Natural bone consists of hard nanostructured hydroxyapatite (HA) in a nanostructured protein-based soft hydrogel template (ie, mostly collagen). For this reason, nanostructured HA has been an intriguing coating material on traditionally used titanium for improving orthopedic applications. In addition, helical rosette nanotubes (HRNs), newly developed materials which form through the self-assembly process of DNA base pair building blocks in body solutions, are soft nanotubes with a helical architecture that mimics natural collagen. Thus, the objective of this in vitro study was for the first time to combine the promising attributes of HRNs and nanocrystalline HA on titanium and assess osteoblast (bone-forming cell) functions. Different sizes of nanocrystalline HA were synthesized in this study through a wet chemical precipitation process following either hydrothermal treatment or sintering. Transmission ...
SummaryThe numerous applications of hydrogelators have led to rapid expansion of this field. In the present work we report the facile synthesis of amphiphilic hydrogelators having a quaternary...Full Text Available
The purpose of the present study was to prepare a novel domperidone hydrogel. The domperidone dispersion was prepared by the solvent evaporation method. The characteristics of domperidone dispersion...Full Text Available
A tobermorite/hydroxyapatite composite was prepared by hydrothermal treatment using diatomaceous earth, ?-tricalcium phosphate and slaked lime starting materials. The XRD patterns of the composite confirmed that tobermorite and hydroxyapatite were formed after the hydrothermal process. The bending strength of the composite reached a level higher than 9?MPa after the hydrothermal process. The development of the bending strength was due to the formation of tobermorite and hydroxyapatite during the hydrothermal process. The composite had a high specific surface area due to these newly formed crystals.
The effects of pH on the calcium phosphate phase, of Tris and of amino acids, such as aspartic acid, glutamic acid, and serine on hydroxyapatite formation and morphology, were studied in double diffusion experiments. In this system, hydroxyapatite was only formed when the pH was around 7.4 or higher for the duration of the reaction. A decrease in pH resulted in the transformation of hydroxyapatite to octacalcium phosphate. Amino acids and Tris or the buffering capacity of Tris have an effect on the morphology of the synthetic hydroxyapatite. The presence of the additive results in spheres consisting of needles, blades or plates depending on the reaction system. PMID:12175941
In this study, we report the physico-chemical and biological properties of a novel biodegradable composite scaffold made of nano-hydroxyapatite and natural derived polymers of chitosan and carboxymethyl...Full Text Available
The gelation kinetics of an in situ gelable hydrogel formulated from oxidized dextran (Odex) and N-carboxyethyl chitosan (CEC) were investigated rheologically. Both Schiff base...Full Text Available
A series of in situ gelable hydrogels were prepared from oxidized dextran (Odex) and N-carboxyethyl chitosan (CEC) without any extraneous crosslinking agent. The gelation readily...Full Text Available
Background Photopolymerizable poly(ethylene glycol) (PEG) hydrogels offer a platform to deliver cells in vivo and support three-dimensional cell culture but should be designed to degrade in sync with neotissue development and endure the physiologic environment. Questions/purposes We asked whether (1) incorporation of degradation into PEG hydrogels facilitates tissue development comprised of essential cartilage macromolecules; (2) with early loading before pericellular matrix formation, the duration of load affects matrix production; and (3) dynamic loading in general influences macroscopic tissue development. Methods Primary bovine chondrocytes were encapsulated in hydrogels (n?=?3 for each condition). The independent variables were hydrogel degradation (nondegrading PEG and degrading olig...
Invasive fungal infections can be devastating, particularly in immunocompromised patients, and difficult to treat with systemic drugs. Furthermore, systemic administration of those medications...Full Text Available
Protein hydrogels were prepared by substituting ovalbumin with different concentrations of ethyl vinyl sulfone (EVS) or acrylic acid (AA) and crosslinking with divinyl sulfone (DVS). Fourier transform-infrared (FT-IR) spectroscopic studies confirmed the addition of EVS, AA, and DVS onto the protein. Swelling was assessed as a function of pH in the range of 2.5 to 9.4 and ionic strength. The elastic modulus of the gels was determined in shear and compression. Stress relaxation was assessed in compression. The substituent highly affected swelling and modulus with both hydrogels displaying non-Gaussian behavior in the range of hydrogel environments studied. Acrylic acid substituted ovalbumin exhibited a decreasing modulus with increasing swelling behaving as a polyelectrolyte with low added s...
Current bioartificial extra-corporeal systems are bioreactors where cells are separated from the surrounding media by porous polymeric membranes. The present work focuses on the design of membranes that allow the differential diffusion of plasma metabolites and proteins such as immunoglobulin (IgG). This design will improve catabolites removal and reduce possible immune response and virus infection. We demonstrate the feasibility to synthesize the hydrogels confined to the macroporous structure of membranes by radiation-induced in situ polymerization. The hollow-fiber membranes were soaked in aqueous monomeric solution, rinsed and irradiated while submerged in oil. This procedure confined the hydrogel to the void internal volume of the pores of the membrane. Hydrogels of polyacrylamide and polyHEMA were synthesized this way by irradiation at 10 kGy. Hydraulic permeability and diffusion of glucose, albumin and IgG were ...
Nanocrystalline and nanostructured materials offer unique microstructure-dependent properties that are superior to coarse-grained materials. These materials have been shown to have very high hardness, strength, and wear resistance. However, most current methods of producing nanostructured materials in weapons-relevant materials create powdered metal that must be consolidated into bulk form to be useful. Conventional consolidation methods are not appropriate due to the need to maintain the nanocrystalline structure. This research investigated new ways of creating nanocrystalline material, new methods of consolidating nanocrystalline material, and an analysis of these different methods of creation and consolidation to evaluate their applicability to mesoscale weapons applications where part features are often under 100 {micro}m wide and the material's microstructure must be very small to give ...
The aim of this study was to develop a nanostructured Nb2O5-natural hydroxyapatite bulk composite to serve as an alternative biocompatible bulk material for implants. A set of samples of hydroxyapatite from fish bones with different concentrations of Nb2O5 were designed. They were prepared through a milling process, compacted under different pressures (350, 450, 550 and 650MPa) and sintered in air atmosphere at 1000^oC for 1h. The results revealed that the prepared composites presented strong interactions between the two elements and showed improvement in the sinterability with significant densification and microstructure changes, suggesting that they are promising for implants meant to replace bone tissues.
In the present paper, the effects of hydroxyapatite (HA) content on the microstructure, thermal and mechanical properties of Ti-based glassy alloy/HA composite prepared by spark plasma sintering (SPS) are investigated. The microstructure of the composites is homogeneous when the HA is lower than 2 wt%. When the HA content is higher than 3 wt%, the crystalline precipitates with size of less than 5 nm are distributed in the glassy matrix. HA decomposes during sintering procedure for the composite with high HA content. With increasing HA addition, compressive strength decreases. Especially for the HA content is over 2 wt%, the strength decreases sharply because of partial crystallization of glassy alloy matrix.
Polyurethane (PU) foam was combined with protein drug-loaded pH-sensitive alginate-bentonite hydrogel for wound dressings. Alginate is a linear copolymer composed of 1?4-linked ?-D-mannuronic acid (M) and its c-5-epimer ?-Lguluronic acid (G). The amount of (M) and (G) and their sequential distribution are varied depending on the alginate source. Soluble sodium alginate can become a hydrogel when cross-linked with divalent cations and has widespread applications in the food, drink, pharmaceutical and bioengineering industries. Recently, it has been also proposed as a biomaterial for drug delivery systems. Bentonites are the natural inorganic polymers consisting of a large proportion of expandable clay minerals with a three-layer structure such as montmorillonite, beidellite, nontronite, etc...
The present study was carried out to exploit the feasibility of using polymeric nanosponges as an alternative carrier for targeting econazole nitrate (EN) to the skin through topical hydrogel formulation. Nanosponges prepared by emulsion solvent diffusion method were evaluated for various physicochemical parameters and in vitro drug release. The nanosponges of EN were discrete free flowing nanosized particles with perforated orange peel like morphology as visualized by SEM. The nanosponge formulated using PVA:EC (3:2) displayed highest in vitro release after 12 ?h in phosphate buffer (pH 6.8) that fitted matrix model. Selected nanosponge was formulated as Carbopol 934 NF hydrogel using varying concentrations of permeation enhancers propylene glycol and N-methyl-2-pyrrolidone. The EN nanosp...
The effect of reinforcement in the cross-linked poly(propylene fumarate-co-caprolactone diol) thermoset composites based on Kevlar fibres and hydroxyapatite was studied. Cross-linked poly(propylene...Full Text Available
Craniofacial injuries require a variety of different cell types to repopulate areas of bone, cartilage, tendon, and fat. Mesenchymal stem cells (MSCs) provide a multipotent cell source for tissue...Full Text Available
The main objective of Phase I of this SBIR project was to demonstrate the feasibility for successful development of an antimicrobial wound dressing based on a hydrogel sustained release matrix. This goal has been achieved. In vitro studies of drug diffusi...
