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Sample records for f-substituted hydroxyapatite nanopowders

  1. Si-substituted hydroxyapatite nanopowders: Synthesis, thermal stability and sinterability

    SciTech Connect

    Bianco, Alessandra Cacciotti, Ilaria; Lombardi, Mariangela Montanaro, Laura

    2009-02-04

    Synthetic hydroxyapatites incorporating small amounts of Si have shown improved biological performances in terms of enhanced bone apposition, bone in-growth and cell-mediated degradation. This paper reports a systematic investigation on Si-substituted hydroxyapatite (Si 1.40 wt%) nanopowders produced following two different conventional wet methodologies: (a) precipitation of Ca(NO{sub 3}){sub 2}.4H{sub 2}O and (b) titration of Ca(OH){sub 2}. The influence of the synthesis process on composition, thermal behaviour and sinterability of the resulting nanopowders is studied. Samples were characterised by electron microscopy, induced coupled plasma atomic emission spectroscopy, thermal analysis, infrared spectroscopy, N{sub 2} adsorption measurements, X-ray diffraction and dilatometry. Semicrystalline Si-substituted hydroxyapatite powders made up of needle-like nanoparticles were obtained, the specific surface area ranged between 84 and 110 m{sup 2}/g. Pure and Si-substituted hydroxyapatite nanopowders derived from Ca(NO{sub 3}){sub 2}.4H{sub 2}O decomposed around 1000 deg. C. Si-substituted hydroxyapatite nanopowders obtained from Ca(OH){sub 2} were thermally stable up to 1200 deg. C and showed a distinct decreased thermal stability with respect to the homologous pure sample. Si-substituted hydroxyapatites exhibited higher sintering temperature and increased total shrinkage with respect to pure powders. Nanostructured dense ceramics were obtained by sintering at 1100 deg. C Si-substituted hydroxyapatites derived from Ca(OH){sub 2}.

  2. Surfactant-assisted hydrothermal synthesis of hydroxyapatite nanopowders.

    PubMed

    Bricha, Meriame; Belmamouni, Younes; Essassi, El Mokhtar; Ferreira, José M F; El Mabrouk, Khalil

    2012-10-01

    Rod-like hydroxyapatite nanoparticles (n-HAp) with a highly ordered nanostructure were prepared by hydrothermal synthesis from calcium chloride, and phosphoric acid, as calcium and phosphorus sources, respectively. Various surfactant families such as cationic (CTAB), anionic (SDS) and nonionic (Triton X-100) were used as regulators of the nucleation and crystal growth. The synthesized nanopowders were characterized using X-ray diffraction (XRD), Fourier transform infrared spectrograph (FTIR) and transmission electron microscopy (TEM). The rod-like morphology was obtained regardless of the surfactant used during the hydrothermal treatment, but the aspect ratio of the crystals was found to be surfactant dependent. The mechanism of crystal growth as well-oriented nanostructure is discussed. PMID:23421176

  3. Bio-nanoplatforms based on carbon dots conjugating with F-substituted nano-hydroxyapatite for cellular imaging.

    PubMed

    Zhao, Yafei; Shi, Liyi; Fang, Jianhui; Feng, Xin

    2015-12-21

    Carbon dots (CDs) have shown great promise in a wide range of bioapplications due to their tunable optical properties and noncytotoxicity. For the first time, a rational strategy was designed to construct new bio-nanoplatforms based on carboxylic acid terminated CDs (CDs-COOH) conjugating with amino terminated F-substituted nano-hydroxyapatite (NFAp) via EDC/NHS coupling chemistry. The monodisperse NFAp nanorods were functionalized with o-phosphoethanolamine (PEA) to provide them with amino groups and render them hydrophilic with respect to the ligand exchange process. The CDs-COOH@PEA-NFAp conjugates exhibits bright blue fluorescence under UV illumination, excellent photostability and colloidal stability. Due to their low cytotoxicity and good biocompatibility as determined by methyl thiazolyl tetrazolium (MTT) assay, the CDs-COOH@PEA-NFAp conjugates were successfully applied as bio-nanoplatforms to MCF-7 breast cancer cells for cellular imaging in vitro. More importantly, the functional CDs conjugated to NFAp provide an extended and general approach to construct different water-soluble NFAp bio-nanoplatforms for other easily functionalised luminescent materials. Therefore, these green nanoplatforms may be a prospective candidate for applications in bioimaging or targeted biological therapy and drug delivery. PMID:26568461

  4. Bio-nanoplatforms based on carbon dots conjugating with F-substituted nano-hydroxyapatite for cellular imaging

    NASA Astrophysics Data System (ADS)

    Zhao, Yafei; Shi, Liyi; Fang, Jianhui; Feng, Xin

    2015-11-01

    Carbon dots (CDs) have shown great promise in a wide range of bioapplications due to their tunable optical properties and noncytotoxicity. For the first time, a rational strategy was designed to construct new bio-nanoplatforms based on carboxylic acid terminated CDs (CDs-COOH) conjugating with amino terminated F-substituted nano-hydroxyapatite (NFAp) via EDC/NHS coupling chemistry. The monodisperse NFAp nanorods were functionalized with o-phosphoethanolamine (PEA) to provide them with amino groups and render them hydrophilic with respect to the ligand exchange process. The CDs-COOH@PEA-NFAp conjugates exhibits bright blue fluorescence under UV illumination, excellent photostability and colloidal stability. Due to their low cytotoxicity and good biocompatibility as determined by methyl thiazolyl tetrazolium (MTT) assay, the CDs-COOH@PEA-NFAp conjugates were successfully applied as bio-nanoplatforms to MCF-7 breast cancer cells for cellular imaging in vitro. More importantly, the functional CDs conjugated to NFAp provide an extended and general approach to construct different water-soluble NFAp bio-nanoplatforms for other easily functionalised luminescent materials. Therefore, these green nanoplatforms may be a prospective candidate for applications in bioimaging or targeted biological therapy and drug delivery.Carbon dots (CDs) have shown great promise in a wide range of bioapplications due to their tunable optical properties and noncytotoxicity. For the first time, a rational strategy was designed to construct new bio-nanoplatforms based on carboxylic acid terminated CDs (CDs-COOH) conjugating with amino terminated F-substituted nano-hydroxyapatite (NFAp) via EDC/NHS coupling chemistry. The monodisperse NFAp nanorods were functionalized with o-phosphoethanolamine (PEA) to provide them with amino groups and render them hydrophilic with respect to the ligand exchange process. The CDs-COOH@PEA-NFAp conjugates exhibits bright blue fluorescence under UV illumination

  5. Study the adsorption of phenol from aqueous solution on hydroxyapatite nanopowders.

    PubMed

    Lin, Kaili; Pan, Jiayong; Chen, Yiwei; Cheng, Rongming; Xu, Xuecheng

    2009-01-15

    In this study, the hydroxyapatite (HAp) nanopowders prepared by chemical precipitation method were used as the adsorbent, and the potential of HAp nanopowders for phenol adsorption from aqueous solution was studied. The effect of contact time, initial phenol concentration, pH, adsorbent dosage, solution temperature and adsorbent calcining temperature on the phenol adsorption, and the adsorption kinetic, equilibrium and thermodynamic parameters were investigated. The results showed that the HAp nanopowders possessed good adsorption ability to phenol. The adsorption process was fast, and it reached equilibrium in 2h of contact. The initial phenol concentration, pH and the adsorbent calcining temperature played obvious effects on the phenol adsorption capacity onto HAp nanopowders. Increase in the initial phenol concentration could effectively increase the phenol adsorption capacity. At the same time, increase in the pH to high-acidity or to high-alkalinity also resulted in the increase in the phenol adsorption capacity. Increase in the HAp dosage could effectively increase the phenol adsorption percent. However, the higher calcining temperature of HAp nanopowders could obviously decrease the adsorption capacity. The maximum phenol adsorption capacity was obtained as 10.33mg/g for 400mg/L initial phenol concentrations at pH 6.4 and 60 degrees C. The adsorption kinetic and the isotherm studies showed that the pseudo-second-order model and the Freundlich isotherm were the best choices to describe the adsorption behaviors. The thermodynamic parameters suggested that the adsorption of phenol onto HAp was physisorption, spontaneous and endothermic in nature. PMID:18573599

  6. Antimicrobial properties of silver-doped hydroxyapatite nano-powders and thin films

    NASA Astrophysics Data System (ADS)

    Sygnatowicz, Michael; Keyshar, Kunttal; Tiwari, Ashutosh

    2010-07-01

    Silver-doped hydroxyapatite nanopowders were prepared using a solution based sol-gel method and thoroughly characterized using x-ray diffraction (XRD), scanning electron microscopy (SEM), and energy dispersive spectroscopy (EDS). Antibacterial tests showed silver-doped HAP powders prevented the growth and reproduction of bacteria. Silver-doped HAP powders were pressed into pellets and on these pellets a pulsed laser deposition (PLD) technique was employed to grow amorphous and crystalline thin films on sapphire substrates. Crystalline films had silver nano-particles present within the HAP matrix. Film stability tests showed crystalline films to be far more stable in prolonged solution submersion than their amorphous counterparts.

  7. O2/Ar Plasma Treatment for Enhancing the Biocompatibility of Hydroxyapatite Nanopowder and Polycaprolactone Composite Film.

    PubMed

    Ko, Yeong-Mu; Myung, Sung-Woon; Kim, Byung-Hoon

    2015-08-01

    In this study we performed O2/Ar plasma treatment to remove the polycaprolactone on hydroxyapatite nanopowder and polycaprolactone (HAp-NP/PCL) composite film. After plasma ashing, the HAp-NP was exposed on the composite film. The 25 wt% HAp-NP/PCL treated with plasma showed the hydrophilic surface property with reducing the aging effect. The MTT and ALP results indicated that the plasma etching increased the biocompatibility of HAp-NP/PCL composite film. The present simple plasma etching technique can be applicable in a development of biomaterials. PMID:26369196

  8. Reverse micelle mediated synthesis, processing, mechanical and biological characterization of hydroxyapatite nanopowders for bone graft application

    NASA Astrophysics Data System (ADS)

    Banerjee, Ashis

    Hydroxyapatite (HA) is the most widely used bioceramic material in bone graft applications because of its compositional similarity with natural bone. However, synthetic HA does not show similar mechanical and biological properties to the inorganic component of bone. Properties of ceramic material depend on starting materials, processing techniques, densification and microstructure of the final product. The objective of this research was to process HA whisker reinforced HA composite using HA nanopowders and whiskers. HA nanopowders with different length scale and morphology were synthesized by reverse micelle system using NP5 and NP12 as surfactants and cyclohexane as organic solvent. The lowest average aspect ratio was 1.357+/-0.39 with average particle size of 66 nm and the highest average aspect ratio was 7.277+/-3.227 with average length of 150 nm and width of 20 nm, were synthesized. Micron sized HA whiskers with aspect ratio between 20 and 50, average particle length of 15 mum and width of 400 nm was synthesized using urea as a precipitating agent. Desired microstructure was obtained after sintering with spherical HA nanopowder and whiskers along with dopants. Addition of whiskers decreased density of the sintered compacts. However, at 10 wt% whisker content sample showed microhardness and fracture toughness of 3.6 GPa and 1.5 MPa.m1/2, respectively, and a compressive strength of 80 MPa was obtained. Mineralization study in simulated body fluid (SBF) showed formation of apatite layer on the dense HA compacts indicating a good tendency of bond formation with natural bone. Cytotoxicity results showed excellent cell attachment on the HA surface. In the Appendices, 3 journal articles have been attached which describe synthesis, processing and characterization of undoped and doped PZT nanopowders. Free standing and agglomerated PZT nanopowders were synthesized by the sucrose templated method and the citrate nitrate autocombustion method. Particle size in the range

  9. Porous hydroxyapatite-TiO2 nanocomposites from natural phosphates and their decolorization properties. Photoactive hydroxyapatite-TiO2 nanopowders

    NASA Astrophysics Data System (ADS)

    Bouyarmane, H.; Saoiabi, S.; El Hanbali, I.; El Karbane, M.; Rami, A.; Masse, S.; Laghzizil, A.; Coradin, T.

    2015-07-01

    Titanium dioxide-hydroxyapatite nanopowders were prepared by the simultaneous gelation of a titanium alkoxide and precipitation of a redisolved natural phosphate mineral. Evolution of the crystallinity, porous features and surface reactivity of these powders as a function of Ti content and heating was studied. Optimal conditions were found for the preparation of a low-cost nanocomposite powder that was as effective as pure titania for the decolorization of methylene blue solutions.

  10. nanopowders

    NASA Astrophysics Data System (ADS)

    Janbutrach, Yutana; Hunpratub, Sitchai; Swatsitang, Ekaphan

    2014-09-01

    La1 - x Al x FeO3 ( x = 0.0, 0.05, 0.1, 0.2, 0.3, 0.4, and 0.5) nanopowders were prepared by polymerization complex method. All prepared samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), and UV-vis spectrophotometry (UV-vis). The magnetic properties were investigated using a vibrating sample magnetometer (VSM). The X-ray results of all samples show the formation of an orthorhombic phase with the second phase of α-Fe2O3 in doped samples. The crystallite sizes of nanoparticles decreased with increasing Al content, and they are found to be in the range of 58.45 ± 5.90 to 15.58 ± 4.64 nm. SEM and TEM images show the agglomeration of nanoparticles with average particle size in the range of 60 to 75 nm. The FT-IR spectra confirm the presence of metal oxygen bonds of O-Fe-O and Fe-O in the FeO6 octahedra. The UV-vis spectra show strong absorption peaks at approximately 285 nm, and the calculated optical band gaps are found to be in the range of 2.05 to 2.09 eV with increasing Al content. The M-H loop of the pure sample is antiferromagnetic, whereas those of the doped samples tend to be ferromagnetic with increasing Al content. The magnetization, remanent magnetization, and coercive field of the Al-doped sample with x = 0.5 are enhanced to 1.665 emu/g, 0.623 emu/g, and 4,087.0 Oe, respectively.

  11. Synthesis, characterization and antimicrobial activity of copper and zinc-doped hydroxyapatite nanopowders

    NASA Astrophysics Data System (ADS)

    Stanić, Vojislav; Dimitrijević, Suzana; Antić-Stanković, Jelena; Mitrić, Miodrag; Jokić, Bojan; Plećaš, Ilija B.; Raičević, Slavica

    2010-08-01

    Antimicrobial materials based on hydroxyapatite are potentially attractive in a wide variety of medical applications. The synthesis of copper and zinc-doped hydroxyapatite was done by neutralization method. This method consists of dissolving CuO or ZnO in solution of H 3PO 4, and the slow addition to suspension of Ca(OH) 2 for obtaining monophasic product. Characterization studies from XRD, SEM, TEM and FTIR spectra showed that particles of all samples are of nano size and they do not contain any discernible crystalline impurity. The quantitative elemental analysis showed that the copper and zinc ions fully incorporated into the hydroxyapatite. The antimicrobial effects of doped hydroxyapatite powders against pathogen bacterial strains Escherichia coli, Staphylococcus aureus and pathogen yeast Candida albicans were tested in solid and liquid media. Quantitative test in liquid media clearly showed that copper and zinc-doped samples had viable cells reduction ability for all tested strains.

  12. Synthesis of antimicrobial monophase silver-doped hydroxyapatite nanopowders for bone tissue engineering

    NASA Astrophysics Data System (ADS)

    Stanić, Vojislav; Janaćković, Djordje; Dimitrijević, Suzana; Tanasković, Sladjana B.; Mitrić, Miodrag; Pavlović, Mirjana S.; Krstić, Aleksandra; Jovanović, Dragoljub; Raičević, Slavica

    2011-02-01

    Monophase silver-doped hydroxyapatite (AgxCa10-x(PO4)6(OH)2; 0.002 ≤ x ≤ 0.04) nanoparticles were prepared using a neutralization method and investigated with respect to potential medical applications. This method consists of dissolving Ag2O in solution of H3PO4, and the slow addition to suspension of Ca(OH)2 was applied for the purpose of homogenous distribution of silver ions. Characterization studies from XRD, TEM and FTIR spectra showed that obtained crystals are monophase hydroxyapatites and that particles of all samples are of nano size, with average length of 70 nm and about 15-25 nm in diameter. Antimicrobial studies have demonstrated that all silver-doped hydroxyapatite samples exhibit excellent antimicrobial activity in vitro against the following pathogens: Staphylococcus aureus, Escherichia coli and Candida albicans. The hydroxyapatite sample with the highest content of silver has shown the highest antimicrobial activity; killed all cells of E. coli and brought to more than 99% reduction in viable counts of S. aureus and C. albicans. The atomic force microscopic studies illustrate that silver-doped hydroxyapatite sample causes considerable morphological changes of microorganism cells which might be the cause of cells' death. Hemolysis ratios of the silver-doped hydroxyapatite samples were below 3%, indicating good blood compatibility and that are promising as biomaterials.

  13. Synthesis of fluorine substituted hydroxyapatite nanopowders and application of the central composite design for determination of its antimicrobial effects

    NASA Astrophysics Data System (ADS)

    Stanić, Vojislav; Dimitrijević, Suzana; Antonović, Dušan G.; Jokić, Bojan M.; Zec, Slavica P.; Tanasković, Sladjana T.; Raičević, Slavica

    2014-01-01

    Synthetic biomaterials based on fluorine substituted hydroxyapatite are potentially attractive for orthopedic and dental implant applications. The new synthesis of fluorine substituted hydroxyapatite samples were done by neutralization, which consists of adding the solution of HF and H3PO4 in suspension of Ca(OH)2. Characterization studies from XRD, SEM and FTIR spectra showed that crystals are obtained with apatite structure and those particles of all samples are nano size, with an average length of 80 nm and about 15-25 nm in diameter. The central composite design was used in order to determine the optimal conditions for the antimicrobial activity of the synthesized samples. In order to evaluate the influence of operating parameters on the percent of viable cell reduction of Streptococcus mutans, three independent variables were chosen: exposure time, pH of saline and floride concentration in apatite samples. The experimental and predicted antimicrobial activities were in close agreement. Antimicrobial activity of the samples increases with the increase of fluoride concentration and the decreased pH of saline. The maximum antimicrobial activity was achieved at the initial pH of 4.

  14. Rheological behavior of oxide nanopowder suspensions

    NASA Astrophysics Data System (ADS)

    Cinar, Simge

    Ceramic nanopowders offer great potential in advanced ceramic materials and many other technologically important applications. Because a material's rheological properties are crucial for most processing routes, control of the rheological behavior has drawn significant attention in the recent past. The control of rheological behavior relies on an understanding of how different parameters affect the suspension viscosities. Even though the suspension stabilization mechanisms are relatively well understood for sub-micron and micron size particle systems, this knowledge cannot be directly transferred to nanopowder suspensions. Nanopowder suspensions exhibit unexpectedly high viscosities that cannot be explained with conventional mechanisms and are still a topic of investigation. This dissertation aims to establish the critical parameters governing the rheological behavior of concentrated oxide nanopowder suspensions, and to elucidate the mechanisms by which these parameters control the rheology of these suspensions. Aqueous alumina nanopowders were chosen as a model system, and the findings were extrapolated to other oxide nanopowder systems such as zirconia, yttria stabilized zirconia, and titania. Processing additives such as fructose, NaCl, HCl, NaOH, and ascorbic acid were used in this study. The effect of solids content and addition of fructose on the viscosity of alumina nanopowder suspensions was investigated by low temperature differential scanning calorimetry (LT-DSC), rheological, and zeta potential measurements. The analysis of bound water events observed in LT-DSC revealed useful information regarding the rheological behavior of nanopowder suspensions. Because of the significance of interparticle interactions in nanopowder suspensions, the electrostatic stabilization was investigated using indifferent and potential determining ions. Different mechanisms, e.g., the effect of the change in effective volume fraction caused by fructose addition and electrostatic

  15. Incorporation of aluminum nanopowder into NTO.

    SciTech Connect

    Lee, K. Y.; Kennedy, J. E.; Peterson, P. D.; Asay, B. W.

    2004-01-01

    Most insensitive high explosives have relatively low output and the user is forced to choose between enhancing operational safety and meeting ordnance performance requirements. The goals of this project are to investigate ways to incorporate Al nanopowder in NTO and to devise formulations that are insensitive and that exhibit high performance. In this paper, the novel method for the preparation of nanoNTO and its formulation with Al nanopowder will be presented, together with the characterization test results. Data from minisandwich velocity test on NTO and NTO/Al mix and the techniques used to verify the potential encapsulation of Al in NTO will also be presented.

  16. Method of preparation of silver nanopowder

    NASA Astrophysics Data System (ADS)

    Jarosz, Mateusz; Mlozniak, Anna; Jakubowska, Malgorzata

    2010-09-01

    In recent years we observe the rapid growth of nanotechnology, including materials, technologies and devices development. Going from micro- to nanoscale can result in new, specific physicochemical, mechanical, optical, electrical, magnetic or catalytical properties. It all emerges from quantum effects and high contribution of surface atoms causing high reactivity. Among others it can cause a reduction of the melting-temperature. The goal of our work was to obtain a silver nanopowder from a thermal decomposition of silver salts of fatty acids.

  17. Production and properties of electrosprayed sericin nanopowder

    NASA Astrophysics Data System (ADS)

    Hazeri, Najmeh; Tavanai, Hossein; Moradi, Ali Reza

    2012-06-01

    Sericin is a proteinous substrate that envelops fibroin (silk) fiber, and its recovery provides significant economical and social benefits. Sericin is an antibacterial agent that resists oxidation and absorbs moisture and UV light. In powder form, sericin has a wide range of applications in food, cosmetics and drug delivery. Asides from other techniques of producing powder, such as precipitation and spray drying, electrospraying can yield solid nanoparticles, particularly in the submicron range. Here, we report the production of sericin nanopowder by electrospraying. Sericin sponge was recovered from Bombyx mori cocoons through a high-temperature, high-pressure process, followed by centrifugation and freeze drying of the sericin solution. The electrospraying solution was prepared by dissolving the sericin sponge in dimethyl sulfoxide. We demonstrate that electrospraying is capable of producing sericin nanopowder with an average particle size of 25 nm, which is by far smaller than the particles produced by other techniques. The electrosprayed sericin nanopowder consists of small crystallites and exhibits a high moisture absorbance.

  18. Preparation of hydroxyapatite/zirconia bioceramic nanocomposites for orthopaedic and dental prosthesis applications

    NASA Astrophysics Data System (ADS)

    Sung, Yun-Mo; Shin, Young-Keun; Ryu, Jae-Jun

    2007-02-01

    Homogeneous mixtures of hydroxyapatite (HAp) and yttria-stabilized zirconia (YSZ) nanoparticles were successfully synthesized using chemical co-precipitation and subsequent calcination. For the synthesis of HAp/YSZ nanopowder, the Ca/P atomic ratio was 1.73 to obtain high-content stoichiometric hydroxyapatite phase and to suppress β-tricalcium phosphate (β-TCP) formation. The agglomerated crystalline powders were milled using YSZ ball media to obtain well-separated nanoparticles. The final particle size of the HAp and YSZ was ~50-70 and ~15-30 nm, respectively. The crystallinity and morphological feature of the nanopowder was analysed using x-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM) analyses. The ball-milled nanopowder mixture was hot pressed at 1100 °C for 1 h under 20 MPa in vacuum atmosphere. The sintered HAp/YSZ nanocomposites exhibited approximately 99% of the theoretical density, due not only to the fine nanoscale of the particles, but also to the homogeneous distribution of the nanoparticle mixture. They also showed fine grain structures of the HAp phase due to the suppressed grain growth by YSZ particles. The nanocomposites showed improved mechanical properties, flexural strength of ~155 MPa and fracture toughness of ~2.1 MP m1/2, due to the YSZ contribution to the HAp matrix.

