presented the highest sensitivity of approximately 6 × 104, confirming a strong dependence on the dopant precursor type. The results obtained in this work show that the use of Cu as a dopant in ZnO films processed by sol-gel produces excellent catalysts for sensing C3H8 gas. PMID:28787885

Magnetron sputtering fabrication and photoelectric properties of WSe2 film solar cell device

NASA Astrophysics Data System (ADS)

Mao, Xu; Zou, Jianpeng; Li, Hongchao; Song, Zhengqi; He, Siru

2018-06-01

Tungsten diselenide (WSe2) films with different growing orientations exhibit diverse photoelectric properties. The WSe2 film with C-axis⊥substrate texture has been prepared and applied to thin-film solar cells. W nanofilms with a thickness of 270 nm were deposited onto the Mo bottom electrode and then heat-treated in selenium vapor to synthesize WSe2 films with a thickness of 1 μm. ZnO films were deposited onto WSe2 films to form a P-N junction and ITO films were deposited subsequently as the conductive layer. X-ray diffractometry, scanning electron microscopy and UV-vis-NIR spectro-analysis instrument were employed to analyze the phase composition, optical absorptivity and micromorphology of WSe2 films and the WSe2 solar cell device. WSe2 films exhibit excellent photoelectric performance with an optical absorption coefficient greater than 105 cm-1 across the visible spectrum. The calculated direct and indirect band gap of the WSe2 films is 1.48 eV and 1.25 eV, respectively. With the application of standard glass/Mo/WSe2/ZnO/ITO/Ag device structure, the open-circuit voltage of the battery device is 82 mV. The short-circuit current density is 2.98 mA/cm2 and the filling factor is 0.32. The photoelectric conversion efficiency of the WSe2 film solar cell device is 0.79%.

Surface modification using the biomimetic method in alumina-zirconia porous ceramics obtained by the replica method.

PubMed

Silva, André D R; Rigoli, Willian R; Osiro, Denise; Mello, Daphne C R; Vasconcellos, Luana M R; Lobo, Anderson O; Pallone, Eliria M J A

2018-01-12

The modification of biomaterials approved by the Food and Drug Administration could be an alternative to reduce the period of use in humans. Porous bioceramics are widely used as support structures for bone formation and repair. This composite has essential characteristics for an implant, including good mechanical properties, high chemical stability, biocompatibility and adequate aesthetic appearance. Here, three-dimensional porous scaffolds of Al 2 O 3 containing 5% by volume of ZrO 2 were produced by the replica method. These scaffolds had their surfaces chemically treated with phosphoric acid and were coated with calcium phosphate using the biomimetic method simulated body fluid (SBF, 5×) for 14 days. The scaffolds, before and after biomimetic coating, were characterized mechanically, morphologically and structurally by axial compression tests, scanning electron microscopy, microtomography, apparent porosity, X-ray diffractometry, near-infrared spectroscopy, inductively coupled plasma optical emission spectroscopy, energy dispersive X-ray spectroscopy and reactivity. The in vitro cell viability and formation of mineralization nodules were used to identify the potential for bone regeneration. The produced scaffols after immersion in SBF were able to induce the nodules formation. These characteristics are advantaged by the formation of different phases of calcium phosphates on the material surface in a reduced incubation period. © 2018 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 2018. © 2018 Wiley Periodicals, Inc.

Effect of graphite addition into mill scale waste as a potential bipolar plates material of proton exchange membrane fuel cells

NASA Astrophysics Data System (ADS)

Khaerudini, D. S.; Prakoso, G. B.; Insiyanda, D. R.; Widodo, H.; Destyorini, F.; Indayaningsih, N.

2018-03-01

Bipolar plates (BPP) is a vital component of proton exchange membrane fuel cells (PEMFC), which supplies fuel and oxidant to reactive sites, remove reaction products, collects produced current and provide mechanical support for the cells in the stack. This work concerns the utilization of mill scale, a by-product of iron and steel formed during the hot rolling of steel, as a potential material for use as BPP in PEMFC. On the other hand, mill scale is considered a very rich in iron source having characteristic required such as for current collector in BPP and would significantly contribute to lower the overall cost of PEMFC based fuel cell systems. In this study, the iron reach source of mill scale powder, after sieving of 150 mesh, was mechanically alloyed with the carbon source containing 5, 10, and 15 wt.% graphite using a shaker mill for 3 h. The mixed powders were then pressed at 300 MPa and sintered at 900 °C for 1 h under inert gas atmosphere. The structural changes of powder particles during mechanical alloying and after sintering were studied by X-ray diffractometry, optical microscopy, scanning electron microscopy, and microhardness measurement. The details of the presence of iron, carbon, and iron carbide (Fe-C) as the products of reactions as well as sufficient mechanical strength of the sintered materials were presented in this report.

Effect of spark plasma sintering on the microstructure and in vitro behavior of plasma sprayed HA coatings.

PubMed

Yu, L-G; Khor, K A; Li, H; Cheang, P

2003-07-01

The crystalline phases and degree of crystallinity in plasma sprayed calcium phosphate coatings on Ti substrates are crucial factors that influence the biological interactions of the materials in vivo. In this study, plasma sprayed hydroxyapatite (HA) coatings underwent post-spray treatment by the spark plasma sintering (SPS) technique at 500 degrees C, 600 degrees C, and 700 degrees C for duration of 5 and 30 min. The activity of the HA coatings before and after SPS are evaluated in vitro in a simulated body fluid. The surface microstructure, crystallinity, and phase composition of each coating is characterized by scanning electron microscopy and X-ray diffractometry before, and after in vitro incubation. Results show that the plasma sprayed coatings treated for 5 min in SPS demonstrated increased proportion of beta-TCP phase with a preferred-orientation in the (214) plane, and the content of beta-TCP phase corresponded to SPS temperature, up to 700 degrees C. SPS treatment at 700 degrees C for 30 min enhanced the HA content in the plasma spray coating as well. The HA coatings treated in SPS for 5 min revealed rapid surface morphological changes during in vitro incubation (up to 12 days), indicating that the surface activity is enhanced by the SPS treatment. The thickest apatite layer was found in the coating treated by SPS at 700 degrees C for 5 min.

Assessment of osteoinduction using a porous hydroxyapatite coating prepared by micro-arc oxidation on a new titanium alloy.

PubMed

Jing, Wensen; Zhang, Minghua; Jin, Lei; Zhao, Jian; Gao, Qing; Ren, Min; Fan, Qingyu

2015-12-01

Surface modification and material improvement is now an important way to improve the osseointegration between bone and uncemented prothesis. The purpose of this study was to investigate the bone ingrowth potential of porous hydroxyapatite (HA) coatings prepared by micro-arc oxidation (MAO) on Ti-3Zr-2Sn-3Mo-25Nb, a new titanium alloy. HA-coated specimens were implanted in the left proximal femoral medullary canal of beagles for 4, 12, and 24 weeks, and uncoated specimens were implanted in the right as a control. The surface morphology and phase composition were investigated with environmental scanning electron microscopy and X-ray diffractometry. The bone ingrowth was assessed by histomorphometry. A pull-out test was performed to assess the mechanical performance of the bone-implant interface. A porous coating was well prepared on the new titanium alloy by using the MAO method. The bone-to-implant contact was significantly higher for the HA-coated group compared to that in the uncoated group. Mechanical tests showed that the HA-coated group had significantly higher maximum force at the bone-implant interface compared to the uncoated specimens. MAO is a suitable coating approach for this new titanium alloy. The HA coating prepared by this approach can significantly promote bone ingrowth and the mechanical performance of the bone-implant interface. Copyright © 2015. Published by Elsevier Ltd.

The negative electrode development for a Ni-MH battery prototype

NASA Astrophysics Data System (ADS)

Cuscueta, D. J.; Ghilarducci, A. A.; Salva, H. R.; Milocco, R. H.; Castro, E. B.

2009-10-01

The negative electrode development for a nickel-metal hydride battery (Ni-MH) prototype was performed with the following procedure: (1) the Lm 0.95Ni 3.8Co 0.3Mn 0.3Al 0.4 (Lm=lanthanum rich mischmetal) intermetallic alloy was elaborated by melting the pure elements in an induction furnace inside a boron nitride crucible under an inert atmosphere, (2) the obtained alloy was crushed and sieved between 44 and 74 μm and mixed with teflonized carbon; (3) the compound was assembled together with a current collector and pressed in a cylindrical matrix. The obtained electrode presented a disc shape, with 11 mm diameter and approximately 1 mm thickness. The crystalline structure of the hydrogen storage alloy was examined using X-ray diffractometry. The measured hcp lattice volume was 1.78% larger than the precursor LaNi 5 intermetallic alloy, increasing the available space for hydrogen movement. Energy dispersive spectroscopy (EDS) and scanning electronic microscopy (SEM) measurements were used before and after hydriding in order to verify the alloy sample homogeneity. The negative electrode was electrochemically tested by using a laboratory cell. It activates almost totally in its first cycle, which is an excellent characteristic from the commercial point of view. The maximum discharge capacity reached was 314.2 mA h/g in the 10th cycle.

Synthesis and characterization of carboxymethyl potato starch and its application in reactive dye printing.

PubMed

Zhang, Bing; Gong, Honghong; Lü, Shaoyu; Ni, Boli; Liu, Mingzhu; Gao, Chunmei; Huang, Yinjuan; Han, Fei

2012-11-01

Carboxymethyl potato starch (CMPS) was synthesized with a simple dry and multi-step method as a product of the reaction of native potato starch and monochloroacetic acid in the presence of sodium hydroxide. The influence of the molar ratio of sodium hydroxide to anhydroglucose unit, the volume of 95% (v/v) ethanol, the rotation rate of motor driven stirrer and the reaction time for degree of substitution (DS) were evaluated. The product was characterized by Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and X-ray diffractometry (XRD). FTIR spectrometry showed new bonds at 1618 and 1424 cm⁻¹ when native starch underwent carboxymethylation. SEM pictures showed that the smooth surface of native starch particles was mostly ruptured. XRD revealed that starch crystallinity was reduced after carboxymethylation. The viscosity of the mixture paste of carboxymethyl starch and sodium alginate (SA) was measured using a rotational viscometer. In addition, the applied effect of mixed paste in reactive dye printing was examined by assessing the fabric stiffness, color yield and sharp edge to the printed image in comparison with SA. And the results indicated that the mixed paste could partially replace SA as thickener in reactive dye printing. The study also showed that the method was low cost and eco-friendly and the product would have an extensive application in reactive dye printing. Copyright © 2012 Elsevier B.V. All rights reserved.

Possible role of Prussian blue nanoparticles in chemical evolution: interaction with ribose nucleotides

NASA Astrophysics Data System (ADS)

Sharma, Rachana; Iqubal, Md. Asif; Kamaluddin

2016-01-01

Ribonucleotides (RMPs) are the building blocks of genetic material consisting of a sugar group, a phosphate group and a nucleobase. Prussian blue (PB) is an ancient compound which is supposed to have formed under the conditions of primitive Earth. The interaction between nucleotides and mineral surfaces is of primary importance in the context of prebiotic chemistry. In the present work, the adsorption of RMPs on PB has been studied in the concentration range 0.4 × 10-4-3.0 × 10-4 M of RMPs at pH 7.5, T = 27°C and found to be 53.1, 41.7, 25.8 and 24.0% for adenosine 5'-monophosphate (5'-AMP), guanosine 5'-monophosphate, cytidine 5'-monophosphate and uridine 5'-monophosphate, respectively. Optimum conditions for the adsorption were studied as a function of concentration, time, amount of adsorbent and pH and data obtained were found to fit the Langmuir adsorption isotherm. Langmuir constants (K L and X m ) values were calculated. Fourier transform infrared spectroscopy, Raman spectroscopy, field-emission scanning electron microscopy and X-ray diffractometry techniques were used to investigate the interaction of RMPs on PB surface. Adsorption kinetics of 5'-AMP on PB has been found to be pseudo-second order. Results obtained from this study should prove valuable for a better understanding of the mechanism of RMP-PB interaction.

Concave Urinary Crystallines: Direct Evidence of Calcium Oxalate Crystals Dissolution by Citrate In Vivo

PubMed Central

Shang, Yun-Feng; Xu, Meng; Zhang, Guang-Na; Ouyang, Jian-Ming

2013-01-01

The changes in urinary crystal properties in patients with calcium oxalate (CaOx) calculi after oral administration of potassium citrate (K3cit) were investigated via atomic force microscopy (AFM), scanning electron microscopy (SEM), X-ray powder diffractometry (XRD), and zeta potential analyzer. The AFM and SEM results showed that the surface of urinary crystals became concave, the edges and corners of crystals became blunt, the average size of urinary crystallines decreased significantly, and aggregation of urinary crystals was reduced. These changes were attributed to the significant increase in concentration of excreted citrate to 492 ± 118 mg/L after K3cit intake from 289 ± 83 mg/L before K3cit intake. After the amount of urinary citrate was increased, it complexed with Ca2+ ions on urinary crystals, which dissolved these crystals. Thus, the appearance of concave urinary crystals was a direct evidence of CaOx dissolution by citrate in vivo. The XRD results showed that the quantities and species of urinary crystals decreased after K3cit intake. The mechanism of inhibition of formation of CaOx stones by K3cit was possibly due to the complexation of Ca2+ with citrate, increase in urine pH, concentration of urinary inhibitor glycosaminoglycans (GAGs), and the absolute value of zeta potential after K3cit intake. PMID:24363634

Magnetic analysis of commercial hematite, magnetite, and their mixtures

NASA Astrophysics Data System (ADS)

Ahmadzadeh, Mostafa; Romero, Camila; McCloy, John

2018-05-01

Magnetic techniques are suitable to detect iron oxides even in trace concentrations. However, since several iron oxides may be simultaneously present in natural and synthetic samples, mixtures of magnetic particles and magnetic interactions between grains can complicate magnetic signatures. Among the iron oxide minerals, hematite (α-Fe2O3) and magnetite (Fe3O4) are the most common. In this work, different commercial hematite powders, normally used as Fe precursor in laboratory synthesis of Fe-containing oxides, were characterized using X-ray diffractometry (XRD), scanning electron microscopy (SEM), and vibrating sample magnetometry (VSM). The effects of different concentrations of the hematite and magnetite on the magnetic properties of a set of mixtures (from 1 to 10 wt% magnetite) were then investigated by measuring the hysteresis loops, first order reversal curves (FORCs), thermal demagnetization, and isothermal remanent magnetization (IRM) curves. The three commercial hematite powders presented different magnetic behaviors mostly due to the effects of particle size. The magnetic results of mixtures reveal that it is very difficult to identify hematite magnetic signals by means of hysteresis loops, FORCs, or thermal demagnetization when even a small amount of magnetite (>5 wt%) is present due to magnetite's high specific magnetization. However, IRM was found to be a sensitive method to determine the presence of hematite when magnetite is simultaneously present as high as 10 wt%.

The Formation Mechanism and Corrosion Resistance of a Composite Phosphate Conversion Film on AM60 Alloy

PubMed Central

Lan, Xiangna; Wang, Chao; Zhang, Qinyong

2018-01-01

Magnesium alloy AM60 has high duc and toughness, which is expected to increase in demand for automotive applications. However, it is too active, and coatings have been extensively studied to prevent corrosion. In this work, a Ba-containing composite phosphate film has been prepared on the surface of AM60. The composition and formation mechanism of the film have been investigated using a scanning electronic microscope equipped with energy dispersive X-ray spectroscopy, Fourier transform infrared, X-ray photoelectron spectroscopy, and X-ray diffractometry tests. The corrosion resistance of the film has been measured by electrochemical and immersion tests. The results show that the deposition film has fully covered the substrate but there are some micro-cracks. The structure of the film is complex, and consists of MgHPO4·3H2O, MnHPO4·2.25H2O, BaHPO4·3H2O, BaMg2(PO4)2, Mg3(PO4)2·22H2O, Ca3(PO4)2·xH2O, and some amorphous phases. The composite phosphate film has better anticorrosion performance than the AM60 and can protect the bare alloy from corrosion for more than 12 h in 0.6 M NaCl. PMID:29518038

Influence of Near-Surface Severe Plastic Deformation of Mild Steel on the Inhibition Performance of Sodium Molybdate and 1H-Benzotriazole in Artificial Sea Water

NASA Astrophysics Data System (ADS)

Sabet Bokati, Kazem; Dehghanian, Changiz; Babaei, Mahdi

2018-02-01

The effects of near-surface severe plastic deformation (NS-SPD) on the inhibition performance of sodium molybdate (SM) and 1H-benzotriazole (BTA) for mild steel were investigated using weight loss, polarization and electrochemical impedance spectroscopy measurements. The crystal grain size of NS-SPD-processed surface was analyzed by x-ray diffractometry and field emission scanning electron microscopy. A deformed layer with thickness of 20 ± 5 µm was produced on mild steel surface after NS-SPD process due to accumulated strains. The NS-SPD process caused more effective adsorption of corrosion inhibitors due to the fabrication of a surface with a high density of preferential adsorption sites. However, the stability of protective layer was predominantly influenced by the effect of NS-SPD process on inhibition efficiency. The fairly good persistence of protective layer formed on the surface by SM-containing solution and also positive effect of NS-SPD process on adsorption of molybdate ions caused higher inhibition performance for sodium molybdate. However, NS-SPD process encouraged deterioration of protective layer formed on steel surface in the presence of BTA inhibitor. It was ascribed to partial coverage of surface, low stability of adsorbed layer and thus more adsorption of aggressive ions on unprotected area which was uncovered during immersion time.

Relationship between crystal structure and solid-state properties of pharmaceuticals

NASA Astrophysics Data System (ADS)

Sheth, Agam R.

This thesis strives to understand the structure-property relationships of some pharmaceutical crystals at the molecular level with emphasis on the effect of secondary processing on the solid phase. Using single crystal X-ray diffractometry (SCXRD), the structure of warfarin sodium 2-propanol adduct (W) was established to be a true solvate, contrary to previous reports. Using dynamic water vapor sorption, optical and environmental scanning electron microscopy, SCXRD, powder X-ray diffractometry (PXRD), volume computations and molecular modeling, the effect of relative humidity and temperature on the crystal structure of W was investigated. Ab initio calculations on piroxicam showed that the difference in energy between the two polymorphs, I and II, arises predominantly from the difference between their lattice energies. The detailed hydrogen bonding networks of the two polymorphs are described and compared using graph sets. Despite stabilization of the polymorphs by hydrogen bonds, pair-wise distribution function transforms show a loss of polymorphic memory upon cryogrinding the two polymorphs, leading to a difference in recrystallization behavior between amorphous piroxicam prepared from polymorphs I and II. Structural and solid-state changes of piroxicam polymorphs under mechanical stress were investigated using cryogenic grinding, PXRD, diffuse-reflectance solid-state ultraviolet-visible spectroscopy, 13C solid-state nuclear magnetic resonance spectroscopy, and diffuse-reflectance solid-state Fourier-transform infrared spectroscopy. Intermolecular proton transfer was found to accompany changes in phase and color observed upon cryogrinding the two polymorphs. Model-free and model-fitting studies of the dehydration kinetics of piroxicam monohydrate (PM) showed the dependence of activation energy ( Ea) on both isothermal and non-isothermal heating conditions, and on the fraction of conversion. In the constant-E a region, isothermal dehydration follows the two-dimensional phase boundary model, while non-isothermal dehydration follows a mechanism intermediate between two- and three-dimensional diffusion that cannot be described by any of the common models. Structural studies suggest that the complex hydrogen bond pattern in PM is responsible for the observed dehydration behavior. Ab initio calculations provide an explanation for the changes in the molecular and crystal structures accompanying the reversible change in hydration state between anhydrous piroxicam Form I and PM. The thesis further demonstrates the utility of model-free analysis in describing complex dehydration kinetics.

Synthesis of magnetic mesoporous metal-organic framework-5 for the effective enrichment of malachite green and crystal violet in fish samples.

PubMed

Zhou, Zhihui; Fu, Yanqing; Qin, Qian; Lu, Xin; Shi, Xianzhe; Zhao, Chunxia; Xu, Guowang

2018-07-27

A novel, magnetic and mesoporous Fe 3 O 4 @PEI-MOF-5 material was synthesized for the effective enrichment of malachite green (MG) and crystal violet (CV) in fish samples. The Fe 3 O 4 @PEI-MOF-5 material was prepared by a facile two-step solvothermal approach in which Fe 3 O 4 @PEI and MOF-5 were connected through chemical bonds. Characterization of the newly synthesized Fe 3 O 4 @PEI-MOF-5 material was performed by Fourier transform infrared spectroscopy, X-ray diffractometry, vibrating sample magnetometry, scanning electron microscopy, transmission electron microscopy, thermogravimetric analysis and X-ray photoelectron spectroscopy. This new material was determined to have high magnetization and chemical stability, a large surface area and a distinctive morphology. An effective enrichment and detection method for MG and CV was subsequently developed by combining the Fe 3 O 4 @PEI-MOF-5 material with ultra-high-performance liquid chromatography-tandem mass spectrometry. The linearity ranges of this approach for MG and CV were 1-500ng/mL and 0.25-500ng/mL, respectively, with correlation coefficients (R 2 ) of 0.999. The limits of detection (LODs) of the method for MG and CV were 0.30ng/mL and 0.08ng/mL, respectively, indicating that the Fe 3 O 4 @PEI-MOF-5 material had good adsorption properties for MG and CV. Fe 3 O 4 @PEI-MOF-5 can be expected to also provide efficient enrichment of MG and CV in other complex matrices. Copyright © 2018 Elsevier B.V. All rights reserved.

Blue–green afterglow of BaAl{sub 2}O{sub 4}:Dy{sup 3+} phosphors

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhai, Bao-gai; Ma, Qing-lan; School of Electronics and Information, Nantong University, Jiangsu 226019

Highlights: • Afterglow can be achieved when Eu{sup 2+} is absent in the DyAl{sub 2}O{sub 4}:Dy{sup 3+} phosphors. • The afterglow of DyAl{sub 2}O{sub 4}:Dy{sup 3+} phosphors is discernible to naked eyes for minutes. • Dy{sup 3+} introduced trap centers are believed to be responsible for the afterglow. - Abstract: Dy{sup 3+} doped barium aluminate (BaAl{sub 2}O{sub 4}:Dy{sup 3+}) phosphors were prepared via the sol–gel combustion route at the ignition temperature of 600 °C. The phosphors were characterized with X-ray diffractometry, scanning electron microscopy, transmission electron microscopy, photoluminescence spectroscopy, Fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy. Regardless of themore » absence of Eu{sup 2+} luminescent centers, broadband blue–green afterglow with its peak at about 490 nm was recorded in the BaAl{sub 2}O{sub 4}:Dy{sup 3+} phosphors. The decay profile of the blue–green afterglow can be best fitted into a two-component exponential function with the two lifetime decay constants to be 8.81 and 45.25 s, respectively. The observation of blue–green afterglow from BaAl{sub 2}O{sub 4}:Dy{sup 3+} in the absence of Eu{sup 2+} provides unique opportunity in unveiling the afterglow mechanisms of rare-earth doped alkaline-metal aluminates. Possible mechanisms on the blue–green afterglow in BaAl{sub 2}O{sub 4}:Dy{sup 3+} phosphors are discussed in terms of the Dy{sup 3+} ions introduced trap centers as well as luminescent centers in the crystal lattice.« less

Effects of solution pH and electrical parameters on hydroxyapatite coatings deposited by a plasma-assisted electrophoresis technique.

PubMed

Nie, X; Leyland, A; Matthews, A; Jiang, J C; Meletis, E I

2001-12-15

Hydroxyapatite (HA) coatings can be deposited using a hybrid process of plasma electrolysis and electrophoresis, called plasma-assisted electrophoretic deposition (PEPD). HA aqueous suspensions with various pH values were prepared using a modified ultrasonic cleaning bath as an agitator/stirrer. Both DC and unbalanced AC power supplies were used to bias the titanium alloy substrate materials employed in this work. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffractometry (XRD), and Fourier transform infrared spectroscopy (FTIR) were used to observe and analyze coating morphology and microstructure. It was shown that the morphology and composition of the calcium phosphate coatings were significantly influenced by solution pH values; the level of "pure" HA in the coatings' composition corresponded to both solution pH and the type of power supply employed. Loss of hydroxyl radials (i.e., dehydroxylation), which degrades the performance of the hydroxyapatite coating in terms of long-term chemical and mechanical stability, can be virtually eliminated by a combination of high pH and unbalanced AC plasma power. In addition, the underlying TiO2 coatings used to support the HA layer (preproduced by plasma electrolysis process) have a nanoscaled (10-20 nm) polycrystalline structure. TEM studies also revealed a dense, continuous amorphous titania layer (10 nm in thickness) at the interface between the Ti alloy substrate and the TiO2 layer, which may play a role in improving the corrosion resistance of the substrate. Such a nanophase TiO2 layer (if used as a coating alone) may also provide a further improvement in osteoinductive properties, compared to a conventional TiO2 coating on the Ti alloy substrate. Copyright 2001 John Wiley & Sons, Inc. J Biomed Mater Res 57: 612-618, 2001

The effect of metal cluster deposition route on structure and photocatalytic activity of mono- and bimetallic nanoparticles supported on TiO2 by radiolytic method

NASA Astrophysics Data System (ADS)

Klein, Marek; Nadolna, Joanna; Gołąbiewska, Anna; Mazierski, Paweł; Klimczuk, Tomasz; Remita, Hynd; Zaleska-Medynska, Adriana

2016-08-01

TiO2 (P25) was modified with small and relatively monodisperse mono- and bimetallic clusters (Ag, Pd, Pt, Ag/Pd, Ag/Pt and Pd/Pt) induced by radiolysis to improve its photocatalytic activity. The as-prepared samples were characterized by X-ray fluorescence spectrometry (XRF), photoluminescence spectrometry (PL), diffuse reflectance spectroscopy (DRS), X-ray powder diffractometry (XRD), scanning transition electron microscopy (STEM) and BET surface area analysis. The effect of metal type (mono- and bimetallic modification) as well as deposition method (simultaneous or subsequent deposition of two metals) on the photocatalytic activity in toluene removal in gas phase under UV-vis irradiation (light-emitting diodes- LEDs) and phenol degradation in liquid phase under visible light irradiation (λ > 420 nm) were investigated. The highest photoactivity under Vis light was observed for TiO2 co-loaded with platinum (0.1%) and palladium (0.1%) clusters. Simultaneous addition of metal precursors results in formation of larger metal nanoparticles (15-30 nm) on TiO2 surface and enhances the Vis-induced activity of Ag/Pd-TiO2 up to four times, while the subsequent metal ions addition results in formation of metal particle size ranging from 4 to 20 nm. Subsequent addition of metal precursors results in formation of BNPs (bimetallic nanoparticle) composites showing higher stability in four cycles of toluene degradation under UV-vis. Obtained results indicated that direct electron transfer from the BNPs to the conduction band of the semiconductor is responsible for visible light photoactivity, whereas superoxide radicals (such as O2rad- and rad OOH) are responsible for pollutants degradation over metal-TiO2 composites.

A potential bioactive wound dressing based on carboxymethyl cellulose/ZnO impregnated MCM-41 nanocomposite hydrogel.

PubMed

Rakhshaei, Rasul; Namazi, Hassan

2017-04-01

Lack of antibacterial activity, deficient water vapor and oxygen permeability, and insufficient mechanical properties are disadvantages of existing wound dressings. Hydrogels could absorb wound exudates due to their strong swelling ratio and give a cooling sensation and a wet environment. To overcome these shortcomings, flexible nanocomposite hydrogel films was prepared through combination of zinc oxide impregnated mesoporous silica (ZnO-MCM-41) as a nano drug carrier with carboxymethyl cellulose (CMC) hydrogel. Citric acid was used as cross linker to avoid the cytotoxicity of conventional cross linkers. The prepared nanocomposite hydrogel was characterized using X-ray diffractometry (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Zeta potential and UV-vis spectroscopy. Results of swelling and erosion tests showed CMC/ZnO nanocomposite hydrogel disintegrated during the first hours of the test. Using MCM-41 as a substrate for ZnO nanoparticles solved this problem and the CMC/ZnO-MCM-41 showed a great improvement in tensile strength (12%), swelling (100%), erosion (53%) and gas permeability (500%) properties. Drug delivery and antibacterial properties of the nanocomposite hydrogel films studied using tetracycline (TC) as a broad spectrum antibiotic and showed a sustained TC release. This could efficiently decrease bandage exchange. Cytocompatibility of the nanocomposite hydrogel films has been analyzed in adipose tissue-derived stem cells (ADSCs) and results showed cytocompatibility of CMC/ZnO-MCM-41. Based on these results the prepared CMC nanocomposite hydrogel containing ZnO impregnated MCM-41, could serve as a kind of promising wound dressing with sustained drug delivery properties. Copyright © 2016 Elsevier B.V. All rights reserved.

Selective removal of monoterpenes from bergamot oil by inclusion in deoxycholic acid.

PubMed

Fantin, Giancarlo; Fogagnolo, Marco; Maietti, Silvia; Rossetti, Stefano

2010-05-12

A new approach for removing monoterpenes (MTs) from bergamot oil by selective inclusion in deoxycholic acid (DCA) is proposed. The inclusion process is very efficient, the included fraction being composed mainly of limonene (71.7%) and gamma-terpinene (19.8%). On the other hand, the deterpenated bergamot oil fraction showed for the linalool and linalyl acetate derivatives significant increases from 16.6 and 21.4% to 18.3 and 42.2%, respectively. The major advantages of this methodology are its simplicity, the mild conditions employed, and the quantitative recovery of both host (DCA) and guest (monoterpenes) compounds. Differential scanning calorimetry (DSC), thermal gravimetry (TG), powder X-ray diffractometry (XRPD), infrared spectroscopy (IR), and proton magnetic resonance ((1)H NMR) analysis were used to investigate and characterize the inclusion compounds.

Synthesis of AlFeCuCrMg{sub x} (x = 0, 0.5, 1, 1.7) alloy powders by mechanical alloying

DOE Office of Scientific and Technical Information (OSTI.GOV)

Maulik, Ornov; Kumar, Vinod, E-mail: vkt.meta@mnit.ac.in; Adjunct Faculty, Materials Research Centre, Malaviya National Institute of Technology, Jaipur 302017

2015-12-15

Novel AlFeCuCrMg{sub x} (x = 0, 0.5, 1, 1.7 mol) high-entropy alloys (HEAs) were synthesized by mechanical alloying. The effect of Mg content on the phase evolution of HEAs was investigated using X-Ray diffractometry (XRD), transmission electron microscopy (TEM) and selected area electron diffraction (SAED) pattern analysis. The particle morphology and composition of HEAs were investigated by scanning electron microscopy (SEM). Thermodynamic parameters were calculated and analyzed to explain the formation of a solid solution. XRD analysis revealed BCC as major phase and FCC as a minor phase in as-milled AlFeCuCr and AlFeCuCrMg{sub 0.5} HEAs. Also, XRD analysis of as-milledmore » AlFeCuCrMg, AlFeCuCrMg{sub 1.7} confirmed the formation of two BCC phases (BCC 1 and BCC 2). TEM–SAED analysis of AlFeCuCrMg{sub x} HEAs concurred with XRD results. Microstructural features and mechanism for solid solution formation have been conferred in detail. Phase formation of the present HEAs has been correlated with calculated thermodynamic parameters. Differential thermal analysis (TGA-DTA) of these alloys confirmed that there is no substantial phase change up to 500 °C. - Highlights: • Novel AlFeCuCrMg{sub x} (x = 0, 0.5, 1, 1.7) HEAs were prepared by mechanical alloying. • Phase evolution and lattice parameter were studied by X-Ray Diffraction. • Crystallite size and lattice microstrain calculated failed to obey the Williamson–Hall method. • Criterions for formation of simple solid solution were compared to the thermodynamic parameters of the present HEAs. • Increase in the Mg concentration in AlMg{sub x}FeCuCr (x = 0, 0.5, 1, 1.7) HEAs supports the formation of BCC phase.« less

Ultrasonic spray pyrolysis synthesis of reduced graphene oxide/anatase TiO2 composite and its application in the photocatalytic degradation of methylene blue in water.

PubMed

Park, Jeong-Ann; Yang, Boram; Lee, Joongki; Kim, In Gyeom; Kim, Jae-Hyun; Choi, Jae-Woo; Park, Hee-Deung; Nah, In Wook; Lee, Sang-Hyup

2018-01-01

Reduced graphene oxide (RGO)/anatase TiO 2 composite was prepared using a simple one-step technique-ultrasonic spray pyrolysis-in order to inhibit the aggregation of TiO 2 nanoparticles and to improve the photocatalytic performance for degradation of methylene blue (MB). Different proportions (0-5 wt%) of RGO/TiO 2 composites were characterized by scanning electronic microscopy (SEM), dispersive X-ray spectrometry (EDS), transmission electron microscopy (TEM), Brunauer-Emmett-Teller (BET) surface area, X-ray photoelectron spectroscopy (XPS), X-ray diffractometry (XRD), Raman spectroscopy, UV-vis spectroscopy, and electrochemical impedance spectroscopy (EIS) to verify mechanism. From these analysis, TiO 2 nanoparticles are distributed uniformly on the RGO sheets with crumpled shape during ultrasonic spray pyrolysis and surface area is increasing by increasing portion of RGO. Band gap of RGO 5 /TiO 2 (5 wt% of RGO) composite is 2.72 eV and band gap was reduced by increasing portion of RGO in RGO/TiO 2 composites. The RGO 5 /TiO 2 composite was superior to other lower content of RGO/TiO 2 composites with a rapid transport of charge carriers and an effective charge separation. The highest removal efficiency of MB was obtained at the RGO 5 /TiO 2 composite under UVC irradiation, which coincided with the EIS, and the optimal dose of the composite was determined to be 0.5 g/L. The RGO 5 /TiO 2 composite improve the photocatalytic degradation rate of MB over the TiO 2 due to a retardation of electron-hole recombination. The MB adsorption capacity and photocatalytic degradation efficiency were greatly affected by pH changes and increased with increasing pH due to electrostatic interactions and generation of more hydroxyl radicals. The reusability of RGO 5 /TiO 2 composite was examined during 3 cycles. Copyright © 2017 Elsevier Ltd. All rights reserved.

A Detailed Study of the Drastic Worldwide Climatic Change by the Cretaceous/Paleogene (K/T)-Impact of Chicxulub

NASA Astrophysics Data System (ADS)

Preisinger, Anton; Aslanian, Selma; Grass, Fritz; Beigelbeck, Roman; Wernisch, Johann

2010-05-01

The impact of Chicxulub (Yucatan, Mexico) was a global event exhibiting a short-time (fallout) and a long-time (boundary clay) sedimentation of the K/T-boundary [1]. The fallout is mainly characterized by iridium, Ni-Cr-rich magnesia-ferrite spinels (K/T-spinels), spherules, as well as shocked quartzes. The amount of the sediments and their distribution depend on the distance from the impact crater. The Cretaceous/Paleogene (K/T) boundaries at three different locations namely Caravaca (Spain), Cerbara (Italy), and Bjala (Bulgaria) have been well analyzed. About 65 million years ago, they were located at the distances from the impact crater ~6000 km, ~7500 km, and ~8800 km, respectively. The boundary clay is characterized by transported minerals like quartzes and feldspars, authigenically formed minerals, as well as biominerals like Mg-calcites and greigites (Fe3S4). The samples were analyzed by scanning X-ray diffractometry (Bruker Analytical X-ray System), scanning electronic microscopy (XL30, ESEM-Philips), neutron activation analyses, Delta13C and Delta18O analyses, and the determination of nannofossils and foraminifera. Owing to the Earth's rotation, the analyzed samples lie along a great circle (crossing the equator under an angle of ~23° ) which covers Chicxulub, Caravaca, Cerbara, and Bjala indicating the existence of only a single impact. The study of this K/T-boundary by means of high resolution scanning X-ray diffractometry in combination with the scanning electron microscopy and neutron activation analyzes revealed the time dependency of the K/T-event in the fallout as well as in the boundary clay. The biomineralization of sulfate-reducing bacteria by greigites provided the duration of the sulfuric acid rain. The reoccurrence of algae is indicated by the appearance of Mg-calcite at the end of the boundary clay. The K/T-spinels were formed on the nucleus of metallic iridium [2]. They were built in the mesosphere (in a height of about 100 km) and grew during the fall to the Earth's surface by forming ferrimagnetic twins, which were etched by the H2SO4 content of the atmosphere. We developed an extensive mathematical model incorporating all relevant physical effects (particle growth, pressure dependence of the atmosphere, fluid resistance, centrifugal and coriolis forces, etc.) in order to study the development of the particles during the fall. For Caravaca, the shortest flight time for the Iridium fallout is approximately 6.5 days, while the shortest flight time for the ejecta near Chicxulub last only a few hours. The K/T-impact took place about 65 million years ago in a sea depth of more than 2000 m. Consequently, the impact heated up the sea water and the water molecules reacted with the CaCO3, CaSO4, and the silicates down to a depth of 28 km. This hydrothermal reaction reduced the melt temperature significantly, especially those of silicates. Therefore, the pyroxenes and plagioclases changed to clay minerals. The sedimentation rate of Chron 29RK is about twice than that of Chron 29RT, which equals to Chron 29N in Caravaca, Cerbara, and Bjala. The precession cycles of Chron 29R and Chron 29N are 22.5 kyears. The time span of the K/T-boundaries between Chron 29RK and Chron 29RT is worldwide about 1 kyear. Concluding all our results, only one big impact took place at Chicxulub (Yucatan, Mexico) about 65 million years ago and caused, during the formation of the K/T-boundary, a worldwide climatic change. References: [1] Eder, G. and Preisinger, A.: Zeitstruktur globaler Ereignisse veranschaulicht an der Kreide/Terziär-Grenze. Naturwissenschaften, Band 74, 35-37, 1987. [2] Preisinger, A., Aslanian, S., Brandstätter, F., Grass, F., Stradner, H., and Summesberger, H.: Cretaceous-Tertiary profile, rhythmic deposition, and geomagnetic polarity reversals of marine sediments near Bjala, Bulgaria. Geo. Soc. Amer. special paper 356, 229-312, 2002.

A mixed valence zinc dithiolene system with spectator metal and reactor ligands.

PubMed

Ratvasky, Stephen C; Mogesa, Benjamin; van Stipdonk, Michael J; Basu, Partha

2016-08-16

Neutral complexes of zinc with N,N'-diisopropylpiperazine-2,3-dithione ( i Pr 2 Dt 0 ) and N,N'-dimethylpiperazine-2,3-dithione (Me 2 Dt 0 ) with chloride or maleonitriledithiolate (mnt 2- ) as coligands have been synthesized and characterized. The molecular structures of these zinc complexes have been determined using single crystal X-ray diffractometry. Complexes recrystallize in monoclinic P type systems with zinc adopting a distorted tetrahedral geometry. Two zinc complexes with mixed-valent dithiolene ligands exhibit ligand-to-ligand charge transfer bands. Optimized geometries, molecular vibrations and electronic structures of charge-transfer complexes were calculated using density functional theory (B3LYP/6-311G+(d,p) level). Redox orbitals are shown to be almost exclusively ligand in nature, with a HOMO based heavily on the electron-rich maleonitriledithiolate ligand, and a LUMO comprised mostly of the electron-deficient dithione ligand. Charge transfer is thus believed to proceed from dithiolate HOMO to dithione LUMO, showing ligand-to-ligand redox interplay across a d 10 metal.

Synthesis of tritium breeder ceramics from metallic lithium

NASA Astrophysics Data System (ADS)

Knitter, R.; Kolb, M. H. H.; Odemer, C.

2012-01-01

For the fabrication of Li-6 enriched ceramic breeder materials for ITER, the availability of Li-6 enriched compounds is limited, and metallic Li-6 is the most widely available compound. As metallic lithium cannot be used directly in ceramic fabrication processes, we investigated different syntheses to obtain lithium orthosilicate or lithium metatitanate directly from molten lithium. In exothermic reactions of molten lithium with silicon, silica, or titania, several intermediate or precursor phases were observed under argon that could easily be transformed to the desired ceramic phases by a subsequent heat treatment under air. The reaction steps and the resulting phases were studied by differential scanning calorimetry and X-ray diffractometry. The synthesis from lithium and silicon seems to be especially suited for the production of larger quantities and has the advantage that silicon is available with a very high grade of purity.

Second amorphous-to-crystalline phase transformation in Cu(60)Ti(20)Zr(20) bulk metallic glass.

PubMed

Cao, Q P; Li, J F; Zhang, P N; Horsewell, A; Jiang, J Z; Zhou, Y H

2007-06-20

The second amorphous-to-crystalline phase transformation in Cu(60)Ti(20)Zr(20) bulk metallic glass was investigated by differential scanning calorimetry and x-ray diffractometry. The difference of the Gibbs free energies between the amorphous phase and the crystalline products during the transformation is estimated to be about 2.46 kJ mol(-1) at 753 K, much smaller than the 61 kJ mol(-1) obtained assuming that it is a polymorphic transformation. It was revealed that the phase transformation occurs through a eutectic crystallization of Cu(51)Zr(14) and Cu(2)TiZr, having an effective activation energy of the order of 400 kJ mol(-1). The average Avrami exponent n is about 2.0, indicating that the crystallization is diffusion controlled.

Thermal behavior of potato starch and water-vaporization behavior of its paste controlled with amino acid and peptide-rich food materials.

PubMed

Sakauchi, Satoshi; Hattori, Makoto; Yoshida, Tadashi; Yagishita, Takahiro; Ito, Koichi; Akemitsu, Shin-Ichi; Takahashi, Koji

2010-03-01

The particular effect of 4 kinds of amino acid and peptide-rich food material (APRM) containing different charged amino acid contents on the gelatinization and retrogradation behavior of potato starch granules and on the water-vaporization behavior was analyzed by differential scanning calorimetry, rapid viscoanalysis, x-ray diffractometry, thermal gravimetry-differential thermal analysis, and pulsed NMR. APRM with a high-charged amino acid content produced unique gelatinization and retrogradation behavior in terms of an elevated gelatinization temperature, reduced viscosity, higher setback, and lower retrograded starch melting enthalpy. The recovered x-ray diffraction intensity decreased with increasing charged amino acid content. APRM with high-charged amino acid content could provide an improved paste having easy vaporization of external water in the swollen starch granules due to the reduced swelling.

Thin calcium phosphate coatings on titanium by electrochemical deposition in modified simulated body fluid.

PubMed

Peng, Ping; Kumar, Sunil; Voelcker, Nicolas H; Szili, Endre; Smart, Roger St C; Griesser, Hans J

2006-02-01

Adherent and optically semitransparent thin calcium phosphate (CaP) films were electrochemically deposited on titanium substrates in a modified simulated body fluid at 37 degrees C. Coatings deposited by using periodic pulsed potentials showed better adhesion and better mechanical properties than coatings deposited with use of a constant potential. Scanning electron microscopy was used to study the morphology of the coatings. The coatings displayed a polydispersed porous structure with pores in the range of a few nanometers to 1 mum. Furthermore, X-ray diffractometry and the O(1s) satellite peaks in X-ray photoelectron spectroscopy indicated that the coatings possessed a similar surface chemistry to that of natural bone minerals. These results were confirmed by inductively coupled plasma optical emission spectrometry, which yielded a Ca:P ratio of 1.65, close to that of hydroxyapatite. Contact mode atomic force microscopy (AFM) showed the average thickness of the coatings was in the order of 200 nm. Root-mean-square (RMS) roughness values, also derived by AFM, were shown to be much higher on the titanium-CaP surfaces in comparison with untreated titanium substrates, with RMS values of about 300 and 110 nm, respectively. Cell culture experiments showed that the CaP surfaces are nontoxic to MG63 osteoblastic cells in vitro and were able to support cell growth for up to 4 days, outperforming the untreated titanium surface in a direct comparison. These easily prepared coatings show promise for hard-tissue biomaterials. (c) 2005 Wiley Periodicals, Inc.

Preparation, characterization and cytotoxic evaluation of bovine serum albumin nanoparticles encapsulating 5-methylmellein: A secondary metabolite isolated from Xylaria psidii.