We propose and demonstrate a facile room-temperature synthetic method for obtaining water-soluble magnetic Fe3O4 nanoparticles (NPs) by combining the in situ synthesis and decomposition of a magnetic polymer hydrogel. The Fe3O4 NPs with average diameters of 6.3-8.3nm were synthesized in a cross-linked polyacrylamide (PAAm) hydrogel by coprecipitating iron ions. The decomposition of the magnetic polymer hydrogel by an aqueous solution of sodium hydroxide led to the transfer of Fe3O4 NPs into the aqueous medium. The NPs can be dispersed stably in water for more than three months. The Fe3O4 NPs were characterized by X-ray photoelectron spectra (XPS), X-ray powder diffraction (XRD), transmission electron microscope (TEM), and Fourier transform infrared spectroscopy (FT-IR). The saturation magn...
Hydroxyapatite samples were produced by two different wet-chemical methods, and characterized by x-ray diffraction, infrared and compression strength measurements. The x-ray diffraction measurements were simulated using the Rietveld method, and structural data as lattice parameters and average crystallite size were obtained. The infrared spectra showed the presence of CO$_3^{2-}$ ions in all samples, indicating a contamination by these ions. By mixing samples produced by both methods, a bioceramic was obtained and, after sintering, samples with very high compression strengths (26--30 MPa) were obtained.
Bulk nanocrystalline pure iron rods were fabricated by the equal channel angular pressure (ECAP) technique up to eight passes. The microstructure and grain size distribution, natural immersion and electrochemical corrosion in simulated body fluid, cellular responses and hemocompatibility were investigated in this study. The results indicate that nanocrystalline pure iron after severe plastic deformation (SPD) would sustain durable span duration and exhibit much stronger corrosion resistance than that of the microcrystalline pure iron. The interaction of different cell lines reveals that the nanocrystalline pure iron stimulates better proliferation of fibroblast cells and preferable promotion of endothelialization, while inhibits effectively the viability of vascular smooth muscle cells (VSMCs). The burst of red cells and adhesion of the platelets were also substantially suppressed on contact with the ...
Parameters of permanent magnets result from the combination of intrinsic properties such as saturation magnetization, magnetic exchange, and magnetocrystalline energy, as well as microstructural parameters such as phase structure, grain size, and orientation. Reduction of grain size into nanocrystalline regime (#approx# 50 nm) leads to the enhanced remanence which derives from ferromagnetic exchange coupling between highly refined grains. In this study the fundamental phenomena, quantities, and structure parameters, which define nanophase permanent magnets are presented and discussed. The theoretical considerations are confronted with experimental data for nanocrystalline Sm-Fe-N type permanent magnets. (author)
Nanocrystalline zeolites with discrete crystal sizes of less than 100 nm have different properties relative to zeolites with larger crystal sizes. Nanocrystalline zeolites have improved mass transfer properties and very large internal and external surface areas that can be exploited for many different applications. The additional external surface active sites and the improved mass transfer properties of nanocrystalline zeolites offer significant advantages for selective catalytic reduction (SCR) catalysis with ammonia as a reductant in coal-fired power plants relative to current zeolite based SCR catalysts. Nanocrystalline NaY was synthesized with a crystal size of 15-20 nm and was thoroughly characterized using x-ray diffraction, electron paramagnetic resonance spectroscopy, nitrogen adsorption isotherms and Fourier Transform Infrared (FT-IR) spectroscopy. Copper ions were exchanged into ...
Recent advances made in the area of amorphous and nanocrystalline alloys exhibiting high saturation inductions are reviewed. A new chemical composition was identified that achieves a saturation induction of 1.64 T in an iron-based amorphous alloy. This alloy, when used in electrical transformers, shows a much improved performance over the existing amorphous alloy. Nanocrystalline FeCoCuNbSiB alloys are found to have saturation induction levels reaching 1.7 T. These materials are suited for use in sensors and inductors carrying large currents. Some of these nanocrystalline alloys show a BH squareness ratio exceeding 90%, which can be utilized in pulse power devices. Recent developments in the applications of these materials are also pointed out.
Nanocrystalline materials can exhibit properties which are considerably different from their coarse-grained counterparts, making them unique for basic or applied research and also very promising for potential applications. The topics which are addressed in the present paper are magnetic properties and magnetic correlations on the nanometer scale, mechanical properties, in particular the influence of grain boundaries on the elastic and plastic behaviour, and vibration models of grain boundary atoms in nanostructured materials. (author)
This report contains detailed information of the research program entitled "Development of Bulk Nanocrystalline Cemented Tungsten Carbide Materials for Industrial Applications". The report include the processes that were developed for producing nanosized WC/Co composite powders, and an ultrahigh pressure rapid hot consolidation process for sintering of nanosized powders. The mechanical properties of consolidated materials using the nanosized powders are also reported.
Ultra-fine ZnAl2O4 spinel hydrogel precursor synthesized from mixed salt solutions of Zn^2^+ and Al^3^+ ions using ammonium hydroxide-hexamethylenetetramine as basic media for co-precipitation was used as bonding material and sintering aid for pure alumina system. The hydrogel powder exhibited some well-defined ZnAl2O4 spinel phases at 800^oC. Alumina compacts were fabricated by incorporating small proportions of the precursor in alumina powder and firing at different temperatures (1350-1500^oC). The degree of densification was studied by measurement of fired shrinkage, apparent porosity, bulk density and cold crushing strength. Phase compositions and microstructural features of sintered samples were evaluated by XRD and SEM respectively. Addition of 0.2% hydrogel powder to alumina exhibit...
Microwave-hydrothermal processing was compared with conventional hydrothermal processing in the crystallization of hematite from 1M ferric nitrate and hydroxyapatite from calcium oxide and phosphoric acid. Microwave-hydrothermal processing led to the crystallization of hematite while convention-hydrothermal process led to the crystallization of a mixture of goethite and hematite under the same temperature conditions. Thus the crystallization of hematite which is the stable iron oxide phase at high temperatures has been catalyzed by microwaves. Microwave-hydrothermal processing also led to highly crystalline hydroxyapatite powders compared to the conventional hydrothermal processing which also points to the catalytic role of microwaves. The microwave induced effects may be attributed to the generation of localized high temperatures at the reaction sites which enhance reaction rates.
Novel fluoroalkyl end-capped vinyltrimethoxysilane oligomer/hydroxyapatite (HAp) nanocomposites were prepared by the reaction of calcium nitrate tetrahydrate and phosphoric acid in the presence of the corresponding oligomer. These fluorinated oligomer/HAp composites thus obtained are nanometer size-controlled fine particles (83-173 nm), and were found to exhibit good dispersibility in methanol, ethanol, and isopropyl alcohol. These fluorinated HAp nanocomposites were applied to the surface modification of glass and poly(methyl methacrylate) (PMMA) to exhibit good hydro- and oleophobic characteristics imparted by fluorine on their surface. In addition, the surface structural changes of the modified polyethylene terephtalate and PMMA films treated with these fluorinated nanocomposites before...
In situ composite coating of hydroxyapatite (HA)/TiO2 were produced on titanium (Ti) substrate by micro-arc oxidation coupled with electrophoretic deposition (MAO&EPD) technique with different concentrations of HA particles in the 0.2M NaOH electrolyte solution. The surface morphology and chemical composition of the hybrid coating were effected by HA concentration. The amount of HA particles incorporated into coating layer increased with increasing HA concentration used in the electrolyte solution. The corrosion behavior of the coating layer in simulated body fluids (SBF) was evaluated using a potentiodynamic polarization test. The corrosion resistance of the coated sample was increased compared to the untreated Ti sample. The in vitro bioactivity assessment showed that the MAO&EPD treated...
The purpose of this study was to investigate whether hydroxyapatite (HAp) coating could induce polyethylene terephthalate (PET) artificial ligament graft osseointegration in the bone tunnel. Twenty-four New Zealand white rabbits underwent artificial ligament graft transplantation in bilateral proximal tibia tunnels. One limb was implanted with HAp-coated PET graft, and the contralateral limb was implanted with non-HAp-coated PET graft as control. The rabbits were randomly sacrificed at four and eight?weeks after surgery. The loads to failure of the experimental group at eight?weeks were significantly higher than those of the control group (p?=?0.0057). Histologically, application of HAp coating induced new bone formation between graft and bone at eight?weeks compared with the controls. Rea...
The formation of a porous coating is the decisive feature for the bio-compatibility of silica-free calcium phosphate glass ceramics on alloy surfaces like the #beta#-Ti structured Ti-29Nb-13Ta-4.6Zr used in this work. The ceramic composition is highly important: 50CaO-40P_2O_5-7Na_2O-3TiO_2 glass powder produces a pore-free coating unable to bind hydroxyapatite, whereas 60CaO-30P_2O_5-7Na_2O-3TiO_2 glass incorporates pores from which a crystalline hydroxyapatite phase can grow over the surface from simulated body fluid (see Figure). (Abstract Copyright [2003], Wiley Periodicals, Inc.)