  19. Oxidation and melting of aluminum nanopowders.

    PubMed

    Trunov, Mikhaylo A; Umbrajkar, Swati M; Schoenitz, Mirko; Mang, Joseph T; Dreizin, Edward L

    2006-07-01

    Recently, nanometer-sized aluminum powders became available commercially, and their use as potential additives to propellants, explosives, and pyrotechnics has attracted significant interest. It has been suggested that very low melting temperatures are expected for nanosized aluminum powders and that such low melting temperatures could accelerate oxidation and trigger ignition much earlier than for regular, micron-sized aluminum powders. The objective of this work was to investigate experimentally the melting and oxidation behavior of nanosized aluminum powders. Powder samples with three different nominal sizes of 44, 80, and 121 nm were provided by Nanotechnologies Inc. The particle size distributions were measured using small-angle X-ray scattering. Melting was studied by differential scanning calorimetry where the powders were heated from room temperature to 750 degrees C in an argon environment. Thermogravimetric analysis was used to measure the mass increase indicative of oxidation while the powders were heated in an oxygen-argon gas mixture. The measured melting curves were compared to those computed using the experimental particle size distributions and thermodynamic models describing the melting temperature and enthalpy as functions of the particle size. The melting behavior predicted by different models correlated with the experimental observations only qualitatively. Characteristic stepwise oxidation was observed for all studied nanopowders. The observed oxidation behavior was well interpreted considering the recently established kinetics of oxidation of micron-sized aluminum powders. No correlation was found between the melting and oxidation of aluminum nanopowders. PMID:16805619

  20. Characterization of hydroxyapatite by time-resolved luminescence and FTIR spectroscopy

    NASA Astrophysics Data System (ADS)

    Grigorjeva, L.; Millers, D.; Smits, K.; Jankovica, Dz; Pukina, L.

    2013-12-01

    Time-resolved luminescence and FTIR absorption spectra of undoped and Eu and Ce doped hydroxyapatite nanocrystalline powders prepared by sol-gel method were studied. The luminescence band at 350-400 nm was detected and two decay times (11 ns and 38 ns) was determinated for Ce doped samples. The luminescence spectra and decay kinetics were analized for Eu doped nanopowders. The Eu3+ ion was incorporated in different Ca sites. The process of energy transfer to Eu3+ excited state (5D0) was detected from luminescence decay kinetics.

  1. Preparation and reactivity of aluminum nanopowders coated by hydroxyl-terminated polybutadiene (HTPB)

    NASA Astrophysics Data System (ADS)

    Guo, Liangui; Song, Wulin; Hu, Mulin; Xie, Changsheng; Chen, Xia

    2008-02-01

    HTPB-coated aluminum (Al) nanopowders were prepared by laser-induction complex heating. The characterization of the nanopowders was revealed using transmission electronic microscopy (TEM), high-resolution transmission electronic microscopy (HRTEM), X-ray diffraction analysis (XRD) and Fourier transform infrared (FTIR) spectrometry. Results showed that HTPB-coated Al nanopowders have a core-shell structure with size ranging from 30 to 100 nm and organic HTPB exists in HTPB-coated Al nanopowders. Differential scanning calorimeter (DSC) and thermal gravimeter (TG) analysis of the HTPB-coated Al nanopowders and Al 2O 3-passivated Al nanopowders stored for 2 years in ambient environment indicated that the reactivity and stability of HTPB-coated Al nanopowders outperform Al 2O 3-passivated Al nanopowders. These findings demonstrate that HTPB is a suitable surface coating material for Al nanopowders.

  2. Growth model of binary alloy nanopowders for thermal plasma synthesis

    SciTech Connect

    Shigeta, Masaya; Watanabe, Takayuki

    2010-08-15

    A new model is developed for numerical analysis of the entire growth process of binary alloy nanopowders in thermal plasma synthesis. The model can express any nanopowder profile in the particle size-composition distribution (PSCD). Moreover, its numerical solution algorithm is arithmetic and straightforward so that the model is easy to use. By virtue of these features, the model effectively simulates the collective and simultaneous combined process of binary homogeneous nucleation, binary heterogeneous cocondensation, and coagulation among nanoparticles. The effect of the freezing point depression due to nanoscale particle diameters is also considered in the model. In this study, the metal-silicon systems are particularly chosen as representative binary systems involving cocondensation processes. In consequence, the numerical calculation with the present model reveals the growth mechanisms of the Mo-Si and Ti-Si nanopowders by exhibiting their PSCD evolutions. The difference of the materials' saturation pressures strongly affects the growth behaviors and mature states of the binary alloy nanopowder.

  3. Studies on synthesis of alumina nanopowder from synthetic Bayer liquor

    SciTech Connect

    Mazloumi, Mahyar; Arami, Hamed; Khalifehzadeh, Razieh; Sadrnezhaad, S.K. . E-mail: sadrnezh@sharif.edu

    2007-06-05

    Procedure for synthesis of alumina nanopowder from Bayer liquor (synthetic sodium aluminate solution) is investigated. Cooling, ageing and then addition of 3 ml/l Tiron (1,2-dihydroxy-3,5-benzene disulfonic acid disodium salt) to the supersaturated liquor affect purity and fineness of the nanopowder product. X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and energy dispersive X-ray (EDAX) analyses indicate that purity of the alumina nanopowder increases with the aging time. Experimental observations show that highly pure alumina nanopowders could be produced by direct calcination of cold gelatinous sodium aluminate solution followed by careful washing at a Tiron concentration of 3 ml/l NaOH.

  4. Pulsed wire discharge apparatus for mass production of copper nanopowders.

    PubMed

    Suematsu, H; Nishimura, S; Murai, K; Hayashi, Y; Suzuki, T; Nakayama, T; Jiang, W; Yamazaki, A; Seki, K; Niihara, K

    2007-05-01

    A pulsed wire discharge (PWD) apparatus for the mass production of nanopowders has been developed. The apparatus has a continuous wire feeder, which is operated in synchronization with a discharging circuit. The apparatus is designed for operation at a maximum repetition rate of 1.4 Hz at a stored energy of 160 J. In the present study, Cu nanopowder was synthesized using the PWD apparatus and the performance of the apparatus was examined. Cu nanopowder of 2.0 g quantity was prepared in N(2) gas at 100 kPa for 90 s. The particle size distribution of the Cu nanopowder was analyzed by transmission electron microscopy and the mean surface diameter was determined to be 65 nm. The ratio of the production mass of the powder to input energy was 362 g/kW h. PMID:17552867

  5. The processing of nanopowders by thermal plasma technology

    NASA Astrophysics Data System (ADS)

    Tong, Lirong; Reddy, Ramana G.

    2006-04-01

    The thermal plasma synthesis of nanopowders is a relatively new technology with great potential for future industrial applications. This article introduces research carried out in the plasma processing laboratory at the University of Alabama in Tuscaloosa, Alabama. Ceramic nanopowders and nanofibers (SiC, TiC, and B4C) and nanocomposite powders (TiC-Al(Ti), TiC-Fe(Ti), and TiN-Fe (Ti)) were successfully synthesized by thermal plasma technology.

  6. The chemical vapor synthesis of inorganic nanopowders

    NASA Astrophysics Data System (ADS)

    Sohn, Hong Yong; Ryu, Taegong; Choi, Jin Won; Hwang, Kyu Sup; Han, Gilsoo; Choi, Young Joon; Fang, Zhigang Zak

    2007-12-01

    Chemical vapor synthesis (CVS) is a process for making fine solid particles by the vapor-phase chemical reactions of precursors. At the University of Utah, this process has been applied to the synthesis of the aluminides of titanium and nickel, other metallic and intermetallic powders, and subsequently aluminum nanopowder and WC-Co nanocomposite powder. This work has demonstrated that it is possible to prepare fine particles of 5-200 nm size by CVS. Further, it has been shown that this technique has a unique capability to produce uniformly mixed powders of different solids. This is possible because the reactants are perfectly mixed in the gas phase. More recently, the CVS process has been carried out in a plasma reactor. This system has shown considerable promise for many applications as a method of producing nanosized powders.

  7. Microemulsion synthesis and magnetic properties of hydroxyapatite-encapsulated nano CoFe2O4

    NASA Astrophysics Data System (ADS)

    Foroughi, Firoozeh; Hassanzadeh-Tabrizi, S. A.; Amighian, Jamshid

    2015-05-01

    Hydroxyapatite-encapsulated cobalt ferrite (CoFe2O4) nanopowders were synthesized by one step microemulsion method. The powders were characterized by X-ray Diffraction, Fourier transform infrared spectroscopy, field emission scanning electron microscopy, transmission electron microscopy and vibrating sample magnetometer. TEM results showed that nanoparticles calcined at 700 °C have core-shell morphology. It was found that the resultant phases, morphology and magnetic properties of the samples depend on calcining temperature. The synthesized nanoparticles showed a maximum saturation magnetization of 7.8 emu/g with a wasp-waisted hysteresis loop. The magnetion was reduced by increasing calcining temperature to 900 °C. This reduction is due to the reaction of cobalt ferrite with hydroxyapatite which leads to CaFe12(PO4)8(OH)12 phase.

  8. Hydroxyapatite with environmental applications

    SciTech Connect

    Popa, C. L.; Ciobanu, C. S.; Predoi, D.; Petre, C. C.; Jiga, G.; Motelica-Heino, M.; Iconaru, S. L.

    2014-05-15

    The aim of this study was to synthetize new nanoparticles based on methyltrimethoxysilane coated hydroxyapatite (MTHAp) for lead removal in aqueous solutions. The morphological and compositional analysis of MTHAp was investigated by scanning electron microscopy (SEM) equipped with an energy dispersive X-ray spectrometer (EDS). Removal experiments of Pb{sup 2+} ions were carried out in aqueous solutions with controlled concentration of Pb{sup 2+} and at fixed pH of 5. After the removal experiment of Pb{sup 2+} ions from solutions, porous hydroxyapatite nanoparticles were transformed into PbMTHAp-5 via the adsorption of Pb{sup 2+} ions followed by a cation exchange reaction. Our results demonstrate that the porous hydroxyapatite nanoparticles can be used as an adsorbent for removing Pb{sup 2+} ions from aqueous solution.

  9. Transformations in Sol-Gel Synthesized Nanoscale Hydroxyapatite Calcined Under Different Temperatures and Time Conditions

    NASA Astrophysics Data System (ADS)

    Seema, Kapoor; Uma, Batra; Suchita, Kohli

    2012-08-01

    Nano-hydroxyapatite (HAP) has been synthesized using sol-gel technique. Calcium nitrate tetrahydrate and potassium dihydrogen phosphate were used as precursors for calcium and phosphorus, respectively. A detailed study on its transformation during calcination at two crucial temperatures has been undertaken. The synthesized nanopowder was calcined at 600 and 800 °C for different time periods. The results revealed that the obtained powders after calcining at 600 and 800 °C are composed of hydroxyapatite nanoparticles. The nano-HAP powders were characterized by x-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy, thermal gravimetric analysis (TGA), and BET surface area analyzer techniques. The results indicate that crystallite size as well as crystallinity of synthesized HAP nanopowders increase with increase in calcination temperature as well as calcination time, but the effect of temperature is more prominent as compared to that of calcination time. TEM micrograph revealed the presence of majority of HAP powder particles as agglomerates and a few as individual particles. It also revealed that HAP produced after sintering at 600 °C is 26-45 nm in size, which is well in agreement with the crystallite size calculated using XRD data. TGA study showed the thermal stability of the as-synthesized nano-HAP powder. The BET surface area decreased with increase in calcination temperature and time. The results clearly demonstrate the significant role of calcination parameters on the characteristics of nano-HAP powders.

  10. Characterization of porous hydroxyapatite.

    PubMed

    Hing, K A; Best, S M; Bonfield, W

    1999-03-01

    Hydroxyapatite has been considered for use in the repair of osseous defects for the last 20 years. Recent developments have led to interest in the potential of porous hydroxyapatite as a synthetic bone graft. However, despite considerable activity in this field, regarding assessment of the biological response to such materials, the basic materials characterization is often inadequate. This paper documents the characterization of the chemical composition, mechanical integrity, macro- and microstructure of a porous hydroxyapatite, Endobon (E. Merck GmbH), intended for the bone-graft market. Specimens possesed a range of apparent densities from 0.35 to 1.44 g cm(-3). Chemical analysis demonstrated that the natural apatite precursor of Endobon was not converted to pure hydroxyapatite, but retained many of the ionic substituents found in bone mineral, notably carbonate, sodium and magnesium ions. Investigation of the microstructure illustrated that the struts of the material were not fully dense, but had retained some traces of the network of osteocyte lacunae. Macrostructural analysis demonstrated the complex inter-relationship between the structural features of an open pore structure. Both pore size and connectivity were found to be inversely dependent on apparent density. Furthermore, measurement of pore aspect ratio and orientation demonstrated a relationship between apparent density and the degree of macrostructural anisotropy within the specimens, while, it was also noted that pore connectivity was sensitive to anisotropy. Compression testing demonstrated the effect of apparent density and macrostructural anisotropy on the mechanical properties. An increase in apparent density from 0.38 to 1.25 g cm(-3) resulted in increases in ultimate compressive stress and compressive modulus of 1 to 11 MPa and 0.2 to 3.1 GPa, respectively. Furthermore, anisotropic high density (> 0.9 g cm(-3)) specimens were found to possess lower compressive moduli than isotropic specimens

  11. Characterisations of collagen-silver-hydroxyapatite nanocomposites

    NASA Astrophysics Data System (ADS)

    Ciobanu, C. S.; Popa, C. L.; Petre, C. C.; Jiga, G.; Trusca, R.; Predoi, D.

    2016-05-01

    The XRD analysis were performed to confirm the formation of hydroxyapatite structure in collagen-silver-hydroxyapatite nanocomposites. The molecular interaction in collagen-hydroxyapatite nanocomposites was highlighted by Fourier transform infrared spectroscopy (FTIR) analysis. The SEM showed a nanostructure of collagen-silverhydroxyapatite nanocomposites composed of nano needle-like particles in a veil with collagen texture. The presence of vibrational groups characteristics to the hydroxyapatite structure in collagen-silver-hydroxyapatite (AgHApColl) nanocomposites was investigated by FTIR.

  12. Ignition and explosion of nanopowders: something new under the dust

    NASA Astrophysics Data System (ADS)

    Dufaud, Olivier; Vignes, Alexis; Henry, François; Perrin, Laurent; Bouillard, Jacques

    2011-07-01

    This work deals with the study of ignition and explosion characteristics of nanoparticles. It has been carried out on various powders: zinc, aluminum, carbon blacks... Specific behaviours have been highlighted during the first phase of this project (Nanosafe 2). For instance, it has been demonstrated that there mainly exists two combustion regimes that are either kinetically controlled, for small size particles, or diffusion controlled, for large size particles (generally with diameters greater than 1 or 2 μm). It has been found that as the particle size decreases, minimum ignition temperature and minimum ignition energy decrease (even lower than 1 mJ), indicating higher potential inflammation and explosion risks for metallic nanopowders. Moreover, the presence of agglomerates in the nanopowders could modify their reactivity. Thus, the explosion severity of Al powders tends to increase as the specific surface area decreases, before reaching a peak for 1 μm particle size. These results are essential for industries producing or handling nanopowders in order to propose/design new and proper prevention and protection means. Nevertheless, the validity of the classical characterization tools with regard to nanopowders should be discussed. For example, the experimental laminar flame velocity of Al dusts has been compared to a theoretical one, determined by Huang's model, which assumes that the propagation of the flame is run mainly by conduction. It has shown a good agreement. However, under certain conditions, the Al flame propagation is expected to be mainly conducted by radiation. Two hypotheses can then be made. On the one hand, it can be assumed that the 20 L sphere probably disturbs the flame propagation and thermal mechanisms by absorbing radiation (wall quenching effect). On the other hand, it has been observed, thanks to the use of a high speed camera that the preheating zone is smaller for some nanopowders than for micro-particles (figure below). It could

  13. Laser transfer of diamond nanopowder induced by metal film blistering

    NASA Astrophysics Data System (ADS)

    Kononenko, T. V.; Alloncle, P.; Konov, V. I.; Sentis, M.

    2009-03-01

    Blister-based laser induced forward transfer (BB-LIFT) is a promising technique to produce surface microstructures of various advanced materials including inorganic and organic micro/nanopowders, suspensions and biological micro-objects embedded in life sustaining medium. The transferred material is spread over a thin metal film irradiated from the far side by single laser pulses through a transparent support. Interaction of the laser pulse with the metal-support interface under optimized conditions causes formation of a quickly expanding blister. Fast movement of the free metal surface provides efficient material transfer, which has been investigated for the case of diamond nanopowder and diamond-containing suspension. The unique features of the given technique are universality, simplicity and efficient isolation of the transferred material from the ablation products and laser heating.

  14. Raman scattering and luminescence of yttria nanopowders and ceramics

    NASA Astrophysics Data System (ADS)

    Osipov, V. V.; Solomonov, V. I.; Spirina, A. V.; Vovkotrub, E. G.; Strekalovskii, V. N.

    2014-06-01

    We have studied Raman scattering in yttria nanopowders and ceramics that was excited by radiation at wavelengths of 514.5 and 632.8 nm. We show that, in undoped nanopowders and cubic phase of doped yttria ceramics, only the Raman scattering by phonons is observed, with no other Raman scattering centers having been revealed. In nanopowders of the monoclinic phase, we have observed an additional Raman line with a Raman shift of 1093 ± 4 cm-1. If all the objects under investigation are excited by the radiation at a wavelength of 514.5 nm, their spectra exhibit four series of photoluminescence lines, two of which (at λ = 521-523 and 538-564 nm) are emitted by Er3+ ions, "impurity" dopants, while the other two lines (at λ = 607-635 and 644-684 nm) are emitted by intrinsic centers. Under excitation by the radiation at a wavelength of 632.8 nm, only a series of bands at λ = 644-684 nm is emitted. In addition to these photoluminescence bands, neodymium-doped ceramics show photoluminescence bands of Nd3+ ions. We have shown that intrinsic luminescence centers, which occur in all the examined specimens, are capable of acting as acceptors with respect to neodymium ions excited to the upper laser level.

  15. Synthesis and Photoluminescence Properties of SnO2 Nanopowder

    NASA Astrophysics Data System (ADS)

    Arai, Takahiro; Adachi, Sadao

    2012-10-01

    SnO2 nanopowder was synthesized by calcining metastannic salt (SnO2·H2O) prepared by chemically etching metallic Sn in aqueous HNO3 solution. The calcined SnO2 nanopowder was investigated by X-ray diffraction (XRD) measurement and photoluminescence (PL) spectroscopy. The XRD and PL intensities increased with increasing calcining temperature, yielding an activation energy of ˜0.65 eV. The PL spectra of the calcined SnO2 nanopowder exhibited green (G) and red (R) emission bands with peaks at ˜2.5 and ˜2.0 eV, respectively, that were clearly dependent not only on the excitation light wavelength but also on the sample temperature. The temperature dependence of the PL intensity between 20 and 300 K was explained by the thermal quenching with activation energies of ˜15 meV (T=20-60 K) and ˜0.12-0.18 eV (T ≥100 K). The G and R emission states were found to originate from the Jahn-Teller effect of the 5s2 (Sn2+) ions in the SnO2 matrix and were similar to those generally observed in many ns2-doped alkali halides and SnCl2.

  16. Hydroxyapatite for Keratoprosthesis Biointegration

    PubMed Central

    Wang, Liqiang; Jeong, Kyung Jae; Chiang, Homer H.; Zurakowski, David; Behlau, Irmgard; Chodosh, James; Dohlman, Claes H.; Langer, Robert

    2011-01-01

    Purpose. Integration of keratoprosthesis with the surrounding cornea is very important in preventing bacterial invasion, which may cause ocular injury. Here the authors investigated whether hydroxyapatite (HAp) coating can improve keratoprosthesis (KPro) biointegration, using polymethyl methacrylate (PMMA)—the principal component of the Boston KPro—as a model polymer. Methods. HAp coatings were induced on PMMA discs after treatment with concentrated NaOH and coating with poly-dopamine (PDA) or polydopamine and then with 11-mercaptoundecanoic acid (11-MUA). Coatings were characterized chemically (Fourier transform infrared spectroscopy [FTIR], energy dispersive X-ray spectroscopy [EDX]) and morphologically (SEM) and were used as substrates for keratocyte growth in vitro. Cylinders of coated PMMA were implanted in porcine corneas ex vivo for 2 weeks, and the force required to pull them out was measured. The inflammatory reaction to coated discs was assessed in the rabbit cornea in vivo. Results. FTIR of the coatings showed absorption bands characteristic of phosphate groups, and EDX showed that the Ca/P ratios were close to those of HAp. By SEM, each method resulted in morphologically distinct HAp films; the 11-MUA group had the most uniform coating. The hydroxyapatite coatings caused comparable enhancement of keratocyte proliferation compared with unmodified PMMA surfaces. HAp coating significantly increased the force and work required to pull PMMA cylinders out of porcine corneas ex vivo. HAp coating of implants reduced the inflammatory response around the PMMA implants in vivo. Conclusions. These results are encouraging for the potential of HAp-coated surfaces for use in keratoprostheses. PMID:21849419

  17. Magnesium incorporation into hydroxyapatite.

    PubMed

    Laurencin, Danielle; Almora-Barrios, Neyvis; de Leeuw, Nora H; Gervais, Christel; Bonhomme, Christian; Mauri, Francesco; Chrzanowski, Wojciech; Knowles, Jonathan C; Newport, Robert J; Wong, Alan; Gan, Zhehong; Smith, Mark E

    2011-03-01

    The incorporation of Mg in hydroxyapatite (HA) was investigated using multinuclear solid state NMR, X-ray absorption spectroscopy (XAS) and computational modeling. High magnetic field (43)Ca solid state NMR and Ca K-edge XAS studies of a ∼10% Mg-substituted HA were performed, bringing direct evidence of the preferential substitution of Mg in the Ca(II) position. (1)H and (31)P solid state NMR show that the environment of the anions is disordered in this substituted apatite phase. Both Density Functional Theory (DFT) and interatomic potential computations of Mg-substituted HA structures are in agreement with these observations. Indeed, the incorporation of low levels of Mg in the Ca(II) site is found to be more favourable energetically, and the NMR parameters calculated from these optimized structures are consistent with the experimental data. Calculations provide direct insight in the structural modifications of the HA lattice, due to the strong contraction of the M⋯O distances around Mg. Finally, extensive interatomic potential calculations also suggest that a local clustering of Mg within the HA lattice is likely to occur. Such structural characterizations of Mg environments in apatites will favour a better understanding of the biological role of this cation. PMID:21144581

  18. Cements from nanocrystalline hydroxyapatite.

    PubMed

    Barralet, J E; Lilley, K J; Grover, L M; Farrar, D F; Ansell, C; Gbureck, U

    2004-04-01

    Calcium phosphate cements are used as bone substitute materials because they may be moulded to fill a void or defect in bone and are osteoconductive. Although apatite cements are stronger than brushite cements, they are potentially less resorbable in vivo. Brushite cements are three-component systems whereby phosphate ions and water react with a soluble calcium phosphate to form brushite (CaHPO4 x 2H2O). Previously reported brushite cement formulations set following the mixture of a calcium phosphate, such as beta-tricalcium phosphate (beta-TCP), with an acidic component such as H3PO4 or monocalcium phosphate monohydrate (MCPM). Due to its low solubility, hydroxyapatite (HA) is yet to be reported as a reactive component in calcium phosphate cement systems. Here we report a new cement system setting to form a matrix consisting predominantly of brushite following the mixture of phosphoric acid with nanocrystalline HA. As a result of the relative ease with which ionic substitutions may be made in apatite this route may offer a novel way to control cement composition or setting characteristics. Since kinetic solubility is dependent on particle size and precipitation temperature is known to affect precipitated HA crystal size, the phase composition and mechanical properties of cements made from HA precipitated at temperatures between 4 and 60 degrees C were investigated. PMID:15332608

  19. Hydroxyapatite in Physiological Environment

    NASA Astrophysics Data System (ADS)

    Slepko, Alexander; Demkov, Alexander A.