PubMed

Arora, Divya; Kumar, Amit; Gupta, Prasoon; Chashoo, Gousia; Jaglan, Sundeep

2017-12-01

In this study, 5-methylmellein (5-MM) loaded bovine serum albumin nanoparticles (BSA NPs) were developed using desolvation technique. The developed nanoparticles were characterized for their mean particle size, polydispersity, zeta potential, loading efficiency, X-ray diffractometry (XRD), differential scanning calorimetry (DSC) and release profile. The developed nanoparticles were spherical in shape under transmission electron microscopy (TEM) and atomic force microscopy (AFM). The developed 5-MM loaded BSA NPs demonstrated a mean particle size with a diameter of 154.95 ± 4.44 nm. The results from XRD and DSC studies demonstrated that the crystal state of the 5-MM was converted to an amorphous state in polymeric matrix. The encapsulation and loading efficiency was found to be 73.26 ± 4.48% and 7.09 ± 0.43%. The in vitro cytotoxicity in human prostate cancer cell line (PC-3), human colon cancer cells (HCT-116) and human breast adenocarcinoma cell line (MCF-7) cells demonstrated enhanced cytotoxicity of 5-MM BSA NPs as compared to native 5-MM after 72-h treatment. The enhancement in cytotoxicity of 5-MM BSA NPs was also supported by increase in cellular apoptosis, mitochondrial membrane potential loss and generation of high reactive oxygen species (ROS). In conclusion, these findings collectively indicated that BSA nanoparticles may serve as promising drug delivery system for improving the efficacy of 5-methylmellein. Copyright © 2017 Elsevier Ltd. All rights reserved.

Thermodynamic effects of calcium and iron oxides on crystal phase formation in synthetic gasifier slags containing from 0 to 27wt.% V 2O 3

DOE PAGES

Nakano, Jinichiro; Duchesne, Marc; Bennett, James; ...

2014-11-15

Thermodynamic phase equilibria in synthetic slags (Al 2O 3–CaO–FeO–SiO 2–V 2O 3) were investigated with 0–27 wt.% vanadium oxide corresponding to industrial coal–petroleum coke (petcoke) feedstock blends in a simulated gasifier environment. Samples encompassing coal–petcoke mixed slag compositions were equilibrated at 1500 °C in a 64 vol.% CO/36 vol.% CO 2 atmosphere (Po 2 ≈ 10 –8 atm at 1500 °C) for 72 h, followed by rapid water quench, then analyzed by inductively coupled plasma optical emission spectrometry, X-ray diffractometry, and scanning electron microscopy with wavelength dispersive spectroscopy. With increasing CaO content, FeO content, or both; the slag homogeneity regionmore » expanded and a composition range exhibiting crystals was reduced. The mullite (Al 6Si 2O 13) crystalline phase was not present in the slags above 9 wt.% FeO while the karelianite (V 2O 3) crystalline phase was always present in compositions studied if a sufficient amount of vanadium existed in the slag. Furthermore, based on the present experimental equilibrium evaluation, a set of isothermal phase diagrams showing effects of CaO and FeO on thermodynamic phase stabilities in the vanadium-bearing slags is proposed. Some uses of the diagrams for potential industrial practice are discussed.« less

Formulation and delivery of itraconazole to the brain using a nanolipid carrier system

PubMed Central

Lim, Wei Meng; Rajinikanth, Paruvathanahalli Siddalingam; Mallikarjun, Chitneni; Kang, Yew Beng

2014-01-01

The objectives of this study were to develop and characterize itraconazole (ITZ)-loaded nanostructured lipid carriers (NLCs) and to study their potential for drug delivery into the brain. Precirol® ATO 5 and Transcutol® HP were selected as the lipid phase, and Tween® 80 and Solutol® HS15 as surfactants. The ITZ-NLCs were prepared by a hot and high-pressure homogenization method. The entrapment efficiency for the best formulation batch was analyzed using high-performance liquid chromatography and was found to be 70.5%±0.6%. The average size, zeta potential, and polydispersity index for the ITZ-NLCs used for animal studies were found to be 313.7±15.3 nm, −18.7±0.30 mV, and 0.562±0.070, respectively. Transmission electron microscopy confirmed that ITZ-NLCs were spherical in shape, with a size of less than 200 nm. Differential scanning calorimetry and X-ray diffractometry analysis showed that ITZ was encapsulated in the lipid matrix and present in the amorphous form. The in vitro release study showed that ITZ-NLCs achieved a sustained release, with cumulative release of 80.6%±5.3% up to 24 hours. An in vivo study showed that ITZ-NLCs could increase the ITZ concentration in the brain by almost twofold. These results suggest that ITZ-NLCs can be exploited as nanocarriers to achieve sustained release and brain-targeted delivery. PMID:24833900

Composition, diagenetic transformation and alkalinity potential of oil shale ash sediments.

PubMed

Mõtlep, Riho; Sild, Terje; Puura, Erik; Kirsimäe, Kalle

2010-12-15

Oil shale is a primary fuel in the Estonian energy sector. After combustion 45-48% of the oil shale is left over as ash, producing about 5-7 Mt of ash, which is deposited on ash plateaus annually almost without any reuse. This study focuses on oil shale ash plateau sediment mineralogy, its hydration and diagenetic transformations, a study that has not been addressed. Oil shale ash wastes are considered as the biggest pollution sources in Estonia and thus determining the composition and properties of oil shale ash sediment are important to assess its environmental implications and also its possible reusability. A study of fresh ash and drillcore samples from ash plateau sediment was conducted by X-ray diffractometry and scanning electron microscopy. The oil shale is highly calcareous, and the ash that remains after combustion is derived from the decomposition of carbonate minerals. It is rich in lime and anhydrite that are unstable phases under hydrous conditions. These processes and the diagenetic alteration of other phases determine the composition of the plateau sediment. Dominant phases in the ash are hydration and associated transformation products: calcite, ettringite, portlandite and hydrocalumite. The prevailing mineral phases (portlandite, ettringite) cause highly alkaline leachates, pH 12-13. Neutralization of these leachates under natural conditions, by rainwater leaching/neutralization and slow transformation (e.g. carbonation) of the aforementioned unstable phases into more stable forms, takes, at best, hundreds or even hundreds of thousands of years. Copyright © 2010 Elsevier B.V. All rights reserved.

Characterization of home-made silver sulphide based iodide selective electrode.

PubMed

Rajbhandari Nyachhyon, A; Yadav, A P; Manandhar, K; Pradhananga, R R

2010-09-15

Polycrystalline silver sulphide/silver iodide ion selective electrodes (ISEs) with four different compositions, 9:1, 2:1, 1:1, 1:9 Ag(2)S-AgI mole ratios, have been fabricated in the laboratory and characterized by X-ray diffractometry (XRD), scanning electron microscopy (SEM), and electrochemical impedance spectroscopy (EIS). X-ray diffraction studies show the presence of Ag(3)SI, Ag(2)S and AgI crystalline phases in the electrode material. The electrode surfaces have been found to become smoother and lustrous with increasing percentage of silver sulphide in silver iodide. ISE 1:1, ISE 2:1 and ISE 9:1 all responded in Nernstian manner with slopes of about 60 mV/decade change in iodide ion concentration in the linear range of 1 x 10(-1) to 1 x 10(-6)M while ISE 1:9 showed sub-Nernstian behavior with slope of about 45 mV up to the concentration 1 x 10(-5)M. Two capacitive loops, one corresponding to the charge transfer process at metal electrode and the back contact and a second loop corresponding to the charge transfer process at membrane-electrolyte interface have been observed at high and low frequency ranges, respectively. Mott-Schottky analysis shows that the materials are n-type semiconductors with donor defect concentrations in the range of 5.1 x 10(14) to 2.4 x 10(19)/cm(3). Copyright (c) 2010 Elsevier B.V. All rights reserved.

SHS synthesis of Si-SiC composite powders using Mg and reactants from industrial waste

NASA Astrophysics Data System (ADS)

Chanadee, Tawat

2017-11-01

Si-SiC composite powders were synthesized by self-propagating high-temperature synthesis (SHS) using reactants of fly ash-based silica, sawdust-based activated carbon, and magnesium. Fly ash-based silica and sawdust-based activated carbon were prepared from coal mining fly ash and Para rubber-wood sawdust, respectively. The work investigated the effects of the synthesis atmosphere (air and Ar) on the phase and morphology of the SHS products. The SHS product was leached by a two-step acid leaching processes, to obtain the Si-SiC composite powder. The SHS product and SHS product after leaching were characterized by X-ray diffractometry, scanning electron microscopy and energy dispersive X-ray spectrometry. The results indicated that the SHS product synthesized in air consisted of Si, SiC, MgO, and intermediate phases (SiO2, Mg, Mg2SiO4, Mg2Si), whereas the SHS product synthesized in Ar consisted of Si, SiC, MgO and a little Mg2SiO4. The SiC content in the leached-SHS product was higher when Ar was used as the synthesis atmosphere. As well as affecting the purity, the synthesis atmospheres also affected the average crystalline sizes of the products. The crystalline size of the product synthesized in Ar was smaller than that of the product synthesized in air. All of the results showed that fly ash and sawdust could be effective waste-material reactants for the synthesis of Si-SiC composite powders.

Synthesis of ZnS films on Si(100) wafers by using chemical bath deposition assisted by the complexing agent ethylenediamine

NASA Astrophysics Data System (ADS)

Zhu, He-Jie; Wang, Xue-Mei; Gao, Xiao-Yong

2015-07-01

Low-cost synthesis of high-quality ZnS films on silicon wafers is of much importance to the ZnSbased heterojunction blue light-emitting device integrated with silicon. Thus, a series of ZnS films were chemically synthesized at low cost on Si(100) wafers at 353 K under a mixed acidic solution with a pH of 4 with zinc acetate and thioacetamide as precursors and with ethylenediamine and hydrochloric acid as the complexing agent and the pH value modifier, respectively. The effects of the ethylenediamine concentration on the crystallization, surface morphology, and optical properties of the ZnS films were investigated by using X-ray diffractometry, scanning electron microscopy, spectrophotometry, and fluorescence spectroscopy. A mechanism for the formation of ZnS film under an acidic condition was also proposed. All of the ZnS films were polycrystalline in nature, with a dominant cubic phase and a small amounts of hexagonal phases. The crystallization and the surface pattern of the films were clearly improved with increasing ethylenediamine concentration due to its enhanced complexing role. The absorption edge of the films almost underwent a blue shift with increasing ethylenediamine concentration, which was largely attributed to the quantum confinement effects caused by the small particle size of the polycrystalline ZnS films. Defect species and the corresponding strengths of the ZnS films were strongly affected by the ethylenediamine concentration.

An Experimental Investigation of Effects of Fluxes (Na3AlF6 and K2TiF6), Element Alloys (Mg), and Composite Powders ((Al + TiC)CP and (Al + B4C)CP) on Distribution of Particles and Phases in Al-B4C and Al-TiC Composites

NASA Astrophysics Data System (ADS)

Mazaheri, Younes; Emadi, Rahmatollah; Meratian, Mahmood; Zarchi, Mehdi Karimi

2017-04-01

The wettability, incorporation, and gravity segregation of TiC and B4C particles into molten aluminum are important problems in the production of Al-TiC and Al-B4C composites by the casting techniques. In order to solve these problems, different methods consisting of adding the Na3AlF6 and K2TiF6 fluxes and Mg (as the alloying element) into the molten aluminum and injection of the (Al + TiC)CP and (Al + B4C)CP composite powders instead of B4C and TiC particles are evaluated. In this work, the conditions of sample preparation, such as particle addition temperature, stirring speed, and stirring time, are determined after many studies and tests. Microstructural characterizations of samples are investigated by scanning electron microscopy equipped with energy dispersive spectroscopy (EDS) and X-ray diffractometry. The results show better distribution and incorporation of TiCp and B4Cp in aluminum matrix when the fluxes are used, as well as EDS analysis of the interface between the matrix and reinforcement-strengthened formation of the different phases such as Al4C3 in the Al-TiC composites and Al3BC, TiB2 in the Al-B4C composites.

Gradient doping - a case study with Ti-Fe2O3 towards an improved photoelectrochemical response.

PubMed

Srivastav, Anupam; Verma, Anuradha; Banerjee, Anamika; Khan, Saif A; Gupta, Mukul; Satsangi, Vibha Rani; Shrivastav, Rohit; Dass, Sahab

2016-12-07

The present study investigates the effect of gradient doping on modifying the photoelectrochemical response of Ti-doped Fe 2 O 3 photoanodes for their use in sunlight based water splitting for hydrogen evolution. The deposition of a thin film over the ITO (tin doped indium oxide) substrate was carried out using a spray pyrolysis method. The concentration of dopant was varied from 0.5-8.0 at% and two sets of samples were also prepared with low to high (0.5-8%) and high to low (8-0.5%) dopant concentrations in the direction towards the substrate. The prepared thin films were characterized using X-ray Diffractometry (XRD), Scanning Electron Microscopy (SEM), Energy Dispersive X-ray (EDX) Spectroscopy, Secondary Ion Mass Spectroscopy (SIMS), X-ray Photoelectron Spectroscopy (XPS) and UV-visible Spectroscopy. The photoelectrochemical studies revealed that the deposition of dopant layers with a low to high concentration towards the substrate exhibited a highly improved photoresponse (200 times) in comparison to the pristine sample and a two fold enhancement in comparison to 2% Ti-doped Fe 2 O 3 . The improvement in the photoresponse has been attributed to the values of a high flat band potential, low resistance, high open circuit voltage, carrier separation efficiency, applied bias photon-to-current conversion efficiency (ABPE), and incident photon-to-current conversion efficiency (IPCE). A reduced charge transfer resistance has been demonstrated with Nyquist plots.

Growth and Characteristic of Amorphous Nano-Granular TeO2-V2O5-NiO Thin Films

NASA Astrophysics Data System (ADS)

Hosseinzadeh, Sh.; Rahmati, A.; Bidadi, H.

2016-12-01

TeO2-V2O5-NiO thin films were deposited using thermal evaporation from 40TeO2-(60-y)V2O5-yNiO (y=0-30mol%) target. Structural analysis of the films was identified by X-ray diffractometry (XRD) and scanning electron microscopy (SEM). The amorphous TeO2-V2O5-NiO films have nanosized clear grain structure and sharp grain boundaries. DC conductivity and current-voltage (I-V) characteristic of TeO2-V2O5-NiO thin films were measured in the temperature range of 300-423K. As nickel oxide (NiO) content increases, the DC conductivity decreases up to two orders in value (10-9-10-11Sṡcm-1). Temperature dependence of conductivity is described using the small polaron hopping (SPH) model as well. Poole-Frenkel effect is observed at high external electric field. The optical absorption spectra of the TeO2-V2O5-NiO thin films were recorded in the wavelength range of 380-1100nm. The absorption coefficient revealed bandgap shrinkage (3.01-2.3eV) and band tail widening, due to an increase in NiO content. Energy dispersive X-ray spectroscopy (EDX) was used to determine elemental composition. In TeO2-V2O5-NiO thin films, the NiO content is around fifth of the initial target.

Diazepam-loaded solid lipid nanoparticles: design and characterization.

PubMed

Abdelbary, Ghada; Fahmy, Rania H

2009-01-01

The aim of the present study was to investigate the feasibility of the inclusion of a water-insoluble drug (diazepam, DZ) into solid lipid nanoparticles (SLNs), which offer combined advantages of rapid onset and prolonged release of the drug. This work also describes a new approach to prepare suppositories containing DZ-loaded SLN dispersions, as potential drug carrier for the rectal route. Modified high-shear homogenization and ultrasound techniques were employed to prepare SLNs. The effect of incorporation of different concentrations of Compritol ATO 888 or Imwitor 900K and Poloxamer 188 or Tween 80 was investigated. Results showed that varying the type or concentration of lipid matrix or surfactant had a noticeable influence on the entrapment efficiencies, particle size, and release profiles of prepared SLNs. Differential scanning calorimetry and X-ray diffraction measurements showed that the majority of SLNs possessed less ordered arrangements of crystals than the corresponding bulk lipids, which was favorable for increasing the drug loading capacity. Transmission electron microscopy and laser diffractometry studies revealed that the prepared nanoparticles were round and homogeneous and 60% of the formulations were less than 500 nm. Additionally, SLN formulations showed significant (P < 0.05) prolonged release than DZ solution. The subsequent step encompassed the preparation and evaluation of SLN-based suppositories utilizing SLN formulations that illustrated optimal release profiles. The in vitro release of DZ from the suppositories prepared using DZ-loaded SLN dispersions (equivalent to 2 mg DZ) was significantly (P < 0.05) extended compared to suppositories containing 2 mg DZ free drug.

Effect of magnetic and thermal properties of iron oxide nanoparticles (IONs) in nitrile butadiene rubber (NBR) latex

NASA Astrophysics Data System (ADS)

Ong, Hun Tiar; Julkapli, Nurhidayatullaili Muhd; Hamid, Sharifah Bee Abd; Boondamnoen, O.; Tai, Mun Foong

2015-12-01

Nitrile butadiene rubber (NBR) gloves are one of the most important personal protective equipments but they are possible to tear off and contaminate food or pharmaceutical and healthcare products during manufacturing and packaging process. High tendency of torn glove remaining in food or products due to white or light flesh-coloured glove is not easy to be detected by naked eyes. In this paper, iron oxide nanoparticles (IONs) selected as additive for NBR to improve its detectability by mean of magnetic properties. IONs synthesized via precipitation method and compounded with NBR latex before casting on petri dish. The properties of IONs were investigated by X-ray Diffractometry (XRD), Transmission Electron Microscope (TEM), Raman Spectroscopy and Vibrating Sample Magnetometer (VSM). Meanwhile NBR/IONs composites were studied by Thermogravimetry Analysis (TGA), Differential Scanning Calorimetry (DSC) and Vibrating Sample Magnetometer (VSM). It observed that, synthesized IONs shows of 25.28 nm crystallite with 25.86 nm semipherical (changed as) shape. Meanwhile, Magnetite and maghemite phase are found in range of 670 cm-1 and 700 cm-1 respectively, which it contributes magnetization saturation of 73.96 emu/g at 10,000 G by VSM. Thermal stability and magnetic properties were increased with incorporating IONs into NBR latex up to 20 phr. NBR/IONs 5 phr has the optimum thermal stability, lowest glass transition temperature (-14.83 °C) and acceptable range of magnetization saturation (3.83 emu/g at 10,000 G) to form NBR gloves with magnetic detectability.

Tribological Properties of Ti(Al,O)/Al2O3 Composite Coating by Thermal Spraying

NASA Astrophysics Data System (ADS)

Salman, Asma; Gabbitas, Brian; Cao, Peng; Zhang, Deliang

The use of thermal spray coatings provides protection to the surfaces operating in severe environments. The main goal of the current work is to investigate the possibility of using a high velocity air fuel (HVAF) thermally sprayed wear resistant Ti(Al,O)/Al2O3 coating on tool steel (H13) which is used for making dies for aluminium high pressure die casting and dummy blocks aluminium extrusion. A feedstock of Ti(Al,O)/Al2O3 composite powder was produced from a mixture of Al and TiO2 powders by high energy mechanical milling, followed by a thermal reaction process. The feedstock was then thermally sprayed using a high velocity air-fuel (HVAF) technique onto H13 steel substrates to produce a composite coating. The present study describes and compares the tribological properties such as friction and sliding wear rate of the coating both at room and high temperature (700°C). The wear resistance of the coating was investigated by a tribometer using a spherical ended alumina pin as a counter body under dry and lubricating conditions. The results showed that composite coating has lower wear rate at high temperature than at room temperature without using lubricant. The composite coating was characterized using scanning electron microscopy (SEM), optical microscopy and X-ray diffractometry (XRD). This paper reports the experimental observations and discusses the wear resistance performance of the coatings at room and high temperatures.

A systematic and mechanistic evaluation of aspartic acid as filler for directly compressed tablets containing trimethoprim and trimethoprim aspartate.

PubMed

ElShaer, Amr; Hanson, Peter; Mohammed, Afzal R

2013-04-01

The generally accepted paradigm of 'inert' and 'mono functional' excipient in dosage form has been recently challenged with the development of individual excipients capable of exhibiting multiple functions (e.g. binder-disintegrants, surfactant which affect P-gp function). The proposed study has been designed within the realm of multifunctionality and is the first and novel investigation towards evaluation of aspartic acid as a filler and disintegration enhancing agent for the delivery of biopharmaceutical class IV model drug trimethoprim. The study investigated powder characteristics using angle of repose, laser diffractometry and scanning electron microscopy (SEM). The prepared tablets were characterised using Heckel analysis, disintegration time and tensile strength measurements. Although Heckel analysis revealed that both TMP and TMP aspartate salt have high elasticity, the salt form produced a stronger compact which was attributed to the formation of agglomerates. Aspartic acid was found to have high plasticity, but its incorporation into the formulations was found to have a negative impact on the compaction properties of TMP and its salt. Surface morphology investigations showed that mechanical interlocking plays a vital role in binding TMP crystals together during compaction, while the small particle size of TMP aspartate agglomerates was found to have significant impact on the tensile strength of the tablets. The study concluded that aspartic acid can be employed as filler and disintegrant and that compactability within tablets was independent of the surface charge of the excipients. Copyright © 2012 Elsevier B.V. All rights reserved.

Surface engineering of nanoparticles with macromolecules for epoxy curing: Development of super-reactive nitrogen-rich nanosilica through surface chemistry manipulation

NASA Astrophysics Data System (ADS)

Jouyandeh, Maryam; Jazani, Omid Moini; Navarchian, Amir H.; Shabanian, Meisam; Vahabi, Henri; Saeb, Mohammad Reza

2018-07-01

Curing behavior of epoxy-based nanocomposites depends on dispersion state of nanofillers and their physical and chemical interactions with the curing moieties. In this work, a systematic approach was introduced for chemical functionalization of nanoparticles with macromolecules in order to enrich crosslinking potential of epoxy/amine systems, particularly at late stages of cure where the curing is diffusion-controlled. Super-reactive hyperbranched polyethylenimine (PEI)-attached nanosilica was materialized in this work to facilitate epoxy-amine curing. Starting from coupling [3-(2,3-epoxypropoxy) propyl] trimethoxysilane (EPPTMS) with hyperbranched PEI, a super-reactive macromolecule was obtained and subsequently grafted onto the nanosilica surface. Eventually, a thermally-stable highly-curable nanocomposite was attained by replacement of amine and imine groups of the PEI with imide and amide groups through the reaction with pyromellitic acid dianhydride. Fourier-transform infrared spectrophotometry, X-ray diffractometry, X-ray photoelectron spectroscopy and transmission electron microscopy approved successful grafting of polymer chains onto the nanosilica surface. Thermogravimetric analyses approved a relatively high grafting ratio of ca. 21%. Curing potential of the developed super-reactive nanoparticle was uncovered through nonisothermal differential scanning calorimetry signifying an enthalpy rise of ca. 120 J/g by addition of 2 wt.% to epoxy at 5 °C/min heating rate. Even at low concentration of 0.5 wt.%, the glass transition temperature of epoxy increased from 128 to 156 °C, demonstrating prolonged crosslinking.

Redox-active ionic-liquid-assisted one-step general method for preparing gold nanoparticle thin films: applications in refractive index sensing and catalysis.

PubMed

Dinda, Enakshi; Rashid, Md Harunar; Biswas, Mrinmoy; Mandal, Tarun K

2010-11-16

We describe a general one-step facile method for depositing gold nanoparticle (GNP) thin films onto any type of substrates by the in situ reduction of AuCl(3) using a newly designed redox-active ionic liquid (IL), tetrabutylphosphonium citrate ([TBP][Ci]). Various substrates such as positively charged glass, negatively charged glass/quartz, neutral hydrophobic glass, polypropylene, polystyrene, plain paper, and cellophane paper are successfully coated with a thin film of GNPs. This IL ([TBP][Ci]) is prepared by the simple neutralization of tetrabutylphosphonium hydroxide with citric acid. We also demonstrate that the [TBP][Ci] ionic liquid can be successfully used to generate GNPs in an aqueous colloidal suspension in situ. The deposited GNP thin films on various surfaces are made up of mostly discrete spherical GNPs that are well distributed throughout the film, as confirmed by field-emission scanning electron microscopy. However, it seems that some GNPs are arranged to form arrays depending on the nature of surface. We also characterize these GNP thin films via UV-vis spectroscopy and X-ray diffractometry. The as-formed GNP thin films show excellent stability toward solvent washing. We demonstrate that the thin film of GNPs on a glass/quartz surface can be successfully used as a refractive index (RI) sensor for different polar and nonpolar organic solvents. The as-formed GNP thin films on different surfaces show excellent catalytic activity in the borohydride reduction of p-nitrophenol.

Are nanostructured lipid carriers (NLCs) better than solid lipid nanoparticles (SLNs): development, characterizations and comparative evaluations of clotrimazole-loaded SLNs and NLCs?

PubMed

Das, Surajit; Ng, Wai Kiong; Tan, Reginald B H

2012-08-30

In recent years, solid lipid nanoparticles (SLNs) and nanostructured lipid carriers (NLCs) are among the popular research topics for the delivery of lipophilic drugs. Although SLNs have demonstrated several beneficial properties as drug-carrier, limited drug-loading and expulsion of drug during storage led to the development of NLCs. However, the superiority of NLCs over SLNs has not been fully established yet due to the contradictory results. In this study, SLNs and NLCs were developed using clotrimazole as model drug. Size, polydispersity index (PI), zeta potential (ZP), drug-loading (L), drug encapsulation efficiency (EE), scanning electron microscopy (SEM), differential scanning calorimetry (DSC), X-ray diffractometry (XRD), drug release and stability of SLNs and NLCs were compared. Critical process parameters exhibited significant impact on the nanoparticles' properties. Size, PI, ZP and EE of the developed SLNs and NLCs were<100 nm, <0.17, <-22 mV and>82%, respectively. SEM images of SLNs and NLCs revealed spherical shaped particles (≈ 100 nm). DSC and XRD studies indicated slight difference between SLNs and NLCs as well as disappearance of the crystalline peak(s) of the encapsulated drug. NLCs demonstrated faster drug release than SLNs at low drug-loading, whereas there was no significant difference in drug release from SLNs and NLCs at high drug-loading. However, sustained/prolonged drug release was observed from both formulations. Furthermore, this study suggests that the drug release experiment should be designed considering the final application (topical/oral/parenteral) of the product. Regarding stability, NLCs showed better stability (in terms of size, PI, EE and L) than SLNs at 25°C. Moreover, there was no significant difference in drug release profile of NLCs after 3 months storage in compare to fresh NLCs, while significant change in drug release rate was observed in case of SLNs. Therefore, NLCs have an edge over SLNs. Copyright © 2012 Elsevier B.V. All rights reserved.

IVABRADINE LOADED SOLID LIPID MICROPARTICLES: FORMULATION, CHARACTERIZATION AND OPTIMIZATION BY CENTRAL COMPOSITE ROTATABLE DESIGN.

PubMed

Hanif, Muhammad; Khan, Hafeez Ullah; Afzal, Samina; Sher, Muhammad

2017-01-01

The current research focused on improvement of oral bioavailability and decrease in dosing frequency of ivabradine (Iva) in order to enhance patient compliance by formulating novel sustained release Iva loaded solid lipid microparticles (SLMs) with the help of melt emulsification technique. SLMs formulations were designed with the help of three level central composite rotatable design (CCRD) to study the impact of independent variables like lipid concentration, surfactant concentration and stirring speed on responses - percentage yield (Y,) and entrapment efficiency (Y2). Compatibility between the drug and bees wax (BW) was checked by conducting Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC) and X-ray powder diffractometry (XRD). SLMs were further evaluated for rheological behavior, zeta potential, particle size and for morphology by scanning'electron microscope (SEM). The release of drug from SLMs was conducted by USP type-Il apparatus at pH 1.2, pH 6.8 and data were analyzed by different kinetic models like zero order, first order, Higuchi model, Korsmeyer-Peppas and Hixon-Crowell models. The rheo- logical studies approved the good flow behavior of SLMs and spherical smooth surface of SLMs was observed from SEM. DSC, FTIR and XRD studies concluded the lack of any possible interaction between formulation components. The size-of SLMs ranged from 300 to 500 pm and zeta potential study showed the presence of higher negative charge (-30 to -52 mV). Response Y, varied from 53 to 90% and response Y2 ranged from 29 to 78% indicating the effect of formulation variables. The obtained outcomes were analyzed by second order polynomial equation and suggested quadratic model was also validated. SLMs released Iva from 54 to 90% at pH 6.8 and was significantly (p 0.05) affected by BW concentration. The release mechanism followed the zero order and Korsmeyer-Peppas (n 0.85) kinetic models suggesting slow erosion along with diffusion mechanism for Iva release.

Mesoporous silica templated zirconia nanoparticles

NASA Astrophysics Data System (ADS)

Ballem, Mohamed A.; Córdoba, José M.; Odén, Magnus

2011-07-01

Nanoparticles of zirconium oxide (ZrO2) were synthesized by infiltration of a zirconia precursor (ZrOCl2·8H2O) into a SBA-15 mesoporous silica mold using a wet-impregnation technique. X-ray diffractometry and high-resolution transmission electron microscopy show formation of stable ZrO2 nanoparticles inside the silica pores after a thermal treatment at 550 °C. Subsequent leaching out of the silica template by NaOH resulted in well-dispersed ZrO2 nanoparticles with an average diameter of 4 nm. The formed single crystal nanoparticles are faceted with 110 surfaces termination suggesting it to be the preferred growth orientation. A growth model of these nanoparticles is also suggested.

Corrosion products of carbonation induced corrosion in existing reinforced concrete facades

DOE Office of Scientific and Technical Information (OSTI.GOV)

Köliö, Arto; Honkanen, Mari; Lahdensivu, Jukka

Active corrosion in reinforced concrete structures is controlled by environmental conditions and material properties. These factors determine the corrosion rate and type of corrosion products which govern the total achieved service life. The type and critical amount of corrosion products were studied by electron microscopy and X-ray diffractometry on concrete and reinforcement samples from existing concrete facades on visually damaged locations. The corrosion products in outdoor environment exposed concrete facades are mostly hydroxides (Feroxyhite, Goethite and Lepidocrocite) with a volume ratio to Fe of approximately 3. The results can be used to calibrate calculation of the critical corrosion penetration ofmore » concrete facade panels.« less

Investigation of recrystallization of amorphous trehalose through hot-humidity stage X-ray powder diffraction.

PubMed

Jójárt-Laczkovich, Orsolya; Katona, Gábor; Aigner, Zoltán; Szabó-Révész, Piroska

2016-12-01

The aim of this work was an investigation of the physical changes of the amorphous model material spray-dried trehalose through the use of various analytical techniques and to identify a suitable, rapid method able to quantify the changes. The crystallinity changes and recrystallization process of amorphous samples were investigated by hot-humidity stage X-ray powder diffractometry (HH-XRPD) with fresh samples, conventional X-ray powder diffractometry (XRPD) used stored samples and by differential scanning calorimetry (DSC). The data from the three methods were compared and the various forms of trehalose were analysed. HH-XRPD demonstrated that the recrystallization began at 40 and 60°C up to 45% RH and at 70°C up to 30% RH into dihydrate form. At 70°C up to 60% RH the anhydrous form of trehalose appeared too. Conventional XRPD results showed, that in the 28days stored samples the dihydrate form was detected at 40°C, 50% RH. Storage at 60°C, 40% RH resulted in the appearance of the anhydrous form and at 60°C, 50% RH both polymorphic forms were detected. By carrying out the DSC measurements at different temperatures the fraction of recrystallized trehalose dihydrate was detected. The recrystallization investigated by HH-XRPD and DSC followed Avrami kinetics, the calculated rate constants of isothermal crystallization (K) were same. Both HH-XRPD and conventional XRPD was suitable for the detection of the physical changes of the amorphous model material. DSC measurements showed similar results as HH-XRPD. Primarily HH-XRPD could be suggested for prediction, because the method is fast and every changes could be studied on one sample. Copyright © 2016 Elsevier B.V. All rights reserved.

Solid state of CG-400549, a novel FabI inhibitor: characterization, dissolution, transformation.

PubMed

Kim, Bo-Yeon; Sohn, Young-Taek

2011-05-01

The polymorphic and pseudopolymorphic forms of CG-400549, a novel FabI inhibitor with potent in vivo activity were prepared and characterized by differential scanning calorimetry (DSC), powder X-ray diffractometry (PXRD) and thermogravimetric analysis (TG). Seven crystal forms of CG-400549, one anhydrate and six solvates, have been isolated by recrystallization and the DSC and PXRD patterns of the seven crystal forms of CG-400549 were different respectively. The dissolution patterns of these seven crystal forms of CG-400549 were studied and they showed significant differences in the dissolution rate. After storage of 1 month at 0% RH (silica gel, 20°C), 52% RH (saturated solution of Na(2)Cr(2)O(7)2H(2)O/20°C) and 95% RH (saturated solution of Na(2)HPO(4)/20°C), all crystal forms were not transformed.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pratapa, S.; Susanti, L.; Insany, Y. A. S.

Simple coprecipitation method has been used to produce nanoparticles of MgO (magnesia), MgO{center_dot}Al{sub 2}O{sub 3}(spinel), Y{sub 2}O{sub 3}(yttria) and Fe{sub 3}O{sub 4}(ferrite). The raw materials were, in respective, magnesium powder, magnesium and aluminium powders, ytrria powder, and natural sand. The coprecipitation included the use of suitable acid and base to dissolve the powders or sand and to produce precipitates, as well as the use of water to wash and purify the precipitates, and drying at relatively low temperatures, namely lower than 100 deg. C, followed by heating at 450 deg. C, 750 deg. C, 600 deg. C and 200 deg.more » C to produce magnesia, spinel, yttria and ferrite nanopowders, respectively. X-ray diffractometry was used to characterise the purity and nanocrystallinity of the final powders. It was found qualitatively that the powders were of high purity. Further line-broadening analysis using single-line and Rietveld-based softwares was performed to reveal the nanocrystallinity of the powders. Different line breadth values were found for the powders, indicating different crystallite sizes. It was also found that, particularly for spinel and yttria, the diffraction peaks exhibited 'longer' tails, indicating broader crystallite size distribution. The average crystallite size for the powders ranged from 3 to 70 nm. The results could then be used as 'fingerprints' for nanocrystallinity using x-ray diffractometry. The XRD crystallite sizes for yttria and ferrite nanocrystals are in fair agreement with their counterparts from electron microscopy observation.« less

Study of multilayered SiGe semiconductor structures by X-ray diffractometry, grazing-incidence X-ray reflectometry, and secondary-ion mass spectrometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yunin, P. A., E-mail: yunin@ipmras.ru; Drozdov, Yu. N.; Drozdov, M. N.

2013-12-15

In this publication, we report the results of studying a multilayerd nonperiodic SiGe/Si structure by the methods of X-ray diffractometry, grazing-angle X-ray reflectometry, and secondary-ion mass spectrometry (SIMS). Special attention is paid to the processing of the component distribution profile using the SIMS method and to consideration of the most significant experimental distortions introduced by this method. A method for processing the measured composition distribution profile with subsequent consideration of the influence of matrix effects, variation in the etching rate, and remnants of ion sputtering is suggested. The results of such processing are compared with a structure model obtained uponmore » combined analysis of X-ray diffractometry and grazing-angle reflectometry data. Good agreement between the results is established. It is shown that the combined use of independent techniques makes it possible to improve the methods of secondary-ion mass spectrometry and grazing-incidence reflectometry as applied to an analysis of multilayered heteroepitaxial structures (to increase the accuracy and informativity of these methods)« less

New insight into the promoting role of process on the CeO₂-WO₃/TiO₂ catalyst for NO reduction with NH₃ at low-temperature.

PubMed

Zhang, Shule; Zhong, Qin; Shen, Yuge; Zhu, Li; Ding, Jie

2015-06-15

This study aimed at investigating the reason of high catalytic activity for CeO2-WO3/TiO2 catalyst from the aspects of WO3 interaction with other species and the NO oxidation process. Analysis by X-ray diffractometry, photoluminescence spectra, diffuse reflectance UV-visible, X-ray photoelectron spectroscopy, density functional theory calculations, electron paramagnetic resonance spectroscopy, temperature-programmed-desorption of NO and in situ diffuse reflectance infrared transform spectroscopy showed that WO3 could interact with CeO2 to improve the electron gaining capability of CeO2 species. In addition, WO3 species acted as electron donating groups to transfer the electrons to CeO2 species. The two aspects enhanced the formation of reduced CeO2 species to improve the formation of superoxide ions. Furthermore, the Ce species were the active sites for the NO adsorption and the superoxide ions over the catalyst needed oxidizing the adsorbed NO to improve the NO oxidation. This process was responsible for the high catalytic activity of CeO2-WO3/TiO2 catalyst. Copyright © 2015 Elsevier Inc. All rights reserved.

A novel strategy to directly fabricate flexible hollow nanofibers with tunable luminescence-electricity-magnetism trifunctionality using one-pot electrospinning.

PubMed

Liu, Yawen; Ma, Qianli; Dong, Xiangting; Yu, Wensheng; Wang, Jinxian; Liu, Guixia

2015-09-21

Novel photoluminescent-electrical-magnetic trifunctional flexible Eu(BA)3phen/PANI/Fe3O4/PVP (BA = benzoic acid, phen = phenanthroline, PANI = polyaniline, PVP = polyvinylpyrrolidone) hollow nanofibers were fabricated by a one-pot electrospinning technique using a specially designed coaxial spinneret for the first time. Very different from the traditional preparation process of hollow fibers via coaxial electrospinning, which needs to firstly fabricate the coaxial fibers and followed by removing the core through high-temperature calcination or solvent extraction, in our current study, no core spinning solution is used to directly fabricate hollow nanofibers. The morphology and properties of the obtained hollow nanofibers were characterized in detail using X-ray diffractometry, scanning electron microscopy, transmission electron microscopy, fluorescence spectroscopy, Fourier-transform infrared spectroscopy, a 4-point probe resistivity measurement system and vibrating sample magnetometry. The Eu(BA)3phen/PANI/Fe3O4/PVP hollow nanofibers, with outer diameters of ca. 305 nm and inner diameters of about 140 nm, exhibit excellent photoluminescence performance, electrical conductivity and magnetic properties. Fluorescence emission peaks of Eu(3+) are observed in the Eu(BA)3phen/PANI/Fe3O4/PVP hollow nanofibers and assigned to the (5)D0→(7)F0 (580 nm), (5)D0→(7)F1 (592 nm) and (5)D0→(7)F2 (616 nm) energy level transitions of Eu(3+) ions, and the (5)D0→(7)F2 hypersensitive transition at 616 nm is the predominant emission peak. The electrical conductivity of the hollow nanofibers reaches up to the order of 10(-3) S cm(-1). The luminescent intensity, electrical conductivity and magnetic properties of the hollow nanofibers can be tuned by adding various amounts of Eu(BA)3phen, PANI and Fe3O4 nanoparticles. The new-type photoluminescent-electrical-magnetic trifunctional flexible hollow nanofibers hold potential for a variety of applications, including electromagnetic interference shielding, microwave absorption, molecular electronics and biomedicine. The design conception and synthetic strategy developed in this study are of universal significance to construct other multifunctional hollow one-dimensional nanomaterials.

Investigating the effect of Cd-Mn co-doped nano-sized BiFeO3 on its physical properties

NASA Astrophysics Data System (ADS)

Ishaq, B.; Murtaza, G.; Sharif, S.; Azhar Khan, M.; Akhtar, Naeem; Will, I. G.; Saleem, Murtaza; Ramay, Shahid M.

This work deals with the investigation of different effects on the structural, magnetic, electronic and dielectric properties of Cd and Mn doped Bi0.75Cd0.25Fe1-xMnxO3 multiferroic samples by taking fixed ratios of Cd and varying the Mn ratio with values of x = 0.0, 0.5, 0.10 and 0.15. Cd-Mn doped samples were synthesized chemically using a microemulsion method. All the samples were finally sintered at 700 °C for 2 h to obtain the single phase perovskites structure of BiFeO3 materials. The synthesized samples were characterized by different techniques, such as X-ray diffractometry (XRD), Scanning Electron Microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), LCR meter and magnetic properties using VSM. XRD results confirm BFO is a perovskite structure having crystallite size in the range of 24-54 nm. XRD results also reveal observed structural distortion due to doping of Cd at the A-site and Mn at the B-site of BFO. SEM results depict that, as the substitution of Cd-Mn increases in BFO, grain size decreases up to 30 nm. FTIR spectra showed prominent absorption bands at 555 cm-1 and 445 cm-1 corresponding to the stretching vibrations of the metal ions complexes at site A and site B, respectively. Variation of dielectric constant (ɛ‧) and loss tangent (tan δ) at room temperature in the range of 1 MHz to 3 GHz have been investigated. Results reveal that with Cd-Mn co doping a slight decrease in dielectric constant have been observed. Magnetic properties of Cd-Mn doped pure BFO samples have been studied at 300 K. Results reveal that undoped BiFeO3 exhibits weak ferromagnetic ordering due to the canting of its spin. Increase in magnetization and decrease in coercivity is a clear indication that a material can be used in high density recording media and memory devices.

Software electron counting for low-dose scanning transmission electron microscopy.

PubMed

Mittelberger, Andreas; Kramberger, Christian; Meyer, Jannik C

2018-05-01

The performance of the detector is of key importance for low-dose imaging in transmission electron microscopy, and counting every single electron can be considered as the ultimate goal. In scanning transmission electron microscopy, low-dose imaging can be realized by very fast scanning, however, this also introduces artifacts and a loss of resolution in the scan direction. We have developed a software approach to correct for artifacts introduced by fast scans, making use of a scintillator and photomultiplier response that extends over several pixels. The parameters for this correction can be directly extracted from the raw image. Finally, the images can be converted into electron counts. This approach enables low-dose imaging in the scanning transmission electron microscope via high scan speeds while retaining the image quality of artifact-free slower scans. Copyright © 2018 The Authors. Published by Elsevier B.V. All rights reserved.

Self-propagating high-temperature synthesis and luminescent properties of ytterbium doped rare earth (Y, Sc, Lu) oxides nanopowders

NASA Astrophysics Data System (ADS)

Permin, D. A.; Novikova, A. V.; Balabanov, S. S.; Gavrishchuk, E. M.; Kurashkin, S. V.; Savikin, A. P.

2018-04-01

This paper describes a comparative study of structural and luminescent properties of 5%Yb-doped yttrium, scandium, and lutetium oxides (Yb:RE2O3) powders and ceramics fabricated by self-propagating high-temperature synthesis. According to X-ray diffractometry and electron microscopy the chosen method ensures preparation of low-agglomerated cubic Ctype crystal structured powders at one step. No crucial differences in luminescence spectra were found the Yb:RE2O3 powders and ceramics. It was shown that the emission lifetimes of the Yb:RE2O3 powders are lowered by crystal structure defects, while its values for ceramics samples are compared to that of monocrystals and more influenced by rare earth impurities.

Characterizing mineral dusts and other aerosols from the Middle East--Part 2: grab samples and re-suspensions.

PubMed

Engelbrecht, Johann P; McDonald, Eric V; Gillies, John A; Jayanty, R K M Jay; Casuccio, Gary; Gertler, Alan W

2009-02-01

The purpose of the Enhanced Particulate Matter Surveillance Program was to provide scientifically founded information on the chemical and physical properties of dust collected during a period of approximately 1 year in Djibouti, Afghanistan (Bagram, Khowst), Qatar, United Arab Emirates, Iraq (Balad, Baghdad, Tallil, Tikrit, Taji, Al Asad), and Kuwait (northern, central, coastal, and southern regions). To fully understand mineral dusts, their chemical and physical properties, as well as mineralogical inter-relationships, were accurately established. In addition to the ambient samples, bulk soil samples were collected at each of the 15 sites. In each case, approximately 1 kg of soil from the top 10 mm at a previously undisturbed area near the aerosol sampling site was collected. The samples were air-dried and sample splits taken for soil analysis. Further sample splits were sieved to separate the < 38 micro m particle fractions for mineralogical analysis. Examples of major-element and trace-element chemistry, mineralogy, and other physical properties of the 15 grab samples are presented. The purpose of the trace-element analysis was to measure levels of potentially harmful metals while the major-element and ion-chemistry analyses provided an estimate of mineral components. X-ray diffractometry provided a measure of the mineral content of the dust. Scanning electron microscopy with energy dispersive spectroscopy was used to analyze chemical composition of small individual particles. From similarities in the chemistry and mineralogy of re-suspended and ambient sample sets, it is evident that portions of the ambient dust are from local soils.