Greenman J, Thorn RMS, Saad S, Austin AJ. In vitro diffusion bed, 3-day repeat challenge `capacity' test for antimicrobial wound dressings. Int Wound J 2006;3:322-329. Abstract The aim of this study was to develop an in vitro wound infection model that allows the comparison of the bacterial kill rate of antimicrobial wound dressings over the course of 3 days, with renewed microbial challenges each day, under realistic wound-like conditions. A test bed model of a moderately exuding wound was constructed from a hydrogel containing releasable foetal calf serum (FCS), and cellulose discs dosed with test microbes (Methicillin-resistant Staphylococcus aureus and Pseudomonas aeruginosa) suspended in 50% FCS applied at the interface between the test dressing and the hydrogel test bed. Freshly prep...
In this study, the thermodynamic stability of the grain boundaries and the grain growth of nanocrystalline Palladium (Pd) at various temperatures were investigated. For this purpose, the Gibbs free energy curves of grain boundaries were plotted in terms of the excess volume by the use of the equation of state (EOS) and Song's thermodynamic models. The results showed that, according to the prediction of these models, the nanocrystalline growth in metals was stopped at the grain sizes less than the critical grain size. Also, the results of the temperature variations and its effect on the Gibbs free energy curves showed that by the increase of the temperature, the possibility for the stoppage of grain growth is facilitated and the critical grain size is increased. To investigate the validity ...
In this study nanocrystalline powders of yttria-stabilized zirconia (ZrO_2-8Y_2O_3) have been synthesized through 'polymerized complex method'. Zirconium chloride, yttrium nitrate, citric acid and ethylene glycol were polymerized at 80 "oC to produce a gel-like mass in which metallic ions were uniformly distributed. During the thermal treatment of dried gel, nanocrystalline powder was formed at 450 "oC and 650 "oC for 2 h. Thermal reactions and crystalline phase formation of the dried gel were investigated through thermal analysis and X-ray diffraction analysis, respectively. The results of thermal analysis and XRD showed the formation of nanocrystalline powder at less than 600 "oC. Chemical bonding of the dried gel was investigated by Fourier transform infrared spectroscopy analysis. Morphology of powder calcined at 650 "oC was analyzed by scanning electron microscope. Yttria-stabilized zirconia powders with the mean ...
Practical procedures were developed for large-scale microbial decontamination of dry egg powder and gelatine with gamma radiation ("6"0Co). The formation and lifes of free organic radicals in these materials were examined by ESR measurements of powder samples. The concentration of these radicals was studied in dependence on the time of storage. Secondary oxidation of egg fats by air oxygen was investigated. Sensoric tests of irradiated gelatine, both in powder and hydrogel form, were performed. (author). 4 figs., 2 tabs., 2 refs.
Urine is a potential source of diagnostic biomarkers for detection of diseases, and is a very attractive means of non-invasive biospecimen collection. Nonetheless, proteomic measurement in urine...Full Text Available
New data about the structure of high-temperature resistant metalloceramic plasma sprayed coatings in micro and nano areas are presented. Application of the new instrumental methods: transmission electron microscopy combined with selected area electron diffraction mode is possible to obtain these data. The first layer in Ni based metallic bond coat shows nanocrystalline structure. External ceramic layer based on stabilised ZrO_2 is polycrystalline and contains both cubic and tetragonal crystalline phases. Local inhomogeneities in coatings phase composition are determined. (author)
A mixture of powders of silica and aluminum nitride is subjected to high-energy ball milling for different milling times. This material is subsequently compacted by uniaxial pressing and sintered at 1450 deg. C. The resulting pellets are crushed and analysed by X-ray diffraction. For short milling times, the amount of phase transformation is minimal and the resulting material mostly consists of cristobalite and aluminum nitride. For long milling times, nanocrystalline #beta#-SiAl_2O_2N_2 is mainly produced.
Nanocrystalline processing by inert gas condensation has the inherent advantages of generating: (1) high surface area nanoclusters, (2) non-stoichiometric oxides, and (3) high dispersions of dopants. This approach is exploited in the synthesis of fluorite-structured catalysts for SO{sub 2} reduction by CO. Nanocrystalline CeO{sub 2{minus}x}, La-doped CeO{sub 2{minus}x}, and Cu-doped CeO{sub 2{minus}x} were produced by magnetron sputtering from a pure or mixed metal target, followed by controlled oxidation of the metallic clusters. The as-prepared doped and undoped nanocrystalline CeO{sub 2{minus}x} materials were found to be excellent catalysts for complete SO{sub 2} conversion to elemental sulfur. Undoped nanocrystalline CeO{sub 2{minus}x} enabled light-off at 460 C, a temperature {approximately} 120 C lower than that over polycrystalline CeO{sub 2}, which is a novel effective catalyst itself. The high ...
Four species of nanocomposites organized by hydroxyapatite (HAp), hyaluronic acid (HyA), chondroitin sulfate (ChS) and type II collagen (Col), i.e. HAp/HyA, HAp/ChS, HAp/HyA/Col and HAp/ChS/Col composites, were synthesized by coprecipitation methods. The composites could retain lots of water: 40%, 32%, 42% and 58% for the HAp/HyA, HAp/ChS, HAp/HyA/Col and HAp/ChS/Col composites, respectively. Transmission electron microscopy observations revealed that the HAp/HyA and HAp/ChS composites consisted of island-like aggregations whose sizes were 300 nm in length and 30 nm in width, and 150 nm in length and 30 nm in width, respectively. In the aggregations, there were many HAp nanocrystals of 20 nm in length, and their c-axes were aligned along the respective polymer molecules through a self-organization process. Animal tests showed that chondrocyte-like cells penetrated into the HAp/ChS/Col composites 4 weeks after implantation. It was shown that the HAp/ChS/Col ...
In this study, Multi-Walled Carbon Nanotubes (MWCNTs) / Hydroxylapatite (HAp) composites were made to improve mechanical properties by using Spark Plasma Sintering (SPS) method. Slurry 6 mol of CaHPO4#centre dot#2H2O (DCPD), 4 mol calcium hydroxide and MWCNTs were mixed and sintered by using SPS at 5-120 MPa pressure, 1200-1250 deg. C and in vacuum or N2 atmosphere. The fracture toughness of sintered MWCNTs/HAp composites was increased.
The concept of nanocrystal conversion chemistry, which involves the use of pre-formed nanoparticles as templates for chemical transformation into derivative solids, has emerged as a powerful approach for designing the synthesis of complex nanocrystalline solids. The general strategy exploits established synthetic capabilities in simple nanocrystal systems and uses these nanocrystals as templates that help to define the composition, crystal structure, and morphology of product nanocrystals. This article highlights key examples of 'conversion chemistry' approaches to the synthesis of nanocrystalline solids using a variety of techniques, including galvanic replacement, diffusion, oxidation, and ion exchange. The discussion is organized according to classes of solids, highlighting the diverse target systems that are accessible using similar chemical concepts: metals, oxides, chalcogenides, phosphides, alloys, intermetallic compounds, sulfides, and ...
Nanocrystalline Fe75Si20M5 (M = Al, B and Cr) powders were synthesized by mechanical alloying in a planetary ball mill from high purity elemental powders. Evolution of non-equilibrium solid solutions of ?-Fe[Si,(Al, B, Cr)] with a nanocrystalline structure was accompanied by the introduction of a large number of dislocation defects in the course of the milling process. Fe sites get substituted by Si and M (M = Al, B, Cr) atoms during the milling process. The structural change and the resulting disorder are reflected in the changes in the lattice parameter and average magnetic moment of the powders milled for various time periods. The effective magnetic anisotropy increases linearly with the milling time. An increase in coercivity with increasing milling time was observed which could be attributed to the introduction of dislocations and the reduction in the powder particle size during milling. The presence of dislocations and grain boundaries ...
Previous investigations have shown that both the early biological response and the mechanical properties of a porous hydroxyapatite bone graft substitute are highly sensitive to its pore structure. The objective of this study was to evaluate whether the pore structure continued to influence bone integration in the medium to long term. Two screened batches of porous hydroxyapatite (PHA) designated as batch A and batch B, with porosities of approximately 60 and 80%, respectively, were selected for this study and implanted for periods of 5, 13, and 26 weeks into the lower femur of New Zealand White rabbits. Histomorphometric analysis of the absolute volume of bone ingrowth within batch A and B implants from 5 to 26 weeks showed that the absolute volume of bone ingrowth was consistently lower in batch A (10-21%), compared to batch B implants (24-31%). However, when the volume of bone ingrowth was normalised for the available pore space, this ...
In this work, a new sol-gel auto-combustion method has been performed to synthesize single phase nickel ferrite nanocrystalline powders by using n-cetyltrimethylammonium bromide, as a cationic surfactant. The gels were prepared from ferric and nickel nitrates and citric acid. Ammonia was used as pH adjusting agent as well. The effects of the surfactant on the after combustion calcination process and the reduction of the resulting powder crystallite size which affects the magnetic properties of the material were investigated by XRD and DTA/TGA techniques. The results showed that the ignition of the gels in air have a self-propagating behavior. Addition of surfactant to the starting solution affected the crystallite size of the synthesized powders and their phase constitution. The crystallit...