    2011-03-01

    A carbonated form of hydroxyapatite (HA) [ Ca 10 (PO4)6 (OH)2 ] is one of the most abundant materials in mammal bone. It crystallizes within the spaces between tropocollagen protein chains in an aqueous solution and strengthens the bone tissue. An emerging application of synthetic HA is bone repair and replacement. Bulk electronic and chemical properties of HA were studied theoretically recently. However, the absorption of H2 O molecules and amino acids of the tropocollagen chains at HA surfaces remains an area of active research. Using density functional theory we analyze the electronic properties and surface energetics of HA for different orientations and terminations and generate a theoretical surface phase diagram of HA. The reactivity of these surface models is analyzed using the frontier orbital approach. We find two dominant surfaces which are most stable over the widest chemical range. However, we expect them to show little surface reactivity. Using a HA slab with a highly reactive surface we build atomistic models of HA covered with up to one monolayer of water and analyze interactions between this surface and the water molecules.

  20. Synthesis, characterization and luminescence properties of Eu3+-doped hydroxyapatite nanocrystal and the thermal treatment effects

    NASA Astrophysics Data System (ADS)

    Silva, Flávia R. O.; de Lima, Nelson B.; Bressiani, Ana Helena A.; Courrol, Lilia C.; Gomes, Laércio

    2015-09-01

    In this work, we present the synthesis, characterization and the luminescence properties of Ca10(PO4)6(OH)2 (hydroxyapatite/HAp) nanocrystals doped with europium trivalent ions. The most important processes that lead to europium emissions in the visible region were identified. Eu:HAp nanopowder excited at 394 nm (or 460 nm) exhibits several emissions: (i) weak emissions at 579 nm, 592 nm and 616 nm due to the 5D0 → 7F0, 5D0 → 7F1 and 5D0 → 7F2 transitions, respectively, with europium ion occupying site I in hydroxyapatite structure and (ii) strong emissions due to the 5D0 → 7F0 (574 nm), 5D0 → 7F1 (602 nm) and 5D0 → 7F2 (610-630 nm) transitions, when Eu3+ is occupying site II. The emission spectrum and the time-resolved luminescence analysis showed that the HAp nanocrystals (nanopowder) thermally treated at temperature (T) between 500 and 800 °C have a change in the initial Eu3+ site distribution of 100 % of Eu3+ at site I to a more stable one where the majority of europium ions are at site II: 30% remains at site I and 70% migrates to site II. In addition, an enhancement of the Eu3+ emission intensity is observed due to the increasing crystallite size. A time-resolved luminescence investigation using a short pulse laser excitation at 460 nm was employed to measure the luminescence decays and to determine the most important mechanisms involved in the deexcitation process of 5D0 excited state of Eu3+, where it is seen a fast (2.9 μs) energy transfer from Eu3+- site I (donor) to Eu3+- site II (acceptor) in the thermally treated nanopowders with T > 500 °C. The initial presence of 100% of Eu3+ at site I in the synthesized nanocrystals is gradually modified by the thermal treatments with temperatures above 500 °C by thermal activation of Ca2+ vacancy (the charge compensator) diffusion through the HAp lattice, which propitiates the Ca2+- vacancies and Eu3+ ions to exchange positions in the lattice. By this thermal activated mechanism, Eu3+ ion migrates

  1. Synthesis, characterization and gas sensing properties of tin oxide nanopowder

    NASA Astrophysics Data System (ADS)

    Choudhary, Meenakshi; Mishra, V. N.; Dwivedi, R.

    2013-06-01

    In the present work, tin oxide nanopowder has been synthesized by solid-state reaction technique. The as-prepared pure and palladium doped (0.5 and 1%) powders have been used for the fabrication of thick film sensors. The influence of particle size of powders and morphology of the thick films has been studied on the sensing performance of thick film sensor. It is observed that the sensors produced from the SnO2 doped with 1% palladium have an excellent ability for the detection of hydrogen gas.

  2. Green upconversion in Y2O3:Yb nanopowder

    NASA Astrophysics Data System (ADS)

    Horvat, Darja; Lazar, Dušan; Možina, Janez; Križan, Janez; Diaci, Janez; Terzić, Mira

    2015-01-01

    Green emission lines, in addition to the blue and the red, were observed upon 980 nm excitation in yttrium oxide (Y2O3) nanopowder codoped with Yb and Tm, synthesized by the chemical combustion method. Upconversion emission studies suggest that the number and characteristics of the green lines are influenced by the annealing temperature as well as by the Yb/Tm concentration ratio, opening possibilities for new customized applications. The chromaticity properties of the upconversion spectra were quantified by the Commission Internationale de l'éclairage coordinate analysis.

  3. Incorporation of chromium into TiO{sub 2} nanopowders

    SciTech Connect

    Kollbek, Kamila; Sikora, Marcin; Kapusta, Czesław; Szlachetko, Jakub; Radecka, Marta; Lyson-Sypien, Barbara; Zakrzewska, Katarzyna

    2015-04-15

    Highlights: • Nanopowders of TiO{sub 2}:Cr with different amount of Cr dopant were obtained by flame spray synthesis, FSS. • Increase in the optical absorption and a shift of the absorption edge were observed upon Cr doping. • HERFD-XANES measurements indicated that the average valence state of titanium ions was preserved. • Increasing magnetic susceptibility of a paramagnetic character was observed upon Cr doping. - Abstract: The paper reports on the results of a study of optical, electronic and magnetic properties of TiO{sub 2} nanopowders doped with Cr ions. Diffused reflectance spectra reveal an increase in the optical absorption and a shift of the absorption edge towards lower energies upon Cr doping. Direct information on the Ti electronic state and the symmetry of its nearest environment is obtained from XANES Ti K-edge spectra. Magnetic behaviour is probed by means of the temperature dependence of DC magnetic susceptibility. Increasing magnetic susceptibility of a paramagnetic character is observed upon increasing chromium doping. The Curie constant of TiO{sub 2}:10 at.% Cr sample (0.12 emu K/mol Oe) is lower than that expected for Cr{sup 3+} (0.1875 emu K/mol Oe) possibly due to the appearance of Cr{sup 4+} or the presence of the orbital contribution to the magnetic moment.

  4. Hydroxyapatite ceramics from hydrothermally prepared powders

    SciTech Connect

    Lin, C.H.; Huang, C.W.; Chang, S.C.

    1994-12-31

    Hydroxyapatite (Ca{sub 5}(PO{sub 4}){sub 3}(OH)) is an effective material for artificial human bone production. Hydroxyapatite powders were hydrothermally produced in this work by reacting Ca(OH){sub 2} with Na{sub 3}PO{sub 4}{center_dot}12H{sub 2}O in an autoclave at various temperature and for various times. The particle size of hydroxyapatite was observed to be very fine, uniform, around 50 nm, as well as independent of reaction time. The hydroxyapatite powders were compacted and sintered at various temperatures for 2 hrs. The density, grain size, and hardness of the hydroxyapatite ceramics were measured and compared with those of the hydroxyapatite ceramics produced by the powders from the commercial source. The hydroxyapatite ceramics from the hydrothermal powders were found to have a higher density, smaller grain size, and higher hardness. After the hydroxyapatite ceramics were dipped in a simulated biological body liquid for 10 days, the density and hardness of the hydroxyapatite ceramics from the hydrothermal powders were less deteriorated than those of the hydroxyapatite ceramics from the commercial powder.

  5. Spark plasma sintering of alumina nanopowders produced by electrical explosion of wires.

    PubMed

    An, Vladimir; Khasanov, Alexey; de Izarra, Charles

    2015-01-01

    Alumina nanopowders produced by electrical explosion of wires were sintered using the spark plasma sintering technique. The results of XRD analysis show that the main phase in the compacted nanopowders is α-Al2O3. According to the SEM observations, the sintered alumina nanopowder consists of micron-sized faceted grains and nano-sized necked grains. The increase in sintering temperature resulted in a higher density of the sintered powders: from 78.44 to 98.21 % of theoretical density. PMID:26543716

  6. Coralline hydroxyapatite in complex acetabular reconstruction.

    PubMed

    Wasielewski, Ray C; Sheridan, Kate C; Lubbers, Melissa A

    2008-04-01

    This retrospective study examined whether a coralline hydroxyapatite bone graft substitute adequately repaired bone defects during complex acetabular reconstructions. Seventeen patients who underwent acetabular revision using Pro Osteon 500 were assessed to determine whether any cups required re-revision, whether bone had incorporated into the coralline hydroxyapatite grafts, and whether the coralline hydroxyapatite grafts resorbed with time. At latest follow-up, no cups required re-revision, but 1 had failed. Radiographic evidence of bone incorporation was observed in every coralline hydroxyapatite graft. Graft resorption was not observed. PMID:19292282

  7. Crystallization of modified hydroxyapatite on titanium implants

    NASA Astrophysics Data System (ADS)

    Golovanova, O. A.; Izmailov, R. R.; Ghyngazov, S. A.; Zaits, A. V.

    2016-02-01

    Carbonated-hydroxyapatite (CHA) and Si-hydroxyapatite (Si-HA) precipitation have been synthesized from the model bioliquid solutions (synovial fluid and SBF). It is found that all the samples synthesized from the model solutions are single-phase and represent hydroxyapatite. The crystallization of the modified hydroxyapatite on alloys of different composition, roughness and subjected to different treatment techniques was investigated. Irradiation of the titanium substrates with the deposited biomimetic coating can facilitate further growth of the crystal and regeneration of the surface.

  8. Synthesis and characterization of porous hydroxyapatite and hydroxyapatite coatings

    SciTech Connect

    Nieh, T G; Choi, B W; Jankowski, A F

    2000-10-25

    A technique is developed to construct bulk hydroxyapatite (HAp) with different cellular structures. The technique involves the initial synthesis of nanocrystalline hydroxyapatite powder from an aqueous solution using water-soluble compounds and then followed by spray drying into agglomerated granules. The granules were further cold pressed and sintered into bulks at elevated temperatures. The sintering behavior of the HAp granules was characterized and compared with those previously reported. Resulting from the fact that the starting HAp powders were extremely fine, a relatively low activation energy for sintering was obtained. In the present study, both porous and dense structures were produced by varying powder morphology and sintering parameters. Porous structures consisting of open cells were constructed. Sintered structures were characterized using scanning electron microscopy and x-ray tomography. In the present paper, hydroxyapatite coatings produced by magnetron sputtering on silicon and titanium substrates will also be presented. The mechanical properties of the coatings were measured using nanoindentation techniques and microstructures examined using transmission electron microscopy.

  9. Chemical vapor synthesis and characterization of aluminum nanopowder

    NASA Astrophysics Data System (ADS)

    Choi, Jin Won; Sohn, Hong Yong; Choi, Young Joon; Fang, Zhigang Zak

    Aluminum is a component in many promising hydrogen storage materials such as aluminum hydride and complex aluminum hydrides. In this research, Al and TiAl 3-containing Al nanopowders were prepared by a chemical vapor synthesis (CVS) process using Mg as the reducing agent. XRD and EDS results indicated that the produced powder was composed of Al or Al with TiAl 3. The shape of the powder was spherical with the average size in the range of 10-50 nm measured by SEM, TEM, BET and ZetaPALS compared with the typically larger than 100 nm for commercially available fine Al powders. In addition, the effects of the operating conditions such as Ar flow rate, precursor feed rate and reaction temperature on the properties of the product powder were investigated.

  10. Effect of deposition parameters on the structural properties of ZnO nanopowders prepared by microwave-assisted hydrothermal synthesis

    NASA Astrophysics Data System (ADS)

    Caglar, Yasemin; Gorgun, Kamuran; Aksoy, Seval

    2015-03-01

    ZnO nanopowders were synthesized via microwave-assisted hydrothermal method at different deposition (microwave irradiation) times and pH values. The effects of pH and deposition (microwave irradiation) time on the crystalline structure and orientation of the ZnO nanopowders have been investigated by X-ray diffraction (XRD) study. XRD observations showed that the crystalline quality of ZnO nanopowders increased with increasing pH value. The crystallite size and texture coefficient values of ZnO nanopowders were calculated. The structural quality of ZnO nanopowder was improved by deposition parameters. Field emission scanning electron microscope (FESEM) was used to analyze the surface morphology of the ZnO nanopowders. Microwave irradiation time and pH value showed a significant effect on the surface morphology.

  11. Cementless Hydroxyapatite Coated Hip Prostheses

    PubMed Central

    Herrera, Antonio; Mateo, Jesús; Gil-Albarova, Jorge; Lobo-Escolar, Antonio; Ibarz, Elena; Gabarre, Sergio; Más, Yolanda

    2015-01-01

    More than twenty years ago, hydroxyapatite (HA), calcium phosphate ceramics, was introduced as a coating for cementless hip prostheses. The choice of this ceramic is due to its composition being similar to organic apatite bone crystals. This ceramic is biocompatible, bioactive, and osteoconductive. These qualities facilitate the primary stability and osseointegration of implants. Our surgical experience includes the implantation of more than 4,000 cementless hydroxyapatite coated hip prostheses since 1990. The models implanted are coated with HA in the acetabulum and in the metaphyseal area of the stem. The results corresponding to survival and stability of implants were very satisfactory in the long-term. From our experience, HA-coated hip implants are a reliable alternative which can achieve long term survival, provided that certain requirements are met: good design selection, sound choice of bearing surfaces based on patient life expectancy, meticulous surgical technique, and indications based on adequate bone quality. PMID:25802848

  12. Structural and physical properties of antibacterial Ag-doped nano-hydroxyapatite synthesized at 100°C

    PubMed Central

    2011-01-01

    Synthesis of nanosized particle of Ag-doped hydroxyapatite with antibacterial properties is in the great interest in the development of new biomedical applications. In this article, we propose a method for synthesized the Ag-doped nanocrystalline hydroxyapatite. A silver-doped nanocrystalline hydroxyapatite was synthesized at 100°C in deionized water. Other phase or impurities were not observed. Silver-doped hydroxyapatite nanoparticles (Ag:HAp) were performed by setting the atomic ratio of Ag/[Ag + Ca] at 20% and [Ca + Ag]/P as 1.67. The X-ray diffraction studies demonstrate that powders made by co-precipitation at 100°C exhibit the apatite characteristics with good crystal structure and no new phase or impurity is found. The scanning electron microscopy (SEM) observations suggest that these materials present a little different morphology, which reveals a homogeneous aspect of the synthesized particles for all samples. The presence of calcium (Ca), phosphor (P), oxygen (O), and silver (Ag) in the Ag:HAp is confirmed by energy dispersive X-ray (EDAX) analysis. FT-IR and FT-Raman spectroscopies revealed that the presence of the various vibrational modes corresponds to phosphates and hydroxyl groups. The strain of Staphylococcus aureus was used to evaluate the antibacterial activity of the Ca10-xAgx(PO4)6(OH)2 (x = 0 and 0.2). In vitro bacterial adhesion study indicated a significant difference between HAp (x = 0) and Ag:HAp (x = 0.2). The Ag:Hap nanopowder showed higher inhibition. PMID:22136671

  13. Electron microscopy of biomaterials based on hydroxyapatite

    SciTech Connect

    Suvorova, E. I. Klechkovskaya, V. V.; Komarov, V. F.; Severin, A. V.; Melikhov, I. V.; Buffat, P. A.

    2006-10-15

    Three types of biomaterials based on hydroxyapatite are synthesized and investigated. Hydroxyapatite nanocrystals or microcrystals precipitated from low-temperature aqueous solutions serve as the initial material used for preparing spherical porous granules approximately 300-500 {mu}m in diameter. Sintering of hydroxyapatite crystals at a temperature of 870 deg. C for 2 h or at 1000 deg. C (for 3 h) + 1200 deg. C (for 2 h) brings about the formation of solid ceramics with different internal structures. According to the electron microscopic data, the ceramic material prepared at 870 deg. C is formed by agglomerated hydroxyapatite nanocrystals, whereas the ceramics sintered at 1200 deg. C (with a bending strength of the order of 100 MPa) are composed of crystal blocks as large as 2 {mu}m. It is established that all the biomaterials have a single-phase composition and consist of the hydroxyapatite with a structure retained up to a temperature of 1200 deg. C.

  14. Mechanical and cytotoxicity evaluation of nanostructured hydroxyapatite-bredigite scaffolds for bone regeneration.

    PubMed

    Eilbagi, Marjan; Emadi, Rahmatollah; Raeissi, Keyvan; Kharaziha, Mahshid; Valiani, Ali

    2016-11-01

    Despite the attractive characteristics of three-dimensional pure hydroxyapatite (HA) scaffolds, due to their weak mechanical properties, researches have focused on the development of composite scaffolds via introducing suitable secondary components. The aim of this study was to develop, for the first time, three-dimensional HA-bredigite (Ca7MgSi4O16) scaffolds containing various amounts of bredigite nanopowder (0, 5, 10 and 15wt.%) using space holder technique. Transmission electron microscopy, scanning electron microscopy, energy-dispersive X-ray spectroscopy and X-ray diffraction spectroscopy were applied in order to study the morphology, fracture surface and phase compositions of nanopowders and scaffolds. Furthermore, the effects of scaffold composition on the mechanical properties, bioactivity, biodegradability, and cytotoxicity were also evaluated. Results showed that the composite scaffolds with average pore size in the range of 220-310μm, appearance porosity of 63.1-75.9% and appearance density of 1.1±0.04g/cm(3) were successfully developed, depending on bredigite content. Indeed, the micropore size of the scaffolds reduced with increasing bredigite content confirming that the sinterability of the scaffolds was improved. Furthermore, the compression strength and modulus of the scaffolds significantly enhanced via incorporation of bredigite content from 0 to 15wt.%. The composite scaffolds revealed superior bioactivity and biodegradability with increasing bredigite content. Moreover, MTT assay confirmed that HA-15wt.% bredigite scaffold significantly promoted cell proliferation compared to tissue culture plate (control) and HA scaffold. Based on these results, three-dimensional HA-bredigite scaffolds could be promising replacements for HA scaffolds in bone regeneration. PMID:27524060

  15. Synthesis and spectral characterizations of trivalent ions (Cr3+, Fe3+) doped CdO nanopowders.

    PubMed

    Aswani, T; Babu, B; Manjari, V Pushpa; Stella, R Joyce; Rao, G Thirumala; Krishna, Ch Rama; Ravikumar, R V S S N

    2014-01-01

    Trivalent transition metal ions (Cr(3+), Fe(3+)) doped CdO nanopowders via sonication in the presence of Sodium lauryl sulfate as stabilizing agent were synthesized and characterized. Powder XRD studies indicate that the obtained CdO has a cubic phase and concluded that the trivalent ions doping induced the lattice constants to change some extent. Optical absorption spectra exhibited the characteristic bands of Cr(3+) and Fe(3+) ions in octahedral site symmetry. Crystal field (Dq) and inter-electronic repulsion (B and C) parameters are evaluated for Cr(3+) doped CdO nanopowders as Dq=1540, B=619 and C=3327 cm(-1) and for Fe(3+) doped CdO nanopowders Dq=920, B=690, C=2750 cm(-1). EPR spectra of the Cr(3+) and Fe(3+) doped CdO nanopowders exhibited resonances at g=1.973 and g=2 respectively which indicate distorted octahedral site for both ions with the host. Photoluminescence spectra shows the emission bands in violet and bluish green regions for Cr(3+) doped CdO, ultraviolet and blue emissions for Fe(3+) doped CdO nanopowders. The CIE chromaticity coordinates were also evaluated from the emission spectrum. FT-IR spectra indicate the presence of various functional groups of host lattice. PMID:24291431

  16. Preparation, structural and linear optical properties of Zn doped CdS nanopowders

    NASA Astrophysics Data System (ADS)

    Sekhar, H.; Rakesh Kumar, Y.; Narayana Rao, D.

    2015-02-01

    A series of Zn doped cadmium sulfide (CdS:Zn) nanopowders were prepared by a simple co-precipitation method at room temperature by mixing the stoichiometric amount of reactants in a Milli Q water solvent. The composition of nanopowders was accurately adjusted by controlling the molar ratio of Cd, Zn acetate in the mixed reactants. Spectroscopic studies on as prepared nanopowders were investigated by using XRD, Raman, UV-Vis absorption, FE- SEM-EDAX and photoluminescence. Extremely broad reflections of XRD peaks of as prepared powders establish the nanometer scale dimensions and cubic structure. Doping with Zn in CdS does not lead to any structural phase transformation but introduces a decrease in the lattice constants. Two characteristics of LO phonon peaks were observed in pure and Zn doped CdS samples. Raman peaks of Zn doped CdS nanopowders shifts slightly towards higher energy side compared to the pure CdS nanopowders. Exciton-phonon confinement factor (S) varies in between 0.3-0.4. At lower wavelength excitation we observed a broad emission peak maximum centered at 404 nm is attributed to localized band edge emission.

  17. Nanopowder production by gas-embedded electrical explosion of wire

    NASA Astrophysics Data System (ADS)

    Zou, Xiao-Bing; Mao, Zhi-Guo; Wang, Xin-Xin; Jiang, Wei-Hua

    2013-04-01

    A small electrical explosion of wire (EEW) setup for nanopowder production is constructed. It consists of a low inductance capacitor bank of 2 μF-4 μF typically charged to 8 kV-30 kV, a triggered gas switch, and a production chamber housing the exploding wire load and ambient gas. With the EEW device, nanosize powders of titanium oxides, titanium nitrides, copper oxides, and zinc oxides are successfully synthesized. The average particle size of synthesized powders under different experimental conditions is in a range of 20 nm-80 nm. The pressure of ambient gas or wire vapor can strongly affect the average particle size. The lower the pressure, the smaller the particle size is. For wire material with relatively high resistivity, such as titanium, whose deposited energy Wd is often less than sublimation energy Ws due to the flashover breakdown along the wire prematurely ending the Joule heating process, the synthesized particle size of titanium oxides or titanium nitrides increases with overheat coefficient k (k = Wd/Ws) increasing.