Effect of cooling rate and Mg addition on the structural evaluation of rapidly solidified Al-20wt%Cu-12wt%Fe alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Karaköse, Ercan, E-mail: ekarakose@karatekin.edu.t

2016-11-15

The present work examines the effect of Mg contents and cooling rate on the morphology and mechanical properties of Al{sub 20}Cu{sub 12}Fe quasicrystalline alloy. The microstructure of the alloys was analyzed by scanning electron microscopy and the phase composition was identified by X-ray diffractometry. The melting characteristics were studied by differential thermal analysis under an Ar atmosphere. The mechanical features of the melt-spun and conventionally solidified alloys were tested by tensile-strength test and Vickers micro-hardness test. It was found that the final microstructure of the Al{sub 20}Cu{sub 12}Fe samples mainly depends on the cooling rate and Mg contents, which suggestsmore » that different cooling rates and Mg contents produce different microstructures and properties. The average grain sizes of the melt spun samples were about 100–300 nm at 35 m/s. The nanosize, dispersed, different shaped quasicrystal particles possessed a remarkable effect to the mechanical characteristics of the rapidly solidified ribbons. The microhardness values of the melt spun samples were approximately 18% higher than those of the conventionally counterparts. - Highlights: •Quasicrystal-creating materials have high potential for applications. •Different shaped nanosize quasicrystal particles were observed. •The addition of Mg has an important impact on the mechanical properties. •H{sub V} values of the MS0, MS3 and MS5 samples at 35 m/s were 8.56, 8.66 and 8.80 GPa. •The volume fraction of IQC increases with increasing cooling rates.« less

[The "silica" component in the PM10 of an urban site].

PubMed

De Berardis, Barbara; Incocciati, Emma; Massera, S; Gargaro, G; Paoletti, L

2007-01-01

In vivo and in vitro toxicological studies have shown that the aged fracturated crystalline silica, which is a component of airborne particulate, exerts an important inflammatory action on airways. The evaluation of the concentration level of airborne crystalline silica in an urban area is an important research subject in order to determine the exposure levels of the general population. The aim was to study the seasonal trend of the quartz (the most common form of crystalline silica) concentration levels in the particulate inhalable faction (PM10) in the urban area of Rome. PM10, sampled by a cascade impactor, was analysed by scanning electron microscopy, equipped with a thin-window system for X-ray microanalysis (SEM/EDX) for qualitative analysis. Parallely the concentration levels of quartz in the particulate were determined by X-ray diffractometry (XRD) for quantitative analysis, using the NIOSH 7500 method (NIOSH, 1994). From September 2004 to October 2005 the abundance of silica particles, evaluated by SEM/EDX was in the range 1.6/10.4%, with a concentration level of free crystalline silica in the range 0.25/2.87 microg/mi. The equivalent diameter of silica particles ranged from 0.3 to 10.5 mircom, moreover, more than 87% of particles showed a diameter less than 2.5 microm. The correlations between SEM/EDX and XRD data seem to suggest that the airborne silica particles in the urban location studied consisted mostly of crystalline silica. Moreover, the data suggest the existence of a significant contribution of silica particles due to southwest wind carrying a fine dust from the Sahara desert to Mediterranean Europe.

Preparation, characterization and millimetre wave attenuation performance of carbon fibers coated with nickel-wolfram-phosphorus and nickel-cobalt-wolfram- phosphorus

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ye, Mingquan; Li, Zhitao; Wang, Chen

2016-04-15

Highlights: • SEM, XRD, EDS and MMW attenuation performances of alloys coated CFs were studied. • Resistivity and P content in alloys were main factors on MMW attenuation property. • The weight gain of coated CFs has effects on the MMW attenuation performance. - Abstract: Carbon fibers (CFs) coated with Ni–X–P (X = W, Co–W or none) alloys were prepared by electroless plating. The morphology, crystal structure, and element composition of alloy-coated CFs were characterized by scanning electron microscopy, X-ray diffractometry, energy-dispersive spectrometry and microwave attenuation. The results showed that CFs were coated with a layer of alloy particles. Pmore » content in Ni–Co–W–P or Ni–W–P alloys was lower than that in Ni–P alloy, and coating alloy Ni–P was amorphous. After W or Co introduction, coating alloys exhibited crystal characteristics. MMW-attenuation performance analysis showed that the 3 mm wave attenuation performance of CFs/Ni–Co–W–P, CFs/Ni–W–P and CFs/Ni–P increased by 7.27 dBm, 4.88 dBm and 3.55 dBm, and the 8 mm wave attenuation effects increased by 11.61 dBm, 6.11 dBm, and 4.06 dBm respectively, compared with those of CFs. MMW-attenuation performance is attributable to the sample bulk resistivity and P content in the alloy. Moreover, an optimal weight gain value existed for the MMW-attenuation performance of alloy-coated CFs.« less

Nanocrystalline Ce 1- xY xO 2- x/2 (0≤ x≤0.35) Oxides via Carbonate Precipitation: Synthesis and Characterization

NASA Astrophysics Data System (ADS)

Li, Ji-Guang; Ikegami, Takayasu; Wang, Yarong; Mori, Toshiyuki

2002-10-01

A novel carbonate (co)precipitation method, employing nitrates as the starting salts and ammonium carbonate as the precipitant, has been used to synthesize nanocrystalline CeO 2 and Ce 1- xY xO 2- x/2 ( x≤0.35) solid-solutions. The resultant powders are characterized by elemental analysis, differential thermal analysis/thermogravimetry (DTA/TG), X-ray diffractometry (XRD), Brunauer-Emmett-Teller (BET) analysis, and high-resolution scanning electron microscopy (HRSEM). Due to the direct formation of carbonate solid-solutions during precipitation, Ce 1- xY xO 2- x/2 solid-solution oxides are formed directly during calcination at a very low temperature of ˜300°C for 2 h. The thus-produced oxide nanopowders are essentially non-agglomerated, as revealed by BET in conjunction with XRD analysis. The solubility of YO 1.5 in CeO 2 is determined via XRD to be somewhere in the range from 27 to 35 mol%, from which a Y 2O 3-related type-C phase appears in the final product. Y 3+-doping promotes the formation of spherical nanoparticles, retards thermal decomposition of the precursors, and suppresses significantly crystallite coarsening of the oxides during calcination. The activation energy for crystallite coarsening increases gradually from 68.7 kJ mol -1 for pure CeO 2 to 138.6 kJ mol -1 for CeO 2 doped with 35 mol% YO 1.5. The dopant effects on crystallite coarsening is elaborated from the view point of solid-state chemistry.

Tribological properties of thermally sprayed TiAl-Al2O3 composite coating

NASA Astrophysics Data System (ADS)

Salman, A.; Gabbitas, B.; Li, J.; Zhang, D.

2009-08-01

The use of thermal spray coatings provides protection to the surfaces operating in severe environments. The main goal of the current work is to investigate the possibility of using a high velocity oxy fuel (HVOF) thermally sprayed wear resistant TiAl/Al2O3 coating on tool steel (H13) which is used for making dies for aluminium high pressure die casting. A feedstock of TiAl/Al2O3 composite powder was produced from a mixture of Al and TiO2 powders by high energy mechanical milling, followed by a thermal reaction process. The feedstock was then thermally sprayed using a high velocity oxy-fuel (HVOF) technique onto H13 steel substrates to produce a composite coating. The present study describes and compares the tribological properties such as friction and sliding wear rate of the coating both at room and high temperature (700°C). The results showed that the composite coating has lower wear rate at high temperature (700°C) than the uncoated H13 sample. At Room temperature without using lubricant there is no much significant difference between the wear rate of the coated and uncoated samples. The experimental results showed that the composite coating has great potential for high temperature application due to its lower wear rate at high temperature in comparison with the uncoated sample at the same temperature. The composite coating was characterized using scanning electron microscopy (SEM), optical microscopy and X-ray diffractometry (XRD). This paper reports the experimental observations and discusses the wear resistance performance of the coatings at room and high temperatures.

System and method for compressive scanning electron microscopy

DOEpatents

Reed, Bryan W

2015-01-13

A scanning transmission electron microscopy (STEM) system is disclosed. The system may make use of an electron beam scanning system configured to generate a plurality of electron beam scans over substantially an entire sample, with each scan varying in electron-illumination intensity over a course of the scan. A signal acquisition system may be used for obtaining at least one of an image, a diffraction pattern, or a spectrum from the scans, the image, diffraction pattern, or spectrum representing only information from at least one of a select subplurality or linear combination of all pixel locations comprising the image. A dataset may be produced from the information. A subsystem may be used for mathematically analyzing the dataset to predict actual information that would have been produced by each pixel location of the image.

Geology and geochemistry of the Arctic prospect, Ambler District, Alaska

NASA Astrophysics Data System (ADS)

Schmidt, J. M.

The Arctic volcanogenic massive sulfide prospect is the largest known (40 million ton) deposit hosted by the low greenschist grade, latest Devonian Ambler Sequence of bimodal, basaltic and rhyolitic volcanic and volcanoclastic rocks, pelitic, graphitic and calcareous metasediments. Detailed field mapping, core logging, petrography, X-ray diffractometry, electron microprobe analyses and whole-rock major element analyses of hydrothermally altered rocks were used to determine the emplacement history and setting of sulfide deposition. Low greenschist grade metamorphism was essentially isochemical on a macroscopic scale, and preserved volcanic compositions, the major element chemistry of alteration and the compositions of individual metamorphic, alteration and relict igneous minerals. Mineralization at Arctic was formed along a synvolcanic fault in a tectonically and volcanically active basin within a rifted continental margin, possibly related to an actively spreading oceanic rift.

In-line metrology for roll-to-roll UV assisted nanoimprint lithography using diffractometry

NASA Astrophysics Data System (ADS)

Kreuzer, Martin; Whitworth, Guy L.; Francone, Achille; Gomis-Bresco, Jordi; Kehagias, Nikolaos; Sotomayor-Torres, Clivia M.

2018-05-01

We describe and discuss the optical design of a diffractometer to carry out in-line quality control during roll-to-roll nanoimprinting. The tool measures diffractograms in reflection geometry, through an aspheric lens to gain fast, non-invasive information of any changes to the critical dimensions of target grating structures. A stepwise tapered linear grating with constant period was fabricated in order to detect the variation in grating linewidth through diffractometry. The minimum feature change detected was ˜40 nm to a precision of 10 nm. The diffractometer was then integrated with a roll-to-roll UV assisted nanoimprint lithography machine to gain dynamic measurements in situ.

Influence of pH and method of crystallization on the solid physical form of indomethacin.

PubMed

Dubbini, Alessandra; Censi, Roberta; Martena, Valentina; Hoti, Ela; Ricciutelli, Massimo; Malaj, Ledjan; Di Martino, Piera

2014-10-01

The purpose of this study was to investigate the effect of pH and method of crystallization on the solid physical form of indomethacin (IDM). IDM, a non steroidal anti-inflammatory drug poorly soluble in water, underwent two different crystallization methods: crystallization by solvent evaporation under reduced pressure at 50.0°C (method A), and crystallization by cooling of solution from 50.0 to 5.0°C (method B). In both cases, several aqueous ethanolic solutions of IDM of different pHs were prepared. pHs were adjusted by adding acidic solutions (HCl 2M) or alkali (NaOH or NH4OH 2M) to an aqueous ethanolic solution of IDM. Thus, several batches were recovered after crystallization. The chemical stability of IDM was verified through (1)H NMR and mass spectroscopy (FIA-ESI-MS), that revealed that IDM degraded in strong alkali media (pH ≥ 12). Crystals obtained under different crystallization conditions at pHs of 1.0, 4.5, 7.0, 8.0, 10.0 and chemically stable were thus characterized for crystal habit by scanning electron microscopy, for thermal behaviour by differential scanning calorimetry, and thermogravimetry, and for solid state by X-ray powder diffractometry. Under the Method A, IDM always crystallized into pure metastable alpha form when solutions were acidified or alkalized respectively with HCl and NH4OH. On the contrary, in presence of NaOH, IDM crystallized under a mixture of alpha and sodium trihydrate form, because the presence of the sodium counter ion orientates the crystallization towards the formation of the trihydrate salt. Under the method B, at pH of 1.0, IDM crystallized under the alpha form; at pH 4.5, IDM crystallized under the form alpha in presence of some nuclei of gamma form; at pH 7.0, 8.0, and 10.0 for NH4OH, IDM crystallized under the most stable polymorph gamma form, whereas in presence of NaOH, a mix of alpha, and salt forms was formed whatever the pH of the solution. Copyright © 2014 Elsevier B.V. All rights reserved.

Electrochemical and Spectroscopic Analysis of Mg2+ Intercalation into Thin Film Electrodes of Layered Oxides: V2O5 and MoO3

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gershinsky, G; Yoo, HD; Gofer, Y

Electrochemical, surface, and structural studies related to rechargeable Mg batteries were carried out with monolithic thin-film cathodes comprising layered V2O5 and MoO3. The reversible intercalation reactions of these electrodes with Mg ion in nonaqueous Mg salt solutions were explored using a variety of analytical tools. These included slow-scan rate cyclic voltammetry (SSCV), chrono-potentiometry (galvanostatic cycling), Raman and photoelectron spectroscopies, high-resolution microscopy, and XRD. The V2O5 electrodes exhibited reversible Mg-ion intercalation at capacities around 150-180 mAh g(-1) with 100% efficiency. A capacity of 220 mAh g(-1) at >95% efficiency was obtained with MoO3 electrodes. By applying the electrochemical driving force sufficientlymore » slowly it was possible to measure the electrodes at equilibrium conditions and verify by spectroscopy, microscopy, and diffractometry that these electrodes undergo fully reversible structural changes upon Mg-ion insertion/deinsertion cycling.« less

Solid-State Characterization of Novel Propylene Glycol Ester Solvates Isolated from Lipid Formulations.

PubMed

Chakravarty, Paroma; Kothari, Sanjeev; Deese, Alan; Lubach, Joseph W

2015-07-06

The purpose of this study was to identify and characterize precipitates obtained from a liquid formulation of GNE068.HCl, a Genentech developmental compound, and lipophilic excipients, such as propylene glycol monocaprylate, and monolaurate. Precipitates were characterized using powder X-ray diffractometry (PXRD), differential scanning calorimetry, thermogravimetry, microscopy, nuclear magnetic resonance spectroscopy (NMR; solution and solid-state) and water sorption analysis. PXRD and NMR revealed the precipitates to be crystalline solvates of propylene glycol esters. The solvates (capryolate and lauroglycolate) were isomorphic and stable up to 70 °C, beyond which melting of the lattice occurred with subsequent dissolution of the active ingredient in the melt (microscopy and variable temperature PXRD). They were found to be mechanically stable (no change in PXRD pattern upon compression) and were nonhygroscopic up to ∼70% RH (25 °C). Our results highlight the outcome of inadvertent drug-excipient interactions in two separate lipid solution formulations with good solid-state properties and, thus, potential for further development.

Formulation and Solid State Characterization of Nicotinamide-based Co-crystals of Fenofibrate

PubMed Central

Shewale, Sheetal; Shete, A. S.; Doijad, R. C.; Kadam, S. S.; Patil, V. A.; Yadav, A. V.

2015-01-01

The present investigation deals with formulation of nicotinamide-based co-crystals of fenofibrate by different methods and solid-state characterization of the prepared co-crystals. Fenofibrate and nicotinamide as a coformer in 1:1 molar ratio were used to formulate molecular complexes by kneading, solution crystallization, antisolvent addition and solvent drop grinding methods. The prepared molecular complexes were characterized by powder X-ray diffractometry, differential scanning calorimetry, Fourier transform infrared spectroscopy, nuclear magnetic resonance spectroscopy and in vitro dissolution study. Considerable improvement in the dissolution rate of fenofibrate from optimized co-crystal formulation was due to an increased solubility that is attributed to the super saturation from the fine co-crystals is faster because of large specific surface area of small particles and prevention of phase transformation to pure fenofibrate. In vitro dissolution study showed that the formation of co-crystals improves the dissolution rate of fenofibrate. Nicotinamide forms the co-crystals with fenofibrate, theoretically and practically. PMID:26180279

Solubility and conversion of carbamazepine polymorphs in supercritical carbon dioxide.

PubMed

Bettini, R; Bonassi, L; Castoro, V; Rossi, A; Zema, L; Gazzaniga, A; Giordano, F

2001-06-01

The aim of this work was to investigate whether mixtures of carbamazepine polymorphs could be processed in supercritical (SC) CO(2) in order to obtain the pure stable crystalline phase. To accomplish this goal the solubility of carbamazepine polymorphs I and III in supercritical CO(2) was first assessed using a low solvent flux dynamic method. Mixtures of Form I and Form III were processed in dynamic or static conditions in SC-CO(2). Differential scanning calorimetry, Fourier transformed infrared spectroscopy, and powder X-ray diffractometry were used to analyse solid samples in terms of polymorph composition. It was found that Form I and Form III of carbamazepine have different solubility in supercritical CO(2) at 55 degrees C above 300 bar. Due to the transformation of the metastable form, conversion of Form I into Form III can be carried out on a binary mixture of the two polymorphs by treating the mixture at 55 degrees C and 350 bar, under both static and dynamic conditions, via its solubilization in supercritical CO(2).

Synchronized voltage contrast display analysis system

NASA Technical Reports Server (NTRS)

Johnston, M. F.; Shumka, A.; Miller, E.; Evans, K. C. (Inventor)

1982-01-01

An apparatus and method for comparing internal voltage potentials of first and second operating electronic components such as large scale integrated circuits (LSI's) in which voltage differentials are visually identified via an appropriate display means are described. More particularly, in a first embodiment of the invention a first and second scanning electron microscope (SEM) are configured to scan a first and second operating electronic component respectively. The scan pattern of the second SEM is synchronized to that of the first SEM so that both simultaneously scan corresponding portions of the two operating electronic components. Video signals from each SEM corresponding to secondary electron signals generated as a result of a primary electron beam intersecting each operating electronic component in accordance with a predetermined scan pattern are provided to a video mixer and color encoder.

An x-ray diffraction study of microstructural deformation induced by cyclic loading of selected steel

NASA Astrophysics Data System (ADS)

Fourspring, Patrick Michael

X-ray double crystal diffractometry (XRDCD) and X-ray scanning diffractometry (XRSD) were used to assess cyclic microstructural deformation in a face centered cubic (fcc) steel (AISI304) and a body centered cubic (bcc) steel (SA508 class 2). The objectives of the investigation were to determine if X-ray diffraction could be used effectively to monitor cyclic microstructural deformation in polycrystalline Fe alloys and to study the distribution of the microstructural deformation induced by cyclic loading in these alloys. The approach used in the investigation was to induce fatigue damage in a material and to characterize the resulting microstructural deformation at discrete fractions of the fatigue life of the material. Also, characterization of microstructural deformation was carried out to identify differences in the accumulation of damage from the surface to the bulk, focusing on the following three regions: near surface (0-10 mum), subsurface (10-300 mum), and bulk. Characterization of the subsurface region was performed only on the AISI304 material because of the limited availability of the SA508 material. The results from the XRDCD data indicate a measurable change induced by fatigue from the initial state to subsequent states of both the AISI304 and the SA508 materials. The results from the XRSD data show similar but less coherent trends than the results from the XRDCD data. Therefore, the XRDCD technique was shown to be sensitive to the microstructural deformation caused by fatigue in steels; thus, the technique can be used to monitor fatigue damage in steels. In addition, for the AISI304 material, the level of cyclic microstructural deformation in the bulk material was found to be greater than the level in the near surface material. In contrast, previous investigations have shown that the deformation is greater in the near surface than the bulk for Al alloys and bcc Fe alloys.

Swept Line Electron Beam Annealing of Ion Implanted Semiconductors.

DTIC Science & Technology

1982-07-01

of my research to the mainstream of technology. The techniques used for beam processing are distinguished by their * ~.* beam source and method by...raster scanned CW lasers (CWL), pulsed ion beams (PI), area pulsed electron beams (PEE), raster scanned (RSEB) or multi - scanned electron beams (MSEB...where high quality or tailored profiles are required. Continuous wave lasers and multi -scanned or swept-line electron beams are the most likely candidates

Scanning Transmission Electron Microscopy | Materials Science | NREL

Science.gov Websites

mode by collecting the EDS and EELS signals point-by-point as one scans the electron probe across the . Examples of Scanning Transmission Electron Microscopy Capabilities Z-contrast image microphoto taken by

Application of environmental scanning electron microscopy to determine biological surface structure.

PubMed

Kirk, S E; Skepper, J N; Donald, A M

2009-02-01

The use of environmental scanning electron microscopy in biology is growing as more becomes understood about the advantages and limitations of the technique. These are discussed and we include new evidence about the effect of environmental scanning electron microscopy imaging on the viability of mammalian cells. We show that although specimen preparation for high-vacuum scanning electron microscopy introduces some artefacts, there are also challenges in the use of environmental scanning electron microscopy, particularly at higher resolutions. This suggests the two technologies are best used in combination. We have used human monocyte-derived macrophages as a test sample, imaging their complicated and delicate membrane ruffles and protrusions. We have also explored the possibility of using environmental scanning electron microscopy for dynamic experiments, finding that mammalian cells cannot be imaged and kept alive in the environmental scanning electron microscopy. The dehydration step in which the cell surface is exposed causes irreversible damage, probably via loss of membrane integrity during liquid removal in the specimen chamber. Therefore, mammalian cells should be imaged after fixation where possible to protect against damage as a result of chamber conditions.

Accurate Virus Quantitation Using a Scanning Transmission Electron Microscopy (STEM) Detector in a Scanning Electron Microscope

DTIC Science & Technology

2017-06-29

Accurate Virus Quantitation Using a Scanning Transmission Electron Microscopy (STEM) Detector in a Scanning Electron Microscope Candace D Blancett1...L Norris2, Cynthia A Rossi4 , Pamela J Glass3, Mei G Sun1,* 1 Pathology Division, United States Army Medical Research Institute of Infectious...Diseases (USAMRIID), 1425 Porter Street, Fort Detrick, Maryland, 21702 2Biostatistics Division, United States Army Medical Research Institute of

Electron probe X-ray microanalysis of cultured myogenic C2C12 cells with scanning and scanning transmission electron microscopy.

PubMed

Tylko, G; Karasiński, J; Wróblewski, R; Roomans, G M; Kilarski, W M

2000-01-01

Heterogeneity of the elemental content of myogenic C2C12 cultured cells was studied by electron probe X-ray microanalysis (EPXMA) with scanning (SEM EPXMA) and scanning transmission electron microscopy (STEM EPXMA). The best plastic substrate for growing cells was Thermanox. For STEM EPXMA, a Formvar film coated with carbon was found to be suitable substrate. The cells examined by scanning transmission electron microscopy showed great heterogeneity in their elemental content in comparison with the cells examined in the scanning electron microscope despite of an almost identical preparation procedure for EPXMA. Nevertheless the K/Na ratios obtained from both methods of EPXMA were very close (4.1 and 4.3). We conclude that the observed discrepancy in the elemental content obtained by the two methods may be due to differences in instrumentation and this must be taken into account when planning a comparative study.

Identifying the hazard characteristics of powder byproducts generated from semiconductor fabrication processes.

PubMed

Choi, Kwang-Min; An, Hee-Chul; Kim, Kwan-Sick

2015-01-01

Semiconductor manufacturing processes generate powder particles as byproducts which potentially could affect workers' health. The chemical composition, size, shape, and crystal structure of these powder particles were investigated by scanning electron microscopy equipped with an energy dispersive spectrometer, Fourier transform infrared spectrometry, and X-ray diffractometry. The powders generated in diffusion and chemical mechanical polishing processes were amorphous silica. The particles in the chemical vapor deposition (CVD) and etch processes were TiO(2) and Al(2)O(3), and Al(2)O(3) particles, respectively. As for metallization, WO(3), TiO(2), and Al(2)O(3) particles were generated from equipment used for tungsten and barrier metal (TiN) operations. In photolithography, the size and shape of the powder particles showed 1-10 μm and were of spherical shape. In addition, the powders generated from high-current and medium-current processes for ion implantation included arsenic (As), whereas the high-energy process did not include As. For all samples collected using a personal air sampler during preventive maintenance of process equipment, the mass concentrations of total airborne particles were < 1 μg, which is the detection limit of the microbalance. In addition, the mean mass concentrations of airborne PM10 (particles less than 10 μm in diameter) using direct-reading aerosol monitor by area sampling were between 0.00 and 0.02 μg/m(3). Although the exposure concentration of airborne particles during preventive maintenance is extremely low, it is necessary to make continuous improvements to the process and work environment, because the influence of chronic low-level exposure cannot be excluded.

A Lower Temperature FDM 3D Printing for the Manufacture of Patient-Specific Immediate Release Tablets.

PubMed

Okwuosa, Tochukwu C; Stefaniak, Dominika; Arafat, Basel; Isreb, Abdullah; Wan, Ka-Wai; Alhnan, Mohamed A

2016-11-01

The fabrication of ready-to-use immediate release tablets via 3D printing provides a powerful tool to on-demand individualization of dosage form. This work aims to adapt a widely used pharmaceutical grade polymer, polyvinylpyrrolidone (PVP), for instant on-demand production of immediate release tablets via FDM 3D printing. Dipyridamole or theophylline loaded filaments were produced via processing a physical mixture of API (10%) and PVP in the presence of plasticizer through hot-melt extrusion (HME). Computer software was utilized to design a caplet-shaped tablet. The surface morphology of the printed tablet was assessed using scanning electron microscopy (SEM). The physical form of the drugs and its integrity following an FDM 3D printing were assessed using x-ray powder diffractometry (XRPD), thermal analysis and HPLC. In vitro drug release studies for all 3D printed tablets were conducted in a USP II dissolution apparatus. Bridging 3D printing process with HME in the presence of a thermostable filler, talc, enabled the fabrication of immediate release tablets at temperatures as low as 110°C. The integrity of two model drugs was maintained following HME and FDM 3D printing. XRPD indicated that a portion of the loaded theophylline remained crystalline in the tablet. The fabricated tablets demonstrated excellent mechanical properties, acceptable in-batch variability and an immediate in vitro release pattern. Combining the advantages of PVP as an impeding polymer with FDM 3D printing at low temperatures, this approach holds a potential in expanding the spectrum of drugs that could be used in FDM 3D printing for on demand manufacturing of individualised dosage forms.

Enhanced oral bioavailability of felodipine by novel solid self-microemulsifying tablets.

PubMed

Jing, Boyu; Wang, Zhiyuan; Yang, Rui; Zheng, Xia; Zhao, Jia; Tang, Si; He, Zhonggui

2016-01-01

The novel self-microemulsifying (SME) tablets were developed to enhance the oral bioavailability of a poor water-soluble drug felodipine (FDP). Firstly, FDP was dissolved in the optimized liquid self-microemusifying drug delivery systems (SMEDDS) containing Miglyol® 812, Cremophor® RH 40, Tween 80 and Transcutol® P, and the mixture was solidified with porous silicon dioxide and crospovidone as adsorbents. Then after combining the solidified powders with other excipients, the solid SME tablets were prepared by wet granulation-compression method. The prepared tablets possessed satisfactory characterization; the droplet size of the SME tablets following self-emulsification in water was nearly equivalent to the liquid SMEDDS (68.4 ± 14.0 and 64.4 ± 12.0 nm); differential scanning calorimetry (DSC) and powder X-ray diffractometry (PXRD) analysis demonstrated that FDP in SME tablets had undergone a polymorphism transition from a crystal form to an amorphous state, which was further confirmed by transmission electron microscopy (TEM). A similar dissolution performance of SME tablets and liquid SMEDDS was also obtained under the sink condition (85% within 10 min), both significantly higher than commercial tablets. The oral bioavailability was evaluated for the SME tablets, liquid SMEDDS and commercial conventional tablets in the fasted beagle dogs. The AUC of FDP from the SME tablets was about 2-fold greater than that of conventional tablets, but no significant difference was found when compared with the liquid SMEDDS. Accordingly, these preliminary results suggest that this formulation approach offers a useful large-scale producing method to prepare the solid SME tablets from the liquid SMEDDS for oral bioavailability equivalent enhancement of poorly soluble FDP.

Kaolinite, illite and quartz dissolution in the karstification of Paleozoic sandstones of the Furnas Formation, Paraná Basin, Southern Brazil

NASA Astrophysics Data System (ADS)

Melo, Mário Sérgio de; Guimarães, Gilson Burigo; Chinelatto, Adilson Luiz; Giannini, Paulo César Fonseca; Pontes, Henrique Simão; Chinelatto, Adriana Scoton Antonio; Atencio, Daniel

2015-11-01

Karstification processes in sandstones of the Furnas Formation, Silurian to Devonian of the Paraná Basin, have been described since the mid-twentieth century. However, some geologists still doubt the idea of true karst in sandstones. Studies carried out in the Campos Gerais region, Paraná State, Southern Brazil, aimed at investigating the nature of erosion processes in Furnas Formation and the role of the dissolution in the development of their notorious erosive features and underground cavities. These studies have led to the recognition of dissolution macro to micro features ('furnas', caves, ponds, sinks, ruiniform relief on cliffs and rocky surfaces, grain corrosion, speleothems, mineral reprecipitation and incrustation). The analysis (scanning electron microscopy, energy dispersive spectrometry and x-ray diffractometry) of sandstones and their alterites has indicated significant dissolution of clay cement along with discrete quartz grain dissolution. This mesodiagenetic cement (kaolinite and illite) is dissolved and reprecipitated as clay minerals with poorly developed crystallinity along with other minerals, such as variscite and minerals of the alunite supergroup, suggesting organic participation in the processes of dissolution and incrustation. The mineral reprecipitation usually forms centimetric speleothems, found in cavities and sheltered rocky surfaces. The cement dissolution associated with other factors (fractures, wet weather, strong hydraulic gradient, antiquity of the landforms) leads to the rock arenisation, the underground erosion and the appearance of the karst features. Carbonate rocks in the basement may locally be increasing the karst forms in the overlying Furnas Formation. The recognition of the karst character of the Furnas Formation sandstones has important implications in the management of underground water resources (increasingly exploited in the region), in the use of the unique geological heritage and in the prevention of geo-environmental accidents resulting from underground erosion phenomena.

Upgrading pyrolytic residue from waste tires to commercial carbon black.

PubMed

Zhang, Xue; Li, Hengxiang; Cao, Qing; Jin, Li'e; Wang, Fumeng

2018-05-01

The managing and recycling of waste tires has become a worldwide environmental challenge. Among the different disposal methods for waste tires, pyrolysis is regarded as a promising route. How to effectively enhance the added value of pyrolytic residue (PR) from waste tires is a matter of great concern. In this study, the PRs were treated with hydrochloric and hydrofluoric acids in turn under ultrasonic waves. The removal efficiency for the ash and sulfur was investigated. The pyrolytic carbon black (PCB) obtained after treating PR with acids was analyzed by X-ray fluorescence spectrophotometry, Fourier transform infrared spectrometry, X-ray diffractometry, laser Raman spectrometry, scanning electron microscopy, thermogravimetric (TG) analysis, and physisorption apparatus. The properties of PCB were compared with those of commercial carbon black (CCB) N326 and N339. Results showed PRs from waste tires were mainly composed of carbon, sulfur, and ash. The carbon in PCB was mainly from the CCB added during tire manufacture rather than from the pyrolysis of pure rubbers. The removal percentages for the ash and sulfur of PR are 98.33% (from 13.98 wt % down to 0.24 wt %) and 70.16% (from 1.81 wt % down to 0.54 wt %), respectively, in the entire process. The ash was mainly composed of metal oxides, sulfides, and silica. The surface properties, porosity, and morphology of the PCB were all close to those of N326. Therefore, PCB will be a potential alternative of N326 and reused in tire manufacture. This route successfully upgrades PR from waste tires to the high value-added CCB and greatly increases the overall efficiency of the waste tire pyrolysis industry.

Toxicological aspects of photocatalytic degradation of selected xenobiotics with nano-sized Mn-doped TiO2.

PubMed

Ozmen, Murat; Güngördü, Abbas; Erdemoglu, Sema; Ozmen, Nesrin; Asilturk, Meltem

2015-08-01

The toxic effects of two selected xenobiotics, bisphenol A (BPA) and atrazine (ATZ), were evaluated after photocatalytic degradation using nano-sized, Mn-doped TiO2. Undoped and Mn-doped TiO2 nanoparticles were synthesized. The samples were characterized by X-ray diffractometry (XRD), scanning electron microscopy (SEM), UV-vis-diffuse reflectance spectra (DRS), X-ray fluorescence spectroscopy (XRF), and BET surface area. The photocatalytic efficiency of the undoped and Mn-doped TiO2 was evaluated for BPA and ATZ. The toxicity of the synthesized photocatalysts and photocatalytic by-products of BPA and ATZ was determined using frog embryos and tadpoles, zebrafish embryos, and bioluminescent bacteria. Possible toxic effects were also evaluated using selected enzyme biomarkers. The results showed that Mn-doped TiO2 nanoparticles did not cause significant lethality in Xenopus laevis embryos and tadpoles, but nonfiltered samples caused lethality in zebrafish. Furthermore, Mn-doping of TiO2 increased the photocatalytic degradation capability of nanoparticles, and it successfully degraded BPA and AZT, but degradation of AZT caused an increase of the lethal effects on both tadpoles and fish embryos. Degradation of BPA caused a significant reduction of lethal effects, especially after 2-4h of degradation. However, biochemical assays showed that both Mn-doped TiO2 and the degradation by-products caused a significant change of selected biomarkers on X. laevis tadpoles; thus, the ecological risks of Mn-doped TiO2 should be considered due to nanomaterial applications and for spilled nanoparticles in an aquatic ecosystem. Also, the risk of nanoparticles should be considered using indicator reference biochemical markers to verify the environmental health impacts. Copyright © 2015 Elsevier B.V. All rights reserved.

Anisotropic magnetic properties of the KMo4O6

NASA Astrophysics Data System (ADS)

Andrade, M.; Maffei, M. L.; Dos Santos, C. A. M.; Ferreira, B.; Sartori, A. F.

2012-02-01

Electrical resistivity measurements in the tetragonal KMo4O6 single crystals show a metal-insulator transition (MIT) near 100K. Magnetization measurements as a function of temperature show no evidence of magnetic ordering at this MIT [1]. Single crystals of KMo4O6 were obtained by electrolysis of a melt with a molar ratio of K2MoO4:MoO3 = 6:1. The process were carried out at 930 C with a current of 20-25mA for 52h in argon atmosphere. After that, electrodes were removed from the melt alloying the crystals to cool down to room temperature rapidly. Scanning Electron Microscopy (SEM) showed that the black single crystals were grown on the platinum cathode. Typical dimensions of the single crystals are 1x0.2x0.2mm^3. X-ray diffractometry confirmed that the single crystals have KMo4O6 tetragonal crystalline structure with space group P4. Magnetization measurements were performed parallel and perpendicular to the c-axis from 2 to 300K. The results show anisotropic behavior between both directions. Furthermore, the temperature independence of the magnetization at high temperature and the upturn at low temperature are observed in agreement with previous results [1]. MxH curves measured at several temperatures show nonlinear behavior and a small magnetic ordering. The magnetic ordering seems to be related to the MIT near 100K. This material is based upon support by FAPESP (2009/14524-6 and 2009/54001-6) and CNPq/NSF (490182/2009-7). M. Andrade is CAPES fellow and C.A.M. dos Santos is CNPq fellow. [4pt] [1] K. V. Ramanujachary et al., J. Sol. State Chem.102 (1993) 69.

Microwave combustion synthesis of Co1-xZnxFe2O4 (0⩽x⩽0.5): Structural, magnetic, optical and vibrational spectroscopic studies.

PubMed

Sundararajan, M; Kennedy, L John; Vijaya, J Judith; Aruldoss, Udaya

2015-04-05

Nanostructured pure and zinc doped cobalt ferrites (Co1-xZnxFe2O4 where x fraction ranging from 0 to 0.5) were prepared by microwave combustion method employing urea as a fuel. The nanostructured samples were characterized by using various instrumental techniques such as X-ray powder diffractometry, high resolution scanning electron microscopy, energy dispersive X-ray analysis, UV-visible diffuse reflectance spectroscopy, photoluminescence spectroscopy and Fourier transformed infrared (FT-IR) spectroscopy. Vibrating sample magnetometry at room temperature was recorded to study the magnetic behavior of the samples. X-ray analysis and the FT-IR spectroscopy revealed the formation of cobalt ferrite cubic spinel-type structure. The average crystallite sizes for the samples were in the range of 3.07-11.30 nm. The direct band gap (Eg) was estimated using Kubelka-Munk method and is obtained from the UV-vis spectra. The band gap value decreased with an increase in zinc fraction (2.56-2.17 eV). The violet and green emission observed in the photoluminescence spectra revealed that cobalt ferrites are governed by defect controlled processes. The elemental analysis of zinc doped cobalt ferrites were obtained from energy dispersive X-ray (EDX) analysis. From the magnetic measurements, it is observed that cobalt ferrite and zinc doped cobalt ferrite systems fall under the soft ferrite category. The saturation magnetization (Ms) value of undoped cobalt ferrite is 14.26 emu/g, and it has reached a maximum of 29.61 emu/g for Co0.7Zn0.3Fe2O4. Copyright © 2014 Elsevier B.V. All rights reserved.

Use of nanoindentation technique for a better understanding of the fracture toughness of Strombus gigas conch shell

DOE Office of Scientific and Technical Information (OSTI.GOV)

Romana, L., E-mail: laurence.romana@univ-ag.fr; Thomas, P.; Bilas, P.

2013-02-15

In this work the nanochemical properties of the composite organomineral biomaterial constituting Strombus gigas conch shell are studied by means of dynamic mechanical analyses associated to nanoidentation technique. The measurements are performed on shell samples presenting different surface orientations relative to the growth axis of the conch shell. The influence of the organic component of the biomaterial on its nanomechanical properties is also investigated by studying fresh and dried S. gigas conch shells. Monocrystalline aragonite is used as a reference. For the understanding of nanochemical behaviour, special attention is paid to the pop in events observed on the load/displacement curvesmore » which results from nanofractures' initiation and propagation occuring during the load process. In order to better understand the mechanical properties systematic studies of the structure and morphology are performed using scanning electron microscopy, atomic force microscopy and X-ray diffractometry. The hardness and Young's modulus values measured on bio aragonite samples are close to those of the aragonite mineral standard. This surprising result shows that, H and E values are not related to the bio composition and lamellar structure of the bio aragonite. However, it was found that the organic layer and the micro architecture strongly influence the nanofracture initiation and propagation processes in the samples. Statistic study of the pop-in events can help to predict the macroscopic mechanical behaviour of the material. - Highlights: ► Nanomechanical properties of Strombus gigas conch shell ► Low influence of the crossed lamellar structure on H and E values at the nano scale ► Strong influence of the crossed lamellar on nanocracks initiation ► Correlation between mechanical behaviors at the macro and nano scales.« less

Valve microstructure and phylomineralogy of New Zealand chitons.

PubMed

Peebles, B A; Smith, A M; Spencer, H G

2017-03-01

The microstructure and mineralogy of chiton valves has been largely ignored in the literature and only described in 29 species to date. Eight species: Acanthochitona zelandica, Notoplax violacea (Family Acanthochitonidae, Suborder Acanthochitonina, Order Chitonida), Chiton glaucus, Onithochiton neglectus, Sypharochiton spelliserpentis, Sypharochiton sinclairi (Family Chitonidae, Suborder, Chitonina, Order Chitonida), Ischnochiton maorianus (Family Ischnochitonidae, Suborder Chitonina, Order Chitonida), and Leptochiton inquinatus (Family Leptochitonidae, Suborder Lepidopleurina, Order Lepidopleurida) were collected from the Otago Peninsula, South Island, New Zealand. The valves of these chitons were analysed with X-ray diffractometry, Raman spectrometry, and Scanning Electron Micrography (SEM) to determine their mineralogy and microstructure. Both the XRD and Raman data show that the valves consisted solely of aragonite. The observed microstructures of the valves were complex, typically composed of four to seven sublayers, and varied among species. The dorsal layer, the tegmentum, of each species was granular and the ventral layer, the articulamentum, was predominately composed of a spherulitic sublayer, a crossed lamellar sublayer, and an acicular sublayer. The chitonids Sypharochiton pelliserpentis and S. sinclairi had the most complex microstructure layering with three crossed lamellar, two spherulitic sublayers, and a ventral acicular sublayer while the acanthochitonids Acanthochitona zelandica and Notoplax violacea as well as the ischnochitonid Ischnochiton maorianus had the simplest structure with one spherulitic, one crossed lamellar sublayer, and a ventral acicular sublayer. Terminal valves were less complex than intermediate valves and tended to be dominated by the crossed lamellar structure. The leptochitonid Leptochiton inquinatus generated a unique crossed lamellar sublayer different from the other analysed chitonids. Acanthochitona zelandica is the only analysed chitonid that utilizes two different crossed lamellar structures. Clearly, many of these properties do not reflect the currently recognized polyplacophoran phylogeny. Copyright © 2016 Elsevier Inc. All rights reserved.

Comparative study of DNA encapsulation into PLGA microparticles using modified double emulsion methods and spray drying techniques.

PubMed

Oster, C G; Kissel, T

2005-05-01

Recently, several research groups have shown the potential of microencapsulated DNA as adjuvant for DNA immunization and in tissue engineering approaches. Among techniques generally used for microencapsulation of hydrophilic drug substances into hydrophobic polymers, modified WOW double emulsion method and spray drying of water-in-oil dispersions take a prominent position. The key parameters for optimized microspheres are particle size, encapsulation efficiency, continuous DNA release and stabilization of DNA against enzymatic and mechanical degradation. This study investigates the possibility to encapsulate DNA avoiding shear forces which readily degrade DNA during this microencapsulation. DNA microparticles were prepared with polyethylenimine (PEI) as a complexation agent for DNA. Polycations are capable of stabilizing DNA against enzymatic, as well as mechanical degradation. Further, complexation was hypothesized to facilitate the encapsulation by reducing the size of the macromolecule. This study additionally evaluated the possibility of encapsulating lyophilized DNA and lyophilized DNA/PEI complexes. For this purpose, the spray drying and double emulsion techniques were compared. The size of the microparticles was characterized by laser diffractometry and the particles were visualized by scanning electron microscopy (SEM). DNA encapsulation efficiencies were investigated photometrically after complete hydrolysis of the particles. Finally, the DNA release characteristics from the particles were studied. Particles with a size of <10 microm which represent the threshold for phagocytic uptake could be prepared with these techniques. The encapsulation efficiency ranged from 100-35% for low theoretical DNA loadings. DNA complexation with PEI 25?kDa prior to the encapsulation process reduced the initial burst release of DNA for all techniques used. Spray-dried particles without PEI exhibited high burst releases, whereas double emulsion techniques showed continuous release rates.

Fabrication of nano-structured HA/CNT coatings on Ti6Al4V by electrophoretic deposition for biomedical applications.

PubMed

Zhang, Bokai; Kwok, Chi Tat; Cheng, Fai Tsun; Man, Hau Chung

2011-12-01

In order to improve the bone bioactivity and osteointegration of metallic implants, hydroxyapatite (HA) is often coated on their surface so that a real bond with the surrounding bone tissue can be formed. In the present study, cathodic electrophoretic deposition (EPD) has been attempted for depositing nanostructured HA coatings on titanium alloy Ti6Al4V followed by sintering at 800 degrees C. Nano-sized HA powder was used in the EPD process to produce dense coatings. Moreover, multiwalled carbon nanotubes (CNTs) were also used to reinforce the HA coating for enhancing its mechanical strength. The surface morphology, compositions and microstructure of the monolithic coating of HA and nanocomposite coatings of HA with different CNT contents (4 to 25%) on Ti6Al4V were investigated by scanning-electron microscopy, energy-dispersive X-ray spectroscopy and Xray diffractometry, respectively. Electrochemical corrosion behavior of the various coatings in Hanks' solution at 37 degrees C was investigated by means of open-circuit potential measurement and cyclic potentiodynamic polarization tests. Surface hardness, adhesion strength and bone bioactivity of the coatings were also studied. The HA and HA/CNT coatings had a thickness of about 10 microm, with corrosion resistance higher than that of the substrate and adhesion strength higher than that of plasma sprayed HA coating. The properties of the composite coatings were optimized by varying the CNT contents. The enhanced properties could be attributed to the use of nano-sized HA particles and CNTs. Compared with the monolithic HA coating, the CNT-reinforced HA coating markedly increased the coating hardness without deteriorating the corrosion resistance or adhesion strength.

Mineralogical characteristics of Cretaceous-Tertiary kaolins of the Douala Sub-Basin, Cameroon

NASA Astrophysics Data System (ADS)

Bukalo, Nenita N.; Ekosse, Georges-Ivo E.; Odiyo, John O.; Ogola, Jason S.