Nanocrystalline MnO thin film has been prepared by a pulsed laser deposition (PLD) method. The reversible lithium storage capacity of the MnO thin film electrodes at 0.125C is over 472 mAh g{sup -1} (3484 mAh cm{sup -3}) and can be retained more than 90% after 25 cycles. At a rate of 6C, 55% value of the capacity at 0.125C rate can be obtained for both charge and discharge. As-prepared MnO thin film electrodes show the lowest values of overpotential for both charge and discharge among transition metal oxides. All these performances make MnO a promising high capacity anode material for Li-ion batteries. (author)
The use of X-ray diffraction line profile analysis for the study of nanocrystalline powders is described. The fundamentals of the theory are presented in terms of crystallite/domain size, size distribution, lattice distortion, dislocations density and stacking faults. Line profile parameters and the methods of pattern fitting introduced to overcome the diffraction-line overlap problem are discussed. The approaches based of the integral breadth of the measured line profiles and the Fourier method are discussed. In addition, simplified approaches are also commented. Representative examples are selected to illustrate various cases of microstructure, such as nanomaterials with strain-free spherical nano crystallites, strain-free crystallites with anisotropic crystallite shape, anisotropic crystallites with microstrains and spherical crystallites with dislocation densities and crystallite size distributions. (author)
Magnetic properties of Fe-Co-Mo-Cu-B alloy system with Co up to 26at.% were investigated. After proper thermal treatment, the nanocrystalline grain remains tiny, the density hardly increases, but the room-temperature saturation attains 1.5T mainly due to a high enough Curie temperature. The generally observed slant hysteresis loops point to ribbon surfaces, which stress the ribbon interior and induce a specific magnetoelastic contribution to hard-ribbon-axis magnetic anisotropy even after vacuum annealing. The effect does not come from cobalt but rather from the lack of silicon. Partial removal of the surfaces resulted in a decrease of the loop tilt.
The EXAFS-study (Fe, Sn and Ge K-edges) of disordered by mechanical activation binary supersaturated nanocrystalline solid solutions Fe-Al, Fe-Ge, Fe-Sn and Fe-Si is presented. The EXAFS-spectra are processed by solving the inverse binary problem, using the EXAFS-spectrum of the Fe K-edge only or combining the EXAFS-spectra on two K-edges, Fe and Ge or Fe and Sn. The parameters of partial correlation functions indicate chemical short-range ordering, high local static distortions in the lattice, increasing with metalloid content. The macrostructure of other type is forming through an initial, 'local' stage within the bcc lattice.
In this project, nanocrystalline SnO2 powders were successfully prepared by (a) citrate sol-gel and (b) direct precipitation methods. Powders were characterized using thermal analysis techniques (DTA-TG-DSC), X-ray powder Diffraction (XRD), surface area (BET) and electrical conductivity measurements. XRD patterns showed the presence of the cassiterite structure. SnO2 particles, prepared through sol-gel method exhibit crystallite sizes in the range from 3.1 to 22.3 nm when the gel is heat treated at different temperatures up to 900?C. SnO2 nanocrystallites prepared by the precipitation method are comparatively larger in size. The higher specific surface area was obtained for the powder prepared using sol-gel method and the obtained average grain size (d) is relatively large compared with th...
In the present work, bulk amorphous and nanocrystalline Al83Fe17 alloys were obtained by consolidation of mechanically alloyed powders. Mechanical alloying of Al-17% Fe powder mixture yielded powder with an amorphous structure. Thermal behaviour of the milling product was examined using differential scanning calorimetry. This investigation revealed that the amorphous phase crystallised above 380^oC. The amorphous powder was compacted under a pressure of 7.7GPa in different conditions: at 380^oC for 600s and at 1000^oC for 180s. Structural investigations of the bulk material revealed that the amorphous structure was retained after consolidation process applied at 380^oC. Compaction under high pressure at 1000^oC caused crystallisation of the amorphous phase and appearance of metastable nano...
A novel single-step synthetic method for the preparation of anatase N-doped TiO"2 nanocrystalline at low temperature has been devoleped. The N-doped anatase TiO"2 nanoparticles were synthesized by sonication of the solution of tetraisopropyl titanium and urea in water and isopropyl alcohol at 80^oC for 150min. The as-prepared sample was characterized by X-ray diffraction, transmission electron microscopy, X-ray photoelectron spectroscopy and UV-vis absorption spectrum. The product structure depends on the reaction temperature and reaction time. The photocatalytic activity of the as-prepared photocatalyst was evaluated via the photodegradation of an azo dye direct sky blue 5B. The results show that the N-doped TiO"2 nanocrystalline prepared via sonication exhibit an excellent photocatalytic...
Structural relaxation, crystallization and optimisation processes in soft magnetic amorphous alloys based on iron are examined by applying different experimental techniques: X-ray diffraction analysis, high-resolution electron microscopy, measurements of magnetic and electric properties (permeability, after-effect resistivity). The presented results are discussed in terms of annealing out of microvoids, formation of nanocrystalline phase and changes of effective magnetostriction constant. (author)
Molecular dynamics computer simulations of a dense nanocrystalline Nickel sample are performed on the parallel Cray T3 (EPFL-Lausanne). The sample contains 50 grains with an average size of 3 nm. By perturbing the relaxed configuration elastic and plastic properties are studied. (author) 1 fig., 1 ref.
It has been shown that mechanical milling of iron in water results in formation of nanocrystalline magnetite Fe3O4 with an average particle size of 0.6 ?m, saturation magnetization of 77 Am2/kg and coercivity of ?150 A/cm. Along with magnetite, an antiferromagnetic Fe-O phase (?10 wt%), which is an aggregate of small iron-oxygen clusters forms.
Abstract A facile and efficient single-step mineralization approach was exploited for achieving nanoscopic hydroxyapatite (HAP) crystal layer in chitosan porous matrix, wherein a mixed water-ethanol solvent was used to control the growth of minerals. The crystallographic structure, morphology, and mechanical properties of the scaffold were analyzed with XRD, FTIR, environmental scanning electric microscopy (ESEM), TEM, and compression tests. The behaviors and responses of MC3T3-E1 pre-osteoblast cells on the scaffolds were studied as well. The results showed that the scaffolds kept woodpile structure with predefined and controlled hierarchical structure after mineralization. The inorganic phase in the mineralized chitosan scaffolds was determined as pure rod-like HAP, which settled densely...
The present study is focused on preparation of nano composite materials and the effect of citric acid on their different properties. The formation of nano HA and its interaction with chitosan (C), gelatin (G) polymers and citric acid (CA) materials were studied. The Fourier Transformed Infrared Spectroscopy (FT-IR), X-ray diffraction (XRD), thermo-gravimetric analysis (TGA), transmission electron microscope (TEM), and scanning electron microscope (SEM) were used to characterize these composite materials. The compressive strength (CS) was also measured to know the reinforcement of the prepared composites. The results show that carboxylic and amino groups play crucial role for HA formation on chitosan-gelatin polymeric matrix in the presence of citric acid (CA). The formation of nano HA part...
We have investigated the effect of manganese (Mn) doping on properties of nanosized biphasic calcium phosphate powders and their dense bodies. Manganese levels of 0.6, 1.3, 1.9, 4.3, 7.0 and 11.9at.% were successfully incorporated into biphasic calcium phosphate via a sol-gel route. The prepared powders were calcined at temperatures of 500-1200^oC. The X-ray diffraction analysis revealed that a mix phase comprising of hydroxyapatite and @b-tricalcium phosphate were present, however the content of each phases in the structure was affected by the Mn content. The studies found that the largest portion of @b-tricalcium phosphate was detected at 4.3at.% Mn doping. The incorporation of Mn has also greatly increased the crystallinity of the biphasic calcium phosphate powder due to progressive den...
We report the fabrication and characterization of glucose-tolerant Raney-platinum cathodes for oxygen reduction in potentially implantable glucose fuel. Fabricated by extraction of aluminum from 1mm thin platinum-aluminum bi-layers annealed at 300^oC, the novel cathodes show excellent resistance against hydrolytic and oxidative attack. This renders them superior over previous cathodes fabricated from hydrogel-bound catalyst particles. Annealing times of 60, 120, and 240min result in approximately 400-550nm thin porous films (roughness factors ~100-150), which contain platinum and aluminum in a ratio of ~9:1. Aluminum release during electrode operation can be expected to have no significant effect on physiological normal levels, which promises good biocompatibility. Annealing time has a dis...
We present a novel fabrication route yielding Raney-platinum film electrodes intended as glucose oxidation anodes for potentially implantable fuel cells. Fabrication roots on thermal alloying of an extractable metal with bulk platinum at 200^oC for 48h. In contrast to earlier works using carcinogenic nickel, we employ zinc as potentially biocompatible alloying partner. Microstructure analysis indicates that after removal of extractable zinc the porous Raney-platinum film (roughness factor ~2700) consists predominantly of the Pt3Zn phase. Release of zinc during electrode operation can be expected to have no significant effect on physiological normal levels in blood and serum, which promises good biocompatibility. In contrast to previous anodes based on hydrogel-bound catalyst particles the ...