  18. Shock induced reaction of Ni/Al nanopowder mixture.

    PubMed

    Meng, C M; Wei, J J; Chen, Q Y

    2012-11-01

    Nanopowder Ni/Al mixture (mixed in Al:Ni = 2:1 stoichiometry) was shock compressed by employing single and two-stage light gas gun. The particle size of Al and Ni are 100-200 nm and 50-70 nm respectively, morphologies of Al and Ni are sphere like either. Recovered product was characterized by scanning electron microscope (SEM) and X-ray diffraction (XRD) analysis. According to the XRD spectrum, the mixed powder undergo complete reaction under shock compression, reaction product consist of Ni2Al3, NiAl and corundum structure Al2O3 compound. Grain size of Ni-Al compound is less than 100 nm. With the shock pressure increasing, the ratio of Ni2Al3 decreased obviously. The corundum crystal size is 400-500 nm according to the SEM observation. The results of shock recovery experiments and analysis show that the threshold pressure for reaction of nano size powder Ni/Al mixture is much less than that of micro size powder. PMID:23421276

  19. Ce, Gd codoped YAG nanopowder for white light emitting device.

    PubMed

    Schiopu, Vasilica; Matei, Alina; Dinescu, Adrian; Danila, Mihai; Cernica, Ileana

    2012-11-01

    In the last years white light emitting devices have received increased attention and have been used in a wide range of applications due to their long lifetime, high luminescence efficiency, low power consumption and environment friendliness, compared to conventional light sources. The discovery and improvement of inorganic phosphors that can be excited by a GaN chip in the wavelength range 370-470 nm is essential for the efficiency and quality of the emitted light. In the white light emitting device technology, the phosphor preparation step is the most important and it's quality defines the "whiteness". The tunable yellow emission property of YAG:Ce phosphor may be improved by the incorporation of an additional codoping element. Ce, Gd codoped YAG phosphor nanopowder with an average grain size of 40 nm has been synthesized by a sol-gel method. Well-crystallized fine nanoparticles and the formation of the garnet phase have been obtained at 1000 degrees C. The chemical structure and morphology of YAG:Ce, Gd was studied. PMID:23421297

  20. A System to Create Stable Nanoparticle Aerosols from Nanopowders.

    PubMed

    Ding, Yaobo; Riediker, Michael

    2016-01-01

    Nanoparticle aerosols released from nanopowders in workplaces are associated with human exposure and health risks. We developed a novel system, requiring minimal amounts of test materials (min. 200 mg), for studying powder aerosolization behavior and aerosol properties. The aerosolization procedure follows the concept of the fluidized-bed process, but occurs in the modified volume of a V-shaped aerosol generator. The airborne particle number concentration is adjustable by controlling the air flow rate. The system supplied stable aerosol generation rates and particle size distributions over long periods (0.5-2 hr and possibly longer), which are important, for example, to study aerosol behavior, but also for toxicological studies. Strict adherence to the operating procedures during the aerosolization experiments ensures the generation of reproducible test results. The critical steps in the standard protocol are the preparation of the material and setup, and the aerosolization operations themselves. The system can be used for experiments requiring stable aerosol concentrations and may also be an alternative method for testing dustiness. The controlled aerosolization made possible with this setup occurs using energy inputs (may be characterized by aerosolization air velocity) that are within the ranges commonly found in occupational environments where nanomaterial powders are handled. This setup and its operating protocol are thus helpful for human exposure and risk assessment. PMID:27501179

  1. Substituted Hydroxyapatites with Antibacterial Properties

    PubMed Central

    Kolmas, Joanna; Groszyk, Ewa; Kwiatkowska-Różycka, Dagmara

    2014-01-01

    Reconstructive surgery is presently struggling with the problem of infections located within implantation biomaterials. Of course, the best antibacterial protection is antibiotic therapy. However, oral antibiotic therapy is sometimes ineffective, while administering an antibiotic at the location of infection is often associated with an unfavourable ratio of dosage efficiency and toxic effect. Thus, the present study aims to find a new factor which may improve antibacterial activity while also presenting low toxicity to the human cells. Such factors are usually implemented along with the implant itself and may be an integral part of it. Many recent studies have focused on inorganic factors, such as metal nanoparticles, salts, and metal oxides. The advantages of inorganic factors include the ease with which they can be combined with ceramic and polymeric biomaterials. The following review focuses on hydroxyapatites substituted with ions with antibacterial properties. It considers materials that have already been applied in regenerative medicine (e.g., hydroxyapatites with silver ions) and those that are only at the preliminary stage of research and which could potentially be used in implantology or dentistry. We present methods for the synthesis of modified apatites and the antibacterial mechanisms of various ions as well as their antibacterial efficiency. PMID:24949423

  2. Sintering Effects on Morphology, Thermal Stability and Surface Area of Sol-Gel Derived Nano-Hydroxyapatite Powder

    NASA Astrophysics Data System (ADS)

    Kapoor, Seema; Batra, Uma; Kohli, Suchita

    2011-12-01

    Hydroxyapatite (HAP) ceramics have been recognized as substitute materials for bone and teeth in orthopedic and dentistry field due to their chemical and biological similarity to human hard tissue. The nanosized and nanocrystalline forms of HAP have great potential to revolutionize the hard tissue-engineering field, starting from bone repair and augmentation to controlled drug delivery systems. This paper reports the synthesis of biomimetic nano-hydroxyapatite (HAP) by sol-gel method using calcium nitrate tetrahydrate (CNT) and potassium dihydrogen phosphate (KDP) as calcium and phosphorus precursors, respectively to obtain a desired Ca/P ratio of 1.67. Deionized water was used as a diluting media for HAP sol preparation and ammonia was used to adjust the pH to 11. After aging, the HAP gel was dried at 55 °C and sintered to different temperatures (200 °C, 400 °C, 600 °C, 800 °C, 1000 °C and 1200 °C). The dried and sintered powders were characterized for phase composition using Fourier transform infrared (FTIR) spectroscopy and X-ray diffraction (XRD). The particle size and morphology was studied using transmission electron microscopy (TEM). The thermal behavior of the dried HAP nanopowder was studied in the temperature range of 55 °C to 1000 °C using thermal gravimetric analyser (TGA). The BET surface area of absorbance was determined by Nitrogen adsorption using Brunauer-Emmett-Teller (BET) method. The presence of characteristic peaks of the phosphate and OH groups in FTIR spectrums confirmed the formation of pure HAP in dried as well as sintered powders. XRD results also confirmed the formation of stoichiometric nano-HAP. Sintering revealed that with increase in temperature, both the crystallinity and crystallite size of nano-HAP particles increased. The synthesized nano-HAP powder was found to be stable upto 1000 °C without any additional phase other than HAP, whereas peak of β-TCP (tricalcium phosphate) was observed at 1200 °C. Photomicrograph of

  3. Sintering Effects on Morphology, Thermal Stability and Surface Area of Sol-Gel Derived Nano-Hydroxyapatite Powder

    SciTech Connect

    Kapoor, Seema; Batra, Uma; Kohli, Suchita

    2011-12-12

    Hydroxyapatite (HAP) ceramics have been recognized as substitute materials for bone and teeth in orthopedic and dentistry field due to their chemical and biological similarity to human hard tissue. The nanosized and nanocrystalline forms of HAP have great potential to revolutionize the hard tissue-engineering field, starting from bone repair and augmentation to controlled drug delivery systems. This paper reports the synthesis of biomimetic nano-hydroxyapatite (HAP) by sol-gel method using calcium nitrate tetrahydrate (CNT) and potassium dihydrogen phosphate (KDP) as calcium and phosphorus precursors, respectively to obtain a desired Ca/P ratio of 1.67. Deionized water was used as a diluting media for HAP sol preparation and ammonia was used to adjust the pH to 11. After aging, the HAP gel was dried at 55 deg. C and sintered to different temperatures (200 deg. C, 400 deg. C, 600 deg. C, 800 deg. C, 1000 deg. C and 1200 deg. C). The dried and sintered powders were characterized for phase composition using Fourier transform infrared (FTIR) spectroscopy and X-ray diffraction (XRD). The particle size and morphology was studied using transmission electron microscopy (TEM). The thermal behavior of the dried HAP nanopowder was studied in the temperature range of 55 deg. C to 1000 deg. C using thermal gravimetric analyser (TGA). The BET surface area of absorbance was determined by Nitrogen adsorption using Brunauer-Emmett-Teller (BET) method. The presence of characteristic peaks of the phosphate and OH groups in FTIR spectrums confirmed the formation of pure HAP in dried as well as sintered powders. XRD results also confirmed the formation of stoichiometric nano-HAP. Sintering revealed that with increase in temperature, both the crystallinity and crystallite size of nano-HAP particles increased. The synthesized nano-HAP powder was found to be stable upto 1000 deg. C without any additional phase other than HAP, whereas peak of {beta}-TCP (tricalcium phosphate) was observed

  4. Influence of Obtaining Conditions on Kinetics of the Initial Sintering Stage of Zirconia Nanopowders.

    PubMed

    Lakusta, Marharyta; Danilenko, Igor; Konstantinova, Tetyana; Volkova, Galina

    2016-12-01

    The present paper is devoted to the problem of sintering ceramics based on yttria-stabilized zirconia (Y-TZP). In this paper, we studied the effect of two obtaining methods (co-precipitation and technical hydrolysis) on sintering kinetics of Y-TZP nanopowders. We used the constant rate of heating (CRH) method at different heating rates for determining the sintering mechanisms. The basic mechanism and activation energy (Q) of diffusion at the initial sintering stage were estimated using the sintering rate equations that are applicable to the CRH data. We found that nanopowder 3Y-TZP produced by the co-precipitation method (DIPE) was sintered according to the volume diffusion mechanism (n = 1/2) and nanopowder TZ-3Y (TOSOH) produced by the technical hydrolysis was sintered according to the grain boundary diffusion mechanism (n = 1/3). PMID:27142876

  5. Influence of Obtaining Conditions on Kinetics of the Initial Sintering Stage of Zirconia Nanopowders

    NASA Astrophysics Data System (ADS)

    Lakusta, Marharyta; Danilenko, Igor; Konstantinova, Tetyana; Volkova, Galina

    2016-05-01

    The present paper is devoted to the problem of sintering ceramics based on yttria-stabilized zirconia (Y-TZP). In this paper, we studied the effect of two obtaining methods (co-precipitation and technical hydrolysis) on sintering kinetics of Y-TZP nanopowders. We used the constant rate of heating (CRH) method at different heating rates for determining the sintering mechanisms. The basic mechanism and activation energy ( Q) of diffusion at the initial sintering stage were estimated using the sintering rate equations that are applicable to the CRH data. We found that nanopowder 3Y-TZP produced by the co-precipitation method (DIPE) was sintered according to the volume diffusion mechanism ( n = 1/2) and nanopowder TZ-3Y (TOSOH) produced by the technical hydrolysis was sintered according to the grain boundary diffusion mechanism ( n = 1/3).

  6. Copper and Graphene activated ZnO nanopowders for enhanced photocatalytic and antibacterial activities

    NASA Astrophysics Data System (ADS)

    Ravichandran, K.; Chidhambaram, N.; Gobalakrishnan, S.

    2016-06-01

    ZnO, ZnO:Cu and ZnO:Cu:Graphene nanopowders were synthesized via a facile wet chemical method. The XRD studies show that the synthesized samples have hexagonal wurtzite structure. It is found that graphene addition induces a decrease in crystallite size. UV-vis absorption spectra of the samples show sharp absorption edges around 380 nm. Photoluminescence studies reveal that the incorporation of copper and graphene in ZnO facilitates the efficient photo generated electron-hole pair separation. It is found that the ZnO:Cu and ZnO:Cu:Graphene nanopowder exhibit improved photocatalytic efficiency for the photodegradation of Methylene Blue (MB) under visible light irradiation. Moreover, improved antibacterial activity of ZnO:Cu:Graphene nanopowder against Escherichia coli and Staphylococcus aureus bacteria is observed.

  7. Bio-ecological consequences of crop seeds treatment with metal nano-powders

    NASA Astrophysics Data System (ADS)

    Churilov, G.

    2015-11-01

    As a result of our investigations we have determined the optimal concentrations of ferrum, cobalt and cuprum nano-powders recommended to be used as micro-fertilizers increasing the yield and feed value of crops at the expense of accumulating biologically active combinations by 25-35%. In unfavorable climate conditions, for example in a case of excess moisture or heat and drought, the plants development and ripening suffer. Our investigations have shown that the stimulating effect of nano-powders has lowered the effect of stress situations on plants development and simultaneously increased the rape seeds yield and quality. Treating the seeds with the drugs being studied has provided the high crop protection. If consider that the maximum efficiency of protectants Chinuk, SK (20 kg/t of seeds) and Cruiser, KS (10 kg/t of seeds) then for the same effect one needs nano-powders 0.1 g per hectare norm of seeds planting.

  8. Dissolution studies of hydroxyapatite and glass-reinforced hydroxyapatite ceramics

    SciTech Connect

    Queiroz, A.C.; Santos, J.D.; Monteiro, F.J.; Prado da Silva, M.H

    2003-03-15

    In the continuous agitation assays, glass-reinforced hydroxyapatite (GR-HA) was shown to form a calcium phosphate (CaP) layer, but hydroxyapatite (HA) only formed dispersed precipitates. The formation of this layer was first detected on the GR-HA with a 7.5% glass addition (7.5 GR-HA) after only 3 days of immersion in simulated body fluid (SBF). The time required for layer formation decreased as the amount of glass added to the HA increased. The dissolution rate of the materials followed a similar pattern, i.e. the dissolution rate for GR-HA was higher than for HA, and increased with the addition of glass. The immersion of 7.5 GR-HA in water showed almost linear dissolution kinetics over the immersion periods (3, 7, 15, 30 and 60 days). The concentration of calcium ions in solution and the scanning electron microscopy (SEM) analysis of the 7.5 GR-HA specimens immersed in water and in SBF revealed a clear competition between the material dissolution and the precipitation of a CaP phase. Fourier transformed infrared spectroscopy with alternated total reflectance (FTIR-ATR) analysis indicated that the CaP phase that formed during longer immersion times (30 and 60 days) could be a carbonate-substituted CaP precipitate. As expected from previous work, the GR-HA behavior in terms of its in vitro bioactivity is higher than HA because a homogeneous CaP layer is formed and the precipitation occurs faster. From the dissolution test and in accordance with the chemical composition of the samples, GR-HA was more soluble than HA.

  9. Corundum ceramic materials modified with silica nanopowders: structure and mechanical properties

    NASA Astrophysics Data System (ADS)

    Kostytsyn, M. A.; Muratov, D. S.; Lysov, D. V.; Chuprunov, K. O.; Yudin, A. G.; Leybo, D. V.

    2016-01-01

    Filtering elements are often used in the metallurgy of rare earth metals. Corundum ceramic is one of the most suitable materials for this purpose. The process of formation and the properties of nanomodified ceramic materials, which are proposed as filtering materials with tunable effective porosity, are described. A silica nanopowder is used as a porosity-increasing agent. Vortex layer apparatus is used for mixing of precursor materials. The obtained results show that nanomodification with the vortex layer apparatus using 0.04 wt. % silica nanopowder as a modifying agent leads to an increase in the compression strength of corundum ceramic by the factor of 1.5.

  10. Optical property degradation of titanium dioxide micro- and nanopowders under irradiation

    NASA Astrophysics Data System (ADS)

    Mikhailov, M. M.; Li, Chundong; Neshchimenko, V. V.

    2014-08-01

    Diffuse reflection spectra and absorption spectra of titanium dioxide (anatase) micro- and nanopowders induced by exposure to 100 keV protons and electrons were analyzed at wavelengths between 250 and 2500 nm. It is established that the radiation stability of the nanopowders is higher than the micropowders in the absorption region λ > 500 nm for proton and electron exposure. This effect is caused by the high concentration of radiation defects in micropowders, which is associated with defects of interstitial titanium ions (Tiirad rad rad , Tiirad rad rad rad ), titanium vacancies (VTi⁗, VTi‴ ) and oxygen vacancies VOX.

  11. Radiation stability of SiO2 micro- and nanopowders under electron and proton exposure

    NASA Astrophysics Data System (ADS)

    Li, Chundong; Mikhailov, M. M.; Neshchimenko, V. V.

    2014-01-01

    The effects of proton and electron (E = 100 keV, F = 5 × 1015 сm-2) exposure on the reflective spectra of SiO2 micro- and nanopowders in wavelength range from 250 to 2500 nm have been investigated. It has been established that the reflectance and radiation stability of nanopowders is less than that of micropowders. This effect is caused by the high concentration of radiation defects, which act as surface absorption centers (Es‧ centers) near the energies 5.47 and 4.45 eV, and peroxide silicon defects (tbnd Sisbnd Osbnd Osbnd Sitbnd) near the energy 3.84 eV.

  12. Far-infrared spectra of dysprosium doped yttrium aluminum garnet nanopowder

    NASA Astrophysics Data System (ADS)

    Trajić, J.; Rabasović, M. S.; Savić-Šević, S.; Ševic, D.; Babić, B.; Romčević, M.; Ristić-Djurović, J. L.; Paunović, N.; Križan, J.; Romčević, N.

    2016-07-01

    The solution combustion synthesis was used to prepare nanopowders of yttrium aluminum garnet (YAG) and YAG doped with dysprosium ions, Dy3+, (YAG:Dy). The morphology, specific surface area, texture, and optical properties of the prepared materials were studied by the means of scanning electron microscopy (SEM), nitrogen adsorption method, and far-infrared spectroscopy at room temperature in the spectral region between 80 and 600 cm-1. It was established that all the examined samples were microporous. The Maxwell-Garnet formula was used to model dielectric function of YAG and YAG:Dy nanopowders as mixtures of homogenous spherical inclusions in air.

  13. On the anisotropic elastic properties of hydroxyapatite.

    NASA Technical Reports Server (NTRS)

    Katz, J. L.; Ukraincik, K.

    1971-01-01

    Experimental measurements of the isotropic elastic moduli on polycrystalline specimens of hydroxyapatite and fluorapatite are compared with elastic constants measured directly from single crystals of fluorapatite in order to derive a set of pseudo single crystal elastic constants for hydroxyapatite. The stiffness coefficients thus derived are given. The anisotropic and isotropic elastic properties are then computed and compared with similar properties derived from experimental observations of the anisotropic behavior of bone.

  14. Detection of Hydroxyapatite in Calcified Cardiovascular Tissues

    PubMed Central

    Lee, Jae Sam; Morrisett, Joel D.; Tung, Ching-Hsuan

    2012-01-01

    Objective The objective of this study is to develop a method for selective detection of the calcific (hydroxyapatite) component in human aortic smooth muscle cells in vitro and in calcified cardiovascular tissues ex vivo. This method uses a novel optical molecular imaging contrast dye, Cy-HABP-19, to target calcified cells and tissues. Methods A peptide that mimics the binding affinity of osteocalcin was used to label hydroxyapatite in vitro and ex vivo. Morphological changes in vascular smooth muscle cells were evaluated at an early stage of the mineralization process induced by extrinsic stimuli, osteogenic factors and a magnetic suspension cell culture. Hydroxyapatite components were detected in monolayers of these cells in the presence of osteogenic factors and a magnetic suspension environment. Results Atherosclerotic plaque contains multiple components including lipidic, fibrotic, thrombotic, and calcific materials. Using optical imaging and the Cy-HABP-19 molecular imaging probe, we demonstrated that hydroxyapatite components could be selectively distinguished from various calcium salts in human aortic smooth muscle cells in vitro and in calcified cardiovascular tissues, carotid endarterectomy samples and aortic valves, ex vivo. Conclusion Hydroxyapatite deposits in cardiovascular tissues were selectively detected in the early stage of the calcification process using our Cy-HABP-19 probe. This new probe makes it possible to study the earliest events associated with vascular hydroxyapatite deposition at the cellular and molecular levels. This target-selective molecular imaging probe approach holds high potential for revealing early pathophysiological changes, leading to progression, regression, or stabilization of cardiovascular diseases. PMID:22877867

  15. Fostering hydroxyapatite bioactivity and mechanical strength by Si-doping and reinforcing with multiwall carbon nanotubes.

    PubMed

    Belmamouni, Younes; Bricha, Meriame; Essassi, El Mokhtar; Ferreira, José M F; El Mabrouk, Khalil

    2014-06-01

    The aim of the present study was to prepare resorbable hydroxyapatite (HA) based bone graft materials reinforced with carbon nanotubes as a way to cope with the inability of pure HA to resorb and its intrinsic brittleness and poor strength that restrict its clinical applications under load-bearing conditions. With this purpose, a Si-doped HA nanopowder (n-Si0.8HA) was prepared by chemical synthesis and used as composite matrix reinforced with different amounts of functionalized multiwall carbon nanotubes (MWCNTs). The effect of the added amounts of MWCNTs on the mechanical properties of nanocomposites and their in vitro biomineralization was assessed by bending strength measurements, immersing tests in simulated body fluid solution (SBF), scanning electron microscopy (SEM), and inductively coupled plasma atomic emission spectroscopy analysis (ICP-AES). The bioactivity and bending strength were enhanced, reaching maximum balanced values for an optimum addition of 3 wt.% f-MWCNTs. These results might contribute to broaden the potential applications of HA-based bone grafts. PMID:24738405

  16. Brushite-based calcium phosphate cement with multichannel hydroxyapatite granule loading for improved bone regeneration.

    PubMed

    Sarkar, Swapan Kumar; Lee, Byung Yeol; Padalhin, Andrew Reyas; Sarker, Avik; Carpena, Nathaniel; Kim, Boram; Paul, Kallyanshish; Choi, Hwan Jun; Bae, Sang-Ho; Lee, Byong Taek

    2016-01-01

    In this work, we report brushite-based calcium phosphate cement (CPC) system to enhance the in vivo biodegradation and tissue in-growth by incorporation of micro-channeled hydroxyapatite (HAp) granule and silicon and sodium addition in calcium phosphate precursor powder. Sodium- and silicon-rich calcium phosphate powder with predominantly tri calcium phosphate (TCP) phase was synthesized by an inexpensive wet chemical route to react with mono calcium phosphate monohydrate (MCPM) for making the CPC. TCP nanopowder also served as a packing filler and moderator of the reaction kinetics of the setting mechanism. Strong sintered cylindrical HAp granules were prepared by fibrous monolithic (FM) process, which is 800 µm in diameter and have seven micro-channels. Acid sodium pyrophosphate and sodium citrate solution was used as the liquid component which acted as a homogenizer and setting time retarder. The granules accelerated the degradation of the brushite cement matrix as well as improved the bone tissue in-growth by permitting an easy access to the interior of the CPC through the micro-channels. The addition of micro-channeled granule in the CPC introduced porosity without sacrificing much of its compressive strength. In vivo investigation by creating a critical size defect in the femur head of a rabbit model for 1 and 2 months showed excellent bone in-growth through the micro-channels. The granules enhanced the implant degradation behavior and bone regeneration in the implanted area was significantly improved after two months of implantation. PMID:26333790

  17. Use of Hydroxyapatite Doping to Enhance Responsiveness of Heat-Inducible Gene Switches to Focused Ultrasound.

    PubMed

    Fabiilli, Mario L; Phanse, Rahul A; Moncion, Alexander; Fowlkes, J Brian; Franceschi, Renny T

    2016-03-01

    Recently, we demonstrated that ultrasound-based hyperthermia can activate cells containing a heat-activated and ligand-inducible gene switch in a spatio-temporally controlled manner. These engineered cells can be incorporated into hydrogel scaffolds (e.g., fibrin) for in vivo implantation, where ultrasound can be used to non-invasively pattern transgene expression. Due to their high water content, the acoustic attenuation of fibrin scaffolds is low. Thus, long ultrasound exposures and high acoustic intensities are needed to generate sufficient hyperthermia for gene activation. Here, we demonstrate that the attenuation of fibrin scaffolds and the resulting hyperthermia achievable with ultrasound can be increased significantly by doping the fibrin with hydroxyapatite (HA) nanopowder. The attenuation of a 1% (w/v) fibrin scaffold with 5% (w/v) HA was similar to soft tissue. Transgene activation of cells harboring the gene switch occurred at lower acoustic intensities and shorter exposures when the cells were encapsulated in HA-doped fibrin scaffolds versus undoped scaffolds. Inclusion of HA in the fibrin scaffold did not affect the viability of the encapsulated cells. PMID:26712417

  18. Microwave processed nanocrystalline hydroxyapatite: Simultaneous enhancement of mechanical and biological properties

    PubMed Central

    Bose, Susmita; Dasgupta, Sudip; Tarafder, Solaiman; Bandyopadhyay, Amit

    2010-01-01

    Despite excellent bioactivity of hydroxyapatite (HA) ceramics, poor mechanical strength has limited its applications primarily to coatings and other non-load bearing areas as bone grafts. Using synthesized HA nanopowder, dense compacts with grain sizes in nanometers to micrometers were processed via microwave sintering between 1000 and 1150 °C for 20 minutes. Here we demonstrate that mechanical properties, such as compressive strength, hardness and indentation fracture toughness of HA compacts increased with a decrease in grain size. HA with 168± 86 nm grain size showed the highest compressive strength of 395±42 MPa, hardness of 8.4±0.4 GPa and indentation fracture toughness of 1.9 ±0.2 MPam1/2. To study the in vitro biological properties, HA compacts with grain size between 168 nm and 1.16 µm were assessed for in vitro bone cell-materials interactions with human osteoblast cell line. Vinculin protein expression for cell attachment and bone cell proliferation using MTT assay showed surfaces with finer grains provided better bone cell-materials interactions than coarse grained samples. Our results indicate simultaneous improvements in mechanical and biological properties in microwave sintered HA compacts with nanoscale grain size. PMID:20230922

  19. Lower sintering temperature of nanostructured dense ceramics compacted from dry nanopowders using powerful ultrasonic action

    NASA Astrophysics Data System (ADS)

    Khasanov, O.; Reichel, U.; Dvilis, E.; Khasanov, A.