2018-05-01

As a step in evaluating the quality of Cretaceous-Tertiary kaolins of the Douala Sub-Basin, their mineralogical characteristics were determined. The X-ray diffractometry technique was used to identify and quantify the mineral phases present in bulk and <2 μm fractions. Scanning electron microscopy was used to determine the micromorphology of <2 μm fractions kaolins. Thermal analyses (derivative thermal gravimetric analysis, thermal gravimetric analysis, and heat flow) were conducted to further characterise the kaolins. The main mineral phases present in the studied Cretaceous-Tertiary kaolins of the Douala Sub-Basin were kaolinite > smectite > illite, with mean values of 33.01 > 11.20 > 4.41 wt %; and 72.23 > 10.69 > 4.69 wt %, in bulk and <2 μm fractions, respectively. The kaolins, micromorphologically, consisted of pseudo-hexagonal and thin platy particles; swirl-textured particles; and books or stacks of kaolinite particles. Three main reactions occurred during heating of the kaolins: a low temperature endothermic reaction, observed between 48 and 109 °C; a second low temperature peak, observed between 223 and 285 °C; and a third endothermic peak was found between 469 and 531 °C. In addition, an exothermic reaction also occurred between 943 and 988 °C in some of the samples. The absence of primary minerals such as feldspars and micas in most of these kaolins is an indication of intensive weathering, probably due to the humid tropical climate of the region. The different morphologies suggested that these kaolins might have been transported. Therefore, a humid tropical climate was responsible for the formation of Cretaceous-Tertiary kaolins of the Douala Sub-Basin through intense weathering of surrounding volcanic and metamorphic rocks.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Moraes, Paulo E.L., E-mail: pauloeduardo.leitedemoraes@gmail.com; Contieri, Rodrigo J., E-mail: contieri@fem.unicamp.br; Lopes, Eder S.N., E-mail: ederlopes@fem.unicamp.br

Ti and Ti alloys are widely used in restorative surgery because of their good biocompatibility, enhanced mechanical behavior and high corrosion resistance in physiological media. The corrosion resistance of Ti-based materials is due to the spontaneous formation of the TiO{sub 2} oxide film on their surface, which exhibits elevated stability in biological fluids. Ti–Nb alloys, depending on the composition and the processing routes to which the alloys are subjected, have high mechanical strength combined with low elastic modulus. The addition of Sn to Ti–Nb alloys allows the phase transformations to be controlled, particularly the precipitation of ω phase. The aimmore » of this study is to discuss the microstructure, mechanical properties and corrosion behavior of cast Ti–Nb alloys to which Sn has been added. Samples were centrifugally cast in a copper mold, and the microstructure was characterized using optical microscopy, scanning electron microscopy and X-ray diffractometry. Mechanical behavior evaluation was performed using Berkovich nanoindentation, Vickers hardness and compression tests. The corrosion behavior was evaluated in Ringer's solution at room temperature using electrochemical techniques. The results obtained suggested that the physical, mechanical and chemical behaviors of the Ti–Nb–Sn alloys are directly dependent on the Sn content. - Graphical abstract: Effects of Sn addition to the Ti–30Nb alloy on the elastic modulus. - Highlights: • Sn addition causes reduction of the ω phase precipitation. • Minimum Vickers hardness and elastic modulus occurred for 6 wt.% Sn content. • Addition of 6 wt.% Sn resulted in maximum ductility and minimum compression strength. • All Ti–30Nb–XSn (X = 0, 2, 4, 6, 8 and 10%) alloys are passive in Ringer's solution. • Highest corrosion resistance was observed for 6 wt.% Sn content.« less

An electron beam linear scanning mode for industrial limited-angle nano-computed tomography.

PubMed

Wang, Chengxiang; Zeng, Li; Yu, Wei; Zhang, Lingli; Guo, Yumeng; Gong, Changcheng

2018-01-01

Nano-computed tomography (nano-CT), which utilizes X-rays to research the inner structure of some small objects and has been widely utilized in biomedical research, electronic technology, geology, material sciences, etc., is a high spatial resolution and non-destructive research technique. A traditional nano-CT scanning model with a very high mechanical precision and stability of object manipulator, which is difficult to reach when the scanned object is continuously rotated, is required for high resolution imaging. To reduce the scanning time and attain a stable and high resolution imaging in industrial non-destructive testing, we study an electron beam linear scanning mode of nano-CT system that can avoid mechanical vibration and object movement caused by the continuously rotated object. Furthermore, to further save the scanning time and study how small the scanning range could be considered with acceptable spatial resolution, an alternating iterative algorithm based on ℓ 0 minimization is utilized to limited-angle nano-CT reconstruction problem with the electron beam linear scanning mode. The experimental results confirm the feasibility of the electron beam linear scanning mode of nano-CT system.

An electron beam linear scanning mode for industrial limited-angle nano-computed tomography

NASA Astrophysics Data System (ADS)

Wang, Chengxiang; Zeng, Li; Yu, Wei; Zhang, Lingli; Guo, Yumeng; Gong, Changcheng

2018-01-01

Nano-computed tomography (nano-CT), which utilizes X-rays to research the inner structure of some small objects and has been widely utilized in biomedical research, electronic technology, geology, material sciences, etc., is a high spatial resolution and non-destructive research technique. A traditional nano-CT scanning model with a very high mechanical precision and stability of object manipulator, which is difficult to reach when the scanned object is continuously rotated, is required for high resolution imaging. To reduce the scanning time and attain a stable and high resolution imaging in industrial non-destructive testing, we study an electron beam linear scanning mode of nano-CT system that can avoid mechanical vibration and object movement caused by the continuously rotated object. Furthermore, to further save the scanning time and study how small the scanning range could be considered with acceptable spatial resolution, an alternating iterative algorithm based on ℓ0 minimization is utilized to limited-angle nano-CT reconstruction problem with the electron beam linear scanning mode. The experimental results confirm the feasibility of the electron beam linear scanning mode of nano-CT system.

Imaging of endodontic biofilms by combined microscopy (FISH/cLSM - SEM).

PubMed

Schaudinn, C; Carr, G; Gorur, A; Jaramillo, D; Costerton, J W; Webster, P

2009-08-01

Scanning electron microscopy is a useful imaging approach for the visualization of bacterial biofilms in their natural environments including their medical and dental habitats, because it allows for the exploration of large surfaces with excellent resolution of topographic features. Most biofilms in nature, however, are embedded in a thick layer of extracellular matrix that prevents a clear identification of individual bacteria by scanning electron microscopy. The use of confocal laser scanning microscopy on the other hand in combination with fluorescence in situ hybridization enables the visualization of matrix embedded bacteria in multi-layered biofilms. In our study, fluorescence in situ hybridization/confocal laser scanning microscopy and scanning electron microscopy were applied to visualize bacterial biofilm in endodontic root canals. The resulting fluorescence in situ hybridization /confocal laser scanning microscopy and scanning electron microscopy and pictures were subsequently combined into one single image to provide high-resolution information on the location of hidden bacteria. The combined use of scanning electron microscopy and fluorescence in situ hybridization / confocal laser scanning microscopy has the potential to overcome the limits of each single technique.

Synthesis and characterization of polyethylenimine-based iron oxide composites as novel contrast agents for MRI.

PubMed

Masotti, A; Pitta, A; Ortaggi, G; Corti, M; Innocenti, C; Lascialfari, A; Marinone, M; Marzola, P; Daducci, A; Sbarbati, A; Micotti, E; Orsini, F; Poletti, G; Sangregorio, C

2009-04-01

Use of polyethylenimines (PEIs) of different molecular weight and selected carboxylated-PEI derivatives (PEI-COOH) in the synthesis and stabilization of iron oxide nanoparticles, to obtain possible multifunctional contrast agents. Oxidation of Fe(II) at slightly elevated pH and temperature resulted in the formation of highly soluble and stable nanocomposites of iron oxides and polymer. Composites were characterized and studied by atomic force microscopy (AFM), transmission electron microscopy (TEM), X-ray diffractometry, AC and DC magnetometry, NMR relaxometry and magnetic resonance imaging (MRI). From AFM the dimensions of the aggregates were found to be in the ~150-250 nm size region; the mean diameter of the magnetic core of the compounds named PEI-25, PEI-500 and PEI-COOH60 resulted d approximately 20 +/- 5 nm for PEI-25, d approximately 9.5 +/- 1.0 nm for PEI-500 and d approximately 6.8 +/- 1.0 nm for PEI-COOH60. In PEI-COOH60 TEM and X-ray diffractometry revealed small assemblies of mineral magnetic cores with clear indications that the main constituents are maghemite and/or magnetite as confirmed by AC and DC SQUID magnetometry. For PEI-COOH60, the study of NMR-dispersion profiles revealed r (1) and r (2) relaxivities comparable to superparamagnetic iron-oxide commercial compounds in the whole investigated frequency range 7 < or = nu < or = 212 MHz. PEI-25 was studied as possible MRI contrast agent (CA) to map the cerebral blood volume (CBV) and cerebral blood flow (CBF) in an animal model obtaining promising results. The reported compounds may be further functionalized to afford novel multifunctional systems for biomedical applications.

Sparse sampling and reconstruction for electron and scanning probe microscope imaging

DOEpatents

Anderson, Hyrum; Helms, Jovana; Wheeler, Jason W.; Larson, Kurt W.; Rohrer, Brandon R.

2015-07-28

Systems and methods for conducting electron or scanning probe microscopy are provided herein. In a general embodiment, the systems and methods for conducting electron or scanning probe microscopy with an undersampled data set include: driving an electron beam or probe to scan across a sample and visit a subset of pixel locations of the sample that are randomly or pseudo-randomly designated; determining actual pixel locations on the sample that are visited by the electron beam or probe; and processing data collected by detectors from the visits of the electron beam or probe at the actual pixel locations and recovering a reconstructed image of the sample.

Scanning ultrafast electron microscopy.

PubMed

Yang, Ding-Shyue; Mohammed, Omar F; Zewail, Ahmed H

2010-08-24

Progress has been made in the development of four-dimensional ultrafast electron microscopy, which enables space-time imaging of structural dynamics in the condensed phase. In ultrafast electron microscopy, the electrons are accelerated, typically to 200 keV, and the microscope operates in the transmission mode. Here, we report the development of scanning ultrafast electron microscopy using a field-emission-source configuration. Scanning of pulses is made in the single-electron mode, for which the pulse contains at most one or a few electrons, thus achieving imaging without the space-charge effect between electrons, and still in ten(s) of seconds. For imaging, the secondary electrons from surface structures are detected, as demonstrated here for material surfaces and biological specimens. By recording backscattered electrons, diffraction patterns from single crystals were also obtained. Scanning pulsed-electron microscopy with the acquired spatiotemporal resolutions, and its efficient heat-dissipation feature, is now poised to provide in situ 4D imaging and with environmental capability.

Atom Optics for Bose-Einstein Condensates (BEC)

DTIC Science & Technology

2012-04-25

Electron Micrograph of the Top View of Test Chip A .......................................29 11. A Scanning Electron Micrograph of the Cross...Sectional View of Test Chip A .....................29 12. A Scanning Electron Micrograph of the Top View of Test Chip B...30 13. A Scanning Electron Micrograph of the Cross Sectional View of Test Chip B .....................30 14. Toner Masks for Etching

Synthesis of Copper-Antimony-Sulfide Nanocrystals for Solution-Processed Solar Cells.

PubMed

Suehiro, Satoshi; Horita, Keisuke; Yuasa, Masayoshi; Tanaka, Tooru; Fujita, Katsuhiko; Ishiwata, Yoichi; Shimanoe, Kengo; Kida, Tetsuya

2015-08-17

The p-type nanocrystals (NCs) of copper-based chalcogenides, such as CuInSe2 and Cu2ZnSnS4, have attracted increasing attention in photovoltaic applications due to their potential to produce cheap solution-processed solar cells. Herein, we report the synthesis of copper-antimony-sulfide (CAS) NCs with different crystal phases including CuSbS2, Cu3SbS4, and Cu12Sb4S13. In addition, their morphology, crystal phase, and optical properties were characterized using transmission electron microscopy, X-ray diffractometry, UV-vis-near-IR spectroscopy, and photoemission yield spectroscopy. The morphology, crystal phase, and electronic structure were significantly dependent on the chemical composition in the CAS system. Devices were fabricated using particulate films consisting of CAS NCs prepared by spin coating without a high-temperature treatment. The CAS NC-based devices exhibited a diode-like current-voltage characteristic when coupled with an n-type CdS layer. In particular, the CuSbS2 NC devices exhibited photovoltaic responses under simulated sunlight, demonstrating its applicability for use in solution-processed solar cells.

Reduced graphene oxide-CdS nanocomposite with enhanced photocatalytic 4-Nitrophenol degradation

NASA Astrophysics Data System (ADS)

Chakraborty, Koushik; Ibrahim, Sk; Das, Poulomi; Ghosh, Surajit; Pal, Tanusri

2017-05-01

We report the photocatalytic activity of reduced graphene oxide cadmium sulfide (RGO-CdS) composite towards the degradation of 4-Nitrophenol (4-NP) under simulated solar light illumination. The solution processable RGO-CdS composite was synthesized by one pot single step low cost solvothermal process, where the reduction of graphene oxide (GO), synthesis and attachment of CdS onto RGO sheets were done simultaneously. The structural and morphological characterization of the RGO-CdS composite and the reduction of GO was confirmed by X-ray diffractometry, TEM imaging and Fourier transform infrared spectroscopy respectively. The photocatalytic efficiency of RGO-CdS composite is 2.6 times higher in compare to controlled CdS. In RGO-CdS composite the photo induced electrons transfer from CdS nanorod to RGO sheets, which reduces the recombination probability of photo generated electron-hole in the CdS. These well separated photoinduced charges enhanced the photocatalytic activity of the RGO-CdS composite. Our study establishes the RGO-CdS composite as a potential photocatalyst for the degradation of organic water pollutant.

Investigations on nucleation, HRXRD, optical, piezoelectric, polarizability and Z-scan analysis of L-arginine maleate dihydrate single crystals

NASA Astrophysics Data System (ADS)

Sakthy Priya, S.; Alexandar, A.; Surendran, P.; Lakshmanan, A.; Rameshkumar, P.; Sagayaraj, P.

2017-04-01

An efficient organic nonlinear optical single crystal of L-arginine maleate dihydrate (LAMD) has been grown by slow evaporation solution technique (SEST) and slow cooling technique (SCT). The crystalline perfection of the crystal was examined using high-resolution X-ray diffractometry (HRXRD) analysis. Photoluminescence study confirmed the optical properties and defects level in the crystal lattice. Electromechanical behaviour was observed using piezoelectric co-efficient (d33) analysis. The photoconductivity analysis confirmed the negative photoconducting nature of the material. The dielectric constant and loss were measured as a function of frequency with varying temperature and vice-versa. The laser damage threshold (LDT) measurement was carried out using Nd:YAG Laser with a wavelength of 1064 nm (Focal length is 35 cm) and the obtained results showed that LDT value of the crystal is high compared to KDP crystal. The high laser damage threshold of the grown crystal makes it a potential candidate for second and higher order nonlinear optical device application. The third order nonlinear optical parameters of LAMD crystal is determined by open-aperture and closed-aperture studies using Z-scan technique. The third order linear and nonlinear optical parameters such as the nonlinear refractive index (n2), two photon absorption coefficient (β), Real part (Reχ3) and imaginary part (Imχ3) of third-order nonlinear optical susceptibility are calculated.

Analysis of NiAlTa precipitates in beta-NiAl + 2 at. pct Ta alloy

NASA Technical Reports Server (NTRS)

Pathare, V.; Michal, G. M.; Vedula, K.; Nathal, M. V.

1987-01-01

Results are reported from experiments performed to identify the precipitates, and their orientation in the matrix, in a beta-NiAl alloy containing 2 at. pct. Ta after undergoing creep test at 1300 K. Test specimens formed by extruding hot powders were compressed at 1300 K for about 50 hr at a strain rate averaging 6/1 million per sec. The specimens were then thinned and examined under an electron microscope and by X-ray diffractometry. An intermetallic NiAlTa compound with a hexagonal Cl4 structure appeared as second phase precipitates in the samples, exhibiting plate-like shapes and a habit plane close to (012). The prism planes of the hexagonal NiAlTa precipitates paralleled the closest packed planes in the cubic beta-NiAl matrix.

Laser formation of titanium nitride films as a result of Ti coating modification in a nitrogen atmosphere

NASA Astrophysics Data System (ADS)

Eskin, Sergei

1998-12-01

Laser treatment of the 303 and 416 stainless steels with Ti precoating was studied. CW CO2 and UV ArF excimer lasers were used. The TiN films were formed at a treatment velocity of 0.5 to 3 - 5 cm/sec and a power density of CO2 laser at (3 - 5) 104 W/cm2. X-ray diffractometry, x-ray mapping and Auger electron spectroscopy techniques indicated a TiN phase on the surface with oxygen content 12 - 25 at%. The thickness of the TiN film was 0.3 - 0.4 micrometers after treatment of the 5 micrometers Ti coating and about 900 angstroms for the 0.3 micrometers coating. Some characteristics of TiN films were examined and features of the nitriding process are discussed.

Method and apparatus for a high-resolution three dimensional confocal scanning transmission electron microscope

DOEpatents

de Jonge, Niels [Oak Ridge, TN

2010-08-17

A confocal scanning transmission electron microscope which includes an electron illumination device providing an incident electron beam propagating in a direction defining a propagation axis, and a precision specimen scanning stage positioned along the propagation axis and movable in at least one direction transverse to the propagation axis. The precision specimen scanning stage is configured for positioning a specimen relative to the incident electron beam. A projector lens receives a transmitted electron beam transmitted through at least part of the specimen and focuses this transmitted beam onto an image plane, where the transmitted beam results from the specimen being illuminated by the incident electron beam. A detection system is placed approximately in the image plane.

Atmospheric scanning electron microscope observes cells and tissues in open medium through silicon nitride film.

PubMed

Nishiyama, Hidetoshi; Suga, Mitsuo; Ogura, Toshihiko; Maruyama, Yuusuke; Koizumi, Mitsuru; Mio, Kazuhiro; Kitamura, Shinichi; Sato, Chikara

2010-03-01

Direct observation of subcellular structures and their characterization is essential for understanding their physiological functions. To observe them in open environment, we have developed an inverted scanning electron microscope with a detachable, open-culture dish, capable of 8 nm resolution, and combined with a fluorescence microscope quasi-simultaneously observing the same area from the top. For scanning electron microscopy from the bottom, a silicon nitride film window in the base of the dish maintains a vacuum between electron gun and open sample dish while allowing electrons to pass through. Electrons are backscattered from the sample and captured by a detector under the dish. Cells cultured on the open dish can be externally manipulated under optical microscopy, fixed, and observed using scanning electron microscopy. Once fine structures have been revealed by scanning electron microscopy, their component proteins may be identified by comparison with separately prepared fluorescence-labeled optical microscopic images of the candidate proteins, with their heavy-metal-labeled or stained ASEM images. Furthermore, cell nuclei in a tissue block stained with platinum-blue were successfully observed without thin-sectioning, which suggests the applicability of this inverted scanning electron microscope to cancer diagnosis. This microscope visualizes mesoscopic-scale structures, and is also applicable to non-bioscience fields including polymer chemistry. (c) 2010 Elsevier Inc. All rights reserved.

Electronic noise in CT detectors: Impact on image noise and artifacts.

PubMed

Duan, Xinhui; Wang, Jia; Leng, Shuai; Schmidt, Bernhard; Allmendinger, Thomas; Grant, Katharine; Flohr, Thomas; McCollough, Cynthia H

2013-10-01

The objective of our study was to evaluate in phantoms the differences in CT image noise and artifact level between two types of commercial CT detectors: one with distributed electronics (conventional) and one with integrated electronics intended to decrease system electronic noise. Cylindric water phantoms of 20, 30, and 40 cm in diameter were scanned using two CT scanners, one equipped with integrated detector electronics and one with distributed detector electronics. All other scanning parameters were identical. Scans were acquired at four tube potentials and 10 tube currents. Semianthropomorphic phantoms were scanned to mimic the shoulder and abdominal regions. Images of two patients were also selected to show the clinical values of the integrated detector. Reduction of image noise with the integrated detector depended on phantom size, tube potential, and tube current. Scans that had low detected signal had the greatest reductions in noise, up to 40% for a 30-cm phantom scanned using 80 kV. This noise reduction translated into up to 50% in dose reduction to achieve equivalent image noise. Streak artifacts through regions of high attenuation were reduced by up to 45% on scans obtained using the integrated detector. Patient images also showed superior image quality for the integrated detector. For the same applied radiation level, the use of integrated electronics in a CT detector showed a substantially reduced level of electronic noise, resulting in reductions in image noise and artifacts, compared with detectors having distributed electronics.

In situ study of the growth and degradation processes in tetragonal lysozyme crystals on a silicon substrate by high-resolution X-ray diffractometry

NASA Astrophysics Data System (ADS)

Kovalchuk, M. V.; Prosekov, P. A.; Marchenkova, M. A.; Blagov, A. E.; D'yakova, Yu. A.; Tereshchenko, E. Yu.; Pisarevskii, Yu. V.; Kondratev, O. A.

2014-09-01

The results of an in situ study of the growth of tetragonal lysozyme crystals by high-resolution X-ray diffractometry are considered. The crystals are grown by the sitting-drop method on crystalline silicon substrates of different types: both on smooth substrates and substrates with artificial surface-relief structures using graphoepitaxy. The crystals are grown in a special hermetically closed crystallization cell, which enables one to obtain images with an optical microscope and perform in situ X-ray diffraction studies in the course of crystal growth. Measurements for lysozyme crystals were carried out in different stages of the crystallization process, including crystal nucleation and growth, developed crystals, the degradation of the crystal structure, and complete destruction.

Physical properties of organic particulate UV-absorbers used in sunscreens. I. Determination of particle size with fiber-optic quasi-elastic light scattering (FOQELS), disc centrifugation, and laser diffractometry.

PubMed

Herzog, Bernd; Katzenstein, Armin; Quass, Katja; Stehlin, Albert; Luther, Helmut

2004-03-01

In this study microparticles consisting of a benzotriazole derivative, which are used as absorbers for UV radiation in cosmetic sunscreens, were investigated. The particles were micronized in presence of a dispersing agent by means of a ball milling process. According to the energy input different particle sizes were produced in the range of 0.16 to 4 microm. The particle sizes obtained after different stages of the micronization process were measured using fiber-optic quasi-elastic light scattering (FOQELS), disc centrifugation, and laser diffractometry. All methods showed satisfactory agreement over the whole range of sizes. With the FOQELS technique the particle size distribution could be resolved to sizes well below 0.1 microm.

The study of in-situ formed alumina and aluminide intermetallic reinforced aluminum-based metal matrix composites

NASA Astrophysics Data System (ADS)

Yu, Peng

Aluminum-based metal matrix composites (MMCs) have been widely used as structural materials in the automobile and aerospace industry due to their specific properties. In this thesis, we report the fabrication of in-situ formed alumina and aluminide intermetallic reinforced aluminum-based metal matrix composites by the displacement reactions between Al and selected metal oxides (NiO, CuO and ZnO). These MMCs were produced when the Al-20wt% NiO, Al-20wt% CuO and Al-10wt% ZnO green compacts were reaction sintered in the tube furnaces. In this work, differential thermal analysis (DTA) was performed on the green samples. The green samples were then sintered separately in different tube furnaces for 30 minutes. In order to study the reaction mechanisms, the x-ray diffractometry (XRD) was used to obtain diffraction patterns of these sintered samples, the scanning electron microscope (SEM) and transmission electron microscope (TEM) were used to study the microstructures of these samples. The elemental quantitative compositions of samples were determined by the energy dispersive x-ray spectrometry (EDX). In order to study the effect of cooling rate on the samples, the green samples were further sintered to 1000°C and cooled down to room temperature in different conditions: by furnace-cooling, air-quenching, oil-quenching or NaCl-solution-quenching. The SEM, TEM and atomic force microscopy (AFM) were conducted to investigate their microstructures. A microhardness tester was used to measure the hardness values of these samples. It was found that during sintering of the Al-20wt% NiO green sample, displacement reaction between Al and NiO initially occurred in solid-solid form and was soon halted by its products that separated the NiO particles from the Al matrix. The reaction then resumed in solid-liquid form as the temperature increased to the eutectic temperature of Al3Ni-Al when liquid (Al, Ni) phase appeared in the sample. After cooling, Al2O 3 particles, Al3Ni proeutectic phase and fiber-like Al 3Ni-Al eutectic were found in the sintered Al-MMC sample. (Abstract shortened by UMI.)

Wear mechanisms in hybrid composites of Graphite-20 Pct SiC in A356 Aluminum Alloy (Al-7 Pct Si-0.3 Pct Mg)

NASA Astrophysics Data System (ADS)

Ames, W.; Alpas, A. T.

1995-01-01

The wear behavior of A356 aluminum alloy (Al-7 Pct Si-0.3 Pct Mg) matrix composites reinforced with 20 vol Pct SiC particles and 3 or 10 vol Pct graphite was investigated. These hybrid composites represent the merging of two philosophies in tribological material design: soft-particle lubrication by graphite and hard-particle reinforcement by carbide particles. The wear tests were performed using a block-on-ring (SAE 52100 steel) wear machine under dry sliding conditions within a load range of 1 to 441 N. The microstructural and compositional changes that took place during wear were characterized using scanning electron microscopy (SEM), Auger electron spectroscopy (AES), energy-dispersive X-ray spectroscopy (EDXA), and X-ray diffractometry (XRD). The wear resistance of 3 Pct graphite-20 Pct SiC-A356 hybrid composite was comparable to 20 Pct SiC-A356 without graphite at low and medium loads. At loads below 20 N, both hybrid and 20 Pct SiC-A356 composites without graphite demonstrated wear rates up to 10 times lower than the unreinforced A356 alloy due to the load-carrying capacity of SiC particles. The wear resistance of 3 Pct graphite 20 Pct SiC-A356 was 1 to 2 times higher than 10 Pct graphite-containing hybrid composites at high loads. However, graphite addition reduced the counterface wear. The unreinforced A356 and 20 Pct SiC-A356 showed a transition from mild to severe wear at 95 N and 225 N, respectively. Hybrid composites with 3 Pct and 10 Pct graphite did not show such a transition over the entire load range, indicating that graphite improved the seizure resistance of the composites. Tribolayers, mainly consisting of a compacted mixture of graphite, iron oxides, and aluminum, were generated on the surfaces of the hybrid composites. In the hybrid composites, the elimination of the severe wear (and hence the improvement in seizure resistance) was attributed to the reduction in friction-induced surface heating due to the presence of graphite- and iron-oxide-containing tribolayers.

Scanning ultrafast electron microscopy

PubMed Central

Yang, Ding-Shyue; Mohammed, Omar F.; Zewail, Ahmed H.

2010-01-01

Progress has been made in the development of four-dimensional ultrafast electron microscopy, which enables space-time imaging of structural dynamics in the condensed phase. In ultrafast electron microscopy, the electrons are accelerated, typically to 200 keV, and the microscope operates in the transmission mode. Here, we report the development of scanning ultrafast electron microscopy using a field-emission-source configuration. Scanning of pulses is made in the single-electron mode, for which the pulse contains at most one or a few electrons, thus achieving imaging without the space-charge effect between electrons, and still in ten(s) of seconds. For imaging, the secondary electrons from surface structures are detected, as demonstrated here for material surfaces and biological specimens. By recording backscattered electrons, diffraction patterns from single crystals were also obtained. Scanning pulsed-electron microscopy with the acquired spatiotemporal resolutions, and its efficient heat-dissipation feature, is now poised to provide in situ 4D imaging and with environmental capability. PMID:20696933

Measurement of particle size distribution of soil and selected aggregate sizes using the hydrometer method and laser diffractometry

NASA Astrophysics Data System (ADS)

Guzmán, G.; Gómez, J. A.; Giráldez, J. V.

2010-05-01

Soil particle size distribution has been traditionally determined by the hydrometer or the sieve-pipette methods, both of them time consuming and requiring a relatively large soil sample. This might be a limitation in situations, such as for instance analysis of suspended sediment, when the sample is small. A possible alternative to these methods are the optical techniques such as laser diffractometry. However the literature indicates that the use of this technique as an alternative to traditional methods is still limited, because the difficulty in replicating the results obtained with the standard methods. In this study we present the percentages of soil grain size determined using laser diffractometry within ranges set between 0.04 - 2000 μm. A Beckman-Coulter ® LS-230 with a 750 nm laser beam and software version 3.2 in five soils, representative of southern Spain: Alameda, Benacazón, Conchuela, Lanjarón and Pedrera. In three of the studied soils (Alameda, Benacazón and Conchuela) the particle size distribution of each aggregate size class was also determined. Aggregate size classes were obtained by dry sieve analysis using a Retsch AS 200 basic ®. Two hundred grams of air dried soil were sieved during 150 s, at amplitude 2 mm, getting nine different sizes between 2000 μm and 10 μm. Analyses were performed by triplicate. The soil sample preparation was also adapted to our conditions. A small amount each soil sample (less than 1 g) was transferred to the fluid module full of running water and disaggregated by ultrasonication at energy level 4 and 80 ml of sodium hexametaphosphate solution during 580 seconds. Two replicates of each sample were performed. Each measurement was made for a 90 second reading at a pump speed of 62. After the laser diffractometry analysis, each soil and its aggregate classes were processed calibrating its own optical model fitting the optical parameters that mainly depends on the color and the shape of the analyzed particle. As a second alternative a unique optical model valid for a broad range of soils developed by the Department of Soil, Water, and Environmental Science of the University of Arizona (personal communication, already submitted) was tested. The results were compared with the particle size distribution measured in the same soils and aggregate classes using the hydrometer method. Preliminary results indicate a better calibration of the technique using the optical model of the Department of Soil, Water, and Environmental Science of the University of Arizona, which obtained a good correlations (r2>0.85). This result suggests that with an appropriate calibration of the optical model laser diffractometry might provide a reliable soil particle characterization.

Scanning electron microscopy of hepatic ultrastructure: secondary, backscattered, and transmitted electron imaging.

PubMed

Miyai, K; Abraham, J L; Linthicum, D S; Wagner, R M

1976-10-01

Several methods of tissue preparation and different modes of operation of the scanning electron microscope were used to study the ultrastructure of rat liver. Rat livers were perfusion fixed with buffered 2 per cent paraformaldehyde or a mixture of 1.5 per cent paraformaldehyde and 1 per cent glutaraldehyde and processed as follows. Tissue blocks were postfixed in buffered 2 per cent osmium tetroxide followed sequentially by the ligand-mediated osmium binding technique, dehydration and cryofracture in ethanol, and critical point drying. They were then examined without metal coating in the scanning electron microscope operating in the secondary electron and backscattered electron modes. Fifty-micrometer sections were cut with a tissue sectioner, stained with lead citrate, postfixed with osmium, dehydrated, critical point dried, and examined in the secondary electron and back-scattered electron modes. Frozen sections (0.25 to 0.75 mum. thick) were cut by the method of Tokuyasu (Toluyasu KT: J Cell Biol 57:551, 1973) and their scanning transmission electron microscope images were examined either with a scanning transmission electron microscope detector or with a conversion stub using the secondary electron detector. Secondary electron images of the liver prepared by ligand-mediated osmium binding and subsequent cryofracture revealed such intracellular structures as cisternae of the endoplasmic reticulum, lysosomes, mitochondria, lipid droplets, nucleolus and nuclear chromatin, as well as the usual surface morphology, Lipocytes in the perisinusoidal space were readily identified. Backscattered electron images. Unembedded frozen sections had little drying artifact and were virtually free of freezing damage. The scanning transmission electron microscope image revealed those organelles visualized by the secondary electron mode in the ligand-mediated osmium binding-treated tissue.

Characterization of two-dimensional hexagonal boron nitride using scanning electron and scanning helium ion microscopy

NASA Astrophysics Data System (ADS)

Guo, Hongxuan; Gao, Jianhua; Ishida, Nobuyuki; Xu, Mingsheng; Fujita, Daisuke

2014-01-01

Characterization of the structural and physical properties of two-dimensional (2D) materials, such as layer number and inelastic mean free path measurements, is very important to optimize their synthesis and application. In this study, we characterize the layer number and morphology of hexagonal boron nitride (h-BN) nanosheets on a metallic substrate using field emission scanning electron microscopy (FE-SEM) and scanning helium ion microscopy (HIM). Using scanning beams of various energies, we could analyze the dependence of the intensities of secondary electrons on the thickness of the h-BN nanosheets. Based on the interaction between the scanning particles (electrons and helium ions) and h-BN nanosheets, we deduced an exponential relationship between the intensities of secondary electrons and number of layers of h-BN. With the attenuation factor of the exponential formula, we calculate the inelastic mean free path of electrons and helium ions in the h-BN nanosheets. Our results show that HIM is more sensitive and consistent than FE-SEM for characterizing the number of layers and morphology of 2D materials.

Electron beams scanning: A novel method

NASA Astrophysics Data System (ADS)

Askarbioki, M.; Zarandi, M. B.; Khakshournia, S.; Shirmardi, S. P.; Sharifian, M.

2018-06-01

In this research, a spatial electron beam scanning is reported. There are various methods for ion and electron beam scanning. The best known of these methods is the wire scanning wherein the parameters of beam are measured by one or more conductive wires. This article suggests a novel method for e-beam scanning without the previous errors of old wire scanning. In this method, the techniques of atomic physics are applied so that a knife edge has a scanner role and the wires have detector roles. It will determine the 2D e-beam profile readily when the positions of the scanner and detectors are specified.

Reprint of: Atmospheric scanning electron microscope observes cells and tissues in open medium through silicon nitride film.

PubMed

Nishiyama, Hidetoshi; Suga, Mitsuo; Ogura, Toshihiko; Maruyama, Yuusuke; Koizumi, Mitsuru; Mio, Kazuhiro; Kitamura, Shinichi; Sato, Chikara

2010-11-01

Direct observation of subcellular structures and their characterization is essential for understanding their physiological functions. To observe them in open environment, we have developed an inverted scanning electron microscope with a detachable, open-culture dish, capable of 8 nm resolution, and combined with a fluorescence microscope quasi-simultaneously observing the same area from the top. For scanning electron microscopy from the bottom, a silicon nitride film window in the base of the dish maintains a vacuum between electron gun and open sample dish while allowing electrons to pass through. Electrons are backscattered from the sample and captured by a detector under the dish. Cells cultured on the open dish can be externally manipulated under optical microscopy, fixed, and observed using scanning electron microscopy. Once fine structures have been revealed by scanning electron microscopy, their component proteins may be identified by comparison with separately prepared fluorescence-labeled optical microscopic images of the candidate proteins, with their heavy-metal-labeled or stained ASEM images. Furthermore, cell nuclei in a tissue block stained with platinum-blue were successfully observed without thin-sectioning, which suggests the applicability of this inverted scanning electron microscope to cancer diagnosis. This microscope visualizes mesoscopic-scale structures, and is also applicable to non-bioscience fields including polymer chemistry. Copyright © 2010 Elsevier Inc. All rights reserved.

A new apparatus for electron tomography in the scanning electron microscope

DOE Office of Scientific and Technical Information (OSTI.GOV)

Morandi, V., E-mail: morandi@bo.imm.cnr.it; Maccagnani, P.; Masini, L.

2015-06-23

The three-dimensional reconstruction of a microscopic specimen has been obtained by applying the tomographic algorithm to a set of images acquired in a Scanning Electron Microscope. This result was achieved starting from a series of projections obtained by stepwise rotating the sample under the beam raster. The Scanning Electron Microscope was operated in the scanning-transmission imaging mode, where the intensity of the transmitted electron beam is a monotonic function of the local mass-density and thickness of the specimen. The detection strategy has been implemented and tailored in order to maintain the projection requirement over the large tilt range, as requiredmore » by the tomographic workflow. A Si-based electron detector and an eucentric-rotation specimen holder have been specifically developed for the purpose.« less

Subsurface examination of a foliar biofilm using scanning electron- and focused-ion-beam microscopy

USDA-ARS?s Scientific Manuscript database

The dual beam scanning electron microscope, equipped with both a focused ion- and scanning electron- beam (FIB SEM) is a novel tool for the exploration of the subsurface structure of biological tissues. The FIB is capable of removing small cross sections to view the subsurface features and may be s...

Spatial Resolution in Scanning Electron Microscopy and Scanning Transmission Electron Microscopy Without a Specimen Vacuum Chamber.

PubMed

Nguyen, Kayla X; Holtz, Megan E; Richmond-Decker, Justin; Muller, David A

2016-08-01

A long-standing goal of electron microscopy has been the high-resolution characterization of specimens in their native environment. However, electron optics require high vacuum to maintain an unscattered and focused probe, a challenge for specimens requiring atmospheric or liquid environments. Here, we use an electron-transparent window at the base of a scanning electron microscope's objective lens to separate column vacuum from the specimen, enabling imaging under ambient conditions, without a specimen vacuum chamber. We demonstrate in-air imaging of specimens at nanoscale resolution using backscattered scanning electron microscopy (airSEM) and scanning transmission electron microscopy. We explore resolution and contrast using Monte Carlo simulations and analytical models. We find that nanometer-scale resolution can be obtained at gas path lengths up to 400 μm, although contrast drops with increasing gas path length. As the electron-transparent window scatters considerably more than gas at our operating conditions, we observe that the densities and thicknesses of the electron-transparent window are the dominant limiting factors for image contrast at lower operating voltages. By enabling a variety of detector configurations, the airSEM is applicable to a wide range of environmental experiments including the imaging of hydrated biological specimens and in situ chemical and electrochemical processes.

Spatial Resolution in Scanning Electron Microscopy and Scanning Transmission Electron Microscopy Without a Specimen Vacuum Chamber

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nguyen, Kayla X.; Holtz, Megan E.; Richmond-Decker, Justin

2016-07-25

Abstract A long-standing goal of electron microscopy has been the high-resolution characterization of specimens in their native environment. However, electron optics require high vacuum to maintain an unscattered and focused probe, a challenge for specimens requiring atmospheric or liquid environments. Here, we use an electron-transparent window at the base of a scanning electron microscope’s objective lens to separate column vacuum from the specimen, enabling imaging under ambient conditions, without a specimen vacuum chamber. We demonstrate in-air imaging of specimens at nanoscale resolution using backscattered scanning electron microscopy (airSEM) and scanning transmission electron microscopy. We explore resolution and contrast using Montemore » Carlo simulations and analytical models. We find that nanometer-scale resolution can be obtained at gas path lengths up to 400μm, although contrast drops with increasing gas path length. As the electron-transparent window scatters considerably more than gas at our operating conditions, we observe that the densities and thicknesses of the electron-transparent window are the dominant limiting factors for image contrast at lower operating voltages. By enabling a variety of detector configurations, the airSEM is applicable to a wide range of environmental experiments including the imaging of hydrated biological specimens andin situchemical and electrochemical processes.« less

Asbestiform minerals in ophiolitic rocks of Calabria (southern Italy).

PubMed

Campopiano, Antonella; Olori, Angelo; Spadafora, Alessandra; Rosaria Bruno, Maria; Angelosanto, Federica; Iannò, Antonino; Casciardi, Stefano; Giardino, Renato; Conte, Maurizio; Oranges, Teresa; Iavicoli, Sergio

2018-03-22

Ophiolitic rocks cropping on Calabria territory, southern Italy, can hold asbestiform minerals potentially harmful for human health. The aim of this work was to detect the fibrous phases of ophiolites along the Coastal Chain of northern Calabria and southern part of the Sila massif. Above 220 massive samples were collected in the study areas and analyzed using optical and electron microscopy, X-ray diffractometry, and Fourier transform infra-red spectrometry. The main fibrous constituent belonged to tremolite-actinolite series followed by fibrous antigorite that becomes more abundant in the samples collected in Reventino Mount surroundings. Results highlighted that serpentinites samples mainly consisted of antigorite and minor chrysotile. Samples collected along the coastal chain of northern Calabria did not hold fibrous materials. The results will be useful for Italian natural occurrences of asbestos (NOA) mapping in order to avoid an unintentional exposition by human activity or weathering processes.

Growth of single crystals of mercuric iodide (HgI/sub 2/) in spacelab III

DOE Office of Scientific and Technical Information (OSTI.GOV)

Van Den Berg, L.; Schnepple, W.F.

1981-01-01

Continued development of a system designed to grow crystals by physical vapor transport in the environment of Spacelab III will be described, with special emphasis on simulation of expected space conditions, adjustment of crystal growth parameters, and on board observation and control of the experiment by crew members and ground personnel. A critical factor in the use of mercuric iodide for semiconductor detectors of x-rays and gamma-rays is the crystalline quality of the material. The twofold purpose of the Spacelab III experiment is therefore to grow single crystals with superior electronic properties as an indirect result of the greatly reducedmore » gravity field during the growth, and to obtain data which will lead to improved understanding of the vapor transport mechanism. The experiments planned to evaluate the space crystals, including gamma-ray diffractometry and measurements of stoichiometry, lattice dimensions, mechanical strength, luminescense, and detector performance are discussed.« less

Gold nanoparticle decorated multi-walled carbon nanotubes as counter electrode for dye sensitized solar cells.

PubMed

Kaniyoor, Adarsh; Ramaprabhu, Sundara

2012-11-01

A novel counter electrode material for dye sensitized solar cells (DSSCs) composed of nanostructured Au particles decorated on functionalized multi-walled carbon nanotubes (f-MWNTs) is demonstrated for the first time. MWNTs synthesized by catalytic chemical vapor deposition technique are purified and functionalized by treating with concentrated acids. Au nanoparticles are decorated on f-MWNTs by a rapid and facile microwave assisted polyol reduction method. The materials are characterized by X-ray diffractometry, Fourier transform infra red spectroscopy and electron microscopy. The DSSC fabricated with Au/f-MWNTs based counter electrode shows enhanced power conversion efficiency (eta) of 4.9% under AM 1.5G simulated solar radiation. In comparison, the reference DSSCs fabricated with f-MWNTs and Pt counter electrodes show eta of 2.1% and 4.5%. This high performance of Au/f-MWNTs counter electrode is investigated using electrochemical impedance spectroscopy and cyclic voltammetry studies.

Physical characterization of dibasic calcium phosphate dihydrate and anhydrate.

PubMed

Miyazaki, Tamaki; Sivaprakasam, Kannan; Tantry, Jaidev; Suryanarayanan, Raj

2009-03-01

The dehydration of different commercial brands of dibasic calcium phosphate dihydrate (DCPD; CaHPO(4).2H(2)O) was examined over a range of temperatures and water vapor pressures. To determine the main factors affecting the physical stability of DCPD, the baseline characterization of DCPD and dibasic calcium phosphate anhydrate (DCPA; CaHPO(4)) was conducted by thermogravimetric analysis, differential scanning calorimetry and X-ray diffractometry. The surface area and the DCPA content (present as an impurity) depended on the commercial source of DCPD. The larger particles contained a higher concentration of DCPA and the anhydrate exhibited a concentration-dependent acceleratory effect on the dehydration of DCPD. Unlike DCPD, DCPA is physically stable and resisted hydration even when dispersed in water for over 7 months in the temperature range of 4-50 degrees C. In dosage forms containing DCPD, there is a potential for phase transformation to DCPA, while the reverse transition, that is, DCPA --> DCPD appears to be extremely unlikely. Thus, the risk of physical transformation can be minimized by using DCPA in formulations. (c) 2008 Wiley-Liss, Inc. and the American Pharmacists Association

Sustained release biodegradable solid lipid microparticles: Formulation, evaluation and statistical optimization by response surface methodology.

PubMed

Hanif, Muhammad; Khan, Hafeez Ullah; Afzal, Samina; Mahmood, Asif; Maheen, Safirah; Afzal, Khurram; Iqbal, Nabila; Andleeb, Mehwish; Abbas, Nazar

2017-12-20

For preparing nebivolol loaded solid lipid microparticles (SLMs) by the solvent evaporation microencapsulation process from carnauba wax and glyceryl monostearate, central composite design was used to study the impact of independent variables on yield (Y1), entrapment efficiency (Y2) and drug release (Y3). SLMs having a 10-40 μm size range, with good rheological behavior and spherical smooth surfaces, were produced. Fourier transform infrared spectroscopy, differential scanning calorimetry and X-ray diffractometry pointed to compatibility between formulation components and the zeta-potential study confirmed better stability due to the presence of negative charge (-20 to -40 mV). The obtained outcomes for Y1 (29-86 %), Y2 (45-83 %) and Y3 (49-86 %) were analyzed by polynomial equations and the suggested quadratic model were validated. Nebivolol release from SLMs at pH 1.2 and 6.8 was significantly (p < 0.05) affected by lipid concentration. The release mechanism followed Higuchi and zero order models, while n > 0.85 value (Korsmeyer- Peppas) suggested slow erosion along with diffusion. The optimized SLMs have the potential to improve nebivolol oral bioavailability.