The development of 'Green Chemistry' requires new materials to replace the conventional organic chemistry by biological catalysts, to produce fine chemicals in an environmentally friendly manner. Microbial whole cells can be directly used as biocatalysts, providing a simple and cheap methodology since enzyme isolation and purification are avoided. High-density polyethylene (HDPE) is a very stable polymer though it can be activated by gamma radiation to induce grafting. Glycidyl methacrylate was grafted onto macroporous HDPE and PP in the range of 1-6%, proportional to the initial monomer concentration. Grafted polymers were further chemically modified with ethylenediamine to generate a cationic hydrogel of micron-size thickness onto the internal polymer surfaces. Modified polymers were able to immobilize Gram-positive and Gram-negative bacteria that can catalyze a chemical reaction as efficient as free cells do.
Abstract The objective of this study was to investigate how a combination of different scaffold architectures and rotational culture would influence the functional properties of thick cartilaginous tissues engineered using either chondrocytes or bone marrow-derived mesenchymal stem cells (BM-MSCs). Expanded porcine chondrocytes and BM-MSCs were suspended in 2% agarose and cast in custom-designed moulds to produce either regular solid or channelled construct cylinders. The study consisted of three seperate experimental arms. First, chondrocyte and BM-MSC constructs were cultured in free swelling conditions for 9 weeks. Second, constructs were subjected to rotational culture for a period of 3 weeks. Finally, BM-MSC-seeded constructs were subjected to delayed rotational culture, in which cons...
Nanocrystalline samples of Fe_8_0Mo_2_0 and Fe_5_0Mo_5_0 alloys were prepared by the mechanical milling method. The structure, lattice parameters, and crystallite size were determined by the X-ray diffraction. The magnetic properties of the milled products were determined by the Moessbauer spectroscopy. It was observed that in the case of the Fe_8_0Mo_2_0 alloy a solid solution of Mo in Fe was formed with the lattice parameters of the Fe increasing from 0.28659 nm to 0.29240 nm and the crystallite size decreasing from 250 nm to 20 nm. In the case of the Fe_5_0Mo_5_0 alloy there were no clear changes in values of the lattice parameters of Fe and Mo during the milling process, but the crystallite size decreased from 200 to 15 nm. Moessbauer spectra revealed different magnetic phases in the machanosynthesized Fe_Mo samples. In the case of the Fe_8_0Mo_2_0 alloy, the spectrum for the milled mixture indicated the formation of solid solution. In contrast, for the ...
Dye-sensitized nanocrystalline TiO{sub 2} solar cells are currently under development. Since these cells contain an electrolyte solution we reviewed the health and safety aspects in view of indoor applications, where personal contact cannot be excluded. Only small amounts of chemicals are present in each cell and so there is no danger of acute toxicity. However, long-term effects often can be caused by incidental contact with minute amounts. For this reason we have tested cis-di(thiocyanato)-bis(4,4'-dicarboxy-2,2'-bipyridine)Ru(II), the sensitizer dye in the Ames test. The dye was not mutagenic in the Salmonella typhimurium reverse mutation assay and in the Escherichia coli reverse mutation assay.
Nanocrystalline ZnO films were fabricated via a simple method involving the oxidation of Zn films at a remarkably low temperature of 380 C. X-ray diffraction study confirmed that the Zn films were completely oxidized even at the low temperature of 380 C and the ZnO films fabricated were of polycrystalline wurtzite structure. Room temperature optical pumping using a frequency-quintupled Q-switched Nd:YAG laser ({lambda}=213 nm) exhibited that sharp peaks at around 3.12 eV emerged above excitation powers of {proportional_to}7 MW/cm{sup 2}, demonstrating lasing in the ZnO films. These results represent that the process is a simple, promising approach for fabricating ZnO of sufficient optical performance for use as ultraviolet (UV) light emitters and an alternative UV laser source; both are key components in short-wavelength photonic devices. (orig.)
In this study, we propose a new bioactive bone cement (BBC), composed of natural bone powder (hydroxyapatite; HA), chitosan powder, and the currently available polymethylmethacrylate (PMMA) bone cement, for use in orthopedic surgeries such as vertebroplasty or as bone filler. Three types of BBCs (BBC I, BBC II, and BBC III) were prepared with different composition ratios. In vitro tests and animal studies were performed with the new BBCs, and with a currently available commercial PMMA bone cement. Surface morphology, chemical composition, changes in pH over time, exothermic temperatures, intrusion, and cellular responses were investigated in vitro. Scanning electron microscopy (SEM) and radiological and histological examinations were performed in animal studies. The results showed that the major components of the BBCs were C, O, Ca, P, Cl, Si, S, Ba, and Mg. The pH values of the BBCs decreased after 1 day, but eventually recovered to 7.2-7.4. The water absorbency, ...
Aim: Rheumatoid arthritis is a limiting disease having, among its pathological features, the inflammation of synovial tissue with progressive and later destruction of the articulation. This leads to joint deformation and loss of its function, generating pain and reducing the mobility of the affected articulation. The aim was to evaluate "1"6"6Ho-Hydroxyapatite ("1"6"6 Ho-HA) as potential radiopharmaceutical for the symptomatic treatment of chronic and acute arthritis. Materials and Methods: Holmiun-166 was produced by irradiation of Ho_2O_3 at La Reina Research Reactor, Nuclear Chilean Energy Commission. Hydroxyapatite was in-house synthesized. Its labelling and quality controls follows the internationally accepted procedures. An antigen's arthritis was induced to eight New Zealand rabbits with the "1"6"6 Ho-HA radiochemical being administered thereafter in two dosage modalities (single and double). The compound therapeutic efficiency was ...
Formation of the soft magnetic nanostructure in amorphous Fe_1_4Ni_4_0Zr_7B_1_2 alloy due to heat treatment is studied by the Moessbauer, differential scanning calorimetry, and X-ray diffraction techniques. Annealing at temperatures 520-580 "oC leads to the formation of extremely soft nanocrystalline alloy as revealed by the rf-Moessbauer measurements. The superparamagnetic behaviour was observed for the alloy annealed at 620-640 "oC. At higher annealing temperatures good soft magnetic properties deteriorate. (author)
Magnetic properties of a recently developed Fe-based amorphous alloy with a high saturation induction of 1.65 T are reviewed. The increased saturation induction is fully utilized in transformers with reduced magnetic losses, physical sizes and audible noises, minimizing some of the drawbacks of amorphous metal-based transformers based on a currently available amorphous alloy. Impacts of this on the worldwide energy savings and reduction of greenhouse gas emissions are discussed. A recent effort in achieving a saturation induction beyond 1.65 T in nanocrystalline alloys is mentioned.
AlN nanocrystalline layers and superstructures are used in the modern optoelectronic technology as reflecting mirrors in semiconductor layers. In the present work the properties of AlN films prepared by sputtering methods from an AlN target in reactive Ar + N plasma were investigated. The characterization was performed with HRTEM, SEM, glancing angle XRD and RBS methods. The present measurements confirmed the polycrystalline structure of AlN layers and enabled the evaluation of their grain size. The roughness and thickness of the layers were additionally determined by ellipsometric and profilometric measurements. (author)
Understanding the mechanical properties of biomedical devices is critical in predicting and preventing their failure in the body. Such knowledge is essential, for example, in the design of biomedical stents, which must undergo repeated strain over their ten year lifetimes without breaking. Computational models are used to predict mechanical response of a device, but these models are not complete; there are significant deviations from the predictions, especially when devices are subjected to repeated multi-axial loads. Improving these models requires comparisons with actual measurements of strained nitinol. Local measurements of the full strain tensor can be made using X-ray diffraction techniques, but they are currently limited to materials whose grain size is larger than the X-ray beam size or require several diffraction patterns produced by rotation of the sample. Nitinol stents are nanocrystalline, with grains smaller than any available X-ray beam. We present a ...
The spectral energy-dependence of the radiation-induced ESR signal has been studied in ovine cortical bone. Crushed bone samples were irradiated using photon beams with effective energies in the range from 0.06 to 6 MeV, and electron beams with mean energies in the range from 2 to 10 MeV. The photon and electron data were normalized to a dose to bone of 50 Gy and the results are reported as response relative to the ESR signal for photon irradiation at 1.25 MeV ("6"0Co). The photon irradiation results show that the ESR response is greatest at low energies with a relative value of 1.2 at 0.06 MeV. The relative response decreases, as the energy increases, to approximately 0.85 in the region of 2 to 3 MeV. These variations in the relative ESR responses are significantly less than the ESR energy-dependent responses reported in the literature for human tooth enamel and synthetic hydroxyapatite. An explanation for this difference is offered. For electron beam ...