    2011-10-01

    Nanostructured high dense zirconia ceramics have been sintered from dry nanopowders compacted by uniaxial pressing with simultaneous powerful ultrasonic action (PUA). Powerful ultrasound with frequency of 21 kHz was supplied from ultrasonic generator to the mold, which was the ultrasonic wave-guide. Previously the mold was filled by non-agglomerated zirconia nanopowder having average particle size of 40 nm. Any binders or plasticizers were excluded at nanopowder processing. Compaction pressure was 240 MPa, power of ultrasonic generator at PUA was 1 kW and 3 kW. The fully dense zirconia ceramics has been sintered at 1345°C and high-dense ceramics with a density of 99.1%, the most grains of which had the sizes Dgr <= 200 nm, has been sintered at low sintering temperature (1325°C). Applied approach prevents essential grain growth owing to uniform packing of nanoparticles under vibrating PU-action at pressing, which provides the friction forces control during dry nanopowder compaction without contaminating binders or plasticizers.

  20. Workplace Exposure to Titanium Dioxide Nanopowder Released from a Bag Filter System

    PubMed Central

    Ji, Jun Ho; Kim, Jong Bum; Lee, Gwangjae; Noh, Jung-Hun; Yook, Se-Jin; Cho, So-Hye; Bae, Gwi-Nam

    2015-01-01

    Many researchers who use laboratory-scale synthesis systems to manufacture nanomaterials could be easily exposed to airborne nanomaterials during the research and development stage. This study used various real-time aerosol detectors to investigate the presence of nanoaerosols in a laboratory used to manufacture titanium dioxide (TiO2). The TiO2 nanopowders were produced via flame synthesis and collected by a bag filter system for subsequent harvesting. Highly concentrated nanopowders were released from the outlet of the bag filter system into the laboratory. The fractional particle collection efficiency of the bag filter system was only 20% at particle diameter of 100 nm, which is much lower than the performance of a high-efficiency particulate air (HEPA) filter. Furthermore, the laboratory hood system was inadequate to fully exhaust the air discharged from the bag filter system. Unbalanced air flow rates between bag filter and laboratory hood systems could result in high exposure to nanopowder in laboratory settings. Finally, we simulated behavior of nanopowders released in the laboratory using computational fluid dynamics (CFD). PMID:26125024

  1. Workplace Exposure to Titanium Dioxide Nanopowder Released from a Bag Filter System.

    PubMed

    Ji, Jun Ho; Kim, Jong Bum; Lee, Gwangjae; Noh, Jung-Hun; Yook, Se-Jin; Cho, So-Hye; Bae, Gwi-Nam

    2015-01-01

    Many researchers who use laboratory-scale synthesis systems to manufacture nanomaterials could be easily exposed to airborne nanomaterials during the research and development stage. This study used various real-time aerosol detectors to investigate the presence of nanoaerosols in a laboratory used to manufacture titanium dioxide (TiO2). The TiO2 nanopowders were produced via flame synthesis and collected by a bag filter system for subsequent harvesting. Highly concentrated nanopowders were released from the outlet of the bag filter system into the laboratory. The fractional particle collection efficiency of the bag filter system was only 20% at particle diameter of 100 nm, which is much lower than the performance of a high-efficiency particulate air (HEPA) filter. Furthermore, the laboratory hood system was inadequate to fully exhaust the air discharged from the bag filter system. Unbalanced air flow rates between bag filter and laboratory hood systems could result in high exposure to nanopowder in laboratory settings. Finally, we simulated behavior of nanopowders released in the laboratory using computational fluid dynamics (CFD). PMID:26125024

  2. Passivation of the surface of aluminum nanopowders by protective coatings of the different chemical origin

    NASA Astrophysics Data System (ADS)

    Kwon, Young-Soon; Gromov, Alexander A.; Strokova, Julia I.

    2007-04-01

    The results of investigation and analysis of electro-exploded aluminum nanopowders, whose surface were passivated with the following substances: liquids - nitrocellulose (NC), oleic acid (C 17H 33COOH) and stearic acid (C 17H 35COOH), suspended in kerosene and ethanol, fluoropolymer; solids - boron and nickel; gases - N 2, CO 2 and air (for a comparison) are discussed. The surface protection for the aluminum nanopowders by coatings of different chemical origins leads to the some advantages of the powders properties for an application in energetic systems, e.g. solid propellants and "green" propellants (Al-H 2O). Aluminum nanopowders with a protected surface showed the increased stability to oxidation in air during the storage period and higher reactivity by heating. The TEM-visual diagram of the formation and stabilization of the coatings on the particles has been proposed on the basis of experimental results. The kinetics of the interaction of aluminum nanopowders with air has been discussed. The recommendations concerning an efficiency of the protective "non-Al 2O 3" layers on aluminum nanoparticles were proposed.

  3. Liquid-feed flame spray pyrolysis synthesis of oxide nanopowders for the processing of ceramic composites

    NASA Astrophysics Data System (ADS)

    Taylor, Nathan John

    In the liquid-feed flame spray pyrolysis (LF-FSP) process, alcohol solutions of metalloorganic precursors are aerosolized by O2 and combusted. The metal oxide combustion products are rapidly quenched (< 10 ms) from flame temperatures of 1500°C to temperatures < 400° C, limiting particle growth. The resulting nanopowders are typically agglomerated but unaggregated. Here, we demonstrate two processing approaches to dense materials: nanopowders with the exact composition, and mixed single metal oxide nanopowders. The effect of the initial degree of phase separation on the final microstructures was determined by sintering studies. Our first studies included the production of yttrium aluminum garnet, Y3Al5O12 (YAG), tubes which we extruded from a thermoplastic/ceramic blend. At equivalent final densities, we found finer grain sizes in the from the mixed Y2O3 and Al2 O3 nanopowders, which was attributed to densification occurring before full transformation to the YAG phase. The enhanced densification in production of pure YAG from the reactive sintering process led us to produce composites in the YAG/alpha-Al 2O3 system. Finally, a third Y2O3 stabilized ZrO2 (YSZ) phase was added to further refine grain sizes using the same two processing approaches. In a separate study, single-phase metastable Al2O3 rich spinels with the composition MO•3Al 2O3 where M = Mg, Ni, and Co were sintered to produce dense MAl2O4/alpha-Al2O3 composites. All of these studies provide a test of the bottom-up approach; that is, how the initial length scale of mixing affects the final composite microstructure. Overall, the length scale of mixing is highly dependent upon the specific oxide composites studied. This work provides a processing framework to be adopted by other researchers to further refine microstructural size. LF-FSP flame temperatures were mapped using different alcohols with different heats of combustion: methanol, ethanol, 1-propanol, and n-butanol. The effect of different

  4. High elastic modulus nanopowder reinforced resin composites for dental applications

    NASA Astrophysics Data System (ADS)

    Wang, Yijun

    2007-12-01

    Dental restorations account for more than $3 billion dollars a year on the market. Among them, all-ceramic dental crowns draw more and more attention and their popularity has risen because of their superior aesthetics and biocompatibility. However, their relatively high failure rate and labor-intensive fabrication procedure still limit their application. In this thesis, a new family of high elastic modulus nanopowder reinforced resin composites and their mechanical properties are studied. Materials with higher elastic modulus, such as alumina and diamond, are used to replace the routine filler material, silica, in dental resin composites to achieve the desired properties. This class of composites is developed to serve (1) as a high stiffness support to all-ceramic crowns and (2) as a means of joining independently fabricated crown core and veneer layers. Most of the work focuses on nano-sized Al2O3 (average particle size 47 nm) reinforcement in a polymeric matrix with 50:50 Bisphenol A glycidyl methacrylate (Bis-GMA): triethylene glycol dimethacrylate (TEGDMA) monomers. Surfactants, silanizing agents and primers are examined to obtain higher filler levels and enhance the bonding between filler and matrix. Silane agents work best. The elastic modulus of a 57.5 vol% alumina/resin composite is 31.5 GPa compared to current commercial resin composites with elastic modulus <15 GPa. Chemical additives can also effectively raise the hardness to as much as 1.34 GPa. Besides>alumina, diamond/resin composites are studied. An elastic modulus of about 45 GPa is obtained for a 57 vol% diamond/resin composite. Our results indicate that with a generally monodispersed nano-sized high modulus filler, relatively high elastic modulus resin-based composite cements are possible. Time-dependent behavior of our resin composites is also investigated. This is valuable for understanding the behavior of our material and possible fatigue testing in the future. Our results indicate that with

  5. Characterisation of Suspension Precipitated Nanocrystalline Hydroxyapatite Powders

    NASA Astrophysics Data System (ADS)

    Mallik, P. K.; Swain, P. K.; Patnaik, S. C.

    2016-02-01

    Hydroxyapatite (HA) is a well-known biomaterial for coating on femoral implants, filling of dental cavity and scaffold for tissue replacement. Hydroxyapatite possess limited load bearing capacity due to their brittleness. In this paper, the synthesis of nanocrystalline hydroxyapatite powders was prepared by dissolving calcium oxide in phosphoric acid, followed by addition of ammonia liquor in a beaker. The prepared solution was stirred by using magnetic stirrer operated at temperature of 80°C for an hour. This leads to the formation of hydroxyapatite precipitate. The precipitate was dried in oven for overnight at 100°C. The dried agglomerated precipitate was calcined at 800°C in conventional furnace for an hour. The influence of calcium oxide concentration and pH on the resulting precipitates was studied using BET, XRD and SEM. As result, a well-defined sub-rounded morphology of powders size of ∼41 nm was obtained with a salt concentration of 0.02 M. Finally, it can be concluded that small changes in the reaction conditions led to large changes in final size, shape and degree of aggregation of the hydroxyapatite particles.

  6. Growth of hydroxyapatite nanoparticles on silica gels.

    PubMed

    Rivera-Muñoz, E M; Huirache-Acuña, R; Velázquez, R; Alonso-Núñez, G; Eguía-Eguía, S

    2011-06-01

    Synthetic, hydroxyapatite nanoparticles were grown on the surface of silica gels. The synthesis of those nanoparticles was obtained by immersing silica gels in a simulated body fluid (SBF) at 37 degrees C. The SBF was replaced every week to keep constant the Ca and P ion concentration and subsequent growth of hydroxyapatite was evaluated after 1-6 weeks of total soaking time in SBF. Hydroxyapatite nanoparticles were observed by scanning electron microscopy (SEM) on the surface of silica gel samples and confirmed by energy dispersive X-ray spectroscopy (EDS), Fourier Transform Infra Red Spectroscopy (FTIR) and powder X-ray Diffractometry (XRD) analysis. These particles show a regular shape and uniform size every week, keeping within the nanoscale always. Both the size and morphology of hydroxyapatite nanoparticles obtained are the result of the use of different chemical additives in the synthesis of silica gels, since they affect the liquid-to-solid interface, and the growth could correspond to a diffusion limited aggregation (DLA) process. A more detailed analysis, with higher magnifications, showed that hydroxyapatite nanoparticles are not solid spheres, showing a branched texture and their size depends on the scale and resolution of the measure instrument. PMID:21770224

  7. Bioactive Surface Modification of Hydroxyapatite

    PubMed Central

    Okazaki, Yohei; Hiasa, Kyou; Yasuda, Keisuke; Nogami, Keisuke; Mizumachi, Wataru; Hirata, Isao

    2013-01-01

    The purpose of this study was to establish an acid-etching procedure for altering the Ca/P ratio of the nanostructured surface of hydroxyapatite (HAP) by using surface chemical and morphological analyses (XPS, XRD, SEM, surface roughness, and wettability) and to evaluate the in vitro response of osteoblast-like cells (MC3T3-E1 cells) to the modified surfaces. This study utilized HAP and HAP treated with 10%, 20%, 30%, 40%, 50%, or 60% phosphoric acid solution for 10 minutes at 25°C, followed by rinsing 3 times with ultrapure water. The 30% phosphoric acid etching process that provided a Ca/P ratio of 1.50, without destruction of the grain boundary of HAP, was selected as a surface-modification procedure. Additionally, HAP treated by the 30% phosphoric acid etching process was stored under dry conditions at 25°C for 12 hours, and the Ca/P ratio approximated to 1.00 accidentally. The initial adhesion, proliferation, and differentiation (alkaline phosphatase (ALP) activity and relative mRNA level for ALP) of MC3T3-E1 cells on the modified surfaces were significantly promoted (P < 0.05 and 0.01). These findings show that the 30% phosphoric acid etching process for the nanostructured HAP surface can alter the Ca/P ratio effectively and may accelerate the initial adhesion, proliferation, and differentiation of MC3T3-E1 cells. PMID:23862150

  8. Monoclonal antibody purification with hydroxyapatite.

    PubMed

    Gagnon, Pete

    2009-06-01

    Hydroxyapatite (HA) has been used for IgG purification since its introduction in the 1950s. Applications expanded to include IgA and IgM in the 1980s, along with elucidation of its primary binding mechanisms and the development of ceramic HA media. With the advent of recombinant monoclonal antibodies, HA was demonstrated to be effective for removal of antibody aggregates, as well as host cell proteins and leached protein A. HA's inherent abilities have been enhanced by the development of elution strategies that permit differential control of its primary binding mechanisms: calcium metal affinity and phosphoryl cation exchange. These strategies support reduction of antibody aggregate content from greater than 60% to less than 0.1%, in conjunction with enhanced removal of DNA, endotoxin, and virus. HA also has a history of discriminating various immunological constructs on the basis of differences in their variable regions, or discriminating Fab fragments from Fc contaminants in papain digests of purified monoclonal IgG. Continuing development of novel elution strategies, alternative forms of HA, and application of robotic high throughput screening systems promise to expand HA's utility in the field. PMID:19491046

  9. Finite Element Simulation of Diametral Strength Test of Hydroxyapatite

    SciTech Connect

    Ozturk, Fahrettin; Toros, Serkan; Evis, Zafer

    2011-01-17

    In this study, the diametral strength test of sintered hydroxyapatite was simulated by the finite element software, ABAQUS/Standard. Stress distributions on diametral test sample were determined. The effect of sintering temperature on stress distribution of hydroxyapatite was studied. It was concluded that high sintering temperatures did not reduce the stress on hydroxyapatite. It had a negative effect on stress distribution of hydroxyapatite after 1300 deg. C. In addition to the porosity, other factors (sintering temperature, presence of phases and the degree of crystallinity) affect the diametral strength of the hydroxyapatite.

  10. Fe{sub 2}O{sub 3} nanopowders prepared by a thermal plasma process for water oxidation

    SciTech Connect

    Lee, Dongeun; Choi, Yong-Wook; Na, Ye-Seul; Choi, Soo-Suk; Park, Dong-Wha; Choi, Jinsub

    2015-08-15

    Highlights: • Hematite nanopowders with a high purity were synthesized by a DC thermal plasma process. • Fe{sub 3}O{sub 4} is formed during the formation of Fe{sub 2}O{sub 3} by thermal plasma with iron and oxygen sources. • Hematite nanopowders with a high purity show higher PEC performance compared to mixed oxides. - Abstract: Hematite (Fe{sub 2}O{sub 3}) nanopowders were synthesized from commercially available micro-sized iron powders by a DC thermal plasma process at atmospheric pressure. The micro-sized iron powders were vaporized in the plasma region, after which the plasma processing equipment was rapidly quenched, resulting in the formation of iron nanopowders with a size of less than 100 nm. Subsequently, the iron nanopowders were heated to convert hematite with a high purity, which was then formed into a thin film with a binder for preparation of electrodes for photoelectrochemical water oxidation. Iron oxide nanopowders were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), particle size analysis (PSA) and transmission electron microscopy (TEM). The photoelectrochemical properties of the Fe{sub 2}O{sub 3} film were characterized in 1 M NaOH under AM 1.5 conditions.

  11. Permeability, drying, and sintering of pressure filtered ceramic nanopowders

    NASA Astrophysics Data System (ADS)

    Sweeney, Sean M.

    2002-01-01

    point of drying (when fracture is most likely during drying). Agreement between maximum safe drying stresses and measured sample strengths is found to be good (to within better than a factor of 2) for boehmite samples, but not very good (off by a factor of ˜7) for nanocrystalline 3Y-TZP samples. Sub-critical crack growth is indicated as the source of this deviation in nanocrystalline 3Y-TZP samples. Literature studies of the sintering of chloride-derived 3Y-TZP nanopowders have documented numerous sintering problems including inability to reach full density, desintering, cracking, and the formation of a dense shell with less dense interior. To explain the poor sintering behavior of samples of one nanocrystalline 3Y-TZP powder, the origin of such a dense shell microstructure is determined. Three possible reasons for a dense shell microstructure are examined and rejected: exothermic reactions with the sintering atmosphere, pre-existing density gradients in the green compact, and thermal gradients occurring during sintering. A combination of gas flow/diffusion, thermodynamic, and sintering calculations are used to show that the evolution of a structure-coarsening gas (hydrogen chloride) during sintering causes the formation of a dense shell microstructure, and explains the poor densification behavior of this system. Two solutions to the problem are compared: (1) a thermal treatment composed of an extended hold at 1000°C to allow HCl gas removal before the onset of closed porosity (at about 90-93% of theoretical density), and (2) a chemical treatment performed by washing pre-sintered (500°C/30 min) samples at room temperature using a concentrated ammonium hydroxide solution to remove chlorides. The thermal treatment is found to be superior for removing residual chlorine and allowing full density to be achieved during sintering.

  12. Preparation of irregular mesoporous hydroxyapatite

    SciTech Connect

    Wang Hualin Zhai Linfeng; Li Yanhong; Shi Tiejun

    2008-06-03

    An irregular mesoporous hydroxyapatite (meso-HA), Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2}, is successfully prepared from Ca(NO{sub 3}){sub 2}.4H{sub 2}O and NH{sub 4}H{sub 2}PO{sub 4} using surfactant cetyltrimethyl ammonium bromide (CTAB) as template. Fourier transform infrared spectroscopy (FTIR) and differential scanning calorimetry (DSC) results reveal that the positive head of CTAB is assembled on the surface precipitated HA and much NH{sub 4}{sup +} is enclosed in precipitated HA before calcination. Field scanning electron microscope (FSEM) reveals that there exist many interconnected pores throughout the HA reticular skeleton. Nitrogen adsorption-desorption experiment exhibits a mesoporous material type IV curve, and pore size distribution calculated from the desorption branch of the isotherms based on Barrett-Joyner-Halenda (BJH) model shows that most pores throughout the HA reticular skeleton are sized at about 40 nm, but the pores are not uniform on the whole, owning to decomposition of the 'organic' CTAB templating structures and ammonium salt enclosed in the precipitated HA. The specific surface area of irregular meso-HA is calculated to be 37.6 m{sup 2}/g according to the Brunauer-Emmett-Teller (BET) equation. Moreover, after polylactic acid/meso-HA (PLA/meso-HA) composites degraded 12 weeks in normal saline at 37 deg. C, the interconnected pores throughout the HA skeleton were enlarged and sized in micron degree, which resemble trabecular bone structure very much.

  13. Highly biocompatible, nanocrystalline hydroxyapatite synthesized in a solvothermal process driven by high energy density microwave radiation.

    PubMed

    Smolen, Dariusz; Chudoba, Tadeusz; Malka, Iwona; Kedzierska, Aleksandra; Lojkowski, Witold; Swieszkowski, Wojciech; Kurzydlowski, Krzysztof Jan; Kolodziejczyk-Mierzynska, Małgorzata; Lewandowska-Szumiel, Małgorzata

    2013-01-01

    A microwave, solvothermal synthesis of highly biocompatible hydroxyapatite (HAp) nanopowder was developed. The process was conducted in a microwave radiation field having a high energy density of 5 W/mL and over a time less than 2 minutes. The sample measurements included: powder X-ray diffraction, density, specific surface area, and chemical composition. The morphology and structure were investigated by scanning electron microscopy as well as transmission electron microscopy (TEM). The thermal behavior analysis was conducted using a simultaneous thermal analysis technique coupled with quadruple mass spectrometry. Additionally, Fourier transform infrared spectroscopy tests of heated samples were performed. A degradation test and a biocompatibility study in vitro using human osteoblast cells were also conducted. The developed method enables the synthesis of pure, fully crystalline hexagonal HAp nanopowder with a specific surface area close to 240 m(2)/g and a Ca/P molar ratio equal to 1.57. TEM measurements showed that this method results in particles with an average grain size below 6 nm. A 28-day degradation test conducted according to the ISO standard indicated a 22% loss of initial weight and a calcium ion concentration at 200 μmol/dm(3) in the tris(hydroxymethyl)aminomethane hydrochloride test solution. The cytocompatibility of the obtained material was confirmed in a culture of human bone derived cells, both in an indirect test using the material extract, and in direct contact. A quantitative analysis was based on the 2,3-bis-(2-methoxy-4-nitro-5-sulfophenyl)-2H-tetrazolium-5-carboxanilide. Viability assay as well as on DNA content measurements in the PicoGreen test. Indirect observations were performed at one point in time according to the ISO standard for in vitro cytotoxicity (ie, after 24 hours of cell exposure to the extracts). The direct contact tests were completed at three time points: after 24 hours, on day 7, and on day 14 of a culture in an

  14. Highly biocompatible, nanocrystalline hydroxyapatite synthesized in a solvothermal process driven by high energy density microwave radiation

    PubMed Central

    Smolen, Dariusz; Chudoba, Tadeusz; Malka, Iwona; Kedzierska, Aleksandra; Lojkowski, Witold; Swieszkowski, Wojciech; Kurzydlowski, Krzysztof Jan; Kolodziejczyk-Mierzynska, Małgorzata; Lewandowska-Szumiel, Małgorzata

    2013-01-01

    A microwave, solvothermal synthesis of highly biocompatible hydroxyapatite (HAp) nanopowder was developed. The process was conducted in a microwave radiation field having a high energy density of 5 W/mL and over a time less than 2 minutes. The sample measurements included: powder X-ray diffraction, density, specific surface area, and chemical composition. The morphology and structure were investigated by scanning electron microscopy as well as transmission electron microscopy (TEM). The thermal behavior analysis was conducted using a simultaneous thermal analysis technique coupled with quadruple mass spectrometry. Additionally, Fourier transform infrared spectroscopy tests of heated samples were performed. A degradation test and a biocompatibility study in vitro using human osteoblast cells were also conducted. The developed method enables the synthesis of pure, fully crystalline hexagonal HAp nanopowder with a specific surface area close to 240 m2/g and a Ca/P molar ratio equal to 1.57. TEM measurements showed that this method results in particles with an average grain size below 6 nm. A 28-day degradation test conducted according to the ISO standard indicated a 22% loss of initial weight and a calcium ion concentration at 200 μmol/dm3 in the tris(hydroxymethyl)aminomethane hydrochloride test solution. The cytocompatibility of the obtained material was confirmed in a culture of human bone derived cells, both in an indirect test using the material extract, and in direct contact. A quantitative analysis was based on the 2,3-bis-(2-methoxy-4-nitro-5-sulfophenyl)-2H-tetrazolium-5-carboxanilide. Viability assay as well as on DNA content measurements in the PicoGreen test. Indirect observations were performed at one point in time according to the ISO standard for in vitro cytotoxicity (ie, after 24 hours of cell exposure to the extracts). The direct contact tests were completed at three time points: after 24 hours, on day 7, and on day 14 of a culture in an osteogenic

  15. Thickness of hydroxyapatite nanocrystal controls mechanical properties of the collagen-hydroxyapatite interface.

    PubMed

    Qin, Zhao; Gautieri, Alfonso; Nair, Arun K; Inbar, Hadass; Buehler, Markus J

    2012-01-31

    Collagen-hydroxyapatite interfaces compose an important building block of bone structures. While it is known that the nanoscale structure of this elementary building block can affect the mechanical properties of bone, a systematic understanding of the effect of the geometry on the mechanical properties of this interface between protein and mineral is lacking. Here we study the effect of geometry, different crystal surfaces, and hydration on the mechanical properties of collagen-hydroxyapatite interfaces from an atomistic perspective, and discuss underlying deformation mechanisms. We find that the presence of hydroxyapatite significantly enhances the tensile modulus and strength compared with a tropocollagen molecule alone. The stiffening effect is strongly dependent on the thickness of the mineral crystal until a plateau is reached at 2 nm crystal thickness. We observe no significant differences due to the mineral surface (Ca surface vs OH surface) or due to the presence of water. Our result shows that the hydroxyapatite crystal with its thickness confined to the nanometer size efficiently increases the tensile modulus and strength of the collagen-hydroxyapatite composite, agreeing well with experimental observations that consistently show the existence of extremely thin mineral flakes in various types of bones. We also show that the collagen-hydroxyapatite interface can be modeled with an elastic network model which, based on the results of atomistic simulations, provides a good estimate of the surface energy and other mechanical features. PMID:22208454

  16. Thermal and Mechanical Characteristics of Polymer Composites Based on Epoxy Resin, Aluminium Nanopowders and Boric Acid

    NASA Astrophysics Data System (ADS)

    Nazarenko, O. B.; Melnikova, T. V.; Visakh, P. M.