Crystal structure and thermal expansion of a CsCe 2Cl 7 scintillator

DOE PAGES

Zhuravleva, M.; Lindsey, A.; Chakoumakos, B. C.; ...

2015-04-06

Here we used single-crystal X-ray diffraction data to determine crystal structure of CsCe 2Cl 7. It crystallizes in a P112 1/b space group with a = 19.352(1) Å, b = 19.352(1) Å, c = 14.838(1) Å, γ = 119.87(2) ° , and V = 4818.6(5) Å 3. Differential scanning calorimetry measurements combined with the structural evolution of CsCe 2Cl 7 via X-ray diffractometry over a temperature range from room temperature to the melting point indicates no obvious intermediate solid-solid phase transitions. The anisotropy in the average linear coefficient of thermal expansion of the a axis (21.3 10 -6/ °C) withmore » respect to the b and c axes (27.0 10 -6/ °C) was determined through lattice parameter refinement of the temperature dependent diffraction patterns. Lastly, these findings suggest that the reported cracking behavior during melt growth of CsCe 2Cl 7 bulk crystals using conventional Bridgman and Czochralski techniques may be largely attributed to the anisotropy in thermal expansion.« less

Enhanced dissolution, stability and physicochemical characterization of ATRA/2-hydroxypropyl-β-cyclodextrin inclusion complex pellets prepared by fluid-bed coating technique.

PubMed

Chen, Zhongjian; Lu, Yi; Qi, Jianping; Wu, Wei

2013-02-01

The aim of this work was to prepare stable all-trans-retinoic acid (ATRA)/2-hydroxypropyl-β-cyclodextrin (HPCD) inclusion complex pellets with industrial feasible technology, the fluid-bed coating technique, using PVP K30 simultaneously as binder and reprecipitation retarder. The coating process was fluent with high coating efficiency. In vitro dissolution of the inclusion complex pellets in 5% w/v Cremopher EL solution was dramatically enhanced with no reprecipitation observed, and significantly improved stability against humidity (92.5% and 75% RH) and illumination (4500 lx ± 500 lx) was achieved by HPCD inclusion. Differential scanning calorimetry and powder X-ray diffractometry confirmed the absence of crystallinity of ATRA. Fourier transform-infrared spectrometry revealed interaction between ATRA and HPCD adding evidence on inclusion of ATRA moieties into HPCD cavities. Solid-state (13)C NMR spectrometry indicated possible inclusion of ATRA through the polyene chain, which was the main reason for the enhanced photostability. It is concluded that the fluid-bed coating technique has the potential use in the industrial preparation of ATRA/HPCD inclusion complex pellets.

A scanning electron microscopy study of the macro-crystalline structure of 2-(2,4-dinitrobenzyl) pyridine

NASA Technical Reports Server (NTRS)

Ware, Jacqueline; Hammond, Ernest C., Jr.

1989-01-01

The compound, 2-(2,4-dinitrobenzyl) pyridine, was synthesized in the laboratory; an introductory level electron microscopy study of the macro-crystalline structure was conducted using the scanning electron microscope (SEM). The structure of these crystals was compared with the macrostructure of the crystal of 2-(2,4-dinitrobenzyl) pyridinium bromide, the hydrobromic salt of the compound which was also synthesized in the laboratory. A scanning electron microscopy crystal study was combined with a study of the principle of the electron microscope.

U-10Mo Sample Preparation and Examination using Optical and Scanning Electron Microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Prabhakaran, Ramprashad; Joshi, Vineet V.; Rhodes, Mark A.

2016-10-01

The purpose of this document is to provide guidelines to prepare specimens of uranium alloyed with 10 weight percent molybdenum (U-10Mo) for optical metallography and scanning electron microscopy. This document also provides instructions to set up an optical microscope and a scanning electron microscope to analyze U-10Mo specimens and to obtain the required information.

U-10Mo Sample Preparation and Examination using Optical and Scanning Electron Microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Prabhakaran, Ramprashad; Joshi, Vineet V.; Rhodes, Mark A.

2016-03-30

The purpose of this document is to provide guidelines to prepare specimens of uranium alloyed with 10 weight percent molybdenum (U-10Mo) for optical metallography and scanning electron microscopy. This document also provides instructions to set up an optical microscope and a scanning electron microscope to analyze U-10Mo specimens and to obtain the required information.

Correcting nonlinear drift distortion of scanning probe and scanning transmission electron microscopies from image pairs with orthogonal scan directions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ophus, Colin; Ciston, Jim; Nelson, Chris T.

Unwanted motion of the probe with respect to the sample is a ubiquitous problem in scanning probe and scanning transmission electron microscopies, causing both linear and nonlinear artifacts in experimental images. We have designed a procedure to correct these artifacts by using orthogonal scan pairs to align each measurement line-by-line along the slow scan direction, by fitting contrast variation along the lines. We demonstrate the accuracy of our algorithm on both synthetic and experimental data and provide an implementation of our method.

Correcting nonlinear drift distortion of scanning probe and scanning transmission electron microscopies from image pairs with orthogonal scan directions

DOE PAGES

Ophus, Colin; Ciston, Jim; Nelson, Chris T.

2015-12-10

Unwanted motion of the probe with respect to the sample is a ubiquitous problem in scanning probe and scanning transmission electron microscopies, causing both linear and nonlinear artifacts in experimental images. We have designed a procedure to correct these artifacts by using orthogonal scan pairs to align each measurement line-by-line along the slow scan direction, by fitting contrast variation along the lines. We demonstrate the accuracy of our algorithm on both synthetic and experimental data and provide an implementation of our method.

High-resolution, high-throughput imaging with a multibeam scanning electron microscope

PubMed Central

EBERLE, AL; MIKULA, S; SCHALEK, R; LICHTMAN, J; TATE, ML KNOTHE; ZEIDLER, D

2015-01-01

Electron–electron interactions and detector bandwidth limit the maximal imaging speed of single-beam scanning electron microscopes. We use multiple electron beams in a single column and detect secondary electrons in parallel to increase the imaging speed by close to two orders of magnitude and demonstrate imaging for a variety of samples ranging from biological brain tissue to semiconductor wafers. Lay Description The composition of our world and our bodies on the very small scale has always fascinated people, making them search for ways to make this visible to the human eye. Where light microscopes reach their resolution limit at a certain magnification, electron microscopes can go beyond. But their capability of visualizing extremely small features comes at the cost of a very small field of view. Some of the questions researchers seek to answer today deal with the ultrafine structure of brains, bones or computer chips. Capturing these objects with electron microscopes takes a lot of time – maybe even exceeding the time span of a human being – or new tools that do the job much faster. A new type of scanning electron microscope scans with 61 electron beams in parallel, acquiring 61 adjacent images of the sample at the same time a conventional scanning electron microscope captures one of these images. In principle, the multibeam scanning electron microscope’s field of view is 61 times larger and therefore coverage of the sample surface can be accomplished in less time. This enables researchers to think about large-scale projects, for example in the rather new field of connectomics. A very good introduction to imaging a brain at nanometre resolution can be found within course material from Harvard University on http://www.mcb80x.org/# as featured media entitled ‘connectomics’. PMID:25627873

High-resolution scanning precession electron diffraction: Alignment and spatial resolution.

PubMed

Barnard, Jonathan S; Johnstone, Duncan N; Midgley, Paul A

2017-03-01

Methods are presented for aligning the pivot point of a precessing electron probe in the scanning transmission electron microscope (STEM) and for assessing the spatial resolution in scanning precession electron diffraction (SPED) experiments. The alignment procedure is performed entirely in diffraction mode, minimising probe wander within the bright-field (BF) convergent beam electron diffraction (CBED) disk and is used to obtain high spatial resolution SPED maps. Through analysis of the power spectra of virtual bright-field images extracted from the SPED data, the precession-induced blur was measured as a function of precession angle. At low precession angles, SPED spatial resolution was limited by electronic noise in the scan coils; whereas at high precession angles SPED spatial resolution was limited by tilt-induced two-fold astigmatism caused by the positive spherical aberration of the probe-forming lens. Copyright © 2016 Elsevier B.V. All rights reserved.

The application of scanning electron microscopy to fractography

DOE Office of Scientific and Technical Information (OSTI.GOV)

Brooks, C.R.; McGill, B.L.

1994-10-01

Many failures involve fracture, and determination of the fracture process is a key factor in understanding the failure. This is frequently accomplished by characterizing the topography of the fracture surface. Scanning electron microscopy has a prominent role in fractography due to three features of the scanning electron microscope (SEM): high resolution, great depth of field, and the ability to obtain chemical information via analysis of the X-rays generated by the electrons. A qualitative treatment is presented of the interaction of electrons with a sample and the effect of the SEM operating parameters on image formation, quality, and X-ray analysis. Fractographsmore » are presented to illustrate these features of scanning electron microscopy and to illustrate the limitations and precautions in obtaining fractographs and x-ray analyses. The review is concluded with examples of fracture surface features of metallic, ceramic, and polymeric materials.« less

Ion-induced crystal damage during plasma-assisted MBE growth of GaN layers

NASA Astrophysics Data System (ADS)

Kirchner, V.; Heinke, H.; Birkle, U.; Einfeldt, S.; Hommel, D.; Selke, H.; Ryder, P. L.

1998-12-01

Gallium nitride layers were grown by plasma-assisted molecular-beam epitaxy on (0001)-oriented sapphire substrates using an electron cyclotron resonance (ECR) and a radio frequency (rf) plasma source. An applied substrate bias was varied from -200 to +250 V, resulting in a change of the density and energy of nitrogen ions impinging the growth surface. The layers were investigated by high-resolution x-ray diffractometry and high-resolution transmission electron microscopy (HRTEM). Applying a negative bias during growth has a marked detrimental effect on the crystal perfection of the layers grown with an ECR plasma source. This is indicated by a change in shape and width of (0002) and (202¯5) reciprocal lattice points as monitored by triple axis x-ray measurements. In HRTEM images, isolated basal plane stacking faults were found, which probably result from precipitation of interstitial atoms. The crystal damage in layers grown with a highly negative substrate bias is comparable to that observed for ion implantation processes at orders of magnitude larger ion energies. This is attributed to the impact of ions on the growing surface. None of the described phenomena was observed for the samples grown with the rf plasma source.

On the Progress of Scanning Transmission Electron Microscopy (STEM) Imaging in a Scanning Electron Microscope.

PubMed

Sun, Cheng; Müller, Erich; Meffert, Matthias; Gerthsen, Dagmar

2018-04-01

Transmission electron microscopy (TEM) with low-energy electrons has been recognized as an important addition to the family of electron microscopies as it may avoid knock-on damage and increase the contrast of weakly scattering objects. Scanning electron microscopes (SEMs) are well suited for low-energy electron microscopy with maximum electron energies of 30 keV, but they are mainly used for topography imaging of bulk samples. Implementation of a scanning transmission electron microscopy (STEM) detector and a charge-coupled-device camera for the acquisition of on-axis transmission electron diffraction (TED) patterns, in combination with recent resolution improvements, make SEMs highly interesting for structure analysis of some electron-transparent specimens which are traditionally investigated by TEM. A new aspect is correlative SEM, STEM, and TED imaging from the same specimen region in a SEM which leads to a wealth of information. Simultaneous image acquisition gives information on surface topography, inner structure including crystal defects and qualitative material contrast. Lattice-fringe resolution is obtained in bright-field STEM imaging. The benefits of correlative SEM/STEM/TED imaging in a SEM are exemplified by structure analyses from representative sample classes such as nanoparticulates and bulk materials.

Imaging of Norway spruce early somatic embryos with the ESEM, Cryo-SEM and laser scanning microscope.

PubMed

Neděla, Vilém; Hřib, Jiří; Havel, Ladislav; Hudec, Jiří; Runštuk, Jiří

2016-05-01

This article describes the surface structure of Norway spruce early somatic embryos (ESEs) as a typical culture with asynchronous development. The microstructure of extracellular matrix covering ESEs were observed using the environmental scanning electron microscope as a primary tool and using the scanning electron microscope with cryo attachment and laser electron microscope as a complementary tool allowing our results to be proven independently. The fresh samples were observed in conditions of the air environment of the environmental scanning electron microscope (ESEM) with the pressure from 550Pa to 690Pa and the low temperature of the sample from -18°C to -22°C. The samples were studied using two different types of detector to allow studying either the thin surface structure or material composition. The scanning electron microscope with cryo attachment was used for imaging frozen extracellular matrix microstructure with higher resolution. The combination of both electron microscopy methods was suitable for observation of "native" plant samples, allowing correct evaluation of our results, free of error and artifacts. Copyright © 2016 Elsevier Ltd. All rights reserved.

A correlative optical microscopy and scanning electron microscopy approach to locating nanoparticles in brain tumors.

PubMed

Kempen, Paul J; Kircher, Moritz F; de la Zerda, Adam; Zavaleta, Cristina L; Jokerst, Jesse V; Mellinghoff, Ingo K; Gambhir, Sanjiv S; Sinclair, Robert

2015-01-01

The growing use of nanoparticles in biomedical applications, including cancer diagnosis and treatment, demands the capability to exactly locate them within complex biological systems. In this work a correlative optical and scanning electron microscopy technique was developed to locate and observe multi-modal gold core nanoparticle accumulation in brain tumor models. Entire brain sections from mice containing orthotopic brain tumors injected intravenously with nanoparticles were imaged using both optical microscopy to identify the brain tumor, and scanning electron microscopy to identify the individual nanoparticles. Gold-based nanoparticles were readily identified in the scanning electron microscope using backscattered electron imaging as bright spots against a darker background. This information was then correlated to determine the exact location of the nanoparticles within the brain tissue. The nanoparticles were located only in areas that contained tumor cells, and not in the surrounding healthy brain tissue. This correlative technique provides a powerful method to relate the macro- and micro-scale features visible in light microscopy with the nanoscale features resolvable in scanning electron microscopy. Copyright © 2014 Elsevier Ltd. All rights reserved.

New developments in electron microscopy for serial image acquisition of neuronal profiles.

PubMed

Kubota, Yoshiyuki

2015-02-01

Recent developments in electron microscopy largely automate the continuous acquisition of serial electron micrographs (EMGs), previously achieved by laborious manual serial ultrathin sectioning using an ultramicrotome and ultrastructural image capture process with transmission electron microscopy. The new systems cut thin sections and capture serial EMGs automatically, allowing for acquisition of large data sets in a reasonably short time. The new methods are focused ion beam/scanning electron microscopy, ultramicrotome/serial block-face scanning electron microscopy, automated tape-collection ultramicrotome/scanning electron microscopy and transmission electron microscope camera array. In this review, their positive and negative aspects are discussed. © The Author 2015. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

Precision controlled atomic resolution scanning transmission electron microscopy using spiral scan pathways

NASA Astrophysics Data System (ADS)

Sang, Xiahan; Lupini, Andrew R.; Ding, Jilai; Kalinin, Sergei V.; Jesse, Stephen; Unocic, Raymond R.

2017-03-01

Atomic-resolution imaging in an aberration-corrected scanning transmission electron microscope (STEM) can enable direct correlation between atomic structure and materials functionality. The fast and precise control of the STEM probe is, however, challenging because the true beam location deviates from the assigned location depending on the properties of the deflectors. To reduce these deviations, i.e. image distortions, we use spiral scanning paths, allowing precise control of a sub-Å sized electron probe within an aberration-corrected STEM. Although spiral scanning avoids the sudden changes in the beam location (fly-back distortion) present in conventional raster scans, it is not distortion-free. “Archimedean” spirals, with a constant angular frequency within each scan, are used to determine the characteristic response at different frequencies. We then show that such characteristic functions can be used to correct image distortions present in more complicated constant linear velocity spirals, where the frequency varies within each scan. Through the combined application of constant linear velocity scanning and beam path corrections, spiral scan images are shown to exhibit less scan distortion than conventional raster scan images. The methodology presented here will be useful for in situ STEM imaging at higher temporal resolution and for imaging beam sensitive materials.

Precision controlled atomic resolution scanning transmission electron microscopy using spiral scan pathways.

PubMed

Sang, Xiahan; Lupini, Andrew R; Ding, Jilai; Kalinin, Sergei V; Jesse, Stephen; Unocic, Raymond R

2017-03-08

Atomic-resolution imaging in an aberration-corrected scanning transmission electron microscope (STEM) can enable direct correlation between atomic structure and materials functionality. The fast and precise control of the STEM probe is, however, challenging because the true beam location deviates from the assigned location depending on the properties of the deflectors. To reduce these deviations, i.e. image distortions, we use spiral scanning paths, allowing precise control of a sub-Å sized electron probe within an aberration-corrected STEM. Although spiral scanning avoids the sudden changes in the beam location (fly-back distortion) present in conventional raster scans, it is not distortion-free. "Archimedean" spirals, with a constant angular frequency within each scan, are used to determine the characteristic response at different frequencies. We then show that such characteristic functions can be used to correct image distortions present in more complicated constant linear velocity spirals, where the frequency varies within each scan. Through the combined application of constant linear velocity scanning and beam path corrections, spiral scan images are shown to exhibit less scan distortion than conventional raster scan images. The methodology presented here will be useful for in situ STEM imaging at higher temporal resolution and for imaging beam sensitive materials.

The Scanning Electron Microscope and the Archaeologist

ERIC Educational Resources Information Center

Ponting, Matthew

2004-01-01

Images from scanning electron microscopy are now quite common and they can be of great value in archaeology. Techniques such as secondary electron imaging, backscattered electron imaging and energy-dispersive x-ray analysis can reveal information such as the presence of weevils in grain in Roman Britain, the composition of Roman coins and the…

Scanning Electron Microscopy (SEM) Procedure for HE Powders on a Zeiss Sigma HD VP SEM

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zaka, F.

This method describes the characterization of inert and HE materials by the Zeiss Sigma HD VP field emission Scanning Electron Microscope (SEM). The SEM uses an accelerated electron beam to generate high-magnification images of explosives and other materials. It is fitted with five detectors (SE, Inlens, STEM, VPSE, HDBSD) to enable imaging of the sample via different secondary electron signatures, angles, and energies. In addition to imaging through electron detection, the microscope is also fitted with two Oxford Instrument Energy Dispersive Spectrometer (EDS) 80 mm detectors to generate elemental constituent spectra and two-dimensional maps of the material being scanned.

Comparative study of image contrast in scanning electron microscope and helium ion microscope.

PubMed

O'Connell, R; Chen, Y; Zhang, H; Zhou, Y; Fox, D; Maguire, P; Wang, J J; Rodenburg, C

2017-12-01

Images of Ga + -implanted amorphous silicon layers in a 110 n-type silicon substrate have been collected by a range of detectors in a scanning electron microscope and a helium ion microscope. The effects of the implantation dose and imaging parameters (beam energy, dwell time, etc.) on the image contrast were investigated. We demonstrate a similar relationship for both the helium ion microscope Everhart-Thornley and scanning electron microscope Inlens detectors between the contrast of the images and the Ga + density and imaging parameters. These results also show that dynamic charging effects have a significant impact on the quantification of the helium ion microscope and scanning electron microscope contrast. © 2017 The Authors Journal of Microscopy © 2017 Royal Microscopical Society.

Pseudomorphic GeSiSn, SiSn and Ge layers in strained heterostructures

NASA Astrophysics Data System (ADS)

Timofeev, V. A.; Nikiforov, A. I.; Tuktamyshev, A. R.; Mashanov, V. I.; Loshkarev, I. D.; Bloshkin, A. A.; Gutakovskii, A. K.

2018-04-01

The GeSiSn, SiSn layer growth mechanisms on Si(100) were investigated and the kinetic diagrams of the morphological GeSiSn, SiSn film states in the temperature range of 150 °C-450 °C at the tin content from 0% to 35% were built. The phase diagram of the superstructural change on the surface of Sn grown on Si(100) in the annealing temperature range of 0 °C-850 °C was established. The specular beam oscillations were first obtained during the SiSn film growth from 150 °C to 300 °C at the Sn content up to 35%. The transmission electron microscopy and x-ray diffractometry data confirm the crystal perfection and the pseudomorphic GeSiSn, SiSn film state, and also the presence of smooth heterointerfaces between GeSiSn or SiSn and Si. The photoluminescence for the multilayer periodic GeSiSn/Si structures in the range of 0.6-0.8 eV was detected. The blue shift with the excitation power increase is observed suggesting the presence of a type II heterostructure. The creation of tensile strained Ge films, which are pseudomorphic to the underlying GeSn layer, is confirmed by the results of the formation and analysis of the reciprocal space map in the x-ray diffractometry. The tensile strain in the Ge films reached the value in the range of 0.86%-1.5%. The GeSn buffer layer growth in the Sn content range from 8% to 12% was studied. The band structure of heterosystems based on pseudomorphic GeSiSn, SiSn and Ge layers was calculated and the valence and conduction band subband position dependences on the Sn content were built. Based on the calculation, the Sn content range in the GeSiSn, SiSn, and GeSn layers, which corresponds to the direct bandgap GeSiSn, SiSn, and Ge material, was obtained.

Correction of image drift and distortion in a scanning electron microscopy.

PubMed

Jin, P; Li, X

2015-12-01

Continuous research on small-scale mechanical structures and systems has attracted strong demand for ultrafine deformation and strain measurements. Conventional optical microscope cannot meet such requirements owing to its lower spatial resolution. Therefore, high-resolution scanning electron microscope has become the preferred system for high spatial resolution imaging and measurements. However, scanning electron microscope usually is contaminated by distortion and drift aberrations which cause serious errors to precise imaging and measurements of tiny structures. This paper develops a new method to correct drift and distortion aberrations of scanning electron microscope images, and evaluates the effect of correction by comparing corrected images with scanning electron microscope image of a standard sample. The drift correction is based on the interpolation scheme, where a series of images are captured at one location of the sample and perform image correlation between the first image and the consequent images to interpolate the drift-time relationship of scanning electron microscope images. The distortion correction employs the axial symmetry model of charged particle imaging theory to two images sharing with the same location of one object under different imaging fields of view. The difference apart from rigid displacement between the mentioned two images will give distortion parameters. Three-order precision is considered in the model and experiment shows that one pixel maximum correction is obtained for the employed high-resolution electron microscopic system. © 2015 The Authors Journal of Microscopy © 2015 Royal Microscopical Society.

High-resolution, high-throughput imaging with a multibeam scanning electron microscope.

PubMed

Eberle, A L; Mikula, S; Schalek, R; Lichtman, J; Knothe Tate, M L; Zeidler, D

2015-08-01

Electron-electron interactions and detector bandwidth limit the maximal imaging speed of single-beam scanning electron microscopes. We use multiple electron beams in a single column and detect secondary electrons in parallel to increase the imaging speed by close to two orders of magnitude and demonstrate imaging for a variety of samples ranging from biological brain tissue to semiconductor wafers. © 2015 The Authors Journal of Microscopy © 2015 Royal Microscopical Society.

Dynamic scan control in STEM: Spiral scans

DOE PAGES

Lupini, Andrew R.; Borisevich, Albina Y.; Kalinin, Sergei V.; ...

2016-06-13

Here, scanning transmission electron microscopy (STEM) has emerged as one of the foremost techniques to analyze materials at atomic resolution. However, two practical difficulties inherent to STEM imaging are: radiation damage imparted by the electron beam, which can potentially damage or otherwise modify the specimen and slow-scan image acquisition, which limits the ability to capture dynamic changes at high temporal resolution. Furthermore, due in part to scan flyback corrections, typical raster scan methods result in an uneven distribution of dose across the scanned area. A method to allow extremely fast scanning with a uniform residence time would enable imaging atmore » low electron doses, ameliorating radiation damage and at the same time permitting image acquisition at higher frame-rates while maintaining atomic resolution. The practical complication is that rastering the STEM probe at higher speeds causes significant image distortions. Non-square scan patterns provide a solution to this dilemma and can be tailored for low dose imaging conditions. Here, we develop a method for imaging with alternative scan patterns and investigate their performance at very high scan speeds. A general analysis for spiral scanning is presented here for the following spiral scan functions: Archimedean, Fermat, and constant linear velocity spirals, which were tested for STEM imaging. The quality of spiral scan STEM images is generally comparable with STEM images from conventional raster scans, and the dose uniformity can be improved.« less

Dynamic scan control in STEM: Spiral scans

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lupini, Andrew R.; Borisevich, Albina Y.; Kalinin, Sergei V.

Here, scanning transmission electron microscopy (STEM) has emerged as one of the foremost techniques to analyze materials at atomic resolution. However, two practical difficulties inherent to STEM imaging are: radiation damage imparted by the electron beam, which can potentially damage or otherwise modify the specimen and slow-scan image acquisition, which limits the ability to capture dynamic changes at high temporal resolution. Furthermore, due in part to scan flyback corrections, typical raster scan methods result in an uneven distribution of dose across the scanned area. A method to allow extremely fast scanning with a uniform residence time would enable imaging atmore » low electron doses, ameliorating radiation damage and at the same time permitting image acquisition at higher frame-rates while maintaining atomic resolution. The practical complication is that rastering the STEM probe at higher speeds causes significant image distortions. Non-square scan patterns provide a solution to this dilemma and can be tailored for low dose imaging conditions. Here, we develop a method for imaging with alternative scan patterns and investigate their performance at very high scan speeds. A general analysis for spiral scanning is presented here for the following spiral scan functions: Archimedean, Fermat, and constant linear velocity spirals, which were tested for STEM imaging. The quality of spiral scan STEM images is generally comparable with STEM images from conventional raster scans, and the dose uniformity can be improved.« less

Expansion of Shockley stacking fault observed by scanning electron microscope and partial dislocation motion in 4H-SiC

NASA Astrophysics Data System (ADS)

Yamashita, Yoshifumi; Nakata, Ryu; Nishikawa, Takeshi; Hada, Masaki; Hayashi, Yasuhiko

2018-04-01

We studied the dynamics of the expansion of a Shockley-type stacking fault (SSF) with 30° Si(g) partial dislocations (PDs) using a scanning electron microscope. We observed SSFs as dark lines (DLs), which formed the contrast at the intersection between the surface and the SSF on the (0001) face inclined by 8° from the surface. We performed experiments at different electron-beam scanning speeds, observing magnifications, and irradiation areas. The results indicated that the elongation of a DL during one-frame scanning depended on the time for which the electron beam irradiated the PD segment in the frame of view. From these results, we derived a formula to express the velocity of the PD using the elongation rate of the corresponding DL during one-frame scanning. We also obtained the result that the elongation velocity of the DL was not influenced by changing the direction in which the electron beam irradiates the PD. From this result, we deduced that the geometrical kink motion of the PD was enhanced by diffusing carriers that were generated by the electron-beam irradiation.

Three-dimensional imaging of adherent cells using FIB/SEM and STEM.

PubMed

Villinger, Clarissa; Schauflinger, Martin; Gregorius, Heiko; Kranz, Christine; Höhn, Katharina; Nafeey, Soufi; Walther, Paul

2014-01-01

In this chapter we describe three different approaches for three-dimensional imaging of electron microscopic samples: serial sectioning transmission electron microscopy (TEM), scanning transmission electron microscopy (STEM) tomography, and focused ion beam/scanning electron microscopy (FIB/SEM) tomography. With these methods, relatively large volumes of resin-embedded biological structures can be analyzed at resolutions of a few nm within a reasonable expenditure of time. The traditional method is serial sectioning and imaging the same area in all sections. Another method is TEM tomography that involves tilting a section in the electron beam and then reconstruction of the volume by back projection of the images. When the scanning transmission (STEM) mode is used, thicker sections (up to 1 μm) can be analyzed. The third approach presented here is focused ion beam/scanning electron microscopy (FIB/SEM) tomography, in which a sample is repeatedly milled with a focused ion beam (FIB) and each newly produced block face is imaged with the scanning electron microscope (SEM). This process can be repeated ad libitum in arbitrary small increments allowing 3D analysis of relatively large volumes such as eukaryotic cells. We show that resolution of this approach is considerably improved when the secondary electron signal is used. However, the most important prerequisite for three-dimensional imaging is good specimen preparation. For all three imaging methods, cryo-fixed (high-pressure frozen) and freeze-substituted samples have been used.

Analysis of improvement in performance and design parameters for enhancing resolution in an atmospheric scanning electron microscope.

PubMed

Yoon, Yeo Hun; Kim, Seung Jae; Kim, Dong Hwan

2015-12-01

The scanning electron microscope is used in various fields to go beyond diffraction limits of the optical microscope. However, the electron pathway should be conducted in a vacuum so as not to scatter electrons. The pretreatment of the sample is needed for use in the vacuum. To directly observe large and fully hydrophilic samples without pretreatment, the atmospheric scanning electron microscope (ASEM) is needed. We developed an electron filter unit and an electron detector unit for implementation of the ASEM. The key of the electron filter unit is that electrons are transmitted while air molecules remain untransmitted through the unit. The electron detector unit collected the backscattered electrons. We conducted experiments using the selected materials with Havar foil, carbon film and SiN film. © The Author 2015. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

High Dynamic Range Pixel Array Detector for Scanning Transmission Electron Microscopy.

PubMed

Tate, Mark W; Purohit, Prafull; Chamberlain, Darol; Nguyen, Kayla X; Hovden, Robert; Chang, Celesta S; Deb, Pratiti; Turgut, Emrah; Heron, John T; Schlom, Darrell G; Ralph, Daniel C; Fuchs, Gregory D; Shanks, Katherine S; Philipp, Hugh T; Muller, David A; Gruner, Sol M

2016-02-01

We describe a hybrid pixel array detector (electron microscope pixel array detector, or EMPAD) adapted for use in electron microscope applications, especially as a universal detector for scanning transmission electron microscopy. The 128×128 pixel detector consists of a 500 µm thick silicon diode array bump-bonded pixel-by-pixel to an application-specific integrated circuit. The in-pixel circuitry provides a 1,000,000:1 dynamic range within a single frame, allowing the direct electron beam to be imaged while still maintaining single electron sensitivity. A 1.1 kHz framing rate enables rapid data collection and minimizes sample drift distortions while scanning. By capturing the entire unsaturated diffraction pattern in scanning mode, one can simultaneously capture bright field, dark field, and phase contrast information, as well as being able to analyze the full scattering distribution, allowing true center of mass imaging. The scattering is recorded on an absolute scale, so that information such as local sample thickness can be directly determined. This paper describes the detector architecture, data acquisition system, and preliminary results from experiments with 80-200 keV electron beams.

Precision controlled atomic resolution scanning transmission electron microscopy using spiral scan pathways

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sang, Xiahan; Lupini, Andrew R.; Ding, Jilai

Atomic-resolution imaging in an aberration-corrected scanning transmission electron microscope (STEM) can enable direct correlation between atomic structure and materials functionality. The fast and precise control of the STEM probe is, however, challenging because the true beam location deviates from the assigned location depending on the properties of the deflectors. To reduce these deviations, i.e. image distortions, we use spiral scanning paths, allowing precise control of a sub-Å sized electron probe within an aberration-corrected STEM. Although spiral scanning avoids the sudden changes in the beam location (fly-back distortion) present in conventional raster scans, it is not distortion-free. “Archimedean” spirals, with amore » constant angular frequency within each scan, are used to determine the characteristic response at different frequencies. We then show that such characteristic functions can be used to correct image distortions present in more complicated constant linear velocity spirals, where the frequency varies within each scan. Through the combined application of constant linear velocity scanning and beam path corrections, spiral scan images are shown to exhibit less scan distortion than conventional raster scan images. The methodology presented here will be useful for in situ STEM imaging at higher temporal resolution and for imaging beam sensitive materials.« less

Precision controlled atomic resolution scanning transmission electron microscopy using spiral scan pathways

DOE PAGES

Sang, Xiahan; Lupini, Andrew R.; Ding, Jilai; ...

2017-03-08

Atomic-resolution imaging in an aberration-corrected scanning transmission electron microscope (STEM) can enable direct correlation between atomic structure and materials functionality. The fast and precise control of the STEM probe is, however, challenging because the true beam location deviates from the assigned location depending on the properties of the deflectors. To reduce these deviations, i.e. image distortions, we use spiral scanning paths, allowing precise control of a sub-Å sized electron probe within an aberration-corrected STEM. Although spiral scanning avoids the sudden changes in the beam location (fly-back distortion) present in conventional raster scans, it is not distortion-free. “Archimedean” spirals, with amore » constant angular frequency within each scan, are used to determine the characteristic response at different frequencies. We then show that such characteristic functions can be used to correct image distortions present in more complicated constant linear velocity spirals, where the frequency varies within each scan. Through the combined application of constant linear velocity scanning and beam path corrections, spiral scan images are shown to exhibit less scan distortion than conventional raster scan images. The methodology presented here will be useful for in situ STEM imaging at higher temporal resolution and for imaging beam sensitive materials.« less

Large area fabrication of plasmonic nanoparticle grating structure by conventional scanning electron microscope

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sudheer,, E-mail: sudheer@rrcat.gov.in; Tiwari, P.; Rai, V. N.

Plasmonic nanoparticle grating (PNG) structure of different periods has been fabricated by electron beam lithography using silver halide based transmission electron microscope film as a substrate. Conventional scanning electron microscope is used as a fabrication tool for electron beam lithography. Optical microscope and energy dispersive spectroscopy (EDS) have been used for its morphological and elemental characterization. Optical characterization is performed by UV-Vis absorption spectroscopic technique.

Note: Electron energy spectroscopy mapping of surface with scanning tunneling microscope.

PubMed

Li, Meng; Xu, Chunkai; Zhang, Panke; Li, Zhean; Chen, Xiangjun

2016-08-01

We report a novel scanning probe electron energy spectrometer (SPEES) which combines a double toroidal analyzer with a scanning tunneling microscope to achieve both topography imaging and electron energy spectroscopy mapping of surface in situ. The spatial resolution of spectroscopy mapping is determined to be better than 0.7 ± 0.2 μm at a tip sample distance of 7 μm. Meanwhile, the size of the field emission electron beam spot on the surface is also measured, and is about 3.6 ± 0.8 μm in diameter. This unambiguously demonstrates that the spatial resolution of SPEES technique can be much better than the size of the incident electron beam.

Development of Scanning Ultrafast Electron Microscope Capability.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Collins, Kimberlee Chiyoko; Talin, Albert Alec; Chandler, David W.

Modern semiconductor devices rely on the transport of minority charge carriers. Direct examination of minority carrier lifetimes in real devices with nanometer-scale features requires a measurement method with simultaneously high spatial and temporal resolutions. Achieving nanometer spatial resolutions at sub-nanosecond temporal resolution is possible with pump-probe methods that utilize electrons as probes. Recently, a stroboscopic scanning electron microscope was developed at Caltech, and used to study carrier transport across a Si p-n junction [ 1 , 2 , 3 ] . In this report, we detail our development of a prototype scanning ultrafast electron microscope system at Sandia National Laboratoriesmore » based on the original Caltech design. This effort represents Sandia's first exploration into ultrafast electron microscopy.« less

Analysis of the EBT3 Gafchromic film irradiated with 6 MV photons and 6 MeV electrons using reflective mode scanners.

PubMed

Farah, Nicolas; Francis, Ziad; Abboud, Marie

2014-09-01

We explore in our study the effects of electrons and X-rays irradiations on the newest version of the Gafchromic EBT3 film. Experiments are performed using the Varian "TrueBeam 1.6" medical accelerator delivering 6 MV X-ray photons and 6 MeV electron beams as desired. The main interest is to compare the responses of EBT3 films exposed to two separate beams of electrons and photons, for radiation doses ranging up to 500 cGy. The analysis is done on a flatbed EPSON 10000 XL scanner and cross checked on a HP Scanjet 4850 scanner. Both scanners are used in reflection mode taking into account landscape and portrait scanning positions. After thorough verifications, the reflective scanning method can be used on EBT3 as an economic alternative to the transmission method which was also one of the goals of this study. A comparison is also done between single scan configuration including all samples in a single A4 (HP) or A3 (EPSON) format area and multiple scan procedure where each sample is scanned separately on its own. The images analyses are done using the ImageJ software. Results show significant influence of the scanning configuration but no significant differences between electron and photon irradiations for both single and multiple scan configurations. In conclusion, the film provides a reliable relative dose measurement method for electrons and photons irradiations in the medical field applications. Copyright © 2014 Associazione Italiana di Fisica Medica. Published by Elsevier Ltd. All rights reserved.

Microstructure and corrosion behavior of porous coatings on titanium alloy by vacuum-brazed method.

PubMed

Lee, T M; Chang, E; Yen, C H

2006-05-01

The microstructural evolution and electrochemical characteristics of brazed porous-coated Ti-6Al-4V alloy were analyzed and compared with respect to the conventionally 1300 degrees C sintering method. The titanium filler metal of low-melting-point (934 degrees C) Ti-15Cu-15Ni was used to braze commercially pure (CP) titanium beads onto the substrate of Ti-6Al-4V alloy at 970 degrees C for 2 and 8 h. Optical microscopy, scanning and transmission electron microscopy, and X-ray diffractometry (XRD) were used to characterize the microstructure and phase of the brazed metal; also, the potentiostat was used for corrosion study. Experimental results indicate that the bead/substrate contact interface of the 970 degrees C brazed specimens show larger contact area and higher radius curvature in comparison with 1300 degrees C sintering method. The microstructure of brazed specimens shows the Widmanstätten structure in the brazed zone and equiaxed alpha plus intergranular beta in the Ti-6Al-4V substrate. The intermetallic Ti2Ni phase existing in the prior filler metal diminishes, while the Ti2Cu phase can be identified for the substrate at 970 for 2 h, but the latter phase decrease with time. In Hank's solution at 37 degrees C, the corrosion rates of the 1300 degrees C sintering and the 970 degrees C brazed samples are similar at corrosion potential (E(corr)) in potentiodynamic test, and the value of E(corr) for the brazed sample is noble to the sintering samples. The current densities of the brazed specimens do not exceed 100 microA/cm2 at 3.5 V (SCE). These results suggest that the vacuum-brazed method exhibits the potentiality to manufacture the porous-coated specimens for biomedical application. (c) 2005 Wiley Periodicals, Inc.

Dual UV irradiation-based metal oxide nanoparticles for enhanced antimicrobial activity in Escherichia coli and M13 bacteriophage

PubMed Central

Jin, Su-Eon; Hwang, Woochul; Lee, Hyo Jung; Jin, Hyo-Eon

2017-01-01

Metal oxide (MO) nanoparticles have been studied as nano-antibiotics due to their antimicrobial activities even in antibiotic-resistant microorganisms. We hypothesized that a hybrid system of dual UV irradiation and MO nanoparticles would have enhanced antimicrobial activities compared with UV or MO nanoparticles alone. In this study, nanoparticles of ZnO, ZnTiO3, MgO, and CuO were selected as model nanoparticles. A dual UV collimated beam device of UV-A and UV-C was developed depending upon the lamp divided by coating. Physicochemical properties of MO nanoparticles were determined using powder X-ray diffractometry (PXRD), Brunauer-Emmett-Teller analysis, and field emission-scanning electron microscopy with energy-dispersive X-ray spectroscopy. Atomic force microscopy with an electrostatic force microscopy mode was used to confirm the surface topology and electrostatic characteristics after dual UV irradiation. For antimicrobial activity test, MO nanoparticles under dual UV irradiation were applied to Escherichia coli and M13 bacteriophage (phage). The UV-A and UV-C showed differential intensities in the coated and uncoated areas (UV-A, coated = uncoated; UV-C, coated ≪ uncoated). MO nanoparticles showed sharp peaks in PXRD patterns, matched to pure materials. Their primary particle sizes were less than 100 nm with irregular shapes, which had an 8.6~25.6 m2/g of specific surface area with mesopores of 22~262 nm. The electrostatic properties of MO nanoparticles were modulated after UV irradiation. ZnO, MgO, and CuO nanoparticles, except ZnTiO3 nanoparticles, showed antibacterial effects on E. coli. Antimicrobial effects on E. coli and phages were also enhanced after cyclic exposure of dual UV and MO nanoparticle treatment using the uncoated area, except ZnO nanoparticles. Our results demonstrate that dual UV-MO nanoparticle hybrid system has a potential for disinfection. We anticipate that it can be developed as a next-generation disinfection system in pharmaceutical industries and water purification systems. PMID:29138562

Crystal doping aided by rapid expansion of supercritical solutions.

PubMed

Vemavarapu, Chandra; Mollan, Matthew J; Needham, Thomas E

2002-01-01

The purpose of this study was to test the utility of rapid expansion of supercritical solution (RESS) based cocrystallizations in inducing polymorph conversion and crystal disruption of chlorpropamide (CPD). CPD crystals were recrystallized by the RESS process utilizing supercritical carbon dioxide as the solvent. The supercritical region investigated for solute extraction ranged from 45 to 100 degrees C and 2000 to 8000 psi. While pure solute recrystallization formed stage I of these studies, stage II involved recrystallization of CPD in the presence of urea (model impurity). The composition, morphology, and crystallinity of the particles thus produced were characterized utilizing techniques such as microscopy, thermal analysis, x-ray powder diffractometry, and high-performance liquid chromatography. Also, comparative evaluation between RESS and evaporative crystallization from liquid solvents was performed. RESS recrystallizations of commercially available CPD (form A) resulted in polymorph conversion to metastable forms C and V, depending on the temperature and pressure of the recrystallizing solvent. Cocrystallization studies revealed the formation of eutectic mixtures and solid solutions of CPD + urea. Formation of the solid solutions resulted in the crystal disruption of CPD and subsequent amorphous conversion at urea levels higher than 40% wt/wt. Consistent with these results were the reductions in melting point (up to 9 degrees C) and in the DeltaH(f) values of CPD (up to 50%). Scanning electron microscopy revealed a particle size reduction of up to an order of magnitude upon RESS processing. Unlike RESS, recrystallizations from liquid organic solvents lacked the ability to affect polymorphic conversions. Also, the incorporation of urea into the lattice of CPD was found to be inadequate. In providing the ability to control both the particle and crystal morphologies of active pharmaceutical ingredients, RESS proved potentially advantageous to crystal engineering. Rapid crystallization kinetics were found vital in making RESS-based doping superior to conventional solvent-based cocrystallizations.

Preparation of Superparamagnetic Zn0.5Mn0.5Fe2O4 Particle by Coprecipitation-Sonochemical Method for Radar Absorbing Material

NASA Astrophysics Data System (ADS)

Taufiq, A.; Bahtiar, S.; Sunaryono; Hidayat, N.; Hidayat, A.; Mufti, N.; Diantoro, M.; Fuad, A.; Munasir; Rahmawati, R.; Adi, W. A.; Pratapa, S.; Darminto

2017-05-01

One of many applications of spinel ferrite nanoparticles is related to their performance as radar absorbing materials. In this work, we report developing synthesis method through combined coprecipitation-sonochemical routes in preparing Zn0.5Mn0.5Fe2O4 nanoparticle from iron sand in Indonesia as a vital raw material. The structure, size, morphology, and elements of the Zn0.5Mn0.5Fe2O4 nanoparticle were investigated via X-Ray diffractometry and Transmission/Scanning Electron Microscopy (TEM/SEM) combining Energy Dispersive Spectroscopy (EDS). The magnetic properties of the Zn0.5Mn0.5Fe2O4 nanoparticle were characterized by using Vibrating Sample Magnetometer (VSM). Furthermore, the reflection loss character of the Zn0.5Mn0.5Fe2O4 nanoparticle was determined via Vector Network Analyzer (VNA). From the qualitative and quantitative analysis of the XRD data, it can be identified that the Zn0.5Mn0.5Fe2O4 particle formed a spinel cubic structure in a single phase with the lattice parameter of approximately 8.401 Å. It is known from the TEM image that the Zn0.5Mn0.5Fe2O4 particle had a size of about 9.7 nm and tended to agglomerate. Furthermore, the data analysis of the M(H) curve presented that the Zn0.5Mn0.5Fe2O4 nanoparticle has a superparamagnetic behavior with the saturation magnetization of approximately 43 emu/g. Finally, the data analysis of the reflection loss as a function of frequency showed that the Zn0.5Mn0.5Fe2O4 nanoparticle performs as a radar absorbing material with the absorption performance of approximately -11.0 dB at the frequency of 10.8 GHz

Oxidation characteristics of porous-nickel prepared by powder metallurgy and cast-nickel at 1273 K in air for total oxidation time of 100 h.