Artificial bone cements (BCs) based on poly(methyl methacrylate) (PMMA) powders and methyl methacrylate (MMA) liquid monomer also present in their formulation small amounts of other substances, including a chemical initiator compound and radiopaque agents. Because inadequate mixing of the recipe components during the manufacture of the bone cement may compromise the mechanical properties of the final pieces, new techniques to incorporate the fillers into the BC and their effect upon the mechanical properties of BC pieces were investigated in the present study. PMMA powder composites were produced in situ in the reaction vessel by addition of X-ray contrasts to the reacting MMA mixture. It is shown that this can lead to much better mechanical properties of test pieces, when compared to standard bone cement formulations, because enhanced dispersion of the radiopaque agents can be achieved. Moreover, it is shown that the addition of hydroxyapatite (HA) and acrylic ...
There is increasing concern among the dental community regarding the damage caused to teeth by the acids in soft drinks. Enamel dissolution in acidic solution can be reduced by addition of calcium and/or phosphate salts to increase the degree of saturation with respect to hydroxyapatite (DS sub H sub A), or by an increase in pH. In soft drinks, however, both of these approaches are associated with a reduced taste quality. The separate effects of each parameter are not known. In the work presented here, enamel dissolution was studied in citric acid solutions with compositions typical of soft drinks. Nanoindentation and atomic force microscopy (AFM) were used to investigate very early stages of enamel dissolution, with typical exposure times of 30-600 s. Preliminary investigations of the application of SIMS, ESEM and XPS to enamel dissolution studies are also reported. The individual effects of DS sub H sub A , pH and calcium and phosphate concentrations on enamel ...
Abstract The objective of this study was to determine the functional properties of cartilaginous tissues generated by porcine MSCs isolated from different tissue sources, and to compare these properties to those derived from chondrocytes (CCs). MSCs were isolated from bone marrow (BM) and infrapatellar fat pad (FP), while CCs were harvested from the articular surface of the femoro-patellar joint. Culture-expanded CCs and MSCs were encapsulated in agarose hydrogels and cultured in the presence of TGF3. Samples were analysed biomechanically, biochemically and histologically at days 0, 21 and 42. After 42 days in free swelling culture, mean GAG content was 1.50% w/w in CC-seeded constructs, compared to 0.95% w/w in FP- and 0.43% w/w in BM-seeded constructs. Total collagen accumulation was hig...
Aim: To systematically review the currently available high quality evidence evaluating treatments for moist desquamation in radiotherapy patients. Design: Systematic literature review. Methods: Electronic databases, websites, reference lists, key journals and conference proceedings were searched. Attempts were also made to uncover unpublished material. Relevant studies proceeded to data extraction and quality assessment. Results: Twenty studies were found; 10 were eligible for inclusion. Although many studies were small, none had unacceptably poor quality. No meta-analysis was undertaken as the studies were not homogenous in their interventions or methods. No convincing evidence for any intervention was found. Conclusion: Despite being recommended by many guidelines (College of Radiographers Summary of Intervention for Acute Radiotherapy Induced Skin Reactions in Cancer Patients (London, 2001); NHS Quality Improvement Scotland Best Practice Statement: Skincare of Patients Receiving ...
An unsymmetrical squaraine dye which contains an arylamino group was synthesized and used in dye-sensitized solar cells. The molar extinction coefficient of the dye is 77793 M-1 cm-1. Because our synthesized molecule may have no diradical character or the contribution of the diradicaloid component to resonance is quite small, the newly designed squaraine dye has a maximum absorption at 546 nm in the visible region compared with the NIR squaraine sensitizers. Cyclic voltammetry and time dependent density function theory calculation were accomplished to scrutinize the sensitized performance of the dye. Meanwhile, the novel sensitizer has been used to sensitize nanocrystalline TiO2-based solar cell. Under standard global AM 1.5 solar conditions, the squaraine dye-sensitized cell gives a short...
The thermal stability of nanoscale grains in cryomilled aluminum powders containing 1% diamantane was investigated. Diamantane is a diamondoid molecule consisting of 14 carbon atoms in a diamond cubic structure that is terminated by hydrogen atoms. The nanostructures of the resulting cryomilled powders were characterized using both transmission electron microscopy (TEM) and X-ray diffraction (XRD) techniques. The average grain size was found to be on the order of 22?nm, a value similar to that obtained for cryomilled Al without diamantane. To determine thermal stability, the powders were heated in an inert gas atmosphere at constant temperatures between 423 and 773?K (0.51T m to 0.83T m) for exposure times of up to 10?h. The average grain size for all powders containing diamantane was obse...
Nanocrystalline chromium oxynitride films were deposited by reactive RF magnetron sputtering of metallic chromium target in argon and helium atmospheres. The paper deals with consequence of increase in oxygen partial pressure on structural, hydrophobic and optical properties of chromium oxynitride films. The film stoichiometry changes from CrN and Cr2O3 to only Cr2O3 with increase in oxygen partial pressure as evident from X-Ray Diffraction analysis in both cases. The average crystallite size decreases with increase in oxygen partial pressure for both gas atmospheres. The thickness calculated from transmission data and surface profilometer are in good harmony with each other. The deposited films are hydrophobic by nature and the contact angle of the films varies as a function of surface ro...
The light-emitting properties of cubic silicon carbide films grown by vacuum vapor phase epitaxy on Si(100) and Si(111) substrates under conditions of decreased growth temperatures (T gr ? 900?700?C) have been discussed. Structural investigations have revealed a nanocrystalline structure and, simultaneously, a homogeneity of the phase composition of the grown 3C-SiC films. Photoluminescence spectra of these structures under excitation of the electronic subsystem by a helium-cadmium laser (?excit = 325 nm) are characterized by a rather intense luminescence band with the maximum shifted toward the ultraviolet (?3 eV) region of the spectral range. It has been found that the integral curve of photoluminescence at low temperatures of measurements is split into a set of Lorentzian components. Th...
Nanocrystalline MnFe"2O"4 ferrite was prepared by using autocombustion technique (flash). The microstructure and magnetic properties are studied. The results of XRD and TEM clarified that, this ferrite is nanosized with particle size (39 nm). Magnetic measurements showed a ferromagnetic behavior with T"C = 613 K, the saturation magnetization M"s = 13.71 emu/g, remanent magnetization M"r = 0.1694 emu/g and, coercivity H"c = 25.6 Oe. Natural material, egg white used as an aqueous medium to extend prepare nanoparticles better than other chemical interesting materials.
A poly(ether urethane) (PEUR)/poly(ethylene oxide) (PEO)/SiO2 based nanocomposite polymer is prepared and employed in the construction of high efficiency all-solid-state dye-sensitized nanocrystalline solar cells. The introduction of low-molecular weight PEUR prepolymer into PEO electrolyte has greatly enhance the electrolyte performance by both improving the interfacial contact properties of electrode/electrolyte and decreasing the PEO crystallization, which were confirmed by XRD and SEM characteristics. The effects of polymer composition, nano SiO2 content on the ionic conductivity and I3- ions diffusion of polymer-blend electrolyte are investigated. The optimized composition yields an energy conversion efficiency of 3.71% under irradiation by white light (100 mW cm-2).
Nanocrystalline powders of GaN with grain sizes ranging from 2 to 30 nm were examined under high external pressures by in situ diffraction techniques in a diamond anvil cell at DESY (HASYLAB, Station F3). The experiments on densification of pure powders under high pressure were performed without a pressure medium. The mechanism of generation and relaxation of internal strains and their distribution in nanoparticles was deduced from Bragg reflections recorded in situ under high pressures at room temperature. The microstrain was calculated from the full-width at half-maximum (FWHM) values of the Bragg lines. It was found that microstrains in GaN crystallites are generated and subsequently relaxed by two mechanisms: generation of stacking faults and change of the size and shape of the grains occurring under external stress. (author)
Indium sulfide thin films were deposited onto indium-tin-oxide coated glass substrate by electrochemical deposition from an aqueous solution containing In2 (SO4) 3 and Na2S2O3. The deposition conditions were optimized on the basis of data obtained by scanning electron microscope, Auger electron spectroscopy and optical transmission measurements. Furthermore, the photosensitivity of the films was observed by means of photoelectrochemical measurements, which confirmed that the indium sulfide showed n-type conduction. The X-ray diffraction and Raman studies revealed that the as-grown films were amorphous or nanocrystalline in nature and became polycrystalline In2S3 after annealing.
TiB{sub 2} appears to be a promising material for the wear protection in various tribological systems, e.g. the diecasting of Al. This study focuses on the development of titanium boride coatings deposited by PACVD, a deposition method which is most suitable for the coating of substrates with complex shapes. All layers analysed are very smooth and exhibit a quasi-amorphous fracture surface. XRD and TEM analysis indicate a nanocrystalline structure with grain sizes in the order of 2 nm. The diffraction patterns can well be correlated to titanium diboride. WDS reveals an over stoichiometric B/Ti ratio. The layer hardness reaches the value of 33 GPa and the critical load in scratch tests rises to 35 N. Neither 100Cr6 nor Al as a counterpart in pin-on-disk tests leads to wear of the coating. (orig.)