    2016-01-01

    The epoxy polymers are characterized by low thermal stability and high flammability. Nanoparticles are considered to be effective fillers of polymer composites for improving their thermal and functional properties. In this work, the epoxy composites were prepared using epoxy resin ED-20, polyethylene polyamine as a hardener, aluminum nanopowder and boric acid fine powder as flame-retardant filler. The thermal characteristics of the obtained samples were studied using thermogravimetric analysis and differential scanning calorimetry. The mechanical characteristics of epoxy composites were also studied. It was found that an addition of all fillers enhances the thermal stability and mechanical characteristics of the epoxy composites. The best thermal stability showed the epoxy composite filled with boric acid. The highest flexural properties showed the epoxy composite based on the combination of boric acid and aluminum nanopowder.

  17. Technology for production of magnetic carbon nanopowders doped with iron and cobalt nanoclusters

    NASA Astrophysics Data System (ADS)

    Gegechkori, T.; Mamniashvili, G.; Kutelia, E.; Rukhadze, L.; Maisuradze, N.; Eristavi, B.; Gventsadze, D.; Akhalkatsi, A.; Gavasheli, T.; Daraselia, D.; Japaridze, D.; Shengelaya, A.

    2015-01-01

    Complex scanning electron microscope and Auger electron spectroscope structure and composition measurements, along with the vibrating sample magnetometer and NMR studies, were carried out on carbon nanoparticles doped with magnetic clusters, which were synthesized by a technology which combines the ethanol vapor pyrolysis method and the chemical vapor deposition process in a horizontal continuous reactor with certain temperature gradients and controlled partial oxygen pressure. The structure and composition data of the synthesized magnetic carbon nanopowders showed that the nanopowders consisted of randomly distributed carbon nanoparticle aggregations that are 200 nm in diameter doped with magnetic clusters. The magnetometry and NMR data are in agreement with the results of the structure analysis, pointing to the existence of a significant superparamagnetic contribution to the synthesized carbon nanoparticles doped with cobalt nanoclusters.

  18. Structural and Optical Characterization of Synthesized TiO2 Nanopowder Using Sol-Gel Technique

    NASA Astrophysics Data System (ADS)

    Lourduraj, S.; Williams, R. Victor

    2016-02-01

    The nanocrystalline TiO2 powder was synthesized by sol-gel method. The XRD analysis reveals that TiO2 powder was highly crystalline (anatase phase) and nanostructured with tetragonal system. The average crystallite size after calcined at 673K is found to be 7.7nm. The surface morphological studies using scanning electron microscopy (SEM) exhibit that the formation of nanosized TiO2 particles with less densification nature. Atomic force microscopy (AFM) topography exhibits the uniform distribution of spherical-shaped particles. The energy dispersive X-ray spectroscopy (EDX) confirms the presence of Titanium and Oxygen in synthesized TiO2 nanopowder. The value of optical bandgap of TiO2 nanopowder calculated from UV-Visible spectrum is 3.45eV. The presence of TiO2 particles is confirmed from the dominant fourier transform infrared (FTIR) peaks at 621cm-1 and 412cm-1.

  19. Synthesis of the thermoelectric nanopowder recovered from the used thermoelectric modules.

    PubMed

    Lee, Kun-Jae; Jin, Yun-Ho; Kong, Man-Sik

    2014-10-01

    We fabricated the thermoelectric powder using the used thermoelectric modules in a vehicle. As a starting material, the used thermoelectric modules were collected and separated to substrate, electrode, solder, and thermoelectric parts by a thermal process. The separation process was performed in a wet process at the critical temperature. The solder in the module was the neighbor part of the thermoelectric material with the lowest melting temperature in the module. We focused on the thermal property of the solder to separate the thermoelectric chips in the module. After the separation process, we prepared the pure thermoelectric material by the chemical etching for an impurity removal. Also the thermoelectric nanopowder was fabricated by a chemical reduction reaction using the recycled thermoelectric materials. The recovered nanopowder was confirmed to the phase of bismuth telluride (Bi2Te3) with the particle size of -15 nm. PMID:25942894

  20. Fast microstructure and phase analyses of nanopowders using combined analysis of transmission electron microscopy scattering patterns.

    PubMed

    Boullay, P; Lutterotti, L; Chateigner, D; Sicard, L

    2014-09-01

    The full quantitative characterization of nanopowders using transmission electron microscopy scattering patterns is shown. This study demonstrates the feasibility of the application of so-called combined analysis, a global approach for phase identification, structure refinement, characterization of anisotropic crystallite sizes and shapes, texture analysis and texture variations with the probed scale, using electron diffraction patterns of TiO2 and Mn3O4 nanocrystal aggregates and platinum films. Electron diffraction pattern misalignments, positioning, and slight changes from pattern to pattern are directly integrated and refined within this approach. The use of a newly developed full-pattern search-match methodology for phase identification of nanopowders and the incorporation of the two-wave dynamical correction for diffraction patterns are also reported and proved to be efficient. PMID:25176993

  1. Production of nickel and iron nanopowders by hydrogen reduction from salts

    NASA Astrophysics Data System (ADS)

    Oglezneva, S. A.; Bulanov, V. Ya.; Kontsevoi, Yu. V.; Ignat'ev, I. E.

    2012-07-01

    The formation of nickel and iron nanoparticles produced by a chemical—metallurgical method and steels made of composite iron powders with nanosized nickel additions is studied. A procedure is developed for calculating the nanopowder particle size and the activation energy of sintering. The results obtained make it possible to decrease the temperature of the process of powder production, to decrease the energy consumed for powder sintering, and to predict the powder nanoparticle size.

  2. Irradiation creep of nano-powder sintered silicon carbide at low neutron fluences

    SciTech Connect

    Koyanagi, Takaaki; Shimoda, Kazuya; Kondo, Sosuke; Hinoki, Tatsuya; Ozawa, Kazumi; Katoh, Yutai

    2014-12-01

    The irradiation creep behavior of nano-powder sintered silicon carbide was investigated using the bend stress relaxation method under neutron irradiation up to 1.9 dpa. The creep deformation was observed at all temperatures ranging from 380 to 1180 °C mainly from the irradiation creep but with the increasing contributions from the thermal creep at higher temperatures. Microstructural observation and data analysis were performed.

  3. [Adsorption of Congo red from aqueous solution on hydroxyapatite].

    PubMed

    Zhan, Yan-Hui; Lin, Jian-Wei

    2013-08-01

    The adsorption of Congo red (CR) from aqueous solution on hydroxyapatite was investigated using batch experiments. The hydroxyapatite was effective for CR removal from aqueous solution. The adsorption kinetics of CR on hydroxyapatite well followed a pseudo-second-order model. The equilibrium adsorption data of CR on hydroxyapatite could be described by the Langmuir, Freundlich and Dubinin-Radushkevich (D-R) isotherm models. Thermodynamic parameters such as Gibbs free energy change, enthalpy change and entropy change were calculated and showed that the adsorption of CR on hydroxyapatite was spontaneous and exothermic in nature. The CR adsorption capacity for hydroxyapatite decreased significantly with increasing pH from 8 to 10. Thermal regeneration showed that hydroxyapatite could be used for six desorption-adsorption cycles with high removal efficiency for CR in each cycle. The mechanisms for CR adsorption on hydroxyapatite with pH value below the pH at point of zero charge (pH(PZC)) include electrostatic attraction, hydrogen bonding and Lewis acid-base interaction. The mechanisms for CR adsorption on hydroxyapatite with pH value above its pH(PZC) include hydrogen bonding and Lewis acid-base interaction. Results of this work indicate that hydroxyapatite is a promising adsorbent for CR removal from aqueous solution. PMID:24191561

  4. Ultrasonic deagglomeration of aluminum nanopowders with multi-walled carbon nanotube mixtures

    SciTech Connect

    Kozulin, Alexander A. Vorozhtsov, Sergey A. Kulkov, Sergey S.; Kulkov, Sergey N.; Teipel, U.

    2015-10-27

    Comprehensive investigations of aluminum nanopowders, multi-walled carbon nanotubes, and aluminum mixtures with multi-walled carbon nanotubes subjected to ultrasonic deagglomeration in a liquid medium were performed, using microstructural, X-ray diffraction, thermogravimetric, and calorimetric analyses, and specific surface area measurements. The regime of ultrasonic deagglomeration of aluminum nanopowders with multi-walled carbon nanotubes in a liquid medium is described, during which the division of large agglomerates and creation of homogeneous distribution of mixtures components in the volume takes place. It was determined that ultrasonic treatment influences the morphology and crystalline structure of investigated mixtures, contributes to the appearance of X-ray amorphous phase, decreases the specific surface area of the aluminum nanopowder from 13 to 12 m{sup 2}/g, and increases the pore volume and average size from 0.04 to 0.06 cm{sup 3}/g and from 12 to 19 nm, respectively. The size of coherently-diffracting domain was determined by the X-ray diffraction analysis is close to that estimated from the specific surface area and corresponds to average crystallites size in the materials under study.

  5. Ultrasonic deagglomeration of aluminum nanopowders with multi-walled carbon nanotube mixtures

    NASA Astrophysics Data System (ADS)

    Kozulin, Alexander A.; Vorozhtsov, Sergey A.; Kulkov, Sergey S.; Teipel, U.; Kulkov, Sergey N.

    2015-10-01

    Comprehensive investigations of aluminum nanopowders, multi-walled carbon nanotubes, and aluminum mixtures with multi-walled carbon nanotubes subjected to ultrasonic deagglomeration in a liquid medium were performed, using microstructural, X-ray diffraction, thermogravimetric, and calorimetric analyses, and specific surface area measurements. The regime of ultrasonic deagglomeration of aluminum nanopowders with multi-walled carbon nanotubes in a liquid medium is described, during which the division of large agglomerates and creation of homogeneous distribution of mixtures components in the volume takes place. It was determined that ultrasonic treatment influences the morphology and crystalline structure of investigated mixtures, contributes to the appearance of X-ray amorphous phase, decreases the specific surface area of the aluminum nanopowder from 13 to 12 m2/g, and increases the pore volume and average size from 0.04 to 0.06 cm3/g and from 12 to 19 nm, respectively. The size of coherently-diffracting domain was determined by the X-ray diffraction analysis is close to that estimated from the specific surface area and corresponds to average crystallites size in the materials under study.

  6. Photoluminescent BaMoO{sub 4} nanopowders prepared by complex polymerization method (CPM)

    SciTech Connect

    Azevedo Marques, Ana Paula de . E-mail: apamarques@liec.ufscar.br; Melo, Dulce M.A. de; Paskocimas, Carlos A.; Pizani, Paulo S.; Joya, Miryam R.; Leite, Edson R.; Longo, Elson

    2006-03-15

    The BaMoO{sub 4} nanopowders were prepared by the Complex Polymerization Method (CPM). The structure properties of the BaMoO{sub 4} powders were characterized by FTIR transmittance spectra, X-ray diffraction (XRD), Raman spectra, photoluminescence spectra (PL) and high-resolution scanning electron microscopy (HR-SEM). The XRD, FTIR and Raman data showed that BaMoO{sub 4} at 300 deg. C was disordered. At 400 deg. C and higher temperature, BaMoO{sub 4} crystalline scheelite-type phases could be identified, without the presence of additional phases, according to the XRD, FTIR and Raman data. The calculated average crystallite sizes, calculated by XRD, around 40 nm, showed the tendency to increase with the temperature. The crystallite sizes, obtained by HR-SEM, were around of 40-50 nm. The sample that presented the highest intensity of the red emission band was the one heat treated at 400 deg. C for 2 h, and the sample that displayed the highest intensity of the green emission band was the one heat treated at 700 deg. C for 2 h. The CPM was shown to be a low cost route for the production of BaMoO{sub 4} nanopowders, with the advantages of lower temperature, smaller time and reduced cost. The optical properties observed for BaMoO{sub 4} nanopowders suggested that this material is a highly promising candidate for photoluminescent applications.

  7. Impact of isoelectric points of nanopowders in electrolytes on electrochemical characteristics of dye sensitized solar cells

    NASA Astrophysics Data System (ADS)

    Mohanty, Shyama Prasad; Bhargava, Parag

    2012-11-01

    Nanoparticle loaded quasi solid electrolytes are important from the view point of developing electrolytes for dye sensitized solar cells (DSSCs) having long term stability. The present work shows the influence of isoelectric point of nanopowders in electrolyte on the photoelectrochemical characteristics of DSSCs. Electrolytes with nanopowders of silica, alumina and magnesia which have widely differing isoelectric points are used in the study. Adsorption of ions from the electrolyte on the nanopowder surface, characterized by zeta potential measurement, show that cations get adsorbed on silica, alumina surface while anions get adsorbed on magnesia surface. The electrochemical characteristics of nanoparticulate loaded electrolytes are examined through cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). DSSCs fabricated using liquid, silica or alumina loaded electrolytes exhibit almost similar performance. But interestingly, the magnesia loaded electrolyte-based cell show lower short circuit current density (JSC) and much higher open circuit voltage (VOC), which is attributed to adsorption of anions. Such anionic adsorption prevents the dark reaction in magnesia loaded electrolyte-based cell and thus, enhances the VOC by almost 100 mV as compared to liquid electrolyte based cell. Also, higher electron life time at the titania/electrolyte interface is observed in magnesia loaded electrolyte-based cell as compared to others.

  8. Nutrient-substituted hydroxyapatites: synthesis and characterization

    NASA Technical Reports Server (NTRS)

    Golden, D. C.; Ming, D. W.

    1999-01-01

    Incorporation of Mg, S, and plant-essential micronutrients into the structure of synthetic hydroxyapatite (HA) may be advantageous for closed-loop systems, such as will be required on Lunar and Martian outposts, because these apatites can be used as slow-release fertilizers. Our objective was to synthesize HA with Ca, P, Mg, S, Fe, Cu, Mn, Zn, Mo, B, and Cl incorporated into the structure, i.e., nutrient-substituted apatites. Hydroxyapatite, carbonate hydroxyapatite (CHA), nutrient-substituted hydroxyapatite (NHA), and nutrient-substituted carbonate hydroxyapatite (NCHA) were synthesized by precipitating from solution. Chemical and mineralogical analysis of precipitated samples indicated a considerable fraction of the added cations were incorporated into HA, without mineral impurities. Particle size of the HA was in the 1 to 40 nm range, and decreased with increased substitution of nutrient elements. The particle shape of HA was elongated in the c-direction in unsubstituted HA and NHA but more spherical in CHA and NCHA. The substitution of cations and anions in the HA structure was confirmed by the decrease of the d[002] spacing of HA with substitution of ions with an ionic radius less than that of Ca or P. The DTPA-extractable Cu ranged from 8 to 8429 mg kg-1, Zn ranged from 57 to 1279 mg kg-1, Fe from 211 to 2573 mg kg-1, and Mn from 190 to 1719 mg kg-1, depending on the substitution level of each element in HA. Nutrient-substituted HA has the potential to be used as a slow-release fertilizer to supply micronutrients, S, and Mg in addition to Ca and P.

  9. Ferroelectric polarization in nanocrystalline hydroxyapatite thin films on silicon.

    PubMed

    Lang, S B; Tofail, S A M; Kholkin, A L; Wojtaś, M; Gregor, M; Gandhi, A A; Wang, Y; Bauer, S; Krause, M; Plecenik, A

    2013-01-01

    Hydroxyapatite nanocrystals in natural form are a major component of bone--a known piezoelectric material. Synthetic hydroxyapatite is widely used in bone grafts and prosthetic pyroelectric coatings as it binds strongly with natural bone. Nanocrystalline synthetic hydroxyapatite films have recently been found to exhibit strong piezoelectricity and pyroelectricity. While a spontaneous polarization in hydroxyapatite has been predicted since 2005, the reversibility of this polarization (i.e. ferroelectricity) requires experimental evidence. Here we use piezoresponse force microscopy to demonstrate that nanocrystalline hydroxyapatite indeed exhibits ferroelectricity: a reversal of polarization under an electrical field. This finding will strengthen investigations on the role of electrical polarization in biomineralization and bone-density related diseases. As hydroxyapatite is one of the most common biocompatible materials, our findings will also stimulate systematic exploration of lead and rare-metal free ferroelectric devices for potential applications in areas as diverse as in vivo and ex vivo energy harvesting, biosensing and electronics. PMID:23884324

  10. Synthesis of Si, Mg substituted hydroxyapatites and their sintering behaviors.

    PubMed

    Kim, S R; Lee, J H; Kim, Y T; Riu, D H; Jung, S J; Lee, Y J; Chung, S C; Kim, Y H

    2003-04-01

    Si, Mg-substituted hydroxyapatites, alone and co-substituted, have been prepared to obtain biomaterials having an improved biocompatibility. From FT-IR, XRD and ICP analyses, it was confirmed that single phases of hydroxyapatite substituted by Si alone or co-substituted by Si, Mg. The XRD data indicated the absence of extra phases related to silicon and magnesium oxide or other calcium phosphate species. Si-substituted hydroxyapatite of up to 2 wt% for Si and Si, Mg co-substituted hydroxyapatite of 1 wt% for the each ion keep their original structures intact for the sintering temperatures of up to 1200 degrees C. However, it is observed that ion substitutions by an amount higher than the above ratios for each hydroxyapatite lead to destabilization of original structures of the hydroxyapatite and to the production of tricalcium phosphate and calcium phosphate silicate phases when the samples were sintered at 1100 degrees C or higher. PMID:12527280

  11. Ferroelectric Polarization in Nanocrystalline Hydroxyapatite Thin Films on Silicon

    NASA Astrophysics Data System (ADS)

    Lang, S. B.; Tofail, S. A. M.; Kholkin, A. L.; Wojtaś, M.; Gregor, M.; Gandhi, A. A.; Wang, Y.; Bauer, S.; Krause, M.; Plecenik, A.

    2013-07-01

    Hydroxyapatite nanocrystals in natural form are a major component of bone- a known piezoelectric material. Synthetic hydroxyapatite is widely used in bone grafts and prosthetic pyroelectric coatings as it binds strongly with natural bone. Nanocrystalline synthetic hydroxyapatite films have recently been found to exhibit strong piezoelectricity and pyroelectricity. While a spontaneous polarization in hydroxyapatite has been predicted since 2005, the reversibility of this polarization (i.e. ferroelectricity) requires experimental evidence. Here we use piezoresponse force microscopy to demonstrate that nanocrystalline hydroxyapatite indeed exhibits ferroelectricity: a reversal of polarization under an electrical field. This finding will strengthen investigations on the role of electrical polarization in biomineralization and bone-density related diseases. As hydroxyapatite is one of the most common biocompatible materials, our findings will also stimulate systematic exploration of lead and rare-metal free ferroelectric devices for potential applications in areas as diverse as in vivo and ex vivo energy harvesting, biosensing and electronics.

  12. Ferroelectric Polarization in Nanocrystalline Hydroxyapatite Thin Films on Silicon

    PubMed Central

    Lang, S. B.; Tofail, S. A. M.; Kholkin, A. L.; Wojtaś, M.; Gregor, M.; Gandhi, A. A.; Wang, Y.; Bauer, S.; Krause, M.; Plecenik, A.