PubMed

Mohamed, Lamiaa Z; Ghanem, Wafaa A; El Kady, Omayma A; Lotfy, Mohamed M; Ahmed, Hafiz A; Elrefaie, Fawzi A

2017-11-01

The oxidation behavior of two types of inhomogeneous nickel was investigated in air at 1273 K for a total oxidation time of 100 h. The two types were porous sintered-nickel and microstructurally inhomogeneous cast-nickel. The porous-nickel samples were fabricated by compacting Ni powder followed by sintering in vacuum at 1473 K for 2 h. The oxidation kinetics of the samples was determined gravimetrically. The topography and the cross-section microstructure of each oxidized sample were observed using optical and scanning electron microscopy. X-ray diffractometry and X-ray energy dispersive analysis were used to determine the nature of the formed oxide phases. The kinetic results revealed that the porous-nickel samples had higher trend for irreproducibility. The average oxidation rate for porous- and cast-nickel samples was initially rapid, and then decreased gradually to become linear. Linear rate constants were 5.5 × 10 -8  g/cm 2  s and 3.4 × 10 -8  g/cm 2  s for the porous- and cast-nickel samples, respectively. Initially a single-porous non-adherent NiO layer was noticed on the porous- and cast-nickel samples. After a longer time of oxidation, a non-adherent duplex NiO scale was formed. The two layers of the duplex scales were different in color. NiO particles were observed in most of the pores of the porous-nickel samples. Finally, the linear oxidation kinetics and the formation of porous non-adherent duplex oxide scales on the inhomogeneous nickel substrates demonstrated that the addition of new layers of NiO occurred at the scale/metal interface due to the thermodynamically possible reaction between Ni and the molecular oxygen migrating inwardly.

Dissolution of Gold and Silver with Ammonium Thiosulfate from Mangano-Argentiferous Ores Treated in Acid-Reductive Conditions

NASA Astrophysics Data System (ADS)

Tiburcio Munive, G.; Encinas Romero, M. A.; Vazquez, V. M.; Valenzuela García, J. L.; Valenzuela Soto, A.; Coronado Lopez, J. H.

2017-10-01

A novel process was studied to extract economic metals from refractory ores that are difficult to leach with cyanide and ammonium thiosulfate, such as the well-known mangano argentiferous minerals, which are minerals of manganese, iron, and silver. The mineral under consideration originates from the tailings of the Monte del Favor, Hostotipaquillo Jalisco, Mexico. The sample was characterized by x-ray diffractometry, atomic absorption spectroscopy, scanning electron microscopy, and microanalysis by energy-dispersive x-ray spectroscopy. First, the material was passed through a 100-mesh screen, and then it was subjected to reductive leaching by varying the liquid-solid ( L/ S) ratio from 2:1 to 10:1 (observations were carried out at a ratio of 5:1, which yielded higher extraction of manganese). With H2SO4 and Na2SO3 as the reducing agents, manganese extraction of up to 96.05% was achieved during the first 3 h with a mineral head of manganese 3.58%, acid consumption of 90.74 g/L, and sulfite consumption of 25.8 g/L. The mineral was then filtered and proceeded to neutralize the acidity, reaching a pH of 8 with calcium hydroxide. Then, the material was subjected to a new leaching of gold and silver values with ammonium thiosulfate. The L/ S ratio was varied (1:1, 2:1, 3:1, 4:1), and the contact time and the concentration of ammonium thiosulfate was investigated, while controlling the pH using Ca(OH)2 and NH4Cl. An L/ S ratio of 2:1 showed the best extraction of silver (97.06%) and gold (86.66%), and the thiosulfate consumption was 10.36 g/L. The mineral head of gold and silver was 0.30 g/ton and 310 g/ton, respectively. The pH was maintained between 9.8 and 8.4, such that ammonium thiosulfate stabilized with lime, and ammonium chloride did not suffer any decomposition.

The adsorptive behavior of albumin and lysozyme proteins on rod-shaped and plate-shaped hydroxyapatite.

PubMed

Ozeki, K; Hoshino, T; Aoki, H; Masuzawa, T

2013-01-01

The adsorption behavior of albumin (BSA) and lysozyme (LSZ) on rod-shaped and plate-shaped hydroxyapatite (HA) was investigated to evaluate the influence of crystal orientation and morphology on the selective protein adsorption of HA. The rod-shaped HA was prepared by hydrothermal treatment from β-tricalcium phosphate (β-TCP) in H3PO4 solution (pH 2.0 and 4.0 for HA-pH 2.0 and HA-pH 4.0). The plate-shaped HA was synthesized by hydrolysis of CaHPO4-2H2O (DCPD) in NaOH solution at 40°C and 80°C (HA-40°C and HA-80°C). The synthesized HA was characterized using scanning electron microscopy (SEM) and X-ray diffractometry (XRD). HA-pH 2.0 and HA-pH 4.0 produced rod-shaped crystals that were highly oriented to the a-face plane, whereas HA-40°C and HA-80°C showed a plate-like shape and a c-face preferred orientation. The peak intensity ratio I(300)/I(002) (a/c intensity ratio) from the XRD patterns increased in the following order: HA-80°C, HA-40°C, HA-pH 2.0 and HA-pH 4.0. It also increased as the Ca/P ratio decreased. The amount of adsorbed BSA increased in the following order: HA-pH 4.0, HA-pH 2.0, HA-40°C and HA-80°C. The amount of adsorbed LSZ on HA increased in the following order--HA-pH 2.0, HA-pH 4.0, HA-40°C and HA-80°C--with a corresponding decrease in the a/c intensity ratio. The BSA/LSA adsorption ratio increased with the a/c intensity ratio in the range of 3.3-8.9, and the BSA and LSZ were selectively adsorbed on HA, depending on the crystal shape.

Vulnerability of the paper Nautilus (Argonauta nodosa) shell to a climate-change ocean: potential for extinction by dissolution.

PubMed

Wolfe, Kennedy; Smith, Abigail M; Trimby, Patrick; Byrne, Maria

2012-10-01

Shell calcification in argonauts is unique. Only females of these cephalopods construct the paper nautilus shell, which is used as a brood chamber for developing embryos in the pelagic realm. As one of the thinnest (225 μm) known adult mollusc shells, and lacking an outer protective periostracum-like cover, this shell may be susceptible to dissolution as the ocean warms and decreases in pH. Vulnerability of the A. nodosa shell was investigated through immersion of shell fragments in multifactorial experiments of control (19 °C/pH 8.1; pCO(2) 419; Ω(Ca) = 4.23) and near-future conditions (24 °C/pH 7.8-7.6; pCO(2) 932-1525; Ω(Ca) = 2.72-1.55) for 14 days. More extreme pH treatments (pH 7.4-7.2; pCO(2) 2454-3882; Ω(Ca) = 1.20-0.67) were used to assess tipping points in shell dissolution. X-ray diffractometry revealed no change in mineralogy between untreated and treated shells. Reduced shell weight due to dissolution was evident in shells incubated at pH 7.8 (projected for 2070) after 14 days at control temperature, with increased dissolution in warmer and lower pH treatments. The greatest dissolution was recorded at 24 °C (projected for local waters by 2100) compared to control temperature across all low-pH treatments. Scanning electron microscopy revealed dissolution and etching of shell mineral in experimental treatments. In the absence of compensatory mineralization, the uncovered female brood chamber will be susceptible to dissolution as ocean pH decreases. Since the shell was a crucial adaptation for the evolution of the argonauts' holopelagic existence, persistence of A. nodosa may be compromised by shell dissolution in an ocean-change world.

Dual UV irradiation-based metal oxide nanoparticles for enhanced antimicrobial activity in Escherichia coli and M13 bacteriophage.

PubMed

Jin, Su-Eon; Hwang, Woochul; Lee, Hyo Jung; Jin, Hyo-Eon

2017-01-01

Metal oxide (MO) nanoparticles have been studied as nano-antibiotics due to their antimicrobial activities even in antibiotic-resistant microorganisms. We hypothesized that a hybrid system of dual UV irradiation and MO nanoparticles would have enhanced antimicrobial activities compared with UV or MO nanoparticles alone. In this study, nanoparticles of ZnO, ZnTiO 3 , MgO, and CuO were selected as model nanoparticles. A dual UV collimated beam device of UV-A and UV-C was developed depending upon the lamp divided by coating. Physicochemical properties of MO nanoparticles were determined using powder X-ray diffractometry (PXRD), Brunauer-Emmett-Teller analysis, and field emission-scanning electron microscopy with energy-dispersive X-ray spectroscopy. Atomic force microscopy with an electrostatic force microscopy mode was used to confirm the surface topology and electrostatic characteristics after dual UV irradiation. For antimicrobial activity test, MO nanoparticles under dual UV irradiation were applied to Escherichia coli and M13 bacteriophage (phage). The UV-A and UV-C showed differential intensities in the coated and uncoated areas (UV-A, coated = uncoated; UV-C, coated ≪ uncoated). MO nanoparticles showed sharp peaks in PXRD patterns, matched to pure materials. Their primary particle sizes were less than 100 nm with irregular shapes, which had an 8.6~25.6 m 2 /g of specific surface area with mesopores of 22~262 nm. The electrostatic properties of MO nanoparticles were modulated after UV irradiation. ZnO, MgO, and CuO nanoparticles, except ZnTiO 3 nanoparticles, showed antibacterial effects on E. coli . Antimicrobial effects on E. coli and phages were also enhanced after cyclic exposure of dual UV and MO nanoparticle treatment using the uncoated area, except ZnO nanoparticles. Our results demonstrate that dual UV-MO nanoparticle hybrid system has a potential for disinfection. We anticipate that it can be developed as a next-generation disinfection system in pharmaceutical industries and water purification systems.

Osteointegration of PLGA implants with nanostructured or microsized β-TCP particles in a minipig model.

PubMed

Kulkova, Julia; Moritz, Niko; Suokas, Esa O; Strandberg, Niko; Leino, Kari A; Laitio, Timo T; Aro, Hannu T

2014-12-01

Bioresorbable suture anchors and interference screws have certain benefits over equivalent titanium-alloy implants. However, there is a need for compositional improvement of currently used bioresorbable implants. We hypothesized that implants made of poly(l-lactide-co-glycolide) (PLGA) compounded with nanostructured particles of beta-tricalcium phosphate (β-TCP) would induce stronger osteointegration than implants made of PLGA compounded with microsized β-TCP particles. The experimental nanostructured self-reinforced PLGA (85L:15G)/β-TCP composite was made by high-energy ball-milling. Self-reinforced microsized PLGA (95L:5G)/β-TCP composite was prepared by melt-compounding. The composites were characterized by gas chromatography, Ubbelohde viscometry, scanning electron microscopy, laser diffractometry, and standard mechanical tests. Four groups of implants were prepared for the controlled laboratory study employing a minipig animal model. Implants in the first two groups were prepared from nanostructured and microsized PLGA/β-TCP composites respectively. Microroughened titanium-alloy (Ti6Al4V) implants served as positive intra-animal control, and pure PLGA implants as negative control. Cone-shaped implants were inserted in a random order unilaterally in the anterior cortex of the femoral shaft. Eight weeks after surgery, the mechanical strength of osteointegration of the implants was measured by a push-out test. The quality of new bone surrounding the implant was assessed by microcomputed tomography and histology. Implants made of nanostructured PLGA/β-TCP composite did not show improved mechanical osteointegration compared with the implants made of microsized PLGA/β-TCP composite. In the intra-animal comparison, the push-out force of two PLGA/β-TCP composites was 35-60% of that obtained with Ti6Al4V implants. The implant materials did not result in distinct differences in quality of new bone surrounding the implant. Copyright © 2014 Elsevier Ltd. All rights reserved.

Synthesis and Characterization of Cu- and Co-Doped Bi4V2O11 for Intermediate-Temperature Solid Oxide Fuel Cell Electrolytes by Carbonate Coprecipitation

NASA Astrophysics Data System (ADS)

Lee, Jin Goo; Yoon, Hyon Hee

2011-01-01

Bi2MexV1-xO5.5-3x/2 (Me = Cu; 0≤x≤0.2) powders were prepared by the ammonium carbonate coprecipitation method. The starting salts were bismuth nitrate, copper nitrate, cobalt nitrate, and vanadium sulphate. The thermal decomposition of Bi2MexV1-xO5.5-3x/2 precursors was completed at about 500 °C. The crystallite structure, surface morphology, and ionic conductivity of the prepared powders and pellets were examined using X-ray diffractometry, field emission scanning electron microscopy, and an impedance analyzer, respectively. The average particle sizes of the Bi2Cu0.1V0.9O5.35 and Bi2Co0.1V0.9O5.35 powders were 10-50 nm. The tetragonal structure (γ-phase) appeared at sintering temperatures higher than 700 °C and the peak intensity increased at higher sintering temperatures. The ionic conductivities of the Bi2Cu0.1V0.9O5.35 and Bi2Co0.1V0.9O5.35 pellets sintered at 800 °C showed the highest values of 6.8×10-2 S cm-1 at 700 °C and 9.1×10-2 S cm-1 at 700 °C, respectively. The optimum concentration of the Cu and Co dopants in Bi2MexV1-xO5.5-3x/2 was determined to be 0.1. The results of this study demonstrated that the ammonium carbonate coprecipitation process could be used as an economical method for the preparation of Bi2MexV1-xO5.5-3x/2 electrolytes for intermediate-temperature solid oxide fuel cells.

Hair dye-incorporated poly-γ-glutamic acid/glycol chitosan nanoparticles based on ion-complex formation.

PubMed

Lee, Hye-Young; Jeong, Young-Il; Choi, Ki-Choon

2011-01-01

p-Phenylenediamine (PDA) or its related chemicals are used more extensively than oxidative hair dyes. However, permanent hair dyes such as PDA are known to have potent contact allergy reactions in humans, and severe allergic reactions are problematic. PDA-incorporated nanoparticles were prepared based on ion-complex formation between the cationic groups of PDA and the anionic groups of poly(γ-glutamic acid) (PGA). To reinforce PDA/PGA ion complexes, glycol chitosan (GC) was added. PDA-incorporated nanoparticles were characterized using field-emission scanning electron microscopy, Fourier- transform infrared (FT-IR) spectroscopy, dynamic light scattering, and powder X-ray diffractometry (XRD). Nanoparticles were formed by ion-complex formation between the amine groups of PDA and the carboxyl groups of PGA. PDA-incorporated nanoparticles are small in size (<100 nm), and morphological observations showed spherical shapes. FT-IR spectra results showed that the carboxylic acid peak of PGA decreased with increasing PDA content, indicating that the ion complexes were formed between the carboxyl groups of PGA and the amine groups of PDA. Furthermore, the intrinsic peak of the carboxyl groups of PGA was also decreased by the addition of GC. Intrinsic crystalline peaks of PDA were observed by XRD. This crystalline peak of PDA was completely nonexistent when nanoparticles were formed by ion complex between PDA, PGA, and GC, indicating that PDA was complexed with PGA and no free drug existed in the formulation. During the drug-release experiment, an initial burst release of PDA was observed, and then PDA was continuously released over 1 week. Cytotoxicity testing against HaCaT human skin keratinocyte cells showed PDA-incorporated nanoparticles had lower toxicity than PDA itself. Furthermore, PDA-incorporated nanoparticles showed reduced apoptosis and necrosis reaction at HaCaT cells. The authors suggest that these microparticles are ideal candidates for a vehicle for decreasing side effects of hair dye.

Hydrophilicity, Viscoelastic, and Physicochemical Properties Variations in Dental Bone Grafting Substitutes.

PubMed

Trajkovski, Branko; Jaunich, Matthias; Müller, Wolf-Dieter; Beuer, Florian; Zafiropoulos, Gregory-George; Houshmand, Alireza

2018-01-30

The indication-oriented Dental Bone Graft Substitutes (DBGS) selection, the correct bone defects classification, and appropriate treatment planning are very crucial for obtaining successful clinical results. However, hydrophilic, viscoelastic, and physicochemical properties' influence on the DBGS regenerative potential has poorly been studied. For that reason, we investigated the dimensional changes and molecular mobility by Dynamic Mechanical Analysis (DMA) of xenograft (cerabone ® ), synthetic (maxresorb ® ), and allograft (maxgraft ® , Puros ® ) blocks in a wet and dry state. While no significant differences could be seen in dry state, cerabone ® and maxresorb ® blocks showed a slight height decrease in wet state, whereas both maxgraft ® and Puros ® had an almost identical height increase. In addition, cerabone ® and maxresorb ® blocks remained highly rigid and their damping behaviour was not influenced by the water. On the other hand, both maxgraft ® and Puros ® had a strong increase in their molecular mobility with different damping behaviour profiles during the wet state. A high-speed microscopical imaging system was used to analyze the hydrophilicity in several naturally derived (cerabone ® , Bio-Oss ® , NuOss ® , SIC ® nature graft) and synthetic DBGS granules (maxresorb ® , BoneCeramic ® , NanoBone ® , Ceros ® ). The highest level of hydrophilicity was detected in cerabone ® and maxresorb ® , while Bio-Oss ® and BoneCeramic ® had the lowest level of hydrophilicity among both naturally derived and synthetic DBGS groups. Deviations among the DBGS were also addressed via physicochemical differences recorded by Micro Computed Tomography, Scanning Electron Microscopy, Fourier Transform Infrared Spectroscopy, X-ray powder Diffractometry, and Thermogravimetric Analysis. Such DBGS variations could influence the volume stability at the grafting site, handling as well as the speed of vascularization and bone regeneration. Therefore, this study initiates a new insight into the DBGS differences and their importance for successful clinical results.

Hydrophilicity, Viscoelastic, and Physicochemical Properties Variations in Dental Bone Grafting Substitutes

PubMed Central

Müller, Wolf-Dieter; Beuer, Florian; Zafiropoulos, Gregory-George; Houshmand, Alireza

2018-01-01

The indication-oriented Dental Bone Graft Substitutes (DBGS) selection, the correct bone defects classification, and appropriate treatment planning are very crucial for obtaining successful clinical results. However, hydrophilic, viscoelastic, and physicochemical properties’ influence on the DBGS regenerative potential has poorly been studied. For that reason, we investigated the dimensional changes and molecular mobility by Dynamic Mechanical Analysis (DMA) of xenograft (cerabone®), synthetic (maxresorb®), and allograft (maxgraft®, Puros®) blocks in a wet and dry state. While no significant differences could be seen in dry state, cerabone® and maxresorb® blocks showed a slight height decrease in wet state, whereas both maxgraft® and Puros® had an almost identical height increase. In addition, cerabone® and maxresorb® blocks remained highly rigid and their damping behaviour was not influenced by the water. On the other hand, both maxgraft® and Puros® had a strong increase in their molecular mobility with different damping behaviour profiles during the wet state. A high-speed microscopical imaging system was used to analyze the hydrophilicity in several naturally derived (cerabone®, Bio-Oss®, NuOss®, SIC® nature graft) and synthetic DBGS granules (maxresorb®, BoneCeramic®, NanoBone®, Ceros®). The highest level of hydrophilicity was detected in cerabone® and maxresorb®, while Bio-Oss® and BoneCeramic® had the lowest level of hydrophilicity among both naturally derived and synthetic DBGS groups. Deviations among the DBGS were also addressed via physicochemical differences recorded by Micro Computed Tomography, Scanning Electron Microscopy, Fourier Transform Infrared Spectroscopy, X-ray powder Diffractometry, and Thermogravimetric Analysis. Such DBGS variations could influence the volume stability at the grafting site, handling as well as the speed of vascularization and bone regeneration. Therefore, this study initiates a new insight into the DBGS differences and their importance for successful clinical results. PMID:29385747

Writing silica structures in liquid with scanning transmission electron microscopy.

PubMed

van de Put, Marcel W P; Carcouët, Camille C M C; Bomans, Paul H H; Friedrich, Heiner; de Jonge, Niels; Sommerdijk, Nico A J M

2015-02-04

Silica nanoparticles are imaged in solution with scanning transmission electron microscopy (STEM) using a liquid cell with silicon nitride (SiN) membrane windows. The STEM images reveal that silica structures are deposited in well-defined patches on the upper SiN membranes upon electron beam irradiation. The thickness of the deposits is linear with the applied electron dose. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) demonstrate that the deposited patches are a result of the merging of the original 20 nm-diameter nanoparticles, and that the related surface roughness depends on the electron dose rate used. Using this approach, sub-micrometer scale structures are written on the SiN in liquid by controlling the electron exposure as function of the lateral position. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Examination of Surveyor 3 parts with the scanning electron microscope and electron microprobe

NASA Technical Reports Server (NTRS)

Chodos, A. A.; Devaney, J. R.; Evens, K. C.

1972-01-01

Two screws and two washers, several small chips of tubing, and a fiber removed from a third screw were examined with the scanning electron microscope and the electron microprobe. The purpose of the examination was to determine the nature of the material on the surface of these samples and to search for the presence of meteoritic material.

Observations on the Role of Hydrogen in Facet Formation in Near-alpha Titanium (Preprint)

DTIC Science & Technology

2011-05-01

using quantitative tilt fractography and electron backscatter diffraction while facet topography was examined using ultra high resolution scanning...quantitative tilt fractography and electron backscatter diffraction while facet topography was examined using ultra high resolution scanning electron...tilt fractography / electron backscatter diffraction (EBSD) technique in which both the crystallographic orientation of the fractured grain and the

Nondestructive determination of the depth of planar p-n junctions by scanning electron microscopy

NASA Technical Reports Server (NTRS)

Chi, J.-Y.; Gatos, H. C.

1977-01-01

A method was developed for measuring nondestructively the depth of planar p-n junctions in simple devices as well as in integrated-circuit structures with the electron-beam induced current (EBIC) by scanning parallel to the junction in a scanning electron microscope (SEM). The results were found to be in good agreement with those obtained by the commonly used destructive method of lapping at an angle to the junction and staining to reveal the junction.

Use of scanning electron microscopy and microanalysis to determine chloride content of concrete and raw materials.

DOT National Transportation Integrated Search

2013-02-01

Standard sample sets of cement and mortar formulations with known levels of Cl as well as concrete samples subject to Cl diffusion were all prepared for and analyzed with scanning electron microscopy (SEM) and electron microprobe (EPMA). Using x-ray ...

Electronically-Scanned Pressure Sensors

NASA Technical Reports Server (NTRS)

Coe, C. F.; Parra, G. T.; Kauffman, R. C.

1984-01-01

Sensors not pneumatically switched. Electronic pressure-transducer scanning system constructed in modular form. Pressure transducer modules and analog to digital converter module small enough to fit within cavities of average-sized wind-tunnel models. All switching done electronically. Temperature controlled environment maintained within sensor modules so accuracy maintained while ambient temperature varies.

41 CFR 301-71.201 - What are the reviewing official's responsibilities?

Code of Federal Regulations, 2013 CFR

2013-07-01

... 41 Public Contracts and Property Management 4 2013-07-01 2012-07-01 true What are the reviewing official's responsibilities? 301-71.201 Section 301-71.201 Public Contracts and Property Management Federal... implements electronic scanning, the electronic travel claim includes scanned electronic images of such...

41 CFR 301-71.201 - What are the reviewing official's responsibilities?

Code of Federal Regulations, 2014 CFR

2014-07-01

... 41 Public Contracts and Property Management 4 2014-07-01 2014-07-01 false What are the reviewing official's responsibilities? 301-71.201 Section 301-71.201 Public Contracts and Property Management Federal... implements electronic scanning, the electronic travel claim includes scanned electronic images of such...

41 CFR 301-71.201 - What are the reviewing official's responsibilities?

Code of Federal Regulations, 2012 CFR

2012-07-01

... 41 Public Contracts and Property Management 4 2012-07-01 2012-07-01 false What are the reviewing official's responsibilities? 301-71.201 Section 301-71.201 Public Contracts and Property Management Federal... implements electronic scanning, the electronic travel claim includes scanned electronic images of such...

41 CFR 301-71.201 - What are the reviewing official's responsibilities?

Code of Federal Regulations, 2011 CFR

2011-07-01

... 41 Public Contracts and Property Management 4 2011-07-01 2011-07-01 false What are the reviewing official's responsibilities? 301-71.201 Section 301-71.201 Public Contracts and Property Management Federal... implements electronic scanning, the electronic travel claim includes scanned electronic images of such...

Chemical mapping and quantification at the atomic scale by scanning transmission electron microscopy.

PubMed

Chu, Ming-Wen; Chen, Cheng Hsuan

2013-06-25

With innovative modern material-growth methods, a broad spectrum of fascinating materials with reduced dimensions-ranging from single-atom catalysts, nanoplasmonic and nanophotonic materials to two-dimensional heterostructural interfaces-is continually emerging and extending the new frontiers of materials research. A persistent central challenge in this grand scientific context has been the detailed characterization of the individual objects in these materials with the highest spatial resolution, a problem prompting the need for experimental techniques that integrate both microscopic and spectroscopic capabilities. To date, several representative microscopy-spectroscopy combinations have become available, such as scanning tunneling microscopy, tip-enhanced scanning optical microscopy, atom probe tomography, scanning transmission X-ray microscopy, and scanning transmission electron microscopy (STEM). Among these tools, STEM boasts unique chemical and electronic sensitivity at unparalleled resolution. In this Perspective, we elucidate the advances in STEM and chemical mapping applications at the atomic scale by energy-dispersive X-ray spectroscopy and electron energy loss spectroscopy with a focus on the ultimate challenge of chemical quantification with atomic accuracy.

Publications - GMC 357 | Alaska Division of Geological & Geophysical

Science.gov Websites

DGGS GMC 357 Publication Details Title: Thin Section and Scanning Electron Microscopy summary Laboratories, Inc., 2008, Thin Section and Scanning Electron Microscopy summary photographs from plugs taken

Microcircuit testing and fabrication, using scanning electron microscopes

NASA Technical Reports Server (NTRS)

Nicolas, D. P.

1975-01-01

Scanning electron microscopes are used to determine both user-induced damages and manufacturing defects subtle enough to be missed by conventional light microscopy. Method offers greater depth of field and increased working distances.

Towards the low-dose characterization of beam sensitive nanostructures via implementation of sparse image acquisition in scanning transmission electron microscopy

NASA Astrophysics Data System (ADS)

Hwang, Sunghwan; Han, Chang Wan; Venkatakrishnan, Singanallur V.; Bouman, Charles A.; Ortalan, Volkan

2017-04-01

Scanning transmission electron microscopy (STEM) has been successfully utilized to investigate atomic structure and chemistry of materials with atomic resolution. However, STEM’s focused electron probe with a high current density causes the electron beam damages including radiolysis and knock-on damage when the focused probe is exposed onto the electron-beam sensitive materials. Therefore, it is highly desirable to decrease the electron dose used in STEM for the investigation of biological/organic molecules, soft materials and nanomaterials in general. With the recent emergence of novel sparse signal processing theories, such as compressive sensing and model-based iterative reconstruction, possibilities of operating STEM under a sparse acquisition scheme to reduce the electron dose have been opened up. In this paper, we report our recent approach to implement a sparse acquisition in STEM mode executed by a random sparse-scan and a signal processing algorithm called model-based iterative reconstruction (MBIR). In this method, a small portion, such as 5% of randomly chosen unit sampling areas (i.e. electron probe positions), which corresponds to pixels of a STEM image, within the region of interest (ROI) of the specimen are scanned with an electron probe to obtain a sparse image. Sparse images are then reconstructed using the MBIR inpainting algorithm to produce an image of the specimen at the original resolution that is consistent with an image obtained using conventional scanning methods. Experimental results for down to 5% sampling show consistency with the full STEM image acquired by the conventional scanning method. Although, practical limitations of the conventional STEM instruments, such as internal delays of the STEM control electronics and the continuous electron gun emission, currently hinder to achieve the full potential of the sparse acquisition STEM in realizing the low dose imaging condition required for the investigation of beam-sensitive materials, the results obtained in our experiments demonstrate the sparse acquisition STEM imaging is potentially capable of reducing the electron dose by at least 20 times expanding the frontiers of our characterization capabilities for investigation of biological/organic molecules, polymers, soft materials and nanostructures in general.

Imaging of high-angle annular dark-field scanning transmission electron microscopy and observations of GaN-based violet laser diodes.

PubMed

Shiojiri, M; Saijo, H

2006-09-01

The first part of this paper is devoted to physics, to explain high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) imaging and to interpret why HAADF-STEM imaging is incoherent, instructing a strict definition of interference and coherence of electron waves. Next, we present our recent investigations of InGaN/GaN multiple quantum wells and AlGaN/GaN strained-layer superlattice claddings in GaN-based violet laser diodes, which have been performed by HAADF-STEM and high-resolution field-emission gun scanning electron microscopy.

Pluronic lecithin organogel as a topical drug delivery system.

PubMed

Pandey, Mohit; Belgamwar, Veena; Gattani, Surendra; Surana, Sanjay; Tekade, Avinash

2010-01-01

The objective of this study was to formulate and evaluate the pluronic lecithin organogel containing flurbiprofen for topical application. Different formulations of pluronic lecithin organogels were prepared by using pluronic F127, lecithin, flurbiprofen, isopropyl palmitate, water, sorbic acid, and potassium sorbate. To study the in vitro potential of these formulations, permeation studies were performed with Keshary-Chien diffusion cells. The results of the in vitro permeation studies found that release of flurbiprofen from dialysis membrane-70 was more than excised dorsal rat skin. Gelation temperature study was carried out to determine the temperature where sol-gel transformation takes place. The viscosities of different formulations were determined by using Brookfield Viscometer at 25°C, the viscosity of formulations increases as the lecithin concentration increases. Also the formulations were tested for appearance and feel psychorheologically, pH, and drug content. Interactions between the components of the gel have been investigated by differential scanning calorimetry and X-ray powder diffractometry. The optimized formulation subjected to differential scanning calorimetry shows no drug-polymer interaction. To investigate the in vivo performance of the formulations, a carrageenan-induced rat paw edema model and skin irritation study was used. The stability studies and freeze-thaw thermal cyclic test were carried out, showing no phase separation of gel, and representing gel stability. Statistical analysis of the data of animal study (anti-inflammatory activity) was done by using one way analysis of variance (ANOVA) followed by Dunnett's test. The formulation shows a statistically significant anti-inflammatory activity and is non-irritant to skin.

Scanning electron microscope observation of dislocations in semiconductor and metal materials.

PubMed

Kuwano, Noriyuki; Itakura, Masaru; Nagatomo, Yoshiyuki; Tachibana, Shigeaki

2010-08-01

Scanning electron microscope (SEM) image contrasts have been investigated for dislocations in semiconductor and metal materials. It is revealed that single dislocations can be observed in a high contrast in SEM images formed by backscattered electrons (BSE) under the condition of a normal configuration of SEM. The BSE images of dislocations were compared with those of the transmission electron microscope and scanning transmission electron microscope (STEM) and the dependence of BSE image contrast on the tilting of specimen was examined to discuss the origin of image contrast. From the experimental results, it is concluded that the BSE images of single dislocations are attributed to the diffraction effect and related with high-angle dark-field images of STEM.

Attainment of 40.5 pm spatial resolution using 300 kV scanning transmission electron microscope equipped with fifth-order aberration corrector.

PubMed

Morishita, Shigeyuki; Ishikawa, Ryo; Kohno, Yuji; Sawada, Hidetaka; Shibata, Naoya; Ikuhara, Yuichi

2018-02-01

The achievement of a fine electron probe for high-resolution imaging in scanning transmission electron microscopy requires technological developments, especially in electron optics. For this purpose, we developed a microscope with a fifth-order aberration corrector that operates at 300 kV. The contrast flat region in an experimental Ronchigram, which indicates the aberration-free angle, was expanded to 70 mrad. By using a probe with convergence angle of 40 mrad in the scanning transmission electron microscope at 300 kV, we attained the spatial resolution of 40.5 pm, which is the projected interatomic distance between Ga-Ga atomic columns of GaN observed along [212] direction.

Note: Electron energy spectroscopy mapping of surface with scanning tunneling microscope

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Meng; Xu, Chunkai, E-mail: xuck@ustc.edu.cn, E-mail: xjun@ustc.edu.cn; Zhang, Panke

We report a novel scanning probe electron energy spectrometer (SPEES) which combines a double toroidal analyzer with a scanning tunneling microscope to achieve both topography imaging and electron energy spectroscopy mapping of surface in situ. The spatial resolution of spectroscopy mapping is determined to be better than 0.7 ± 0.2 μm at a tip sample distance of 7 μm. Meanwhile, the size of the field emission electron beam spot on the surface is also measured, and is about 3.6 ± 0.8 μm in diameter. This unambiguously demonstrates that the spatial resolution of SPEES technique can be much better than themore » size of the incident electron beam.« less

Measurement of Strain and Stress Distributions in Structural Materials by Electron Moiré Method

NASA Astrophysics Data System (ADS)

Kishimoto, Satoshi; Xing, Yougming; Tanaka, Yoshihisa; Kagawa, Yutaka

A method for measuring the strain and stress distributions in structural materials has been introduced. Fine model grids were fabricated by electron beam lithography, and an electron beam scan by a scanning electron microscope (SEM) was used as the master grid. Exposure of the electron beam scan onto the model grid in an SEM produced the electron beam moiré fringes of bright and dark parts caused by the different amounts of the secondary electrons per a primary electron. For demonstration, the micro-creep deformation of pure copper was observed. The creep strain distribution and the grain boundary sliding were analyzed. The residual strain and stress at the interface between a fiber and a matrix of a fiber reinforced plastic (FRP) were measured using the pushing-out test and this electron moiré method. Also, a non-uniform deformation around the boundary of 3-point bended laminated steel was observed and the strain distribution analyzed.

Compatibility of 2, 4, 6, 8, 10,12-Hexanitrohexaazaisowurtzitane with a Selection of Insensitive Explosives

NASA Astrophysics Data System (ADS)

Li, Xi; Lin, Qiu-han; Zhao, Xin-Ying; Han, Zhi-Wei; Wang, Bo-liang

2017-04-01

Thermal techniques (differential scanning calorimetry (DSC) and the vacuum stability test (VST)), according to STANAG 4147, and non-thermal techniques (Fourier transform infrared (FTIR) spectrometry and X-ray diffractometry (XRD)) were used to examine compatibility issues for 2,4,6,8,10,12-hexanitrohexaazaisowurtzitane (CL-20) with a selection of insensitive explosives, including nitroguanidine (NQ), 2,4,6-trinitrotoluene (TNT), 2,6-diamino-3,5-dinitropyridine-1-oxide (ANPyO), 2,4,6-triamino-1,3,5-trinitrobenzene (TATB), 3-nitro-1,2,4-triazol-5-one (NTO) and 2,6-diamino-3,5-dinitropyrazine-1-oxide (LLM-105). DSC measurements showed that ANPyO, TATB, NTO and LLM-105 were compatible with CL-20. The compatibility of CL-20/NQ, CL-20/TNT, CL-20/ANPyO, CL-20/TATB, CL-20/NTO and CL-20/LLM-105 mixtures was further explored using the VST, which revealed that all the selected insensitive explosives were compatible with CL-20. Possible chemical interactions were suspected for CL-20/TATB from the FTIR results and for CL-20/NTO from XRD analysis. In summary, ANPyO and LLM-105 demonstrated the optimal compatibility with CL-20.

Role of the Strength of Drug-Polymer Interactions on the Molecular Mobility and Crystallization Inhibition in Ketoconazole Solid Dispersions.

PubMed

Mistry, Pinal; Mohapatra, Sarat; Gopinath, Tata; Vogt, Frederick G; Suryanarayanan, Raj

2015-09-08

The effects of specific drug-polymer interactions (ionic or hydrogen-bonding) on the molecular mobility of model amorphous solid dispersions (ASDs) were investigated. ASDs of ketoconazole (KTZ), a weakly basic drug, with each of poly(acrylic acid) (PAA), poly(2-hydroxyethyl methacrylate) (PHEMA), and polyvinylpyrrolidone (PVP) were prepared. Drug-polymer interactions in the ASDs were evaluated by infrared and solid-state NMR, the molecular mobility quantified by dielectric spectroscopy, and crystallization onset monitored by differential scanning calorimetry (DSC) and variable temperature X-ray diffractometry (VTXRD). KTZ likely exhibited ionic interactions with PAA, hydrogen-bonding with PHEMA, and weaker dipole-dipole interactions with PVP. On the basis of dielectric spectroscopy, the α-relaxation times of the ASDs followed the order: PAA > PHEMA > PVP. In addition, the presence of ionic interactions also translated to a dramatic and disproportionate decrease in mobility as a function of polymer concentration. On the basis of both DSC and VTXRD, an increase in strength of interaction translated to higher crystallization onset temperature and a decrease in extent of crystallization. Stronger drug-polymer interactions, by reducing the molecular mobility, can potentially delay the crystallization onset temperature as well as crystallization extent.

Modification of solid-state property of sulfasalazine by using the supercritical antisolvent process

NASA Astrophysics Data System (ADS)

Wu, Wei-Yi; Su, Chie-Shaan

2017-02-01

In this study, the supercritical antisolvent (SAS) process was used to recrystallize an active pharmaceutical ingredient, sulfasalazine, to modify the solid-state properties including particle size, crystal habit and polymorphic form. Supercritical CO2 and tetrahydrofuran were used as the antisolvent and solvent, respectively. SAS results obtained from different operating temperatures (35, 45, 55 and 65 °C) were compared and discussed. The results indicate that at 55 °C, spherical sulfasalazine crystals were produced and that their mean particle size was micronized to approximately 1 μm. In addition, according to the analytical results of powder X-ray diffractometry (PXRD), a novel polymorphic form of sulfasalazine was obtained after SAS. Furthermore, the spectroscopic and thermal behavior of produced sulfasalazine crystals were also studied by Fourier transform infrared spectrometry (FTIR), differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). Finally, SAS results obtained from different operating temperature was discussed on the basis of the mixture critical point (MCP) of CO2 and tetrahydrofuran. Operation at slightly higher than the MCP is favorable for recrystallization of sulfasalazine through SAS. These results demonstrate that the SAS process is an efficient tool for controlling and modifying the solid-state property of sulfasalazine.

DSC, X-ray and FTIR studies of a gemfibrozil/dimethyl-β-cyclodextrin inclusion complex produced by co-grinding.

PubMed

Aigner, Z; Berkesi, O; Farkas, G; Szabó-Révész, P

2012-01-05

The steps of formation of an inclusion complex produced by the co-grinding of gemfibrozil and dimethyl-β-cyclodextrin were investigated by differential scanning calorimetry (DSC), X-ray powder diffractometry (XRPD) and Fourier transform infrared (FTIR) spectroscopy with curve-fitting analysis. The endothermic peak at 59.25°C reflecting the melting of gemfibrozil progressively disappeared from the DSC curves of the products on increase of the duration of co-grinding. The crystallinity of the samples too gradually decreased, and after 35min of co-grinding the product was totally amorphous. Up to this co-grinding time, XRPD and FTIR investigations indicated a linear correlation between the cyclodextrin complexation and the co-grinding time. After co-grinding for 30min, the ratio of complex formation did not increase. These studies demonstrated that co-grinding is a suitable method for the complexation of gemfibrozil with dimethyl-β-cyclodextrin. XRPD analysis revealed the amorphous state of the gemfibrozil-dimethyl-β-cyclodextrin product. FTIR spectroscopy with curve-fitting analysis may be useful as a semiquantitative analytical method for discriminating the molecular and amorphous states of gemfibrozil. Copyright © 2011 Elsevier B.V. All rights reserved.

Formation of β-cyclodextrin inclusion enhances the stability and aqueous solubility of natural borneol.

PubMed

Su, Jianyu; Chen, Jianping; Li, Lin; Li, Bing; Shi, Lei; Chen, Ling; Xu, Zhenbo

2012-06-01

The aims of this study were to optimize the preparation conditions of natural borneol/β-cyclodextrin (NB/β-CD) inclusion complex by ultrasound method, and to investigate its improvement of stability and solubility. The complex was characterized by different various spectroscopic techniques including Fourier transform infrared spectroscopy, X-ray diffractometry, and differential scanning calorimetry. The results demonstrate that NB could be efficiently loaded into β-CD to form an inclusion complex by ultrasound method at a molar ratio of 1: 1and mass ratio of 1: 6. The complex exhibited different physicochemical characteristics from that of free NB. Typically, formation of β-CD inclusion significantly enhanced the stability and aqueous solubility of NB. Natural borneol (NB) has the potential to be widely used in the fields of medical and functional food, due to its specificity. However, the disadvantages of unstability in the preparation and storage process due to its easy sublimation and the low water solubility limit its application. This research provides an effective way to improve the solubility and stability of NB by preparing NB/β-CD inclusion complex. Furthermore, theoretical basis is also provided for the application development of NB. © 2012 Institute of Food Technologists®

Insights into radiation damage from atomic resolution scanning transmission electron microscopy imaging of mono-layer CuPcCl16 films on graphene.

PubMed

Mittelberger, Andreas; Kramberger, Christian; Meyer, Jannik C

2018-03-19

Atomically resolved images of monolayer organic crystals have only been obtained with scanning probe methods so far. On the one hand, they are usually prepared on surfaces of bulk materials, which are not accessible by (scanning) transmission electron microscopy. On the other hand, the critical electron dose of a monolayer organic crystal is orders of magnitudes lower than the one for bulk crystals, making (scanning) transmission electron microscopy characterization very challenging. In this work we present an atomically resolved study on the dynamics of a monolayer CuPcCl 16 crystal under the electron beam as well as an image of the undamaged molecules obtained by low-dose electron microscopy. The results show the dynamics and the radiation damage mechanisms in the 2D layer of this material, complementing what has been found for bulk crystals in earlier studies. Furthermore, being able to image the undamaged molecular crystal allows the characterization of new composites consisting of 2D materials and organic molecules.

Crystalline inclusions in the cytoplasm and nuclei of cells of acute myeloid leukaemia.

PubMed

Pearson, E C

1989-01-01

In a survey by electron microscopy of peripheral blood and/or bone marrow from 230 adult patients with acute myeloid leukaemia, five were observed to contain crystalline inclusions in the cytoplasm of the leukaemic cells and a sixth contained crystals in the nuclei. In four cases, two of FAB type M2 and two of M4, the cytoplasmic crystals were hexagonal in section and 1-2 micron long. Two examples showed internal periodicities in the range 3.3-4.0 nm when the electronmicrographs were analysed by optical diffractometry. A single case of M1 contained smaller trapezoidal crystals with a 4.9nm periodicity. The sixth patient, with unusual cytological abnormalities and a rare t(3; 6) chromosomal translocation, contained six-sided crystals in the nuclei of some relatively undifferentiated cells. To the best of our knowledge such intranuclear crystals have not previously been reported in leukaemia. The relevance of the crystals to the leukaemic process is discussed.

Analysis of microstructure and mechanical properties of aluminium-copper joints welded by FSW process

NASA Astrophysics Data System (ADS)

Iordache, M.; Sicoe, G.; Iacomi, D.; Niţu, E.; Ducu, C.

2017-08-01

The research conducted in this article aimed to check the quality of joining some dissimilar materials Al-Cu by determining the mechanical properties and microstructure analysis. For the experimental measurements there were used tin alloy Al - EN-AW-1050A with a thickness of 2 mm and Cu99 sheet with a thickness of 2 mm, joined by FSW weld overlay. The main welding parameters were: rotating speed of the rotating element 1400 rev/min, speed of the rotating element 50 mm/min. The experimental results were determined on samples specially prepared for metallographic analysis. In order to prepare samples for their characterization, there was designed and built a device that allowed simultaneous positioning and fixing for grinding. The characteristics analyzed in the joint welded samples were mictrostructure, microhardness and residual stresses. The techniques used to determine these characteristics were optical microscopy, electron microscopy with fluorescence radioactive elemental analysis (EDS), Vickers microhardness line - HV0.3 and X-ray diffractometry.

Change Spectrum Characteristics Modification of Films Deposited by Magnetron Sputtering with the Assistance of Argon Ions Beam

NASA Astrophysics Data System (ADS)

Umnov, S.; Asainov, O.

2015-04-01

Thin aluminum films were prepared using the method of magnetron sputtering with and without argon ion beam assistance. The influence of argon ion beam on the reflectivity in the UV range and the structure of aluminum films was studied. The structure of the films was studied by transmission electron microscopy (TEM), X-ray diffractometry (XRD) and atomic- force microscope (AFM). The study has shown that the films deposed with the assistance of the argon ion beam have more significant microstresses associated with an increase of crystallites microstructure defects as compared to the films deposed without ion assistance. Comparison of the measured reflectivity of aluminum films deposed without and with the assistance of the ion beam has shown that the films characterized by a higher level of microstructure def ects have increased reflectivity in the UV range. The studies suggest that the defects of thin aluminum films crystal structure influence its optical properties.

Structural properties of H-implanted InP crystals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bocchi, C.; Franzosi, P.; Lazzarini, L.