The corrosion behavior of the sputter-deposited amorphous or nanocrystalline W-Nb alloys is studied in 10% NaCl, 0.1 and 1 M NaOH solutions at 24 deg. C, open to air using immersion tests and electrochemical measurements. Niobium metal acts synergistically with tungsten in enhancing the corrosion resistance of the W-Nb alloys so as to show lower corrosion rates than the corrosion rates of the alloy-constituting elements in almost all examined solutions. Corrosion rates of W-Nb alloys are about more than one order of magnitude less than that of the sputter-deposited tungsten and even lower than that of sputter-deposited niobium. The stability of the anodic passive films formed on the W-Nb alloys increase with niobium content.
In this study a novel sol-gel auto-combustion method, using n-decyltrimethylammonium bromide as a cationic surfactant, has been used to synthesize strontium hexaferrite nanocrystalline powder. The dried nitrate-citrate gel, prepared from a solution of ferric nitrate, strontium nitrate, citric acid, trimethylamine and cationic surfactant, exhibited an auto-combustion behavior after ignition in air. The formation reaction temperature, phase identification, crystallites size, particles size distribution and morphology of resultant strontium hexaferrite powder were investigated by DTA/TGA, FTIR, XRD, LPSA, TEM and SEM techniques. The results showed that in presence of the cationic surfactant, the combustion intensity increases and the crystallite size decreases. The crystallite size of stronti...
Highly water-repellent surfaces have been prepared from arrayed nanowires of zinc oxide (ZnO) by a treatment with stearic acid. The layers are electrochemically deposited on a nanocrystalline seed layer from an oxygenated aqueous zinc chloride solution. An advancing contact angle (CA) as high as 176{sup 0} is obtained with a very small hysteresis {approx}1{sup 0}. These results, supplemented by infrared spectroscopy, show that the stearic acid forms a very well-packed self-assembled monolayer. The CA measurements show a very good stability of the treated surface even when exposed to harsh conditions or long-term ambient illumination.
Solid oxide fuel cell (SOFC) is a promising source of power generation in terms of conversion efficiency which is higher than the conventional one, as it is not limited by the Carnot efficiency. Theoretically, the SOFC have an efficiency of the order of 60-80 % but it is limited by the number of active side available for the reaction i.e. TPB (triple phase boundary) at the electrode-electrolyte interface which depends on the particle size of the materials employed during the fabrication of SOFC components (i.e. the method employed during the synthesis). Literally, there are several methods used in the syntheses of oxide materials such as conventional solid-state reaction, co-precipitation, hydrothermal rout, sol-gel and Glycine nitrate process (GNP) but among these GNP found to be effective over the other because of homogeneity, phase purity and smaller particle size of final product. In this work, the Nano-crystalline Ln_0_._6Sr_0_._4Co_0_._8Fe_0_._2O_3_-_#delta# ...
Full text: It was recently-established for hexagonal barium ferrite-industrially important magnetically hard material that refinement of the crystallite dimensions into the nanoscale regime, typically #<=# 10 nm, leads after heat treatment at temperatures 800-1000 deg C to significant coercivity increase of up to 6.5 kOe (#approx#3-4 times) with saturation magnetisation values of 50-55 emu/g (#approx#95% of bulk at room temperature). High-energy mechanochemical processing has been applied to prepare nanostructural (nanocrystalline-amorphous) composites. High resolution electron microscopy studies reveal that the enhancement of the final magnetic properties was due to formation of magnetically noninteracting #approx#l,#mu#m Ba-ferrite particles with 5-10 nm amorphous surface layer - depending on annealing parameters. Similar situation was established also for ball milled strontium ferrite (SrFe_1_2O_1_9) powders where short annealing 4 h at 1000 deg C produced ...
Chlorophyll-a (Chl-a) assembled in hydrophobic domain by fatty acid with long alkyl hydrocarbon chain such as myristic acid (Myr), stearic acid (Ste) and cholic acid (Cho) modified onto nanocrystalline TiO{sub 2} electrode is prepared and the photovoltaic properties of the nanocrystalline TiO{sub 2} film by Chl-a are studied. Incident photon to current efficiency (IPCE) value at 660 nm in photocurrent action spectrum of Chl-a/Ste-TiO{sub 2}, Chl-a/Myr-TiO{sub 2} and Chl-a/Cho-TiO{sub 2} electrodes are 5.0%, 4.1% and 4.1%, respectively. Thus, the IPCE is maximum using Chl-a/Ste-TiO{sub 2} electrode. From the results of photocurrent responses with light intensity of 100 mW cm{sup -2} irradiation or monochromatic light with 660 nm, generated photocurrent increases using Chl-a/Ste-TiO{sub 2} electrode compared with the other Chl-a assembled TiO{sub 2} electrodes. These results show that the hydrophobic domain formed by stearic acid with long alkyl ...
The crystallite size and orientation in molybdenum films prepared by magnetron sputtering at a low rate of typical 1 (angstrom)s and a pressure of 0.45 Pa was investigated by X-ray diffraction and texture analysis. The surface topography was studied using atomic force microscopy. Increasing the film thickness from 20 nm to 3 microm, the films show a turnover from a (110) fiber texture to a (211) mosaic-like texture. In the early state of growth (20 nm thickness) the development of dome-like structures on the surface is observed. The number of these structures increases with film thickness, whereas their size is weakly influenced. The effect of texture turnover is reduced by increasing the deposition rate by a factor of six, and it is absent for samples mounted above the center of the magnetron source. The effect of texture turnover is related to the bombardment of the films with high energetic argon neutrals resulting from backscattering at the target under oblique angle and causing ...
Electrodeposition of semiconducting iron oxide (Fe_2O_3) thin film was carried out from an alkaline sulphate bath. A 0.1 M ferrous sulphate (FeSO_4#centre dot#7H_2O) was complexed with 0.1 M citric acid. By addition of 1 N NaOH, pH of the solution was made alkaline (pH=9) and deposition of iron oxide (Fe_2O_3) thin films was carried out potentiostatically at room temperature (300 K). From cyclic voltametry (CV), electrochemical studies were carried out for deposition of iron oxide thin films. The XRD studies reveal that Fe_2O_3 with epsilon (#epsilon#) phase having monoclinic crystal structure is formed. By observing scanning electron microscope (SEM), it is seen that iron oxide films were homogeneous, uniform and well covered to surface of the substrate. Grain size was found to be in nanometers range from XRD analysis. The optical band gap of Fe_2O_3 thin film was estimated to be 1.90 eV. Electrical resistivity was order of 10"4 #OMEGA# cm. Dielectric constant and loss (tan #delta#) ...
Nanocrystalline cemented tungsten carbide has attracted considerable interests for use in cutting tool because of its superior mechanical properties. In this study, nano-sized powders of mixed WC and Co were prepared from attrition-milled oxides by a gas reduction-carburization process. The effects of compacting pressure, heating schedule, additional ball-milling, and the presence of a grain growth inhibitor on the sintering properties of the nano-sized WC-Co powders were examined. The grain size and phases in WC-Co alloy were clearly affected by compacting pressure. Because of the trapped gases and the lower melting point of the cobalt binder, when a compact of nano-sized WC-Co powder was sintered through a heating schedule with holding steps, the sintered alloy maintained the small size of WC grains without any {eta} phase. In addition, the additional ball-milling improved the microstructure and mechanical properties of the nano-sized WC-Co powder by producing a ...
Nanocrystalline cemented tungsten carbide has attracted considerable interests for use in cutting tool because of its superior mechanical properties. In this study, nano-sized powders of mixed WC and Co were prepared from attrition-milled oxides by a gas reduction-carburization process. The effects of compacting pressure, heating schedule, additional ball-milling, and the presence of a grain growth inhibitor on the sintering properties of the nano-sized WC-Co powders were examined. The grain size and phases in WC-Co alloy were clearly affected by compacting pressure. Because of the trapped gases and the lower melting point of the cobalt binder, when a compact of nano-sized WC-Co powder was sintered through a heating schedule with holding steps, the sintered alloy maintained the small size of WC grains without any #eta# phase. In addition, the additional ball-milling improved the microstructure and mechanical properties of the nano-sized WC-Co powder by producing a ...
Iron oxide thin films have been obtained by spray pyrolysis using 100% methanolic and ethanolic solutions of iron tri-chloride. The films were deposited onto ITO-coated glass substrates. The preparative conditions have been optimized to obtain compact, pin-hole-free and smooth thin films which are adherent to the substrate. The structural, morphological and compositional characterizations have been carried out by X-ray diffraction, scanning electron microscopy and energy dispersive X-ray analysis. The films deposited using ethanolic solution results into pure hematite; #alpha#-Fe_2O_3 thin films, however, films deposited using methanolic solution consists of hematite and maghemite-c phases of iron oxide. The films are nanocrystalline with particle size of 30-40 nm. The optical absorbance of the film was of the order of 10"5 cm"-"1. The optical band gap of films was found to be 2.26 and 2.20 eV for the films deposited using methanolic and ethanolic solutions, ...