    2013-01-01

    Hydroxyapatite nanocrystals in natural form are a major component of bone- a known piezoelectric material. Synthetic hydroxyapatite is widely used in bone grafts and prosthetic pyroelectric coatings as it binds strongly with natural bone. Nanocrystalline synthetic hydroxyapatite films have recently been found to exhibit strong piezoelectricity and pyroelectricity. While a spontaneous polarization in hydroxyapatite has been predicted since 2005, the reversibility of this polarization (i.e. ferroelectricity) requires experimental evidence. Here we use piezoresponse force microscopy to demonstrate that nanocrystalline hydroxyapatite indeed exhibits ferroelectricity: a reversal of polarization under an electrical field. This finding will strengthen investigations on the role of electrical polarization in biomineralization and bone-density related diseases. As hydroxyapatite is one of the most common biocompatible materials, our findings will also stimulate systematic exploration of lead and rare-metal free ferroelectric devices for potential applications in areas as diverse as in vivo and ex vivo energy harvesting, biosensing and electronics. PMID:23884324

  13. Simple route for nano-hydroxyapatite properties expansion.

    PubMed

    Rojas, L; Olmedo, H; García-Piñeres, A J; Silveira, C; Tasic, L; Fraga, F; Montero, M L

    2015-09-01

    Simple surface modification of nano-hydroxyapatite, through acid-basic reactions, allows expanding the properties of this material. Introduction of organic groups such as hydrophobic alkyl chains, carboxylic acid, and amide or amine basic groups on the hydroxyapatite surface systematically change the polarity, surface area, and reactivity of hydroxyapatite without modifying its phase. Physical and chemical properties of the new derivative particles were analyzed. The biocompatibility of modified Nano-Hap on Raw 264.7 cells was also assessed. PMID:26481455

  14. Porous hydroxyapatite and gelatin/hydroxyapatite microspheres obtained by calcium phosphate cement emulsion.

    PubMed

    Perez, Roman A; Del Valle, Sergio; Altankov, George; Ginebra, Maria-Pau

    2011-04-01

    Hydroxyapatite and hybrid gelatine/hydroxyapatite microspheres were obtained through a water in oil emulsion of a calcium phosphate cement (CPC). The setting reaction of the CPC, in this case the hydrolysis of α-tricalcium phosphate, was responsible for the consolidation of the microspheres. After the setting reaction, the microspheres consisted of an entangled network of hydroxyapatite crystals, with a high porosity and pore sizes ranging between 0.5 and 5 μm. The size of the microspheres was tailored by controlling the viscosity of the hydrophobic phase, the rotation speed, and the initial powder size of the CPC. The incorporation of gelatin increased the sphericity of the microspheres, as well as their size and size dispersion. To assess the feasibility of using the microspheres as cell microcarriers, Saos-2 cells were cultured on the microspheres. Fluorescent staining, SEM studies, and LDH quantification showed that the microspheres were able to sustain cell growth. Cell adhesion and proliferation was significantly improved in the hybrid gelatin/hydroxyapatite microspheres as compared to the hydroxyapatite ones. PMID:21290594

  15. Mechanical properties and biocompatibility of the sputtered Ti doped hydroxyapatite.

    PubMed

    Vladescu, A; Padmanabhan, S C; Ak Azem, F; Braic, M; Titorencu, I; Birlik, I; Morris, M A; Braic, V

    2016-10-01

    The hydroxyapatite enriched with Ti were prepared as possible candidates for biomedical applications especially for implantable devices that are in direct contact to the bone. The hydroxyapatites with different Ti content were prepared by RF magnetron sputtering on Ti-6Al-4V alloy using pure hydroxyapatite and TiO2 targets. The content of Ti was modified by changing the RF power fed on TiO2 target. The XPS and FTIR analyses revealed the presence of hydroxyapatite structure. The hardness and elastic modulus of the hydroxyapatite were increased by Ti addition. After 5 days of culture, the cell viability of the Ti-6Al-4V was enhanced by depositing with undoped or doped hydroxyapatite. The Ti additions led to an increase in cell viability of hydroxyapatite, after 5 days of culture. The electron microscopy showed the presence of more cells on the surface of Ti-enriched hydroxyapatite than those observed on the surface of the uncoated alloys or undoped hydroxyapatite. PMID:27450034

  16. Morphology and electronic structure of nanoscale powders of calcium hydroxyapatite

    NASA Astrophysics Data System (ADS)

    Kurgan, Nataly; Karbivskyy, Volodymyr; Kasyanenko, Vasyl

    2015-02-01

    Atomic force microscopy, infrared spectroscopy and NMR studied morphological and physicochemical properties of calcium hydroxyapatite powders produced by changing the temperature parameters of synthesis. Features of morphology formation of calcium hydroxyapatite nanoparticles with an annealing temperature within 200°C to 1,100°C were determined. It is shown that the particle size of the apatite obtained that annealed 700°C is 40 nm corresponding to the particle size of apatite in native bone. The effect of dimension factor on structural parameters of calcium hydroxyapatite is manifested in a more local symmetry of the PO4 3- tetrahedra at nanodispersed calcium hydroxyapatite.

  17. Fabrication of alpha-Fe2O3 nanopowder modified glassy carbon electrode for applications in electrochemical sensing.

    PubMed

    Goyal, Rajendra N; Pandey, Ashish K; Kaur, Davinder; Kumar, Ashvani

    2009-08-01

    In the present study, Fe2O3 nanopowder has been grown by Ultrasonic mist chemical vapor deposition (UM-CVD), which is a promising method for large area deposition at low temperatures taking in to account of its simplicity, inexpensiveness and safety. Room temperature XRD results revealed prominent hematite phase with intense (104) reflection and was also in agreement with the HR-TEM results. In situ high temperature X-ray diffraction (XRD) studies clearly indicated the change of phase from hematite to magnetite as the temperature increases above 300 degrees C. The surface morphology and particle size distribution of Fe2O3 nanopowder were characterized using field emission scanning electron microscope (FE-SEM) and high resolution transmission electron microscope (HR-TEM), which revealed that the particles were spherical in nature and distributed in range of 50-100 nm. SQUID magnetometry results indicate the ferromagnetic nature of the nanopowder with crystallite size of 6 nm as calculated from M-H curve. Transmittance of approximately 55% and estimated direct band gap of 2.5 eV was observed. Further, the nanopowder was used to modify glassy carbon electrode (GCE) and the modified electrode was found to exhibit electrocatalytic activity for the oxidation of dopamine. It is expected that the nanopowder will exhibit promising applications in the development of sensors. PMID:19928136

  18. Synthesis of hollow cobalt oxide nanopowders by a salt-assisted spray pyrolysis process applying nanoscale Kirkendall diffusion and their electrochemical properties.

    PubMed

    Ju, Hyeon Seok; Cho, Jung Sang; Kim, Jong Hwa; Choi, Yun Ju; Kang, Yun Chan

    2015-12-21

    A new concept for preparing hollow metal oxide nanopowders by salt-assisted spray pyrolysis applying nanoscale Kirkendall diffusion is introduced. The composite powders of metal oxide and indecomposable metal salt are prepared by spray pyrolysis. Post-treatment under a reducing atmosphere and subsequent washing using distilled water produce aggregation-free metal nanopowders. The metal nanopowders are then transformed into metal oxide hollow nanopowders by nanoscale Kirkendall diffusion. Co3O4 hollow nanopowders are prepared as first target materials. A cobalt oxide-NaCl composite powder prepared by spray pyrolysis transforms into several Co3O4 hollow nanopowders by several treatment processes. The discharge capacities of the Co3O4 nanopowders with filled and hollow structures at a current density of 1 A g(-1) for the 150th cycle are 605 and 775 mA h g(-1), respectively. The hollow structure formed by nanoscale Kirkendall diffusion improves the lithium-ion storage properties of Co3O4 nanopowders. PMID:26571144

  19. Reactive hydroxyapatite fillers for pectin biocomposites.

    PubMed

    Munarin, Fabiola; Petrini, Paola; Barcellona, Giulia; Roversi, Tommaso; Piazza, Laura; Visai, Livia; Tanzi, Maria Cristina

    2014-12-01

    In this work, a novel injectable biocomposite hydrogel is produced by internal gelation, using pectin as organic matrix and hydroxyapatite either as crosslinking agent and inorganic reinforcement. Tunable gelling kinetics and rheological properties are obtained varying the hydrogels' composition, with the final aim of developing systems for cell immobilization. The reversibility by dissolution of pectin-hydroxyapatite hydrogels is achieved with saline solutions, to possibly accelerate the release of the cells or active agents immobilized. Texture analysis confirms the possibility of extruding the biocomposites from needles with diameters from 20 G to 30 G, indicating that they can be implanted with minimally-invasive approaches, minimizing the pain during injection and the side effects of the open surgery. L929 fibroblasts entrapped in the hydrogels survive to the immobilization procedure and exhibit high cell viability. On the overall, these systems result to be suitable supports for the immobilization of cells for tissue regeneration applications. PMID:25491814

  20. Biomineralization of nanoscale single crystal hydroxyapatite.

    PubMed

    Omokanwaye, Tiffany; Wilson, Otto C; Gugssa, Ayelle; Anderson, Winston

    2015-11-01

    The chemical and physical characteristics of nanocrystalline hydroxyapatite particles which formed during the subcutaneous implantation of crab shell in Sprague-Dawley rats were studied using selected area electron diffraction (SAED) and high resolution transmission electron microscopy (HRTEM). The initial SAED characterization evidence indicated the presence of an amorphous calcium phosphate phase. The electron dense nanophase particles which formed in the wound healing zone displayed broad diffuse rings which usually indicate a low crystalline order or amorphous phase. High resolution transmission electron microscopy (HRTEM) revealed that these mineralized regions contained discrete single crystal particles less than 5nm in size. Micrographs taken at successively higher magnifications revealed very small nanoparticles with a hexagonal arrangement of ion channels with characteristic spacing of 0.54nm and 0.23nm. This study revealed that single crystal hydroxyapatite nanoparticles consisting of only a few unit cells formed via a biomineralization directed process. PMID:26249568

  1. Mechanical properties of hydroxyapatite/mica composite.

    PubMed

    Nordström, E G; Herø, H; Jørgensen, R B

    1994-01-01

    Bend specimens of the inorganic synthetic materials hydroxyapatite (HA) and a composite of hydroxyapatite/muscovite mica have been prepared and tested mechanically. Sintering followed by hot isostatic pressing (HIP) without encapsulation gave an increased strength for HA alone, but no significant increase in strength compared with sintering alone for HA/mica composites. The bend strength of the HA/mica composite was inferior to that of HA alone, the reason being inadequate bonding between HA and mica. HIP in glass capsules and an increased cold compaction pressure tended to improve the bend strength of the composite. Corrosion in tris for 7 d did not affect the bend strength of the investigated materials significantly. PMID:7950878

  2. Fracture toughness of hydroxyapatite/mica composite, packed hydroxyapatite, alumina ceramics, silicon nitride and -carbide.

    PubMed

    Nordström, E G; Yokobori, A T; Yokobori, T; Aizawa, Y

    1998-01-01

    By using the fracture toughness estimation method based on two-dimensional map, it was found that the ductility of the high porosity hydroxyapatite/mice composite was comparable with silicon carbide. It was measured to be higher than that of packed hydroxyapatite. Alumina ceramics with more than 96% aluminium oxide showed a higher fracture toughness than the composite material. When bending strength was compared, the strength of the composite was two or three times lower than that of packed hydroxyapatite and much lower than the other studied materials. The composite material showed high porosity, which in turn gives it a lower bending strength. However, the high porosity is more favourable for biocompatibility. PMID:9713684

  3. Chemical characterization of silicon-substituted hydroxyapatite.

    PubMed

    Gibson, I R; Best, S M; Bonfield, W

    1999-03-15

    Bioceramic specimens have been prepared by incorporating a small amount of silicon (0.4 wt %) into the structure of hydroxyapatite [Ca10(PO4)6(OH)2, HA] via an aqueous precipitation reaction to produce a silicon-substituted hydroxyapatite (Si-HA). The results of chemical analysis confirmed the proposed substitution of the silicon (or silicate) ion for the phosphorus (or phosphate) ion in hydroxyapatite. The Si-HA was produced by first preparing a silicon-substituted apatite (Si-Ap) by a precipitation process. A single-phase Si-HA was obtained by heating/calcining the as-prepared Si-Ap to temperatures above 700 degrees C; no secondary phases, such as tricalcium phosphate (TCP), tetracalcium phosphate (TeCP), or calcium oxide (CaO), were observed by X-ray diffraction analysis. Although the X-ray diffraction patterns of Si-HA and stoichiometric HA appeared to be identical, refinement of the diffraction data revealed some small structural differences between the two materials. The silicon substitution in the HA lattice resulted in a small decrease in the a axis and an increase in the c axis of the unit cell. This substitution also caused a decrease in the number of hydroxyl (OH) groups in the unit cell, which was expected from the proposed substitution mechanism. The incorporation of silicon in the HA lattice resulted in an increase in the distortion of the PO4 tetrahedra, indicated by an increase in the distortion index. Analysis of the Si-HA by Fourier transform infrared (FTIR) spectroscopy indicated that although the amount of silicon incorporated into the HA lattice was small, silicon substitution appeared to affect the FTIR spectra of HA, in particular the P-O vibrational bands. The results demonstrate that phase-pure silicon-substituted hydroxyapatite may be prepared using a simple precipitation technique. PMID:10397946

  4. Identification of hydroxyapatite crystals in synovial fluid.

    PubMed

    Halverson, P B; McCarty, D J

    1979-04-01

    A semiquantitative technique employing (14C) ethane-1-hydroxy 1, -1-diphosphonate (EHDP) binding has been used to detect crystals, presumably hydroxyapatite, in human synovial fluid samples which were handled to prevent the formation of artifactual mineral phase. Binding material was found in 29% of non-inflammatory and in none of inflammatory joint fluids. Nuclide binding material was strongly correlated with the presence of CPPD crystals and with radiographic evidence of cartilaginous degeneration. PMID:106859

  5. Electrophoretic deposition of composite hydroxyapatite-chitosan coatings

    SciTech Connect

    Pang Xin; Zhitomirsky, Igor . E-mail: zhitom@mcmaster.ca

    2007-04-15

    Cathodic electrophoretic deposition has been utilized for the fabrication of composite hydroxyapatite-chitosan coatings on 316L stainless steel substrates. The addition of chitosan to the hydroxyapatite suspensions promoted the electrophoretic deposition of the hydroxyapatite nanoparticles and resulted in the formation of composite coatings. The obtained coatings were investigated by X-ray diffraction, thermogravimetric and differential thermal analysis, scanning and transmission electron microscopy, potentiodynamic polarization measurements, and electrochemical impedance spectroscopy. It was shown that the deposit composition can be changed by a variation of the chitosan or hydroxyapatite concentration in the solutions. Experimental conditions were developed for the fabrication of hydroxyapatite-chitosan nanocomposites containing 40.9-89.8 wt.% hydroxyapatite. The method enabled the formation of adherent and uniform coatings of thicknesses up to 60 {mu}m. X-ray studies revealed that the preferred orientation of the hydroxyapatite nanoparticles in the chitosan matrix increases with decreasing hydroxyapatite content in the composite coatings. The obtained coatings provided the corrosion protection for the 316L stainless steel substrates00.

  6. Silicide Nanopowders as Low-Cost and High-Performance Thermoelectric Materials

    NASA Astrophysics Data System (ADS)

    Chen, Renkun

    2013-06-01

    Thermoelectric devices directly convert heat into electricity and are very attractive for waste heat recovery and solar energy utilization. If thermoelectric devices can be made sufficiently efficient and inexpensive, then they will become a transformative energy technology that can tap a significant portion (10-20%) of the vast amount of heat existing in nature as well as industrial processes. Nanopowders of Earth-abundant, silicide-based materials, such as Mg2Si and its alloys, provide a unique opportunity to realize this goal. This article will present an overview of recent advances in the synthesis and thermoelectric properties of silicide-based nanostructured materials.

  7. Microstructural and optical characterization of PZT nanopowder prepared at low temperature

    NASA Astrophysics Data System (ADS)

    Ghasemifard, M.; Hosseini, S. M.; Khorsand Zak, A.; Khorrami, Gh. H.

    2009-01-01

    Lead zirconate titanate (PZT) nanopowders were synthesized by the metal organic and salt precursor's sol-gel combustion technique. Single-phase perovskite PZT powders were obtained after heat treatment at temperature of 500 °C. The effects of calcination temperature on lattice parameters and tetragonality of PZT powders have been discussed. The average particles size is estimated to be around 70-80 nm by SEM observations. The absorption coefficient ( α) and the band-gap energy ( Eg) of the perovskite oxide have been estimated using Fourier transform infrared (FTIR) spectroscopy.

  8. Optical properties and radiation stability of submicro- and nanopowders titanium dioxide measured in situ

    NASA Astrophysics Data System (ADS)

    Mikhailov, M. M.; Neshchimenko, V. V.; Yuryev, S. A.

    2016-04-01

    This study carried out an in situ and external investigation on the reflective spectra of micro- and nanopowders titanium dioxide before and after irradiation by 30 keV electrons. The particle sizes range from 60-240 nm. It was established that the decrease in the particle size leads to an increase in intrinsic defects. The particles with intrinsic defects are then transformed into absorption centers during irradiation as a result of optical degradation of TiO2 powders. High radiation stability has particle sizes range from 80-160 nm.

  9. Photocatalytic degradation of betamethasone sodium phosphate in aqueous solution using ZnO nanopowder

    NASA Astrophysics Data System (ADS)

    Giahi, M.; Taghavi, H.; Habibi, S.

    2012-12-01

    The photocatalytic degradation of betamethasone sodium phosphate has been investigated in aqueous phase by using ultraviolet (UV) light and ZnO nanopowder. The effect of catalyst loading, irradiation time, pH, addition of oxidizers, effect of alcohol and anion presence on the reaction rate was ascertained and optimum conditions for maximum degradation were determined. The photocatalytic degradation of betamethasone sodium phosphate was strongly influenced by these parameters. The optimum amount of the photocatalyst used is 0.44 g/L. The efficiency of betamethasone sodium phosphate increases with the photo-degradation increase of the irradiation time.

  10. Spatio-temporal dynamics behind the shock front from compacted metal nanopowders.

    PubMed

    Leela, Ch; Venkateshwarlu, P; Singh, Raja V; Verma, Pankaj; Kiran, P Prem

    2014-03-10

    Laser ablated shock waves from compacted metal nanoenergetic powders of Aluminum (Al), Nickel coated Aluminum (Ni-Al) was characterized using shadowgraphy technique and compared with that from Boron Potassium Nitrate (BKN), Ammonium Perchlorate (AP) and Potassium Bromide (KBr) powders. Ablation is created by focused second harmonic (532 nm, 7 ns) of Nd:YAG laser. Time resolved shadowgraphs of propagating shock front and contact front revealed dynamics and the precise time of energy release of materials under extreme ablative pressures. Among the different compacted materials studied, Al nanopowders have maximum shock velocity and pressure behind the shock front compared to others. PMID:24800282

  11. Spatio-temporal dynamics behind the shock front from compacted metal nanopowders.

    PubMed

    Leela, Ch; Venkateshwarlu, P; Singh, Raja V; Verma, Pankaj; Kiran, P Prem

    2014-03-10

    Laser ablated shock waves from compacted metal nanoenergetic powders of Aluminum (Al), Nickel coated Aluminum (Ni-Al) was characterized using shadowgraphy technique and compared with that from Boron Potassium Nitrate (BKN), Ammonium Perchlorate (AP) and Potassium Bromide (KBr) powders. Ablation is created by focused second harmonic (532 nm, 7 ns) of Nd:YAG laser. Time resolved shadowgraphs of propagating shock front and contact front revealed dynamics and the precise time of energy release of materials under extreme ablative pressures. Among the different compacted materials studied, Al nanopowders have maximum shock velocity and pressure behind the shock front compared to others. PMID:24922235

  12. Plasma Synthesized Doped Boron Nanopowder for MgB2 Superconductors

    SciTech Connect

    James V. Marzik

    2012-03-26

    Under this program, a process to synthesize nano-sized doped boron powder by a plasma synthesis process was developed and scaled up from 20 gram batches at program start to over 200 grams by program end. Over 75 batches of boron nanopowder were made by RF plasma synthesis. Particle sizes were typically in the 20-200 nm range. The powder was synthesized by the reductive pyrolysis of BCl{sub 3} in hydrogen in an RF plasma. A wide range of process parameters were investigated including plasma power, torch geometry, gas flow rates, and process pressure. The powder-in-tube technique was used to make monofilament and multifilament superconducting wires. MgB{sub 2} wire made with Specialty Materials plasma synthesized boron nanopowder exhibited superconducting properties that significantly exceeded the program goals. Superconducting critical currents, J{sub c}, in excess of 10{sup 5} A cm{sup -2} at magnetic fields of 8 tesla were reproducibly achieved. The upper critical magnetic field in wires fabricated with program boron powder were H{sub c2}(0) = 37 tesla, demonstrating the potential of these materials for high field magnet applications. T{sub c} in carbon-doped MgB{sub 2} powder showed a systematic decrease with increasing carbon precursor gas flows, indicating the plasma synthesis process can give precise control over dopant concentrations. Synthesis rates increased by a factor of 400% over the course of the program, demonstrating the scalability of the powder synthesis process. The plasma synthesis equipment at Specialty Materials has successfully and reproducibly made high quality boron nanopowder for MgB{sub 2} superconductors. Research and development from this program enabled Specialty Materials to successfully scale up the powder synthesis process by a factor of ten and to double the size of its powder pilot plant. Thus far the program has been a technical success. It is anticipated that continued systematic development of plasma processing parameters, dopant

  13. Adhesion to and decalcification of hydroxyapatite by carboxylic acids.

    PubMed

    Yoshida, Y; Van Meerbeek, B; Nakayama, Y; Yoshioka, M; Snauwaert, J; Abe, Y; Lambrechts, P; Vanherle, G; Okazaki, M

    2001-06-01

    Fundamental to the processes of decalcification of or adhesion to mineralized tissues is the molecular interaction of acids with hydroxyapatite. This study was undertaken to chemically analyze the interaction of 1 mono-, 2 di-, 1 tri-, and 2 polycarboxylic acids with hydroxyapatite in an attempt to elucidate the underlying mechanism. Maleic, citric, and lactic acid decalcified hydroxyapatite, in contrast to oxalic acid and the two polycarboxylic acids that were chemically bonded to hydroxyapatite. Solubility tests showed that the calcium salts of the former were very soluble, whereas those of the latter could hardly be dissolved in the respective acid solutions. Based on these data, an adhesion/decalcification concept was advanced that predicts that carboxylic acids, regardless of concentration/pH, either adhere to or decalcify hydroxyapatite, depending on the dissolution rate of the respective calcium salts in the acid solution. This contrasting behavior of organic acids most likely results from their differential structural conformations. PMID:11499514

  14. Methods of synthesizing hydroxyapatite powders and bulk materials

    DOEpatents

    Luo, P.

    1999-01-12

    Methods are provided for producing non-porous controlled morphology hydroxyapatite granules of less than 8 {micro}m by a spray-drying process. Solid or hollow spheres or doughnuts can be formed by controlling the volume fraction and viscosity of the slurry as well as the spray-drying conditions. Methods of providing for homogeneous cellular structure hydroxyapatite granules are also provided. Pores or channels or varying size and number can be formed by varying the temperature at which a hydroxyapatite slurry formed in basic, saturated ammonium hydroxide is spray-dried. Methods of providing non-porous controlled morphology hydroxyapatite granules in ammonium hydroxide are also provided. The hydroxyapatite granules and bulk materials formed by these methods are also provided. 26 figs.

  15. Methods of synthesizing hydroxyapatite powders and bulk materials

    DOEpatents

    Luo, Ping

    1999-01-12

    Methods are provided for producing non-porous controlled morphology hydroxyapatite granules of less than 8 .mu.m by a spray-drying process. Solid or hollow spheres or doughnuts can be formed by controlling the volume fraction and viscosity of the slurry as well as the spray-drying conditions. Methods of providing for homogenous cellular structure hydroxyapatite granules are also provided. Pores or channels or varying size and number can be formed by varying the temperature at which a hydroxyapatite slurry formed in basic, saturated ammonium hydroxide is spray-dried. Methods of providing non-porous controlled morphology hydroxyapatite granules in ammonium hydroxide are also provided. The hydroxyapatite granules and bulk materials formed by these methods are also provided.

  16. Effect of zeta potentials on bovine serum albumin adsorption to hydroxyapatite surfaces.

    PubMed

    Miyake, Nahoko; Sato, Toru; Maki, Yoshinobu

    2013-01-01

    The aim of the present study was to examine the adsorption of bovine serum albumin (BSA) to hydroxyapatite surfaces by means of zeta potential. The electrophoretic mobility of both hydroxyapatite and BSA were negative, with BSA itself less negative than hydroxyapatite. The zeta potential of the surface of BSA-adsorbed hydroxyapatite was significantly more negative than that of hydroxyapatite alone (p<0.0001). The BSA histogram indicated two negative peaks, and the zeta potential of BSA-adsorbed hydroxyapatite also showed two similar negative peaks. These results suggest that BSA adsorption to hydroxyapatite surfaces is related to electrostatic interaction. PMID:23903580

  17. Ultrastructure of regenerated bone mineral surrounding hydroxyapatite-alginate composite and sintered hydroxyapatite.