1993-07-01

H has been implanted in InP crystals at the energy E [equals] 100 keV and at different doses ranging from [sigma] [equals] 1 x 10[sup 13] to [sigma] [equals] 5 x 10[sup 16] cm[sup [minus]2]. The depth dependence of the elastic lattice strain has been investigated by high resolution X-ray diffractometry. The implantation produces a lattice dilation. The strain increases with increasing depth, reaches the maximum at about 0.75 [mu]m, and then decreases rapidly; moreover the maximum strain is proportional to the dose. No extended crystal defects have been detected by transmission electron microscopy up to [sigma] <1 x 10[supmore » 16] cm[sup [minus]2] a buried amorphous layer 28 nm in thickness has been observed at the same depth where the strain is maximum. The thickness of the amorphous layer increases by further increasing the dose and reaches a value of about 0.18 [mu]m for [sigma] [equals] 5 x 10[sup 16] cm[sup [minus]2].« less

Accurate virus quantitation using a Scanning Transmission Electron Microscopy (STEM) detector in a scanning electron microscope.

PubMed

Blancett, Candace D; Fetterer, David P; Koistinen, Keith A; Morazzani, Elaine M; Monninger, Mitchell K; Piper, Ashley E; Kuehl, Kathleen A; Kearney, Brian J; Norris, Sarah L; Rossi, Cynthia A; Glass, Pamela J; Sun, Mei G

2017-10-01

A method for accurate quantitation of virus particles has long been sought, but a perfect method still eludes the scientific community. Electron Microscopy (EM) quantitation is a valuable technique because it provides direct morphology information and counts of all viral particles, whether or not they are infectious. In the past, EM negative stain quantitation methods have been cited as inaccurate, non-reproducible, and with detection limits that were too high to be useful. To improve accuracy and reproducibility, we have developed a method termed Scanning Transmission Electron Microscopy - Virus Quantitation (STEM-VQ), which simplifies sample preparation and uses a high throughput STEM detector in a Scanning Electron Microscope (SEM) coupled with commercially available software. In this paper, we demonstrate STEM-VQ with an alphavirus stock preparation to present the method's accuracy and reproducibility, including a comparison of STEM-VQ to viral plaque assay and the ViroCyt Virus Counter. Copyright © 2017 The Authors. Published by Elsevier B.V. All rights reserved.

Correlation of live-cell imaging with volume scanning electron microscopy.

PubMed

Lucas, Miriam S; Günthert, Maja; Bittermann, Anne Greet; de Marco, Alex; Wepf, Roger

2017-01-01

Live-cell imaging is one of the most widely applied methods in live science. Here we describe two setups for live-cell imaging, which can easily be combined with volume SEM for correlative studies. The first procedure applies cell culture dishes with a gridded glass support, which can be used for any light microscopy modality. The second approach is a flow-chamber setup based on Ibidi μ-slides. Both live-cell imaging strategies can be followed up with serial blockface- or focused ion beam-scanning electron microscopy. Two types of resin embedding after heavy metal staining and dehydration are presented making best use of the particular advantages of each imaging modality: classical en-bloc embedding and thin-layer plastification. The latter can be used only for focused ion beam-scanning electron microscopy, but is advantageous for studying cell-interactions with specific substrates, or when the substrate cannot be removed. En-bloc embedding has diverse applications and can be applied for both described volume scanning electron microscopy techniques. Finally, strategies for relocating the cell of interest are discussed for both embedding approaches and in respect to the applied light and scanning electron microscopy methods. Copyright © 2017 Elsevier Inc. All rights reserved.

Scanning electron microscope fractography in failure analysis of steels

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wouters, R.; Froyen, L.

1996-04-01

For many failure cases, macroscopic examination of the fracture surface permits discrimination of fatigue fractures from overload fractures. For clarifying fatigue fractures, the practical significance of microfractography is limited to an investigation of the crack initiation areas. Scanning electron microscopy is successfully used in tracing local material abnormalities that act as fatigue crack initiators. The task for the scanning electron microscope, however, is much more substantial in failure analysis of overload fractures, especially for steels. By revealing specific fractographic characteristics, complemented by information about the material and the loading conditions, scanning electron microscopy provides a strong indication of the probablemore » cause of failure. A complete dimple fracture is indicative of acceptable bulk material properties; overloading, by subdimensioning or excessive external loading, has to be verified. The presence of cleavage fracture makes the material properties questionable if external conditions causing embrittlement are absent. Intergranular brittle fracture requires verification of grain-boundary weakening conditions--a sensitized structure, whether or not combined with a local stress state or a specific environment. The role of scanning electron microscopy in failure analysis is illustrated by case histories of the aforementioned fracture types.« less

Field Emission Auger Electron Spectroscopy with Scanning Auger Microscopy |

Science.gov Websites

0.5 at.% for elements from lithium to uranium. Depth Profiling Removes successive layers by using size (> ~25 nm). Imaging Obtains SEM micrographs with up to 20,000x magnification by using raster scanning with a highly focused electron beam ≥25 nm in diameter. Using the same raster scan, SAM can

Analysis of synthetic diamond single crystals by X-ray topography and double-crystal diffractometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Prokhorov, I. A., E-mail: igor.prokhorov@mail.ru; Ralchenko, V. G.; Bolshakov, A. P.

2013-12-15

Structural features of diamond single crystals synthesized under high pressure and homoepitaxial films grown by chemical vapor deposition (CVD) have been analyzed by double-crystal X-ray diffractometry and topography. The conditions of a diffraction analysis of diamond crystals using Ge monochromators have been optimized. The main structural defects (dislocations, stacking faults, growth striations, second-phase inclusions, etc.) formed during crystal growth have been revealed. The nitrogen concentration in high-pressure/high-temperature (HPHT) diamond substrates is estimated based on X-ray diffraction data. The formation of dislocation bundles at the film-substrate interface in the epitaxial structures has been revealed by plane-wave topography; these dislocations are likelymore » due to the relaxation of elastic macroscopic stresses caused by the lattice mismatch between the substrate and film. The critical thicknesses of plastic relaxation onset in CVD diamond films are calculated. The experimental techniques for studying the real diamond structure in optimizing crystal-growth technology are proven to be highly efficient.« less

Microwave assisted synthesis and characterisation of a zinc oxide/tobacco mosaic virus hybrid material. An active hybrid semiconductor in a field-effect transistor device.

PubMed

Sanctis, Shawn; Hoffmann, Rudolf C; Eiben, Sabine; Schneider, Jörg J

2015-01-01

Tobacco mosaic virus (TMV) has been employed as a robust functional template for the fabrication of a TMV/zinc oxide field effect transistor (FET). A microwave based approach, under mild conditions was employed to synthesize stable zinc oxide (ZnO) nanoparticles, employing a molecular precursor. Insightful studies of the decomposition of the precursor were done using NMR spectroscopy and material characterization of the hybrid material derived from the decomposition was achieved using dynamic light scattering (DLS), transmission electron microscopy (TEM), grazing incidence X-ray diffractometry (GI-XRD) and atomic force microscopy (AFM). TEM and DLS data confirm the formation of crystalline ZnO nanoparticles tethered on top of the virus template. GI-XRD investigations exhibit an orientated nature of the deposited ZnO film along the c-axis. FET devices fabricated using the zinc oxide mineralized virus template material demonstrates an operational transistor performance which was achieved without any high-temperature post-processing steps. Moreover, a further improvement in FET performance was observed by adjusting an optimal layer thickness of the deposited ZnO on top of the TMV. Such a bio-inorganic nanocomposite semiconductor material accessible using a mild and straightforward microwave processing technique could open up new future avenues within the field of bio-electronics.

A study of Bi-Pb-Sn-Cd-Sb penta-alloys rapidly quenched from melt

NASA Astrophysics Data System (ADS)

Kamal, M.; El-Bediwi, A. B.

2004-11-01

Optical microscopy, X-ray diffractometry, the double bridge method, the Vickers microhardness testing and dynamic resonance techniques have been used to investigate structure, electrical resistivity, hardness, internal friction and elastic modulus of quenched Bi-Pb-Sn-Cd-Sb penta-alloys. The properties of these penta-alloys are greatly affected by rapid quenching. The intermetallic compound chi(Pb-Bi) or Bi3Pb7 is obtained after rapid quenching using the melt-spinning technique, and this is in agreement with reports by other authors [Marshall, T.J., Mott, G. T. and Grieverson, M. H. (1975). Br. J. Radiol., 48, 924, Kamal, M., El-Bediwi, A. B. and Karman, M. B. (1998). Structure, mechanical properties and electrical resistivity of rapidly solidified Pb-Sn-Cd and Pb-Bi-Sn-Cd alloys. J. Mater. Sci.: Mater. Electron., 9, 425, Borromee-Gautier, C., Giessen, B. C. and Grrant, N. J. (1968). J. Chem. Phys., 48,1905, Moon, K.-W., Boettinger, W. J., Kanner, U. R., Handwerker, C. A. and Lee, D.-J. (2001). The effect of Pb contamination on the solidification behavior of Sn-Bi solders. J. Electron. Mater, 30, 45.]. The quenched Bi43.5Pb44.5Cd5Sn2Sb5 alloy has important properties for safety devices in fire detection and extinguishing systems.

Iron-antimony-based hybrid oxides as high-performance anodes for lithium-ion storage

NASA Astrophysics Data System (ADS)

Nguyen, Tuan Loi; Kim, Doo Soo; Hur, Jaehyun; Park, Min Sang; Yoon, Sukeun; Kim, Il Tae

2018-06-01

We report a facile approach to synthesize Fe-Sb-based hybrid oxides nanocomposites consisting of Sb, Sb2O3, and Fe3O4 for use as new anode materials for lithium-ion batteries. The composites are synthesized via galvanic replacement between Fe3+ and Sb at high temperature in triethylene glycol medium. The phase, morphology, and composition changes of the composites involved in the various stages of the replacement reaction are characterized using X-ray diffractometry, high-resolution transmission electron microscopy, and energy dispersive X-ray spectroscopy. The as-prepared composites have different compositions with very small particle sizes (<< 10 nm). The FexSbyOz-18 h composite, for instance, exhibits high capacity, better cyclic stability, and rate performance than other composites, with a highly stable specific capacity of 434 mAh g-1 at 500 cycles. The excellent electrochemical performance can be ascribed to the high interfacial contact area between the nanocomposite and electrolyte, stable structure of the composites owing to a mixture of inactive phases generated by the conversion reaction between Li+ and oxide metal-whose structure serves as an electron conductor, inhibits agglomeration of Sb particles, and acts as an effective buffer against volume change of Sb during cycling-and high Li+ diffusion ability.

Refixation of Osteochondral Fractures by an Ultrasound-Activated Pin System - An Ovine In Vivo Examination Using CT and Scanning Electron Microscope.

PubMed

H, Neumann; A P, Schulz; S, Breer; A, Unger; B, Kienast

2015-01-01

Osteochondral injuries, if not treated appropriately, often lead to severe osteoarthritis of the affected joint. Without refixation of the osteochondral fragment, human cartilage only repairs these defects imperfectly. All existing refixation systems for chondral defects have disadvantages, for instance bad MRI quality in the postoperative follow-up or low anchoring forces. To address the problem of reduced stability in resorbable implants, ultrasound-activated pins were developed. By ultrasound-activated melting of the tip of these implants a higher anchoring is assumed. Aim of the study was to investigate, if ultrasound-activated pins can provide a secure refixation of osteochondral fractures comparing to conventional screw and conventional, resorbable pin osteosynthesis. CT scans and scanning electron microscopy should proovegood refixation results with no further tissue damage by the melting of the ultrasound-activated pins in comparison to conventional osteosynthesis. Femoral osteochondral fragments in sheep were refixated with ultrasound-activated pins (SonicPin™), Ethipins(®) and screws (Asnis™). The quality of the refixated fragments was examined after three month of full weight bearing by CT scans and scanning electron microscopy of the cartilage surface. The CT examination found almost no statistically significant difference in the quality of refixation between the three different implants used. Concerning the CT morphology, ultrasound-activated pins demonstrated at least the same quality in refixation of osteochondral fragments as conventional resorbable pins or screws. The scanning electron microscopy showed no major surface damage by the three implants, especially any postulated cartilage damage induced by the heat of the ultrasound-activated pin. The screws protruded above the cartilage surface, which may affect the opposingtibial surface. Using CT scans and scanning electron microscopy, the SonicPin™, the Ethipin(®) and screws were at least equivalent in refixation quality of osteochondral fragments.

Analytical and numerical analysis of imaging mechanism of dynamic scanning electron microscopy.

PubMed

Schröter, M-A; Holschneider, M; Sturm, H

2012-11-02

The direct observation of small oscillating structures with the help of a scanning electron beam is a new approach to study the vibrational dynamics of cantilevers and microelectromechanical systems. In the scanning electron microscope, the conventional signal of secondary electrons (SE, dc part) is separated from the signal response of the SE detector, which is correlated to the respective excitation frequency for vibration by means of a lock-in amplifier. The dynamic response is separated either into images of amplitude and phase shift or into real and imaginary parts. Spatial resolution is limited to the diameter of the electron beam. The sensitivity limit to vibrational motion is estimated to be sub-nanometer for high integration times. Due to complex imaging mechanisms, a theoretical model was developed for the interpretation of the obtained measurements, relating cantilever shapes to interaction processes consisting of incident electron beam, electron-lever interaction, emitted electrons and detector response. Conclusions drawn from this new model are compared with numerical results based on the Euler-Bernoulli equation.

Publications - GMC 58 | Alaska Division of Geological & Geophysical Surveys

Science.gov Websites

DGGS GMC 58 Publication Details Title: X-ray diffraction and scanning electron microscopy mineral , Michael, and Core Laboratories, 1985, X-ray diffraction and scanning electron microscopy mineral analyses

Scanning electron microscope fine tuning using four-bar piezoelectric actuated mechanism

NASA Astrophysics Data System (ADS)

Hatamleh, Khaled S.; Khasawneh, Qais A.; Al-Ghasem, Adnan; Jaradat, Mohammad A.; Sawaqed, Laith; Al-Shabi, Mohammad

2018-01-01

Scanning Electron Microscopes are extensively used for accurate micro/nano images exploring. Several strategies have been proposed to fine tune those microscopes in the past few years. This work presents a new fine tuning strategy of a scanning electron microscope sample table using four bar piezoelectric actuated mechanisms. The introduced paper presents an algorithm to find all possible inverse kinematics solutions of the proposed mechanism. In addition, another algorithm is presented to search for the optimal inverse kinematic solution. Both algorithms are used simultaneously by means of a simulation study to fine tune a scanning electron microscope sample table through a pre-specified circular or linear path of motion. Results of the study shows that, proposed algorithms were able to minimize the power required to drive the piezoelectric actuated mechanism by a ratio of 97.5% for all simulated paths of motion when compared to general non-optimized solution.

STEM VQ Method, Using Scanning Transmission Electron Microscopy (STEM) for Accurate Virus Quantification

DTIC Science & Technology

2017-02-02

Corresponding Author Abstract Accurate virus quantification is sought, but a perfect method still eludes the scientific community. Electron...unlimited. UNCLASSIFIED 2 provides morphology data and counts all viral particles, including partial or noninfectious particles; however, EM methods ...consistent, reproducible virus quantification method called Scanning Transmission Electron Microscopy – Virus Quantification (STEM-VQ) which simplifies

Direct observation of iron-induced conformational changes of mitochondrial DNA by high-resolution field-emission in-lens scanning electron microscopy.

PubMed Central

Yaffee, M; Walter, P; Richter, C; Müller, M

1996-01-01

When respiring rat liver mitochondria are incubated in the presence of Fe(III) gluconate, their DNA (mtDNA) relaxes from the supercoiled to the open circular form dependent on the iron dose. Anaerobiosis or antioxidants fail to completely inhibit the unwinding. High-resolution field-emission in-lens scanning electron microscopy imaging, in concert with backscattered electron detection, pinpoints nanometer-range iron colloids bound to mtDNA isolated from iron-exposed mitochondria. High-resolution field-emission in-lens scanning electron microscopy with backscattered electron detection imaging permits simultaneous detailed visual analysis of DNA topology, iron dose-dependent mtDNA unwinding, and assessment of iron colloid formation on mtDNA strands. Images Fig. 1 Fig. 2 Fig. 3 Fig. 4 PMID:8643576

Sub-nanometre resolution imaging of polymer-fullerene photovoltaic blends using energy-filtered scanning electron microscopy.

PubMed

Masters, Robert C; Pearson, Andrew J; Glen, Tom S; Sasam, Fabian-Cyril; Li, Letian; Dapor, Maurizio; Donald, Athene M; Lidzey, David G; Rodenburg, Cornelia

2015-04-24

The resolution capability of the scanning electron microscope has increased immensely in recent years, and is now within the sub-nanometre range, at least for inorganic materials. An equivalent advance has not yet been achieved for imaging the morphologies of nanostructured organic materials, such as organic photovoltaic blends. Here we show that energy-selective secondary electron detection can be used to obtain high-contrast, material-specific images of an organic photovoltaic blend. We also find that we can differentiate mixed phases from pure material phases in our data. The lateral resolution demonstrated is twice that previously reported from secondary electron imaging. Our results suggest that our energy-filtered scanning electron microscopy approach will be able to make major inroads into the understanding of complex, nano-structured organic materials.

Fabrication of [001]-oriented tungsten tips for high resolution scanning tunneling microscopy

PubMed Central

Chaika, A. N.; Orlova, N. N.; Semenov, V. N.; Postnova, E. Yu.; Krasnikov, S. A.; Lazarev, M. G.; Chekmazov, S. V.; Aristov, V. Yu.; Glebovsky, V. G.; Bozhko, S. I.; Shvets, I. V.

2014-01-01

The structure of the [001]-oriented single crystalline tungsten probes sharpened in ultra-high vacuum using electron beam heating and ion sputtering has been studied using scanning and transmission electron microscopy. The electron microscopy data prove reproducible fabrication of the single-apex tips with nanoscale pyramids grained by the {011} planes at the apexes. These sharp, [001]-oriented tungsten tips have been successfully utilized in high resolution scanning tunneling microscopy imaging of HOPG(0001), SiC(001) and graphene/SiC(001) surfaces. The electron microscopy characterization performed before and after the high resolution STM experiments provides direct correlation between the tip structure and picoscale spatial resolution achieved in the experiments. PMID:24434734

The nanosphere iron mineral(s) in Mars soil

NASA Technical Reports Server (NTRS)

Banin, A.; Ben-Shlomo, T.; Margulies, L.; Blake, D. F.; Mancinelli, R. L.; Gehring, A. U.

1993-01-01

A series of surface-modified clays containing nanophase (np) iron/oxyhydroxides of extremely small particle sizes, with total iron contents as high as found in Mars soil, were prepared by iron deposition on the clay surface from ferrous chloride solution. Comprehensive studies of the iron mineralogy in these 'Mars-soil analogs' were conducted using chemical extractions, solubility analyses, pH and redox, x ray and electron diffractometry, electron microscopic imaging specific surface area and particle size determinations, differential thermal analyses, magnetic properties characterization, spectral reflectance, and Viking biology simulation experiments. The clay matrix and the procedure used for synthesis produced nanophase iron oxides containing a certain proportion of divalent iron, which slowly converts to more stable, fully oxidized iron minerals. The noncrystalline nature of the iron compounds precipitated on the surface of the clay was verified by their complete extractability in oxalate. Lepidocrocite (gamma-FeOOH) was detected by selected area electron diffraction. It is formed from a double iron Fe(II)/Fe(III) hydroxyl mineral such as 'green rust', or ferrosic hydroxide. Magnetic measurements suggested that lepidocrocite converted to the more stable meaghemite (gamma-Fe203) by mild heat treatment and then to nanophase hematite (aplha-Fe203) by extensive heat treatment. Their chemical reactivity offers a plausible mechanism for the somewhat puzzling observations of the Viking biology experiments. Their unique chemical reactivities are attributed to the combined catalytic effects of the iron oxide/oxyhydroxide and silicate phase surfaces. The mode of formation of these (nanophase) iron oxides on Mars is still unknown.

Qualitative and quantitative interpretation of SEM image using digital image processing.

PubMed

Saladra, Dawid; Kopernik, Magdalena

2016-10-01

The aim of the this study is improvement of qualitative and quantitative analysis of scanning electron microscope micrographs by development of computer program, which enables automatic crack analysis of scanning electron microscopy (SEM) micrographs. Micromechanical tests of pneumatic ventricular assist devices result in a large number of micrographs. Therefore, the analysis must be automatic. Tests for athrombogenic titanium nitride/gold coatings deposited on polymeric substrates (Bionate II) are performed. These tests include microshear, microtension and fatigue analysis. Anisotropic surface defects observed in the SEM micrographs require support for qualitative and quantitative interpretation. Improvement of qualitative analysis of scanning electron microscope images was achieved by a set of computational tools that includes binarization, simplified expanding, expanding, simple image statistic thresholding, the filters Laplacian 1, and Laplacian 2, Otsu and reverse binarization. Several modifications of the known image processing techniques and combinations of the selected image processing techniques were applied. The introduced quantitative analysis of digital scanning electron microscope images enables computation of stereological parameters such as area, crack angle, crack length, and total crack length per unit area. This study also compares the functionality of the developed computer program of digital image processing with existing applications. The described pre- and postprocessing may be helpful in scanning electron microscopy and transmission electron microscopy surface investigations. © 2016 The Authors Journal of Microscopy © 2016 Royal Microscopical Society.

Using the scanning electron microscope on the production line to assure quality semiconductors

NASA Technical Reports Server (NTRS)

Adolphsen, J. W.; Anstead, R. J.

1972-01-01

The use of the scanning electron microscope to detect metallization defects introduced during batch processing of semiconductor devices is discussed. A method of determining metallization integrity was developed which culminates in a procurement specification using the scanning microscope on the production line as a quality control tool. Batch process control of the metallization operation is monitored early in the manufacturing cycle.

Soil Particle Size Analysis by Laser Diffractometry: Result Comparison with Pipette Method

NASA Astrophysics Data System (ADS)

Šinkovičová, Miroslava; Igaz, Dušan; Kondrlová, Elena; Jarošová, Miriam

2017-10-01

Soil texture as the basic soil physical property provides a basic information on the soil grain size distribution as well as grain size fraction representation. Currently, there are several methods of particle dimension measurement available that are based on different physical principles. Pipette method based on the different sedimentation velocity of particles with different diameter is considered to be one of the standard methods of individual grain size fraction distribution determination. Following the technical advancement, optical methods such as laser diffraction can be also used nowadays for grain size distribution determination in the soil. According to the literature review of domestic as well as international sources related to this topic, it is obvious that the results obtained by laser diffractometry do not correspond with the results obtained by pipette method. The main aim of this paper was to analyse 132 samples of medium fine soil, taken from the Nitra River catchment in Slovakia, from depths of 15-20 cm and 40-45 cm, respectively, using laser analysers: ANALYSETTE 22 MicroTec plus (Fritsch GmbH) and Mastersizer 2000 (Malvern Instruments Ltd). The results obtained by laser diffractometry were compared with pipette method and the regression relationships using linear, exponential, power and polynomial trend were derived. Regressions with the three highest regression coefficients (R2) were further investigated. The fit with the highest tightness was observed for the polynomial regression. In view of the results obtained, we recommend using the estimate of the representation of the clay fraction (<0.01 mm) polynomial regression, to achieve a highest confidence value R2 at the depths of 15-20 cm 0.72 (Analysette 22 MicroTec plus) and 0.95 (Mastersizer 2000), from a depth of 40-45 cm 0.90 (Analysette 22 MicroTec plus) and 0.96 (Mastersizer 2000). Since the percentage representation of clayey particles (2nd fraction according to the methodology of Complex Soil Survey done in Slovakia) in soil is the determinant for soil type specification, we recommend using the derived relationships in soil science when the soil texture analysis is done according to laser diffractometry. The advantages of laser diffraction method comprise the short analysis time, usage of small sample amount, application for the various grain size fraction and soil type classification systems, and a wide range of determined fractions. Therefore, it is necessary to focus on this issue further to address the needs of soil science research and attempt to replace the standard pipette method with more progressive laser diffraction method.

Scanning electron microscopy combined with image processing technique: Analysis of microstructure, texture and tenderness in Semitendinous and Gluteus Medius bovine muscles.

PubMed

Pieniazek, Facundo; Messina, Valeria

2016-11-01

In this study the effect of freeze drying on the microstructure, texture, and tenderness of Semitendinous and Gluteus Medius bovine muscles were analyzed applying Scanning Electron Microscopy combined with image analysis. Samples were analyzed by Scanning Electron Microscopy at different magnifications (250, 500, and 1,000×). Texture parameters were analyzed by Texture analyzer and by image analysis. Tenderness by Warner-Bratzler shear force. Significant differences (p < 0.05) were obtained for image and instrumental texture features. A linear trend with a linear correlation was applied for instrumental and image features. Image texture features calculated from Gray Level Co-occurrence Matrix (homogeneity, contrast, entropy, correlation and energy) at 1,000× in both muscles had high correlations with instrumental features (chewiness, hardness, cohesiveness, and springiness). Tenderness showed a positive correlation in both muscles with image features (energy and homogeneity). Combing Scanning Electron Microscopy with image analysis can be a useful tool to analyze quality parameters in meat.Summary SCANNING 38:727-734, 2016. © 2016 Wiley Periodicals, Inc. © Wiley Periodicals, Inc.

Flat panel ferroelectric electron emission display system

DOEpatents

Sampayan, Stephen E.; Orvis, William J.; Caporaso, George J.; Wieskamp, Ted F.

1996-01-01

A device which can produce a bright, raster scanned or non-raster scanned image from a flat panel. Unlike many flat panel technologies, this device does not require ambient light or auxiliary illumination for viewing the image. Rather, this device relies on electrons emitted from a ferroelectric emitter impinging on a phosphor. This device takes advantage of a new electron emitter technology which emits electrons with significant kinetic energy and beam current density.

Three-dimensional electron microscopy simulation with the CASINO Monte Carlo software.

PubMed

Demers, Hendrix; Poirier-Demers, Nicolas; Couture, Alexandre Réal; Joly, Dany; Guilmain, Marc; de Jonge, Niels; Drouin, Dominique

2011-01-01

Monte Carlo softwares are widely used to understand the capabilities of electron microscopes. To study more realistic applications with complex samples, 3D Monte Carlo softwares are needed. In this article, the development of the 3D version of CASINO is presented. The software feature a graphical user interface, an efficient (in relation to simulation time and memory use) 3D simulation model, accurate physic models for electron microscopy applications, and it is available freely to the scientific community at this website: www.gel.usherbrooke.ca/casino/index.html. It can be used to model backscattered, secondary, and transmitted electron signals as well as absorbed energy. The software features like scan points and shot noise allow the simulation and study of realistic experimental conditions. This software has an improved energy range for scanning electron microscopy and scanning transmission electron microscopy applications. Copyright © 2011 Wiley Periodicals, Inc.

Three-Dimensional Electron Microscopy Simulation with the CASINO Monte Carlo Software

PubMed Central

Demers, Hendrix; Poirier-Demers, Nicolas; Couture, Alexandre Réal; Joly, Dany; Guilmain, Marc; de Jonge, Niels; Drouin, Dominique

2011-01-01

Monte Carlo softwares are widely used to understand the capabilities of electron microscopes. To study more realistic applications with complex samples, 3D Monte Carlo softwares are needed. In this paper, the development of the 3D version of CASINO is presented. The software feature a graphical user interface, an efficient (in relation to simulation time and memory use) 3D simulation model, accurate physic models for electron microscopy applications, and it is available freely to the scientific community at this website: www.gel.usherbrooke.ca/casino/index.html. It can be used to model backscattered, secondary, and transmitted electron signals as well as absorbed energy. The software features like scan points and shot noise allow the simulation and study of realistic experimental conditions. This software has an improved energy range for scanning electron microscopy and scanning transmission electron microscopy applications. PMID:21769885

The spatial coherence function in scanning transmission electron microscopy and spectroscopy.

PubMed

Nguyen, D T; Findlay, S D; Etheridge, J

2014-11-01

We investigate the implications of the form of the spatial coherence function, also referred to as the effective source distribution, for quantitative analysis in scanning transmission electron microscopy, and in particular for interpreting the spatial origin of imaging and spectroscopy signals. These questions are explored using three different source distribution models applied to a GaAs crystal case study. The shape of the effective source distribution was found to have a strong influence not only on the scanning transmission electron microscopy (STEM) image contrast, but also on the distribution of the scattered electron wavefield and hence on the spatial origin of the detected electron intensities. The implications this has for measuring structure, composition and bonding at atomic resolution via annular dark field, X-ray and electron energy loss STEM imaging are discussed. Copyright © 2014 Elsevier B.V. All rights reserved.

Symposium N: Materials and Devices for Thermal-to-Electric Energy Conversion

DTIC Science & Technology

2010-08-24

X - ray diffraction, transmission electron microscopy, scanning electron microscopy, and dynamic light scattering. Thermal conductivity measurements...SEM), X - ray diffraction (XRD) measurements as well as Raman spectroscopy. The results from these techniques indicate a clear modification...was examined by using scanning electron microscope (SEM; HITACHI S-4500 model) attached with an energy dispersive x - ray spectroscopy. The electrical

The use of a fully integrated electronic medical record to minimize cumulative lifetime radiation exposure from CT scanning to detect urinary tract calculi.

PubMed

Kohler, Steven W; Chen, Richard; Kagan, Alex; Helvey, Dustin W; Buccigrossi, David

2013-06-01

In order to determine the effects of implementation of an electronic medical record on rates of repeat computed tomography (CT) scanning in the emergency department (ED) setting, we analyzed the utilization of CT of the kidneys, ureters, and bladder (CT KUB) for the detection of urinary tract calculi for periods before and after the implementation of a hospital-wide electronic medical record system. Rates of repeat CT scanning within a 6-month period of previous scan were determined pre- and post-implementation and compared. Prior to implementation, there was a 6-month repeat rate of 6.2 % compared with the post-implementation period, which was associated with a 6-month repeat rate of 4.1 %. Statistical analysis using a two-sample, one-tailed t test for difference of means was associated with a p value of 0.00007. This indicates that the implementation of the electronic medical record system was associated with a 34 % decrease in 6-month repeat CT KUB scans. We conclude that the use of an electronic medical record can be associated with a decrease in utilization of unnecessary repeat CT imaging, leading to decreased cumulative lifetime risk for cancer in these patients and more efficient utilization of ED and radiologic resources.

Electron tomography of HEK293T cells using scanning electron microscope-based scanning transmission electron microscopy.

PubMed

You, Yun-Wen; Chang, Hsun-Yun; Liao, Hua-Yang; Kao, Wei-Lun; Yen, Guo-Ji; Chang, Chi-Jen; Tsai, Meng-Hung; Shyue, Jing-Jong

2012-10-01

Based on a scanning electron microscope operated at 30 kV with a homemade specimen holder and a multiangle solid-state detector behind the sample, low-kV scanning transmission electron microscopy (STEM) is presented with subsequent electron tomography for three-dimensional (3D) volume structure. Because of the low acceleration voltage, the stronger electron-atom scattering leads to a stronger contrast in the resulting image than standard TEM, especially for light elements. Furthermore, the low-kV STEM yields less radiation damage to the specimen, hence the structure can be preserved. In this work, two-dimensional STEM images of a 1-μm-thick cell section with projection angles between ±50° were collected, and the 3D volume structure was reconstructed using the simultaneous iterative reconstructive technique algorithm with the TomoJ plugin for ImageJ, which are both public domain software. Furthermore, the cross-sectional structure was obtained with the Volume Viewer plugin in ImageJ. Although the tilting angle is constrained and limits the resulting structural resolution, slicing the reconstructed volume generated the depth profile of the thick specimen with sufficient resolution to examine cellular uptake of Au nanoparticles, and the final position of these nanoparticles inside the cell was imaged.

Anisotropic Shape Changes of Silica Nanoparticles Induced in Liquid with Scanning Transmission Electron Microscopy.

PubMed

Zečević, Jovana; Hermannsdörfer, Justus; Schuh, Tobias; de Jong, Krijn P; de Jonge, Niels

2017-01-01

Liquid-phase transmission electron microscopy (TEM) is used for in-situ imaging of nanoscale processes taking place in liquid, such as the evolution of nanoparticles during synthesis or structural changes of nanomaterials in liquid environment. Here, it is shown that the focused electron beam of scanning TEM (STEM) brings about the dissolution of silica nanoparticles in water by a gradual reduction of their sizes, and that silica redeposites at the sides of the nanoparticles in the scanning direction of the electron beam, such that elongated nanoparticles are formed. Nanoparticles with an elongation in a different direction are obtained simply by changing the scan direction. Material is expelled from the center of the nanoparticles at higher electron dose, leading to the formation of doughnut-shaped objects. Nanoparticles assembled in an aggregate gradually fuse, and the electron beam exposed section of the aggregate reduces in size and is elongated. Under TEM conditions with a stationary electron beam, the nanoparticles dissolve but do not elongate. The observed phenomena are important to consider when conducting liquid-phase STEM experiments on silica-based materials and may find future application for controlled anisotropic manipulation of the size and the shape of nanoparticles in liquid. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Quantitation of polymorphic impurity in entecavir polymorphic mixtures using powder X-ray diffractometry and Raman spectroscopy.

PubMed

Kang, Yanlei; Shao, Zhanying; Wang, Qiang; Hu, Xiurong; Yu, Dongdong

2018-05-26

Entecavir was used for the treatment of chronic hepatitis B through inhibiting hepatitis B virus. The anhydrous form of entecavir (ENT-A) often appeared as impurity polymorph in the manufacturing process of entecavir monohydrate (ENT-H) such as granulation, drying and compression. Since different crystal forms might affect drug bioavailability and therapeutic effect, it was vital to control the ENT-A content of the drug product. The work aimed to develop useful methods to assess ENT-A weight percentage in ENT-H. Powder X-ray diffractometry (PXRD) and Raman spectrometric methods were applied. Binary mixtures with different ratios of pure ENT-H and pure ENT-A were scanned using PXRD and Raman to obtain spectra. Then peak heights and peak areas versus weight percentage were used to construct calibration curves. The best linear regression analysis data for PXRD and Raman method were found to be R 2  = 0.9923 and R 2  = 0.9953, in the weight ratio range of 2.1-20.2% w/w% of ENT-A in binary mixtures. Limit of detection (LOD) of ENT-A was 0.38% and limit of quantitation (LOQ) was 1.15% for PXRD method. LOD and LOQ for Raman method were 0.48% and 1.16%. The results showed that PXRD and Raman methods: both were precise and accurate, and could be used for measurement of ENT-A content in the selected weight percentage range. Partial least squares (PLS) algorithm with four data pre-processing methods: including multiplicative scatter correlation (MSC), standard normal variate (SNV), first and second derivatives were applied and evaluated using prediction errors. The best performance of PLS was R 2  = 0.9958 with RMSEC (0.44%) and RMSEP (0.65%). Multivariate analysis for Raman spectra showed similar good results with univariate analysis, and would be an advantageous method when there were overlapped peaks in the spectra. In summary, the proposed PXRD and Raman method could be developed for the quality control of ENT-H. And Raman was a more promising method in industrial practice due to its slightly better precision, accuracy and time-saving advantage. Copyright © 2018 Elsevier B.V. All rights reserved.

Strain mapping in TEM using precession electron diffraction

DOEpatents

Taheri, Mitra Lenore; Leff, Asher Calvin

2017-02-14

A sample material is scanned with a transmission electron microscope (TEM) over multiple steps having a predetermined size at a predetermined angle. Each scan at a predetermined step and angle is compared to a template, wherein the template is generated from parameters of the material and the scanning. The data is then analyzed using local mis-orientation mapping and/or Nye's tensor analysis to provide information about local strain states.

Sparse imaging for fast electron microscopy

NASA Astrophysics Data System (ADS)

Anderson, Hyrum S.; Ilic-Helms, Jovana; Rohrer, Brandon; Wheeler, Jason; Larson, Kurt

2013-02-01

Scanning electron microscopes (SEMs) are used in neuroscience and materials science to image centimeters of sample area at nanometer scales. Since imaging rates are in large part SNR-limited, large collections can lead to weeks of around-the-clock imaging time. To increase data collection speed, we propose and demonstrate on an operational SEM a fast method to sparsely sample and reconstruct smooth images. To accurately localize the electron probe position at fast scan rates, we model the dynamics of the scan coils, and use the model to rapidly and accurately visit a randomly selected subset of pixel locations. Images are reconstructed from the undersampled data by compressed sensing inversion using image smoothness as a prior. We report image fidelity as a function of acquisition speed by comparing traditional raster to sparse imaging modes. Our approach is equally applicable to other domains of nanometer microscopy in which the time to position a probe is a limiting factor (e.g., atomic force microscopy), or in which excessive electron doses might otherwise alter the sample being observed (e.g., scanning transmission electron microscopy).

A Boundary Scan Test Vehicle for Direct Chip Attach Testing

NASA Technical Reports Server (NTRS)

Parsons, Heather A.; DAgostino, Saverio; Arakaki, Genji

2000-01-01

To facilitate the new faster, better and cheaper spacecraft designs, smaller more mass efficient avionics and instruments are using higher density electronic packaging technologies such as direct chip attach (DCA). For space flight applications, these technologies need to have demonstrated reliability and reasonably well defined fabrication and assembly processes before they will be accepted as baseline designs in new missions. As electronics shrink in size, not only can repair be more difficult, but 49 probing" circuitry can be very risky and it becomes increasingly more difficult to identify the specific source of a problem. To test and monitor these new technologies, the Direct Chip Attach Task, under NASA's Electronic Parts and Packaging Program (NEPP), chose the test methodology of boundary scan testing. The boundary scan methodology was developed for interconnect integrity and functional testing at hard to access electrical nodes. With boundary scan testing, active devices are used and failures can be identified to the specific device and lead. This technology permits the incorporation of "built in test" into almost any circuit and thus gives detailed test access to the highly integrated electronic assemblies. This presentation will describe boundary scan, discuss the development of the boundary scan test vehicle for DCA and current plans for testing of direct chip attach configurations.

Sub-nanometre resolution imaging of polymer–fullerene photovoltaic blends using energy-filtered scanning electron microscopy

PubMed Central

Masters, Robert C.; Pearson, Andrew J.; Glen, Tom S.; Sasam, Fabian-Cyril; Li, Letian; Dapor, Maurizio; Donald, Athene M.; Lidzey, David G.; Rodenburg, Cornelia

2015-01-01

The resolution capability of the scanning electron microscope has increased immensely in recent years, and is now within the sub-nanometre range, at least for inorganic materials. An equivalent advance has not yet been achieved for imaging the morphologies of nanostructured organic materials, such as organic photovoltaic blends. Here we show that energy-selective secondary electron detection can be used to obtain high-contrast, material-specific images of an organic photovoltaic blend. We also find that we can differentiate mixed phases from pure material phases in our data. The lateral resolution demonstrated is twice that previously reported from secondary electron imaging. Our results suggest that our energy-filtered scanning electron microscopy approach will be able to make major inroads into the understanding of complex, nano-structured organic materials. PMID:25906738

Flat panel ferroelectric electron emission display system

DOEpatents

Sampayan, S.E.; Orvis, W.J.; Caporaso, G.J.; Wieskamp, T.F.

1996-04-16

A device is disclosed which can produce a bright, raster scanned or non-raster scanned image from a flat panel. Unlike many flat panel technologies, this device does not require ambient light or auxiliary illumination for viewing the image. Rather, this device relies on electrons emitted from a ferroelectric emitter impinging on a phosphor. This device takes advantage of a new electron emitter technology which emits electrons with significant kinetic energy and beam current density. 6 figs.

Electron Beam-Induced Writing of Nanoscale Iron Wires on a Functional Metal Oxide

PubMed Central

2013-01-01

Electron beam-induced surface activation (EBISA) has been used to grow wires of iron on rutile TiO2(110)-(1 × 1) in ultrahigh vacuum. The wires have a width down to ∼20 nm and hence have potential utility as interconnects on this dielectric substrate. Wire formation was achieved using an electron beam from a scanning electron microscope to activate the surface, which was subsequently exposed to Fe(CO)5. On the basis of scanning tunneling microscopy and Auger electron spectroscopy measurements, the activation mechanism involves electron beam-induced surface reduction and restructuring. PMID:24159366

Tunneling rates in electron transport through double-barrier molecular junctions in a scanning tunneling microscope

PubMed Central

Nazin, G. V.; Wu, S. W.; Ho, W.

2005-01-01

The scanning tunneling microscope enables atomic-scale measurements of electron transport through individual molecules. Copper phthalocyanine and magnesium porphine molecules adsorbed on a thin oxide film grown on the NiAl(110) surface were probed. The single-molecule junctions contained two tunneling barriers, vacuum gap, and oxide film. Differential conductance spectroscopy shows that electron transport occurs via vibronic states of the molecules. The intensity of spectral peaks corresponding to the individual vibronic states depends on the relative electron tunneling rates through the two barriers of the junction, as found by varying the vacuum gap tunneling rate by changing the height of the scanning tunneling microscope tip above the molecule. A simple, sequential tunneling model explains the observed trends. PMID:15956189

Tunneling rates in electron transport through double-barrier molecular junctions in a scanning tunneling microscope.

PubMed

Nazin, G V; Wu, S W; Ho, W

2005-06-21

The scanning tunneling microscope enables atomic-scale measurements of electron transport through individual molecules. Copper phthalocyanine and magnesium porphine molecules adsorbed on a thin oxide film grown on the NiAl(110) surface were probed. The single-molecule junctions contained two tunneling barriers, vacuum gap, and oxide film. Differential conductance spectroscopy shows that electron transport occurs via vibronic states of the molecules. The intensity of spectral peaks corresponding to the individual vibronic states depends on the relative electron tunneling rates through the two barriers of the junction, as found by varying the vacuum gap tunneling rate by changing the height of the scanning tunneling microscope tip above the molecule. A simple, sequential tunneling model explains the observed trends.

EVALUATION OF COMPUTER-CONTROLLED SCANNING ELECTRON MICROSCOPY APPLIED TO AN AMBIENT URBAN AEROSOL SAMPLE

EPA Science Inventory

Concerns about the environmental and public health effects of particulate matter (PM) have stimulated interest in analytical techniques capable of measuring the size and chemical composition of individual aerosol particles. Computer-controlled scanning electron microscopy (CCSE...

Scanning electron microscopy of dentition: methodology and ultrastructural morphology of tooth wear.

PubMed

Shkurkin, G V; Almquist, A J; Pfeihofer, A A; Stoddard, E L

1975-01-01

Scanning electron micrographs were taken of sets of human molars-those of paleo-Indians used in mastication of, ostensibly, a highly abrasive diet, and those of contemporary Americans. Different ultrastructural patterns of enamel wear were observed between the groups.

Scanning-electron-microscope used in real-time study of friction and wear

NASA Technical Reports Server (NTRS)

Brainard, W. A.; Buckley, D. H.

1975-01-01

Small friction and wear apparatus built directly into scanning-electron-microscope provides both dynamic observation and microscopic view of wear process. Friction and wear tests conducted using this system have indicated that considerable information can readily be gained.

Beam distribution reconstruction simulation for electron beam probe

NASA Astrophysics Data System (ADS)

Feng, Yong-Chun; Mao, Rui-Shi; Li, Peng; Kang, Xin-Cai; Yin, Yan; Liu, Tong; You, Yao-Yao; Chen, Yu-Cong; Zhao, Tie-Cheng; Xu, Zhi-Guo; Wang, Yan-Yu; Yuan, You-Jin

2017-07-01

An electron beam probe (EBP) is a detector which makes use of a low-intensity and low-energy electron beam to measure the transverse profile, bunch shape, beam neutralization and beam wake field of an intense beam with small dimensions. While it can be applied to many aspects, we limit our analysis to beam distribution reconstruction. This kind of detector is almost non-interceptive for all of the beam and does not disturb the machine environment. In this paper, we present the theoretical aspects behind this technique for beam distribution measurement and some simulation results of the detector involved. First, a method to obtain a parallel electron beam is introduced and a simulation code is developed. An EBP as a profile monitor for dense beams is then simulated using the fast scan method for various target beam profiles, including KV distribution, waterbag distribution, parabolic distribution, Gaussian distribution and halo distribution. Profile reconstruction from the deflected electron beam trajectory is implemented and compared with the actual profile, and the expected agreement is achieved. Furthermore, as well as fast scan, a slow scan, i.e. step-by-step scan, is considered, which lowers the requirement for hardware, i.e. Radio Frequency deflector. We calculate the three-dimensional electric field of a Gaussian distribution and simulate the electron motion in this field. In addition, a fast scan along the target beam direction and slow scan across the beam are also presented, and can provide a measurement of longitudinal distribution as well as transverse profile simultaneously. As an example, simulation results for the China Accelerator Driven Sub-critical System (CADS) and High Intensity Heavy Ion Accelerator Facility (HIAF) are given. Finally, a potential system design for an EBP is described.