The microstructure, microhardness, corrosion, and wear resistance of d.c.-plated Ni electrodeposits prepared from different types of electrolysing Watts-type baths, without or with organic compounds, ceramic powder - SiC and polymer - polytetrafluoroethylene (PTFE), on Cu substrate, which was subsequently removed from the deposits, were investigated. With the change of the type of bath, the deposit grain size was found to decrease markedly, e.g. deposits with an average grain size of about 50 nm could be produced from the bath containing 45 g/dm"3 Ni"2"+ ions, 5 g/dm"3 SiC, and 20 g/dm"3 PTFE. The surface morphology on the bath side of the electrode-posited Ni or Ni-SiC-PTFE foils was characteristic of the type of bath, and its roughness correlated well with the observed grain size. Microhardness and wear resistance increased with decreasing grain size, as expected. On discussing the factors controlling deposit grain size, it is concluded that the Ni"2"+ ion content in the bath and the ...
There has been considerable interest in producing and studying nanoparticle materials because of the effect of size on their structure, physical and chemical structure. Most studied nanoparticle semiconductors belong to the II-VI group, as they are relatively easy to synthesize and are generally prepared as particulates or in thin film form. Among II-VI compounds, CdS is one of the most studied materials. There are different ways to synthesize CdS nanoparticles such as colloidal particles, chemical decomposition, sol-gel, gas evaporation, magnetron sputtering, electrostatic deposition, and etc. {gamma}-irradiation is one of the effective methods for synthesis of nanomaterials. These nonomaterials have been extensively used in the preparation of nanocrystalline metals, metal oxides, and metal-polymer composites. However, The preparation of CdS nanoparticle and CdS/ polyacrylonitrile nanocomposite by {gamma}-irradiation method at room temperature and ambient ...
The synthesis of narrowly dispersed nanocrystalline TiO_2 was investigated with a surfactant aided solvothermal synthetic method in toluene solutions. When a sufficient amount of titanium isopropoxide, Ti[OCH(CH_3)_2]_4 (TIP), was added to the solution, the shapes of TiO_2 nanoparticles changed from spheres to rods. The aggregated microstructures of the nano-sized TiO_2 in systems of spheres, rods, and mixtures of spheres and rods was studied using TEM. The morphological shape of the aggregation was described in terms of the fractal dimensions. We used a box-counting method to get the fractal dimension of these systems. The fitted fractal dimensions for spheres, sphere/rod mixtures, and rods are D = 1.54, D = 1.81, and D = 1.89, respectively. The fractal dimension changed from 1.54 to 1.9 with the TIP/toluene ratio, indicating that the growth mechanism for aggregations showed different behaviors.
MmMg{sub 12}-Ni amorphous or nanocrystalline composites (Mm: Ce-rich mischmetal) were prepared through the ball-milling method, and their electrochemical hydrogen storage performance was investigated and compared with that of ball-milled CeMg{sub 12}-Ni composites. It was found that the ball-milled MmMg{sub 12}-Ni composites had larger initial discharge capacities and better high rate dischargeability. Analysis of electrochemical impedance spectra (EIS) shows that the reaction resistance and hydrogen diffusion resistance of the ball-milled MmMg{sub 12}-Ni composites are lower as a result of the decrease in Ce content, and thus can contribute to the larger discharge capacity and better high rate dischargeability. Additionally, the cycle performance of the ball-milled MmMg{sub 12}-Ni composites is better than those of the ball-milled CeMg{sub 12}-Ni composites. This may be related to the formation of a Nd oxide or Nd(OH){sub 3} film on surface of the MmMg{sub 12} ...
Aim: Compounds such "9"9"mTc-MDP and "9"9"mTc-HEDP are used regularly in bone scintigraphy for metastasis detection. The therapeutics properties of beta emitter radionuclides like "1"5"3Sm, "1"6"6Ho and "1"7"7Lu has been widely reported in literature being "1"7"7Lu the less developed for medical applications. With the purpose of study different radiopharmaceuticals alternatives, for metastasis bone palliation, we have evaluated, on a comparative basis, the labeling of "1"5"3Sm-MDP, "1"5"3Sm-HEDP, "1"6"6Ho-MDP, "1"6"6Ho-HEDP, "1"7"7Lu-MDP and "1"7"7Lu-HEDP from the exhibited radionuclidic purity and biological distribution point of view. Material and Methods: The radionuclides were produced at La Reina Research Reactor, Chilean Nuclear Energy Commission. The radionuclidic purity was determined by gamma-Ray spectrometry. The labeling was accomplished with MDP (Plenum) and HEDP synthesized in-house. The in-vitro affinity of labeled compounds to the mineral bone matrix was determined using ...
By magnetron sputtering model steel films with specific properties can be prepared for purposive surveys. By changing the deposition parameters certain properties of these films can be influenced. For this thesis steel films with 18% Cr and 8% Ni have been prepared in order to study specific parameters on the corrosion resistance of bulk stainless steel. Chemical composition, microstructure, and surface morphology of these films have been characterized. In comparison to bulk steel sheets with the same chemical composition they have a smaller grain size and a ferritic structure. In contrast to bulk steel sheets they don`t contain any nonmetallic inclusions like Mn-sulfides. The influence of these structural differences on the corrosion resistance has been studied. For this purpose the electrochemical properties of the sputter-deposited steels have been compared with the properties of steel sheets with a similar chemical composition (DIN 1.4301, AISI 304) in neutral and acidic Cl{sup ...
The paper generalizes some results of the United States/Moldova program on advanced composite organic and semiconductor light emitters. High density exciton system bound to N impurity superlattice grown by modern technologies and GaP:N, GaP:N:Sm nanocrystals distributed in transparent fluorine-containing polymers will be used as the base elements for new generation of optoelectronic devices. The work seeks to expand further the applications of GaP itself through the formation of nanocomposites. Classic and new methods are applied for preparation of GaP:N nanoparticles with the controlled dimensions developed clear quantum confinement effect. The long-term ordered bulk GaP crystals as well as their nanoparticles have been investigated by TEM, XRD, Raman scattering, and luminescent methods. The evolution of the Raman Light Scattering and luminescence spectra is reported from pure and doped GaP single crystals grown over 40 years ago and evaluated approximately every 15 years. For the ...
We have investigated the nanocrystalline microstructure and the hard magnetic properties of Sm(Co{sub 0.725}Fe{sub 0.1}Cu{sub 0.12}Zr{sub 0.04}B{sub 0.015}){sub 7.4} melt-spun ribbons. The coercivity (H{sub c}) of the as-spun ribbons increased with the wheel surface speed from 2.8kOe for 10m/s to 14.5kOe for 40m/s. The post-annealing of the melt-spun ribbons from 700 to 900 deg. C for 10min did not lead to a substantial increase of H{sub c}. However, after isothermal aging at 820 deg. C and subsequent slow cooling (0.5 deg. C/min) to 120 deg. C, H{sub c} increased from 2.8 to 10.9kOe for 10m/s, while it decreased from 14.5 to 13.5kOe for 40m/s ribbons. The grain size of the melt-spun ribbon reduced with structural transformation from 2:17H (Th{sub 2}Ni{sub 17}-hexagonal type) to 1:7H (TbCu{sub 7}-hexagonal type) as the wheel surface speed was increased. Three-dimensional atom probe analysis showed a boron enriched precipitate at the grain boundaries in the as-spun ...
We have investigated the nanocrystalline microstructure and the hard magnetic properties of Sm(Co_0_._7_2_5Fe_0_._1Cu_0_._1_2Zr_0_._0_4B_0_._0_1_5)_7_._4 melt-spun ribbons. The coercivity (H_c) of the as-spun ribbons increased with the wheel surface speed from 2.8kOe for 10m/s to 14.5kOe for 40m/s. The post-annealing of the melt-spun ribbons from 700 to 900 deg. C for 10min did not lead to a substantial increase of H_c. However, after isothermal aging at 820 deg. C and subsequent slow cooling (0.5 deg. C/min) to 120 deg. C, H_c increased from 2.8 to 10.9kOe for 10m/s, while it decreased from 14.5 to 13.5kOe for 40m/s ribbons. The grain size of the melt-spun ribbon reduced with structural transformation from 2:17H (Th_2Ni_1_7-hexagonal type) to 1:7H (TbCu_7-hexagonal type) as the wheel surface speed was increased. Three-dimensional atom probe analysis showed a boron enriched precipitate at the grain boundaries in the as-spun ribbons, which acts as the grain growth ...
The behaviour of the packaging materials under radiation field has a great importance in radiation processing, because, in most cases, they are finally responsible for the preservation of the beneficent changes achieved in irradiated products. For example, in radiation sterilisation and food irradiation, the packages must preserve the sterilisation, respectively the sanitisation. They must preserve also the physical barrier feature. The radiation effects on plastics were extensively studied in the last decades for nuclear industry and more recently for radiation processing. The two major effects of nuclear radiation on polymeric materials are the degradation and cross-linking. The degradation consists in breaking of macromolecules after interaction with nuclear particles, amplified by the free radicals which persist long periods, especially in crystalline polymers. Oxygen could penetrate the sample and interact with free radicals so that the degradation process continues after the ...