Recombinant Reflectin-Based Optical Materials

DTIC Science & Technology

2012-01-01

sili- con substrates were placed in a sealed plastic box. The RH was controlled using a Dydra electronic cigar humidifier and monitored using a Fisher...diffraction gratings to generate diffraction patterns. Nano-spheres and la- mellar microstructures of refCBA samples were observed by scanning electron ...samples were observed by scanning electron microscopy and atomic force microscopy. Despite the reduced complexity of the refCBA protein compared to natural

Bilayer Tablet Formulation of Metformin HCl and Acarbose: A Novel Approach To Control Diabetes.

PubMed

Tiwari, Ruchi; Gupta, Ankita; Joshi, Meenakshi; Tiwari, Gaurav

2014-01-01

The present investigation studied a novel bilayer tablet having an extended release system of metformin HCl with Eudragit RS 100 and RL 100 and an immediate release system of acarbose with polyvinylpyrrolidone K30 (PVP K30) and polyethylene glycol 6000 (PEG 6000) in different ratios using solvent evaporation and cogrinding techniques. Solid dispersions (SDs) were characterized by Fourier transform infrared spectroscopy (FT-IR), differential scanning calorimetry (DSC), powder x-ray diffractometry (XRD), scanning electron microscopy (SEM), as well as by content uniformity, in vitro dissolution studies, and release kinetics. The selected SD system was subjected to bilayer tablet preparation by direct compression. Compressed tablets were evaluated for drug content, weight variation, friability, hardness, and thickness, and they underwent in vitro dissolution studies. The progressive disappearance of IR, x-ray, and thermotropic drug signals in SDs and physical mixtures were related to increasing amount of polymer. SEM studies suggested the homogenous dispersion of drug in polymers. FT-IR studies confirmed the formation of hydrogen bonding between drug and polymer. All tablet formulations showed compliance with pharmacopoeial standards. The formulations gave an initial burst effect to provide the loading dose of the drug followed by extended release for 12 h (Higuchi model via a non-Fickian diffusion controlled release mechanism). Stability studies conducted for the optimized formulation did not show any change in physical properties, drug content, or in vitro drug release. The goal of diabetes therapy today is to achieve and maintain as near normal glycemia as possible to prevent the long-term microvascular and macrovascular complications of elevated blood glucose levels. Oral therapeutic options for the treatment of type 2 diabetes mellitus, until recently, have been severely limited. Metformin, a biguanide, targets additional mechanisms of hyperglycemia by inhibiting hepatic glucose production and enhancing peripheral glucose uptake and thereby reducing insulin resistance; acarbose reversibly bind to pancreatic alpha-amylase and membrane-bound intestinal alpha-glucoside hydrolases. These enzymes inhibit hydrolysis of complex starches to oligosaccharides in the lumen of the small intestine and hydrolysis of oligosaccharides, trisaccharides, and disaccharides to glucose and other monosaccharides in the brush border of the small intestine. The two agents were found to have a remarkable effect on glycemic control. In the present investigation a bilayer tablet was prepared in which one layer gives instant action against diabetes and another layer maintain concentration of drug in plasma for longer periods.

Scanning Electron Microanalysis and Analytical Challenges of Mapping Elements in Urban Atmospheric Particles

EPA Science Inventory

Elemental mapping with energy-dispersive X-ray spectroscopy (EDX) associated with scanning electron microscopy is highly useful for studying internally mixed atmospheric particles. Presented is a study of individual particles from urban airsheds and the analytical challenges in q...

Microstructure of milk

USDA-ARS?s Scientific Manuscript database

The fat and protein in milk may be examined by scanning electron microscopy, transmission electron microscopy, and confocal laser scanning microscopy, and any bacteria present may be viewed by light microscopy. The fat exists as globules, the bulk of the protein is in the form of casein micelles, a...

Three-Dimensional Intercalated Porous Graphene on Si(111)

NASA Astrophysics Data System (ADS)

Pham, Trung T.; Sporken, Robert

2018-02-01

Three-dimensional intercalated porous graphene has been formed on Si(111) by electron beam evaporation under appropriate conditions and its structural and electronic properties investigated in detail by reflection high-energy electron diffraction, x-ray photoemission spectroscopy, Raman spectroscopy, high-resolution scanning electron microscopy, atomic force microscopy, and scanning tunneling microscopy. The results show that the crystalline quality of the porous graphene depended not only on the substrate temperature but also on the SiC layer thickness during carbon atom deposition.

Scanning electron microscope/energy dispersive x ray analysis of impact residues in LDEF tray clamps

NASA Technical Reports Server (NTRS)

Bernhard, Ronald P.; Durin, Christian; Zolensky, Michael E.

1993-01-01

Detailed optical scanning of tray clamps is being conducted in the Facility for the Optical Inspection of Large Surfaces at JSC to locate and document impacts as small as 40 microns in diameter. Residues from selected impacts are then being characterized by Scanning Electron Microscopy/Energy Dispersive X-ray Analysis at CNES. Results from this analysis will be the initial step to classifying projectile residues into specific sources.

Local 2D-2D tunneling in high mobility electron systems

NASA Astrophysics Data System (ADS)

Pelliccione, Matthew; Sciambi, Adam; Bartel, John; Goldhaber-Gordon, David; Pfeiffer, Loren; West, Ken; Lilly, Michael; Bank, Seth; Gossard, Arthur

2012-02-01

Many scanning probe techniques have been utilized in recent years to measure local properties of high mobility two-dimensional (2D) electron systems in GaAs. However, most techniques lack the ability to tunnel into the buried 2D system and measure local spectroscopic information. We report scanning gate measurements on a bilayer GaAs/AlGaAs heterostructure that allows for a local modulation of tunneling between two 2D electron layers. We call this technique Virtual Scanning Tunneling Microscopy (VSTM) [1,2] as the influence of the scanning gate is analogous to an STM tip, except at a GaAs/AlGaAs interface instead of a surface. We will discuss the spectroscopic capabilities of the technique, and show preliminary results of measurements on a high mobility 2D electron system.[1] A. Sciambi, M. Pelliccione et al., Appl. Phys. Lett. 97, 132103 (2010).[2] A. Sciambi, M. Pelliccione et al., Phys. Rev. B 84, 085301 (2011).

Comparison of macroscopic and microscopic (stereomicroscopy and scanning electron microscopy) features of bone lesions due to hatchet hacking trauma.

PubMed

Nogueira, Luísa; Quatrehomme, Gérald; Bertrand, Marie-France; Rallon, Christophe; Ceinos, Romain; du Jardin, Philippe; Adalian, Pascal; Alunni, Véronique

2017-03-01

This experimental study examined the lesions produced by a hatchet on human bones (tibiae). A total of 30 lesions were produced and examined macroscopically (naked eye) and by stereomicroscopy. 13 of them were also analyzed using scanning electron microscopy. The general shape of the lesion, both edges, both walls, the kerf floor and the extremities were described. The length and maximum width of the lesions were also recorded. The microscopic analysis of the lesions led to the description of a sharp-blunt mechanism. Specific criteria were identified (lateral pushing back, fragmentation of the upraising, fossa dug laterally to the edge and vertical striae) enabling the forensic expert to conclude that a hacking instrument was used. These criteria are easily identifiable using scanning electron microscopy, but can also be observed with stereomicroscopy. Overall, lateral pushing back and vertical striae visible using stereomicroscopy and scanning electron microscopy signal the use of a hacking tool.

Two-dimensional simulation and modeling in scanning electron microscope imaging and metrology research.

PubMed

Postek, Michael T; Vladár, András E; Lowney, Jeremiah R; Keery, William J

2002-01-01

Traditional Monte Carlo modeling of the electron beam-specimen interactions in a scanning electron microscope (SEM) produces information about electron beam penetration and output signal generation at either a single beam-landing location, or multiple landing positions. If the multiple landings lie on a line, the results can be graphed in a line scan-like format. Monte Carlo results formatted as line scans have proven useful in providing one-dimensional information about the sample (e.g., linewidth). When used this way, this process is called forward line scan modeling. In the present work, the concept of image simulation (or the first step in the inverse modeling of images) is introduced where the forward-modeled line scan data are carried one step further to construct theoretical two-dimensional (2-D) micrographs (i.e., theoretical SEM images) for comparison with similar experimentally obtained micrographs. This provides an ability to mimic and closely match theory and experiment using SEM images. Calculated and/or measured libraries of simulated images can be developed with this technique. The library concept will prove to be very useful in the determination of dimensional and other properties of simple structures, such as integrated circuit parts, where the shape of the features is preferably measured from a single top-down image or a line scan. This paper presents one approach to the generation of 2-D simulated images and presents some suggestions as to their application to critical dimension metrology.

Neuroanatomy from Mesoscopic to Nanoscopic Scales: An Improved Method for the Observation of Semithin Sections by High-Resolution Scanning Electron Microscopy

PubMed Central

Rodríguez, José-Rodrigo; Turégano-López, Marta; DeFelipe, Javier; Merchán-Pérez, Angel

2018-01-01

Semithin sections are commonly used to examine large areas of tissue with an optical microscope, in order to locate and trim the regions that will later be studied with the electron microscope. Ideally, the observation of semithin sections would be from mesoscopic to nanoscopic scales directly, instead of using light microscopy and then electron microscopy (EM). Here we propose a method that makes it possible to obtain high-resolution scanning EM images of large areas of the brain in the millimeter to nanometer range. Since our method is compatible with light microscopy, it is also feasible to generate hybrid light and electron microscopic maps. Additionally, the same tissue blocks that have been used to obtain semithin sections can later be used, if necessary, for transmission EM, or for focused ion beam milling and scanning electron microscopy (FIB-SEM). PMID:29568263

Neuroanatomy from Mesoscopic to Nanoscopic Scales: An Improved Method for the Observation of Semithin Sections by High-Resolution Scanning Electron Microscopy.

PubMed

Rodríguez, José-Rodrigo; Turégano-López, Marta; DeFelipe, Javier; Merchán-Pérez, Angel

2018-01-01

Semithin sections are commonly used to examine large areas of tissue with an optical microscope, in order to locate and trim the regions that will later be studied with the electron microscope. Ideally, the observation of semithin sections would be from mesoscopic to nanoscopic scales directly, instead of using light microscopy and then electron microscopy (EM). Here we propose a method that makes it possible to obtain high-resolution scanning EM images of large areas of the brain in the millimeter to nanometer range. Since our method is compatible with light microscopy, it is also feasible to generate hybrid light and electron microscopic maps. Additionally, the same tissue blocks that have been used to obtain semithin sections can later be used, if necessary, for transmission EM, or for focused ion beam milling and scanning electron microscopy (FIB-SEM).

a High-Density Electron Beam and Quad-Scan Measurements at Pleiades Thomson X-Ray Source

NASA Astrophysics Data System (ADS)

Lim, J. K.; Rosenzweig, J. B.; Anderson, S. G.; Tremaine, A. M.

2007-09-01

A recent development of the photo-cathode injector technology has greatly enhanced the beam quality necessary for the creation of high density/high brightness electron beam sources. In the Thomson backscattering x-ray experiment, there is an immense need for under 20 micron electron beam spot at the interaction point with a high-intensity laser in order to produce a large x-ray flux. This has been demonstrated successfully at PLEIADES in Lawrence Livermore National Laboratory. For this Thomson backscattering experiment, we employed an asymmetric triplet, high remanence permanent-magnet quads to produce smaller electron beams. Utilizing highly efficient optical transition radiation (OTR) beam spot imaging technique and varying electron focal spot sizes enabled a quadrupole scan at the interaction zone. Comparisons between Twiss parameters obtained upstream to those parameter values deduced from PMQ scan will be presented in this report.

a High-Density Electron Beam and Quad-Scan Measurements at Pleiades Thomson X-Ray Source

NASA Astrophysics Data System (ADS)

Lim, J. K.; Rosenzweig, J. B.; Anderson, S. G.; Tremaine, A. M.

A recent development of the photo-cathode injector technology has greatly enhanced the beam quality necessary for the creation of high density/high brightness electron beam sources. In the Thomson backscattering x-ray experiment, there is an immense need for under 20 micron electron beam spot at the interaction point with a high-intensity laser in order to produce a large x-ray flux. This has been demonstrated successfully at PLEIADES in Lawrence Livermore National Laboratory. For this Thomson backscattering experiment, we employed an asymmetric triplet, high remanence permanent-magnet quads to produce smaller electron beams. Utilizing highly efficient optical transition radiation (OTR) beam spot imaging technique and varying electron focal spot sizes enabled a quadrupole scan at the interaction zone. Comparisons between Twiss parameters obtained upstream to those parameter values deduced from PMQ scan will be presented in this report.

Study on the parameters of the scanning system for the 300 keV electron accelerator

DOE Office of Scientific and Technical Information (OSTI.GOV)

Leo, K. W.; Chulan, R. M., E-mail: leo@nm.gov.my; Hashim, S. A.

2016-01-22

This paper describes the method to identify the magnetic coil parameters of the scanning system. This locally designed low energy electron accelerator with the present energy of 140 keV will be upgraded to 300 keV. In this accelerator, scanning system is required to deflect the energetic electron beam across a titanium foil in vertical and horizontal direction. The excitation current of the magnetic coil is determined by the energy of the electron beam. Therefore, the magnetic coil parameters must be identified to ensure the matching of the beam energy and excitation coil current. As the result, the essential parameters ofmore » the effective lengths for X-axis and Y-axis have been found as 0.1198 m and 0.1134 m and the required excitation coil currents which is dependenton the electron beam energies have be identified.« less

EBIC spectroscopy - A new approach to microscale characterization of deep levels in semi-insulating GaAs

NASA Technical Reports Server (NTRS)

Li, C.-J.; Sun, Q.; Lagowski, J.; Gatos, H. C.

1985-01-01

The microscale characterization of electronic defects in (SI) GaAs has been a challenging issue in connection with materials problems encountered in GaAs IC technology. The main obstacle which limits the applicability of high resolution electron beam methods such as Electron Beam-Induced Current (EBIC) and cathodoluminescence (CL) is the low concentration of free carriers in semiinsulating (SI) GaAs. The present paper provides a new photo-EBIC characterization approach which combines the spectroscopic advantages of optical methods with the high spatial resolution and scanning capability of EBIC. A scanning electron microscope modified for electronic characterization studies is shown schematically. The instrument can operate in the standard SEM mode, in the EBIC modes (including photo-EBIC and thermally stimulated EBIC /TS-EBIC/), and in the cathodo-luminescence (CL) and scanning modes. Attention is given to the use of CL, Photo-EBIC, and TS-EBIC techniques.

Refixation of Osteochondral Fractures by an Ultrasound-Activated Pin System – An Ovine In Vivo Examination Using CT and Scanning Electron Microscope

PubMed Central

H, Neumann; A.P, Schulz; S, Breer; A, Unger; B, Kienast

2015-01-01

Background: Osteochondral injuries, if not treated appropriately, often lead to severe osteoarthritis of the affected joint. Without refixation of the osteochondral fragment, human cartilage only repairs these defects imperfectly. All existing refixation systems for chondral defects have disadvantages, for instance bad MRI quality in the postoperative follow-up or low anchoring forces. To address the problem of reduced stability in resorbable implants, ultrasound-activated pins were developed. By ultrasound-activated melting of the tip of these implants a higher anchoring is assumed. Aim of the study was to investigate, if ultrasound-activated pins can provide a secure refixation of osteochondral fractures comparing to conventional screw and conventional, resorbable pin osteosynthesis. CT scans and scanning electron microscopy should proovegood refixation results with no further tissue damage by the melting of the ultrasound-activated pins in comparison to conventional osteosynthesis. Methods: Femoral osteochondral fragments in sheep were refixated with ultrasound-activated pins (SonicPin™), Ethipins® and screws (Asnis™). The quality of the refixated fragments was examined after three month of full weight bearing by CT scans and scanning electron microscopy of the cartilage surface. Results: The CT examination found almost no statistically significant difference in the quality of refixation between the three different implants used. Concerning the CT morphology, ultrasound-activated pins demonstrated at least the same quality in refixation of osteochondral fragments as conventional resorbable pins or screws. The scanning electron microscopy showed no major surface damage by the three implants, especially any postulated cartilage damage induced by the heat of the ultrasound-activated pin. The screws protruded above the cartilage surface, which may affect the opposingtibial surface. Conclusion: Using CT scans and scanning electron microscopy, the SonicPin™, the Ethipin® and screws were at least equivalent in refixation quality of osteochondral fragments. PMID:25674184

Design and performance of a beetle-type double-tip scanning tunneling microscope

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jaschinsky, Philipp; Coenen, Peter; Pirug, Gerhard

2006-09-15

A combination of a double-tip scanning tunneling microscope with a scanning electron microscope in ultrahigh vacuum environment is presented. The compact beetle-type design made it possible to integrate two independently driven scanning tunneling microscopes in a small space. Moreover, an additional level for coarse movement allows the decoupling of the translation and approach of the tunneling tip. The position of the two tips can be controlled from the millimeter scale down to 50 nm with the help of an add-on electron microscope. The instrument is capable of atomic resolution imaging with each tip.

[Scanning electron microscope study of chemically disinfected endodontic files].

PubMed

Navarro, G; Mateos, M; Navarro, J L; Canalda, C

1991-01-01

Forty stainless steel endodontic files were observed at scanning electron microscopy after being subjected to ten disinfection cycles of 10 minutes each one, immersed in different chemical disinfectants. Corrosion was not observed on the surface of the files in circumstances that this study was made.

Keggin-type polyoxometalate nanosheets: synthesis and characterization via scanning transmission electron microscopy.

PubMed

Hiyoshi, Norihito

2018-05-17

Polyoxometalate nanosheets were synthesized at the gas/liquid interface of an aqueous solution of Keggin-type silicotungstic acid, cesium chloride, and n-octylamine. The structure of the nanosheets was elucidated via aberration-corrected scanning transmission electron microscopy at the atomic and molecular levels.

Scanning electron microscopy analysis of corrosion degradation on tinplate substrates.

PubMed

Zumelzu, E; Cabezas, C; Vera, A

2003-01-01

The degradation of electrolytic tinplate used in food containers was analysed and evaluated, using scanning electron microscopy and electrochemical measurements of microcorrosion and ion dissolution by atomic absorption to prevent food contamination caused by metal traces and to increase the durability of such tinplates.

EVALUATION OF COMPUTER-CONTROLLED SCANNING ELECTRON MICROSCOPY APPLIED TO AN AMBIENT URBAN AEROSOL SAMPLE

EPA Science Inventory

Recent interest in monitoring and speciation of particulate matter has led to increased application of scanning electron microscopy (SEM) coupled with energy-dispersive x-ray analysis (EDX) to individual particle analysis. SEM/EDX provides information on the size, shape, co...

Path-separated electron interferometry in a scanning transmission electron microscope

NASA Astrophysics Data System (ADS)

Yasin, Fehmi S.; Harvey, Tyler R.; Chess, Jordan J.; Pierce, Jordan S.; McMorran, Benjamin J.

2018-05-01

We report a path-separated electron interferometer within a scanning transmission electron microscope. In this setup, we use a nanofabricated grating as an amplitude-division beamsplitter to prepare multiple spatially separated, coherent electron probe beams. We achieve path separations of 30 nm. We pass the  +1 diffraction order probe through amorphous carbon while passing the 0th and  ‑1 orders through vacuum. The probes are then made to interfere via imaging optics, and we observe an interference pattern at the CCD detector with up to 39.7% fringe visibility. We show preliminary experimental results in which the interference pattern was recorded during a 1D scan of the diffracted probes across a test phase object. These results qualitatively agree with a modeled interference predicted by an independent measurement of the specimen thickness. This experimental design can potentially be applied to phase contrast imaging and fundamental physics experiments, such as an exploration of electron wave packet coherence length.

Local electric field direct writing – Electron-beam lithography and mechanism

DOE PAGES

Jiang, Nan; Su, Dong; Spence, John C. H.

2017-08-24

Local electric field induced by a focused electron probe in silicate glass thin films is evaluated in this paper by the migration of cations. Extremely strong local electric fields can be obtained by the focused electron probe from a scanning transmission electron microscope. As a result, collective atomic displacements occur. This newly revised mechanism provides an efficient tool to write patterned nanostructures directly, and thus overcome the low efficiency of the conventional electron-beam lithography. Applying this technique to silicate glass thin films, as an example, a grid of rods of nanometer dimension can be efficiently produced by rapidly scanning amore » focused electron probe. This nanopatterning is achieved through swift phase separation in the sample, without any post-development processes. The controlled phase separation is induced by massive displacements of cations (glass modifiers) within the glass-former network, driven by the strong local electric fields. The electric field is induced by accumulated charge within the electron probed region, which is generated by the excitation of atomic electrons by the incident electron. Throughput is much improved compared to other scanning probe techniques. Finally, the half-pitch spatial resolution of nanostructure in this particular specimen is 2.5 nm.« less

Local electric field direct writing – Electron-beam lithography and mechanism

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jiang, Nan; Su, Dong; Spence, John C. H.

Local electric field induced by a focused electron probe in silicate glass thin films is evaluated in this paper by the migration of cations. Extremely strong local electric fields can be obtained by the focused electron probe from a scanning transmission electron microscope. As a result, collective atomic displacements occur. This newly revised mechanism provides an efficient tool to write patterned nanostructures directly, and thus overcome the low efficiency of the conventional electron-beam lithography. Applying this technique to silicate glass thin films, as an example, a grid of rods of nanometer dimension can be efficiently produced by rapidly scanning amore » focused electron probe. This nanopatterning is achieved through swift phase separation in the sample, without any post-development processes. The controlled phase separation is induced by massive displacements of cations (glass modifiers) within the glass-former network, driven by the strong local electric fields. The electric field is induced by accumulated charge within the electron probed region, which is generated by the excitation of atomic electrons by the incident electron. Throughput is much improved compared to other scanning probe techniques. Finally, the half-pitch spatial resolution of nanostructure in this particular specimen is 2.5 nm.« less

Electronic properties of conductive pili of the metal-reducing bacterium Geobacter sulfurreducens probed by scanning tunneling microscopy.

PubMed

Veazey, Joshua P; Reguera, Gemma; Tessmer, Stuart H

2011-12-01

The metal-reducing bacterium Geobacter sulfurreducens produces conductive protein appendages known as "pilus nanowires" to transfer electrons to metal oxides and to other cells. These processes can be harnessed for the bioremediation of toxic metals and the generation of electricity in bioelectrochemical cells. Key to these applications is a detailed understanding of how these nanostructures conduct electrons. However, to the best of our knowledge, their mechanism of electron transport is not known. We used the capability of scanning tunneling microscopy (STM) to probe conductive materials with higher spatial resolution than other scanning probe methods to gain insights into the transversal electronic behavior of native, cell-anchored pili. Despite the presence of insulating cellular components, the STM topography resolved electronic molecular substructures with periodicities similar to those reported for the pilus shaft. STM spectroscopy revealed electronic states near the Fermi level, consistent with a conducting material, but did not reveal electronic states expected for cytochromes. Furthermore, the transversal conductance was asymmetric, as previously reported for assemblies of helical peptides. Our results thus indicate that the Geobacter pilus shaft has an intrinsic electronic structure that could play a role in charge transport.

The Effect of Scan Length on the Structure and Mechanical Properties of Electron Beam-Melted Ti-6Al-4V

NASA Astrophysics Data System (ADS)

Everhart, Wesley; Dinardo, Joseph; Barr, Christian

2017-02-01

Electron beam melting (EBM) is a powder bed fusion-based additive manufacturing process in which selective areas of a layer of powder are melted with an electron beam and a part is built layer by layer. EBM scanning strategies within the Arcam AB® A2X EBM system rely upon governing relationships between the scan length of the beam path, the beam current, and speed. As a result, a large parameter process window exists for Ti-6Al-4V. Many studies have reviewed various properties of EBM materials without accounting for this effect. The work performed in this study demonstrates the relationship between scan length and the resulting density, microstructure, and mechanical properties of EBM-produced Ti-6Al-4V using the scanning strategies set by the EBM control software. This emphasizes the criticality of process knowledge and careful experimental design, and provides an alternate explanation for reported orientation-influenced strength differences.

Heart CT scan

MedlinePlus

... Computed tomography scan - heart; Calcium scoring; Multi-detector CT scan - heart; Electron beam computed tomography - heart; Agatston ... table that slides into the center of the CT scanner. You will lie on your back with ...

An inexpensive approach for bright-field and dark-field imaging by scanning transmission electron microscopy in scanning electron microscopy.

PubMed

Patel, Binay; Watanabe, Masashi

2014-02-01

Scanning transmission electron microscopy in scanning electron microscopy (STEM-in-SEM) is a convenient technique for soft materials characterization. Various specimen-holder geometries and detector arrangements have been used for bright-field (BF) STEM-in-SEM imaging. In this study, to further the characterization potential of STEM-IN-SEM, a new specimen holder has been developed to facilitate direct detection of BF signals and indirect detection of dark-field (DF) signals without the need for substantial instrument modification. DF imaging is conducted with the use of a gold (Au)-coated copper (Cu) plate attached to the specimen holder which directs highly scattered transmitted electrons to an off-axis yttrium-aluminum-garnet (YAG) detector. A hole in the copper plate allows for BF imaging with a transmission electron (TE) detector. The inclusion of an Au-coated Cu plate enhanced DF signal intensity. Experiments validating the acquisition of true DF signals revealed that atomic number (Z) contrast may be achieved for materials with large lattice spacing. However, materials with small lattice spacing still exhibit diffraction contrast effects in this approach. The calculated theoretical fine probe size is 1.8 nm. At 30 kV, in this indirect approach, DF spatial resolution is limited to 3.2 nm as confirmed experimentally.

Sample preparation methods for scanning electron microscopy of homogenized Al-Mg-Si billets: A comparative study

DOE Office of Scientific and Technical Information (OSTI.GOV)

Österreicher, Johannes Albert; Kumar, Manoj

Characterization of Mg-Si precipitates is crucial for optimizing the homogenization heat treatment of Al-Mg-Si alloys. Although sample preparation is key for high quality scanning electron microscopy imaging, most common methods lead to dealloying of Mg-Si precipitates. In this article we systematically evaluate different sample preparation methods: mechanical polishing, etching with various reagents, and electropolishing using different electrolytes. We demonstrate that the use of a nitric acid and methanol electrolyte for electropolishing a homogenized Al-Mg-Si alloy prevents the dissolution of Mg-Si precipitates, resulting in micrographs of higher quality. This preparation method is investigated in depth and the obtained scanning electron microscopymore » images are compared with transmission electron micrographs: the shape and size of Mg-Si precipitates appear very similar in either method. The scanning electron micrographs allow proper identification and measurement of the Mg-Si phases including needles with lengths of roughly 200 nm. These needles are β″ precipitates as confirmed by high resolution transmission electron microscopy. - Highlights: •Secondary precipitation in homogenized 6xxx Al alloys is crucial for extrudability. •Existing sample preparation methods for SEM are improvable. •Electropolishing with nitric acid/methanol yields superior quality in SEM. •The obtained micrographs are compared to TEM micrographs.« less

Transfer doping of single isolated nanodiamonds, studied by scanning probe microscopy techniques.

PubMed

Bolker, Asaf; Saguy, Cecile; Kalish, Rafi

2014-09-26

The transfer doping of diamond surfaces has been applied in various novel two-dimensional electronic devices. Its extension to nanodiamonds (ND) is essential for ND-based applications in many fields. In particular, understanding the influence of the crystallite size on transfer doping is desirable. Here, we report the results of a detailed study of the electronic energetic band structure of single, isolated transfer-doped nanodiamonds with nanometric resolution using a combination of scanning tunneling spectroscopy and Kelvin force microscopy measurements. The results show how the band gap, the valence band maximum, the electron affinity and the work function all depend on the ND's size and nanoparticle surface properties. The present analysis, which combines information from both scanning tunneling spectroscopy and Kelvin force microscopy, should be applicable to any nanoparticle or surface that can be measured with scanning probe techniques.

Differences between Subjective Balanced Occlusion and Measurements Reported With T-Scan III

PubMed Central

Lila-Krasniqi, Zana; Shala, Kujtim; Krasniqi, Teuta Pustina; Bicaj, Teuta; Ahmedi, Enis; Dula, Linda; Dragusha, Arlinda Tmava; Guguvcevski, Ljuben

2017-01-01

BACKGROUND: The aetiology of Temporomandibular disorder is multifactorial, and numerous studies have addressed that occlusion may be of great importance in the pathogenesis of Temporomandibular disorder. AIM: The aim of this study is to determine if any direct relationship exists between balanced occlusion and Temporomandibular disorder and to evaluate the differences between subjective balanced occlusion and measurements reported with T-scan III electronic system. MATERIAL AND METHODS: A total of 54 subjects were divided into three groups, selection based on anamnesis-responded to a Fonseca questionnaire and clinical measurements analysed with electronic system T-scan III. In the I study group were participants with fixed dentures with prosthetic ceramic restorations. In the II study group were symptomatic participants with TMD. In the third control group were healthy participants with full arch dentition that completed a subjective questionnaire that documented the absence of jaw pain, joint noise, locking and subjects without a history of TMD. The occlusal balance was reported subjectively through Fonseca questionnaire and compared with occlusion analysed with electronic system T-scan III. RESULTS: For attributive data were used percentage of the structure. Differences in P < 0.05 were considered significant. After distributing attributive data of occlusal balance subjectively reported and compared with measurements analysed with electronic system T-scan III were found significant difference P < 0.001 in all three groups. CONCLUSION: In our study, it was concluded that there were statistically significant differences of balanced occlusion in all three groups. Also it was concluded that subjective data are not exact with measurements reported with electronic device T-scan III. PMID:28932311

Low-Temperature Scanning Capacitance Probe for Imaging Electron Motion

NASA Astrophysics Data System (ADS)

Bhandari, S.; Westervelt, R. M.

2014-12-01

Novel techniques to probe electronic properties at the nanoscale can shed light on the physics of nanoscale devices. In particular, studying the scattering of electrons from edges and apertures at the nanoscale and imaging the electron profile in a quantum dot, have been of interest [1]. In this paper, we present the design and implementation of a cooled scanning capacitance probe that operates at liquid He temperatures to image electron waves in nanodevices. The conducting tip of a scanned probe microscope is held above the nanoscale structure, and an applied sample-to-tip voltage creates an image charge that is measured by a cooled charge amplifier [2] adjacent to the tip. The circuit is based on a low-capacitance, high- electron-mobility transistor (Fujitsu FHX35X). The input is a capacitance bridge formed by a low capacitance pinched-off HEMT transistor and tip-sample capacitance. We have achieved low noise level (0.13 e/VHz) and high spatial resolution (100 nm) for this technique, which promises to be a useful tool to study electronic behavior in nanoscale devices.

The Effect of Electron Beam Irradiation in Environmental Scanning Transmission Electron Microscopy of Whole Cells in Liquid.

PubMed

Hermannsdörfer, Justus; Tinnemann, Verena; Peckys, Diana B; de Jonge, Niels

2016-06-01

Whole cells can be studied in their native liquid environment using electron microscopy, and unique information about the locations and stoichiometry of individual membrane proteins can be obtained from many cells thus taking cell heterogeneity into account. Of key importance for the further development of this microscopy technology is knowledge about the effect of electron beam radiation on the samples under investigation. We used environmental scanning electron microscopy (ESEM) with scanning transmission electron microscopy (STEM) detection to examine the effect of radiation for whole fixed COS7 fibroblasts in liquid. The main observation was the localization of nanoparticle labels attached to epidermal growth factor receptors (EGFRs). It was found that the relative distances between the labels remained mostly unchanged (<1.5%) for electron doses ranging from the undamaged native state at 10 e-/Å2 toward 103 e-/Å2. This dose range was sufficient to determine the EGFR locations with nanometer resolution and to distinguish between monomers and dimers. Various different forms of radiation damage became visible at higher doses, including severe dislocation, and the dissolution of labels.

Fast imaging with inelastically scattered electrons by off-axis chromatic confocal electron microscopy.

PubMed

Zheng, Changlin; Zhu, Ye; Lazar, Sorin; Etheridge, Joanne

2014-04-25

We introduce off-axis chromatic scanning confocal electron microscopy, a technique for fast mapping of inelastically scattered electrons in a scanning transmission electron microscope without a spectrometer. The off-axis confocal mode enables the inelastically scattered electrons to be chromatically dispersed both parallel and perpendicular to the optic axis. This enables electrons with different energy losses to be separated and detected in the image plane, enabling efficient energy filtering in a confocal mode with an integrating detector. We describe the experimental configuration and demonstrate the method with nanoscale core-loss chemical mapping of silver (M4,5) in an aluminium-silver alloy and atomic scale imaging of the low intensity core-loss La (M4,5@840  eV) signal in LaB6. Scan rates up to 2 orders of magnitude faster than conventional methods were used, enabling a corresponding reduction in radiation dose and increase in the field of view. If coupled with the enhanced depth and lateral resolution of the incoherent confocal configuration, this offers an approach for nanoscale three-dimensional chemical mapping.

Ultra-thin resin embedding method for scanning electron microscopy of individual cells on high and low aspect ratio 3D nanostructures.

PubMed

Belu, A; Schnitker, J; Bertazzo, S; Neumann, E; Mayer, D; Offenhäusser, A; Santoro, F

2016-07-01

The preparation of biological cells for either scanning or transmission electron microscopy requires a complex process of fixation, dehydration and drying. Critical point drying is commonly used for samples investigated with a scanning electron beam, whereas resin-infiltration is typically used for transmission electron microscopy. Critical point drying may cause cracks at the cellular surface and a sponge-like morphology of nondistinguishable intracellular compartments. Resin-infiltrated biological samples result in a solid block of resin, which can be further processed by mechanical sectioning, however that does not allow a top view examination of small cell-cell and cell-surface contacts. Here, we propose a method for removing resin excess on biological samples before effective polymerization. In this way the cells result to be embedded in an ultra-thin layer of epoxy resin. This novel method highlights in contrast to standard methods the imaging of individual cells not only on nanostructured planar surfaces but also on topologically challenging substrates with high aspect ratio three-dimensional features by scanning electron microscopy. © 2016 The Authors Journal of Microscopy © 2016 Royal Microscopical Society.

TU-F-18A-06: Dual Energy CT Using One Full Scan and a Second Scan with Very Few Projections

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, T; Zhu, L

Purpose: The conventional dual energy CT (DECT) requires two full CT scans at different energy levels, resulting in dose increase as well as imaging errors from patient motion between the two scans. To shorten the scan time of DECT and thus overcome these drawbacks, we propose a new DECT algorithm using one full scan and a second scan with very few projections by preserving structural information. Methods: We first reconstruct a CT image on the full scan using a standard filtered-backprojection (FBP) algorithm. We then use a compressed sensing (CS) based iterative algorithm on the second scan for reconstruction frommore » very few projections. The edges extracted from the first scan are used as weights in the Objectives: function of the CS-based reconstruction to substantially improve the image quality of CT reconstruction. The basis material images are then obtained by an iterative image-domain decomposition method and an electron density map is finally calculated. The proposed method is evaluated on phantoms. Results: On the Catphan 600 phantom, the CT reconstruction mean error using the proposed method on 20 and 5 projections are 4.76% and 5.02%, respectively. Compared with conventional iterative reconstruction, the proposed edge weighting preserves object structures and achieves a better spatial resolution. With basis materials of Iodine and Teflon, our method on 20 projections obtains similar quality of decomposed material images compared with FBP on a full scan and the mean error of electron density in the selected regions of interest is 0.29%. Conclusion: We propose an effective method for reducing projections and therefore scan time in DECT. We show that a full scan plus a 20-projection scan are sufficient to provide DECT images and electron density with similar quality compared with two full scans. Our future work includes more phantom studies to validate the performance of our method.« less

Minority carrier diffusion length and edge surface-recombination velocity in InP

NASA Technical Reports Server (NTRS)

Hakimzadeh, Roshanak; Bailey, Sheila G.

1993-01-01

A scanning electron microscope was used to obtain the electron-beam-induced current (EBIC) profiles in InP specimens containing a Schottky barrier perpendicular to the scanned (edge) surface. An independent technique was used to measure the edge surface-recombination velocity. These values were used in a fit of the experimental EBIC data with a theoretical expression for normalized EBIC (Donolato, 1982) to obtain the electron (minority carrier) diffusion length.

Choice of range-energy relationship for the analysis of electron-beam-induced-current line scans

NASA Astrophysics Data System (ADS)

Luke, Keung, L.

1994-07-01

The electron range in a material is an important parameter in the analysis of electron-beam-induced-current (EBIC) line scans. Both the Kanaya-Okayama (KO) and Everhart-Hoff (EH) range-energy relationships have been widely used by investigators for this purpose. Although the KO range is significantly larer than the EH range, no study has been done to examine the effect of choosing one range over the other on the values of the surface recombination velocity S(sub T) and minority-carrier diffusion length L evaluated from EBICF line scans. Such a study has been carried out, focusing on two major questions: (1) When the KO range is used in different reported methods to evaluate either or both S(sub T) and L from EBIC line scans, how different are their values thus determined in comparison to those using the EH range?; (2) from EBIC line scans of a given material, is there a way to discriminate between the KO and the EH ranges which should be used to analyze these scans? Answers to these questions are presented to assist investigators in extracting more reliable values of either or both S(sub T) and L and in finding the right range to use in the analysis of these line scans.

Serial block face scanning electron microscopy--the future of cell ultrastructure imaging.

PubMed

Hughes, Louise; Hawes, Chris; Monteith, Sandy; Vaughan, Sue

2014-03-01

One of the major drawbacks in transmission electron microscopy has been the production of three-dimensional views of cells and tissues. Currently, there is no one suitable 3D microscopy technique that answers all questions and serial block face scanning electron microscopy (SEM) fills the gap between 3D imaging using high-end fluorescence microscopy and the high resolution offered by electron tomography. In this review, we discuss the potential of the serial block face SEM technique for studying the three-dimensional organisation of animal, plant and microbial cells.

Realistic representation of Bacillus subtilis biofilms architecture using combined microscopy (CLSM, ESEM and FESEM).

PubMed

Bridier, A; Meylheuc, T; Briandet, R

2013-05-01

In this contribution, we used a set of microscopic techniques including confocal laser scanning microscopy (CLSM), environmental scanning electron microscopy (ESEM) and field emission scanning electron microscopy (FESEM) to analyze the three-dimensional spatial arrangement of cells and their surrounding matrix in Bacillus subtilis biofilm. The combination of the different techniques enabled a deeper and realistic deciphering of biofilm architecture by providing the opportunity to overcome the limits of each single technique. Copyright © 2013 Elsevier Ltd. All rights reserved.

Low-temperature and conventional scanning electron microscopy of human urothelial neoplasms.

PubMed

Hopkins, D M; Morris, J A; Oates, K; Huddart, H; Staff, W G

1989-05-01

The appearance of neoplastic human urothelium viewed by low-temperature scanning electron microscopy (LTSEM) and conventional scanning electron microscopy (CSEM) was compared. Fixed, dehydrated neoplastic cells viewed by CSEM had well-defined, often raised cell junctions; no intercellular gaps; and varying degrees of pleomorphic surface microvilli. The frozen hydrated material viewed by LTSEM, however, was quite different. The cells had a flat or dimpled surface, but no microvilli. There were labyrinthine lateral processes which interdigitated with those of adjacent cells and outlined large intercellular gaps. The process of fixation and dehydration will inevitably distort cell contours and on theoretical grounds, the images of frozen hydrated material should more closely resemble the in vivo appearance.

Use of light, scanning electron microscopy and bioassays to evaluate parasitism by entomopathogenic fungi of the red scale insect of palms (Phoenicococcus marlatti Ckll., 1899).

PubMed

Asensio, L; Lopez-Llorca, L V; López-Jiménez, J A

2005-01-01

We have evaluated the parasitism of the red scale insect of the date palm (Phoenicococcus marlatti) by entomopathogenic fungi, using light microscopy (LM), scanning electron microscopy (SEM) and low temperature scanning electron microscopy (LTSEM). Beauveria bassiana, Lecanicillium dimorphum and Lecanicillium cf. psalliotae, were inoculated directly on the scale insects or on insect infested plant material. We found that L. dimorphum and L. cf. psalliotae developed on plant material and on scale insects, making infection structures. B. bassiana was a bad colonizer of date palm leaves (Phoenix dactylifera L.) and did not parasite the scale insects.

Further description of Cruzia tentaculata (Rudolphi, 1819) Travassos, 1917 (Nematoda: Cruzidae) by light and scanning electron microscopy.

PubMed

Adnet, F A O; Anjos, D H S; Menezes-Oliveira, A; Lanfredi, R M

2009-04-01

Species of Cruzia are parasites of the large intestine of marsupials, reptiles, amphibians, and mammalians. Cruzia tentaculata specimens were collected from the large intestine of Didelphis marsupialis (Mammalia: Didelphidae) from Colombia (new geographical record) and from Brazil and analyzed by light and scanning electron microscopy. The morphology of males and females by light microscopy corroborated most of the previous description and the ultrastructure by scanning electron microscopy evidence: the topography of the cuticle, deirids, amphids, phasmids in both sexes, a pair of papillae near the vulva opening, and the number and location of male caudal papillae, adding new features for species identification only observed by this technique.

Ionic liquid compatibility in polyethylene oxide/siloxane ion gel membranes

DOE PAGES

Kusuma, Victor A.; Macala, Megan K.; Liu, Jian; ...

2018-10-02

Ion gel films were prepared by incorporating eight commercially available ionic liquids in two different cross-linked polymer matrices to evaluate their phase miscibility, gas permeability and ionic conductivity for potential applications as gas separation membranes and solid electrolyte materials. The ionic liquids cations were 1-ethyl-3-methylimidazolium, 1-ethyl-3-methylpyridinium, 1-butyl-1-methylpyrrolidinium, tributylmethylphosphonium, and butyltrimethylammonium with a common anion (bis(trifluoromethylsulfonyl)imide). In addition, ionic liquids with 1-ethyl-3-methylimidazolium cation with acetate, dicyanamide and tetrafluoroborate counterions were evaluated. The two polymers were cross-linked poly(ethylene oxide) and cross-linked poly(ethylene oxide)/siloxane copolymer. Differential scanning calorimetry, X-ray diffractometry and visual observations were performed to evaluate the ion gels’ miscibility, thermal stabilitymore » and homogeneity. Ionic liquids with the least basic anion (bis(trifluoromethylsulfonyl)imide) and aromatic cations containing acidic proton (e.g. imidazolium and pyridinium) gave the most stable and miscible ion gels. Phase stability was shown to be a function of both ionic liquid content and temperature, with phase separation observed at elevated temperatures. In conclusion, gas permeability testing with carbon dioxide and nitrogen and ionic conductivity measurements confirmed that these ionic liquids increased the gas permeability and ionic conductivity of the polymers.« less

Ionic liquid compatibility in polyethylene oxide/siloxane ion gel membranes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kusuma, Victor A.; Macala, Megan K.; Liu, Jian

Ion gel films were prepared by incorporating eight commercially available ionic liquids in two different cross-linked polymer matrices to evaluate their phase miscibility, gas permeability and ionic conductivity for potential applications as gas separation membranes and solid electrolyte materials. The ionic liquids cations were 1-ethyl-3-methylimidazolium, 1-ethyl-3-methylpyridinium, 1-butyl-1-methylpyrrolidinium, tributylmethylphosphonium, and butyltrimethylammonium with a common anion (bis(trifluoromethylsulfonyl)imide). In addition, ionic liquids with 1-ethyl-3-methylimidazolium cation with acetate, dicyanamide and tetrafluoroborate counterions were evaluated. The two polymers were cross-linked poly(ethylene oxide) and cross-linked poly(ethylene oxide)/siloxane copolymer. Differential scanning calorimetry, X-ray diffractometry and visual observations were performed to evaluate the ion gels’ miscibility, thermal stabilitymore » and homogeneity. Ionic liquids with the least basic anion (bis(trifluoromethylsulfonyl)imide) and aromatic cations containing acidic proton (e.g. imidazolium and pyridinium) gave the most stable and miscible ion gels. Phase stability was shown to be a function of both ionic liquid content and temperature, with phase separation observed at elevated temperatures. In conclusion, gas permeability testing with carbon dioxide and nitrogen and ionic conductivity measurements confirmed that these ionic liquids increased the gas permeability and ionic conductivity of the polymers.« less