    PubMed

    Rossi, Andre L; Barreto, Isabela C; Maciel, William Q; Rosa, Fabiana P; Rocha-Leão, Maria H; Werckmann, Jacques; Rossi, Alexandre M; Borojevic, Radovan; Farina, Marcos

    2012-01-01

    We report the ultrastructure of regenerated bone surrounding two types of biomaterials: hydroxyapatite-alginate composite and sintered hydroxyapatite. Critical defects in the calvaria of Wistar rats were filled with micrometer-sized spherical biomaterials and analyzed after 90 and 120 days of implantation by high-resolution transmission electron microscopy and Fourier transform infrared attenuated total reflectance microscopy, respectively. Infrared spectroscopy showed that hydroxyapatite of both biomaterials became more disordered after implantation in the rat calvaria, indicating that the biological environment induced modifications in biomaterials structure. We observed that the regenerated bone surrounding both biomaterials had a lamellar structure with type I collagen fibers alternating in adjacent lamella with angles of approximately 90°. In each lamella, plate-like apatite crystals were aligned in the c-axis direction, although a rotation around the c-axis could be present. Bone plate-like crystal dimensions were similar in regenerated bone around biomaterials and pre-existing bone in the rat calvaria. No epitaxial growth was observed around any of the biomaterials. A distinct mineralized layer was observed between new bone and hydroxyapatite-alginate biomaterial. This region presented a particular ultrastructure with crystallites smaller than those of the bulk of the biomaterial, and was possibly formed during the synthesis of alginate-containing composite or in the biological environment after implantation. Round nanoparticles were observed in regions of newly formed bone. The findings of this work contribute to a better understanding of the role of hydroxyapatite based biomaterials in bone regeneration processes at the nanoscale. PMID:22057083

  18. Properties of magnesium-substituted hydroxyapatite and the plasma coatings based on it

    NASA Astrophysics Data System (ADS)

    Lyasnikova, A. V.; Pichkhidze, S. Ya.; Dudareva, O. A.; Markelova, O. A.

    2015-11-01

    Magnesium-substituted hydroxyapatite is synthesized and deposited by plasma spraying, and the coating and the products of hydroxyapatite decomposition are analyzed. The phase composition of magnesium- substituted hydroxyapatite deposited by plasma spraying undergoes changes. The coating consisting of molten magnesium-substituted hydroxyapatite powder particles with pores between them has a homogeneous structure over the surface and throughout the internal structure and adhesion characteristics that exceed those of hydroxyapatite coatings.

  19. A study on the effect factors of sol-gel synthesis of yttrium aluminum garnet nanopowders

    NASA Astrophysics Data System (ADS)

    Yang, Lin; Lu, Tiecheng; Xu, Hui; Zhang, Wei; Ma, Benyuan

    2010-03-01

    Yttrium aluminum garnet (YAG) nanopowders were synthesized by sol-gel method using aluminum nitrate, yttrium nitrate, and citric acid as starting materials, de-ionized water, ethanol, and ethylene glycol as solvents, respectively. The phase formation process, state of particle size distribution (PSD), compositions, morphological characteristics, and thermal behavior of the powders were investigated by means of x-ray diffractometry, PSD, Fourier transform infrared, transmission electronic microscope, and thermogravimetry-differential scanning calorimetry. Results indicate that the formation and characteristics of precursor gel and YAG powder, such as the rate of gelation, average particle size, and powder agglomerate state, strongly depend on the stoichiometric amount of citric acid, the solvent composition, and the precalcination process. Highly crystalline, well-dispersed YAG nanopowder was obtained by calcining at 800 °C for 2 h in the presence of citric acid to nitrate ratio of 3, ethanol solvent, and precalcination process. According to the analysis of experimental results, sol-gel chemistry, DLVO theory, and steric effect, the effects of stoichiometric amount of citric acid, solvent composition, and precalcination process on the formation and characteristics of precursor gel and YAG powder have been discussed. Meanwhile, the overall synthesis mechanism in sol-gel method has been suggested.

  20. Aluminum doped zirconia nanopowders: Wet-chemical synthesis and structural analysis by Rietveld refinement

    SciTech Connect

    Srdic, Vladimir V. Rakic, Srdan; Cvejic, Zeljka

    2008-10-02

    Alumina/zirconia nanopowders, with up to 20 mol% Al{sub 2}O{sub 3}, were prepared by wet-chemical synthesis technique, using controlled hydrolysis of alkoxides. The as-synthesized powders are amorphous, have very high specific surface area and the corresponding particle size smaller than 4 nm. Amorphous powders with 0, 10 and 20 mol% Al{sub 2}O{sub 3} crystallize at 460, 692 and 749 deg. C, respectively, as a single-phase tetragonal zirconia, without any traces of alumina phases. Rietvled refinement of X-ray diffraction data, used for the detailed structural analysis of annealed nanopowders, showed that the high-temperature zirconia phase is stabilized due to the formation of ZrO{sub 2}/Al{sub 2}O{sub 3} solid solutions. High solubility of alumina in the tetragonal zirconia (up to 28.6 at% Al{sup 3+}) and stabilization of tetragonal zirconia solid solution up to high temperature (as high as 1150 deg. C) were also confirmed.

  1. Dependence of viscosity of suspensions of ceramic nanopowders in ethyl alcohol on concentration and temperature

    PubMed Central

    2012-01-01

    This work presents results of measurements of viscosity of suspensions including yttrium oxide (Y2O3), yttrium aluminum garnet (Y3Al5O12) and magnesium aluminum spinel (MgAl2O4) nanopowders in ethanol. Nanoparticles used in our research were either commercially available (Baikowski) or nanopowders newly developed in the Institute of Ceramics and Building Materials in Warsaw, Poland. The study was conducted in a wide range of shear rates (0.01 to 2,000 s−1) and temperature interval from -15°C to 20°C. A Haake Mars 2 rheometer from Thermo Fisher, Germany, was used in the Biophysics Laboratory at Rzeszów University of Technology. Most of the samples show a non-Newtonian behaviour. It was confirmed with a Rheo-NMR system from Bruker that 10% by weight of Y2O3 suspension is a non-Newtonian fluid. In this work, we also report an unexpected behaviour of the viscosity of some samples (Y2O3 and Y3Al5O12) due to sedimentation effect. PMID:22824064

  2. Synthesis and characterization of NiO nanopowder by sol-gel process

    SciTech Connect

    Ningsih, Sherly Kasuma Warda

    2015-09-30

    Preparation of nickel oxide (NiO) nanopowder by sol-gel process has been studied. NiO nanopowders were obtained by sol-gel method by using nickel nitrate hexahydrate and sodium hydroxide and aquadest were used as precursor, agent precipitator and solvent, respectively. The powders were formed by drying at 110°C and followed by heating in the furnace at 400°C for 1.5 hours. The product was obtained black powder. The product was characterized by Energy Dispesive X-ray Fluorescence (ED-XRF), X-ray diffraction (XRD) and Scanning Electron Microscopy (SEM). The ED-XRF pattern shows the composition of NiO produced was 97.1%. The XRD pattern showed NiO forms were produced generally in monoclinic stucture. The crystalline size of NiO was obtained in the range 40-85 nm. SEM micrograph clearly showed that powder had a spherical with uniform distribution size is 0.1-1.0 µm approximately.

  3. Synthesis and characterization of NiO nanopowder by sol-gel process

    NASA Astrophysics Data System (ADS)

    Ningsih, Sherly Kasuma Warda

    2015-09-01

    Preparation of nickel oxide (NiO) nanopowder by sol-gel process has been studied. NiO nanopowders were obtained by sol-gel method by using nickel nitrate hexahydrate and sodium hydroxide and aquadest were used as precursor, agent precipitator and solvent, respectively. The powders were formed by drying at 110°C and followed by heating in the furnace at 400°C for 1.5 hours. The product was obtained black powder. The product was characterized by Energy Dispesive X-ray Fluorescence (ED-XRF), X-ray diffraction (XRD) and Scanning Electron Microscopy (SEM). The ED-XRF pattern shows the composition of NiO produced was 97.1%. The XRD pattern showed NiO forms were produced generally in monoclinic stucture. The crystalline size of NiO was obtained in the range 40-85 nm. SEM micrograph clearly showed that powder had a spherical with uniform distribution size is 0.1-1.0 µm approximately.

  4. Dependence of viscosity of suspensions of ceramic nanopowders in ethyl alcohol on concentration and temperature.

    PubMed

    Zyła, Gaweł; Cholewa, Marian; Witek, Adam

    2012-01-01

    : This work presents results of measurements of viscosity of suspensions including yttrium oxide (Y2O3), yttrium aluminum garnet (Y3Al5O12) and magnesium aluminum spinel (MgAl2O4) nanopowders in ethanol. Nanoparticles used in our research were either commercially available (Baikowski) or nanopowders newly developed in the Institute of Ceramics and Building Materials in Warsaw, Poland. The study was conducted in a wide range of shear rates (0.01 to 2,000 s-1) and temperature interval from -15°C to 20°C. A Haake Mars 2 rheometer from Thermo Fisher, Germany, was used in the Biophysics Laboratory at Rzeszów University of Technology. Most of the samples show a non-Newtonian behaviour. It was confirmed with a Rheo-NMR system from Bruker that 10% by weight of Y2O3 suspension is a non-Newtonian fluid. In this work, we also report an unexpected behaviour of the viscosity of some samples (Y2O3 and Y3Al5O12) due to sedimentation effect. PMID:22824064

  5. Three-dimensional simulations of nanopowder compaction processes by granular dynamics method

    NASA Astrophysics Data System (ADS)

    Boltachev, G. Sh.; Lukyashin, K. E.; Shitov, V. A.; Volkov, N. B.

    2013-07-01

    In order to describe and to study the processes of cold compaction within the discrete element method a three-dimensional model of nanosized powder is developed. The elastic forces of repulsion, the tangential forces of “friction” (Cattaneo-Mindlin), and the dispersion forces of attraction (van der Waals-Hamaker), as well as the formation and destruction of hard bonds between the individual particles are taken into account. The monosized powders with the size of particles in the range 10-40 nm are simulated. The simulation results are compared to the experimental data of the alumina nanopowders compaction. It is shown that the model allows us to reproduce experimental data reliably and, in particular, describes the size effect in the compaction processes. A number of different external loading conditions is used in order to perform the theoretical and experimental researches. The uniaxial compaction (the closed-die compaction), the biaxial (radial) compaction, and the isotropic compaction (the cold isostatic pressing) are studied. The real and computed results are in a good agreement with each other. They reveal a weak sensitivity of the oxide nanopowders to the loading condition (compaction geometry). The application of the continuum theory of the plastically hardening porous body, which is usually used for the description of powders, is discussed.

  6. Low temperature synthesis of pure cubic ZrO2 nanopowder: Structural and luminescence studies

    NASA Astrophysics Data System (ADS)

    Prakashbabu, D.; Hari Krishna, R.; Nagabhushana, B. M.; Nagabhushana, H.; Shivakumara, C.; Chakradar, R. P. S.; Ramalingam, H. B.; Sharma, S. C.; Chandramohan, R.

    2014-03-01

    Pure cubic zirconia (ZrO2) nanopowder is prepared for the first time by simple low temperature solution combustion method without calcination. The product is characterized by Powder X-ray Diffraction (PXRD), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), Fourier Transform Infra Red spectroscopy (FTIR) and Ultraviolet-Visible spectroscopy (UV-Vis). The PXRD showed the formation of pure stable cubic ZrO2 nanopowders with average crystallite size ranging from 6 to 12 nm. The lattice parameters were calculated from Rietveld refinement method. SEM micrograph shows fluffy, mesoporous, agglomerated particles with large number of voids. TEM micrograph shows honey comb like arrangement of particles with particle size ∼10 nm. The PL emission spectrum excited at 210 nm and 240 nm consists of intense bands centered at ∼365 and ∼390 nm. Both the samples show shoulder peak at ∼420 nm, along with four weak emission bands at ∼484, ∼528, ∼614 and ∼726 nm. TL studies were carried out pre-irradiating samples with γ-rays ranging from 1 to 5 KGy at room temperature. A well resolved glow peak at 377 °C is recorded which can be ascribed to deep traps. With increase in γ radiation there is linear increase in TL intensity which shows the possible use of ZrO2 as dosimetric material.

  7. EGCG assisted green synthesis of ZnO nanopowders: Photodegradative, antimicrobial and antioxidant activities

    NASA Astrophysics Data System (ADS)

    Suresh, D.; Udayabhanu; Nethravathi, P. C.; Lingaraju, K.; Rajanaika, H.; Sharma, S. C.; Nagabhushana, H.

    2015-02-01

    Zinc oxide nanopowders were synthesized by solution combustion method using Epigallocatechin gallate (EGCG) a tea catechin as fuel. The structure and morphology of the product was characterized by Powder X-ray Diffraction, Scanning Electron Microscopy, photoluminescence and UV-Visible spectroscopy. The nanopowders (Nps) were subjected to photocatalytic and biological activities such as antimicrobial and antioxidant studies. PXRD patterns demonstrate that the formed product belongs to hexagonal wurtzite system. SEM images show that the particles are agglomerated to form sponge like structure and the average crystallite sizes were found to be ∼10-20 nm. PL spectra exhibit broad and strong peak at 590 nm due to the Zn-vacancies, and O-vacancies. The prepared ZnO Nps exhibit excellent photocatalytic activity for the photodegradation of malachite green (MG) and methylene blue (MB) indicating that the ZnO NPs are potential photocatalytic semiconductor materials. ZnO NPs exhibit significant bactericidal activity against Klebsiella aerogenes, Pseudomonas aeruginosa, Escherichia coli and Staphylococcus aureus using the agar well diffusion method. Furthermore, the ZnO nano powders show good antioxidant activity by potentially scavenging DPPH radicals. The study successfully demonstrates synthesis of ZnO NPs by simple ecofriendly route employing EGCG as fuel that exhibit superior photodegradative, antibacterial and antioxidant activities.

  8. Synthesis and characterization of InNbO₄ nanopowder for gas sensors.

    PubMed

    Balamurugan, C; Vijayakumar, E; Subramania, A

    2012-01-15

    Indium niobate (InNbO(4)) nanopowder was prepared by a comparatively low temperature niobium citrate complex process. The prepared InNbO(4) was characterized by thermal analysis, X-ray diffraction analysis (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy, diffuse reflectance spectroscopy (DRS), and impedance studies. It revealed that the well crystalline monoclinic InNbO(4) nanopowder was obtained at the calcination temperature of 600°C. The average particle diameter was 22nm. The optical band gap was found to be 2.66eV. The temperature dependent conductivity obeyed Arrhenius relation. The activation energy of the conductivity process was calculated to be 0.43eV. The gas sensing behaviour of the prepared InNbO(4) was studied by measuring the change in resistance of the sensor material as a function of various concentrations of the test gases such as liquid petroleum gas (LPG), ammonia (NH(3)) and ethanol (C(2)H(5)OH) at their optimized operating temperature. InNbO(4) had a better sensitivity to LPG (0.97) and NH(3) (0.70) gas than ethanol (0.46). The sensor responses of InNbO(4) as a function of gas concentrations and with recovery time were also studied in detail. PMID:22265476

  9. Employing Ti nano-powder dielectric to enhance surface characteristics in electrical discharge machining of AISI D2 steel

    NASA Astrophysics Data System (ADS)

    Marashi, Houriyeh; Sarhan, Ahmed A. D.; Hamdi, Mohd

    2015-12-01

    Manufacturing components with superior surface characteristics is challenging when electrical discharge machining (EDM) is employed for mass production. The aim of this research is to enhance the characteristics of AISI D2 steel surface machined with EDM through adding Ti nano-powder to dielectric under various machining parameters, including discharge duration (Ton) and peak current (I). Surface roughness profilometer, FESEM and AFM analysis were utilized to reveal the machined surface characteristics in terms of surface roughness, surface morphology and surface micro-defects. Moreover, EDX analysis was performed in order to evaluate the atomic deposition of Ti nano-powder on the surface. The concentration of Ti nano-powder in dielectric was also examined using ESEM and EDX. According to the results, the addition of Ti nano-powder to dielectric notably enhanced the surface morphology and surface roughness at all machining parameters except Ton = 340 μs. Of these parameters, maximum enhancement was observed at Ton = 210 μs, where the material removal rate and average surface roughness improved by ∼69 and ∼35% for peak current of 6 and 12 A, respectively. Elemental analysis signified negligible Ti deposition on the machined surface while the atomic concentration of Ti was increased around the crack areas.

  10. Hydroxyapatite-silver nanoparticles coatings on porous polyurethane scaffold.

    PubMed

    Ciobanu, Gabriela; Ilisei, Simona; Luca, Constantin

    2014-02-01

    The present paper is focused on a study regarding the possibility of obtaining hydroxyapatite-silver nanoparticle coatings on porous polyurethane scaffold. The method applied is based on a combined strategy involving hydroxyapatite biomimetic deposition on polyurethane surface using a Supersaturated Calcification Solution (SCS), combined with silver ions reduction and in-situ crystallization processes on hydroxyapatite-polyurethane surface by sample immersing in AgNO3 solution. The morphology, composition and phase structure of the prepared samples were characterized by scanning electron microscopy coupled with energy dispersive X-ray spectroscopy (SEM-EDX), X-ray diffraction (XRD), UV-Vis spectroscopy and X-ray photoelectron spectroscopy (XPS) measurements. The data obtained show that a layer of hydroxyapatite was deposited on porous polyurethane support and the silver nanoparticles (average size 34.71 nm) were dispersed among and even on the hydroxyapatite crystals. Hydroxyapatite/polyurethane surface acts as a reducer and a stabilizing agent for silver ions. The surface plasmon resonance peak in UV-Vis absorption spectra showed an absorption maximum at 415 nm, indicating formation of silver nanoparticles. The hydroxyapatite-silver polyurethane scaffolds were tested against Staphylococcus aureus and Escherichia coli and the obtained data were indicative of good antibacterial properties of the materials. PMID:24411349

  11. Hydroxyapatite Reinforced Coatings with Incorporated Detonationally Generated Nanodiamonds

    SciTech Connect

    Pramatarova, L.; Pecheva, E.; Hikov, T.; Fingarova, D.; Dimitrova, R.; Spassov, T.; Krasteva, N.; Mitev, D.

    2010-01-21

    We studied the effect of the substrate chemistry on the morphology of hydroxyapatite-detonational nanodiamond composite coatings grown by a biomimetic approach (immersion in a supersaturated simulated body fluid). When detonational nanodiamond particles were added to the solution, the morphology of the grown for 2 h composite particles was porous but more compact then that of pure hydroxyapatite particles. The nanodiamond particles stimulated the hydroxyapatite growth with different morphology on the various substrates (Ti, Ti alloys, glasses, Si, opal). Biocompatibility assay with MG63 osteoblast cells revealed that the detonational nanodiamond water suspension with low and average concentration of the detonational nanodiamond powder is not toxic to living cells.

  12. In-situ deposition of hydroxyapatite on graphene nanosheets

    PubMed Central

    Neelgund, Gururaj M.; Oki, Aderemi; Luo, Zhiping

    2014-01-01

    Graphene nanosheets were effectively functionalized by in-situ deposition of hydroxyaptite through a facile chemical precipitation method. Prior to grafting of hydroxyapatite, chemically modified graphene nanosheets were obtained by the reduction of graphene oxide in presence of ethylenediamine. The resulting hydroxyapatite functionalized graphene nanosheets were characterized by attenuated total reflection IR spectroscopy, X-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy, X-ray energy dispersive spectroscopy, Raman spectroscopy and thermogravimetric analysis. These characterization techniques revealed the successful grafting of hydroxyapatite over well exfoliated graphene nanosheets without destroying their structure. PMID:25110359

  13. Hydroxyapatite Reinforced Coatings with Incorporated Detonationally Generated Nanodiamonds

    NASA Astrophysics Data System (ADS)

    Pramatarova, L.; Pecheva, E.; Dimitrova, R.; Spassov, T.; Krasteva, N.; Hikov, T.; Fingarova, D.; Mitev, D.

    2010-01-01

    We studied the effect of the substrate chemistry on the morphology of hydroxyapatite-detonational nanodiamond composite coatings grown by a biomimetic approach (immersion in a supersaturated simulated body fluid). When detonational nanodiamond particles were added to the solution, the morphology of the grown for 2 h composite particles was porous but more compact then that of pure hydroxyapatite particles. The nanodiamond particles stimulated the hydroxyapatite growth with different morphology on the various substrates (Ti, Ti alloys, glasses, Si, opal). Biocompatibility assay with MG63 osteoblast cells revealed that the detonational nanodiamond water suspension with low and average concentration of the detonational nanodiamond powder is not toxic to living cells.

  14. EXAFS study of structural disorder in carbonate-containing hydroxyapatites.

    PubMed

    Harries, J E; Hasnain, S S; Shah, J S

    1987-12-01

    A structural characterization of pure hydroxyapatite and partially carbonated hydroxyapatites has been performed using EXAFS spectroscopy, X-ray diffraction, and infrared spectroscopy. Our findings show that marked structural changes within the hydroxyapatite unit cell accompany the substitution of the phosphate anion. Extended X-ray Absorption Fine Structure (EXAFS) spectroscopy has shown that the incorporation of carbonate into the phosphate site alters the structural geometry beyond the nearest neighbor oxygen coordination to calcium in a manner consistent with an increase in structural disorder. The nearest neighbor coordination to calcium is not detectably affected by the presence of carbonate. PMID:2830003

  15. An X-ray electron study of nanodisperse hydroxyapatite

    NASA Astrophysics Data System (ADS)

    Melikhov, I. V.; Teterin, Yu. A.; Rudin, V. N.; Teterin, A. Yu.; Maslakov, K. I.; Severin, A. V.

    2009-01-01

    Two states of surface valence electrons localized on faces with different molecular reliefs were observed for nanodisperse hydroxyapatite. Thermal treatment of nanocrystals caused a shift Δ E b = 0.5 eV of the spectrum of valence electrons on molecularly rough faces and a shift of 0.8 eV of the spectrum from smooth faces. Similar electron spectrum shifts were observed for sorption, in particular, of sodium succinate. These results are of importance for the diagnostics of various hydroxyapatite kinds, since hydroxyapatite is a constituent mineral component of living organisms, and for the synthesis of medicines with enhanced biological activity used in treatment of various bone diseases.

  16. Dissolution of human teeth-derived hydroxyapatite.

    PubMed

    Seo, Dong Seok; Lee, Jong Kook

    2008-01-01

    We have been interested in human teeth which consist of hydroxyapatite (HA), but do not degrade for a long time. In order to overcome dissolution and mechanical degradation of man-made HA, biologically derived hydroxyapatite (BHA) ceramics were prepared from human teeth and their dissolving behavior was investigated in distilled water for 3-14 days and compared with an artificial HA made of synthetic HA powder. BHA ceramics were prepared by calcining freshly extracted human teeth at 900 degrees C and followed by sintering at 1200 degrees C for 2 h. All detectable peaks in the artificial HA are identical to HA lattice planes, whereas BHA consisted of a mixture of HA and beta-tricalcium phosphate (TCP). Although the artificial HA was expected to be stable in water, the surface dissolution initiated at grain boundaries followed by generated many separated grains and their associated pores. On the other hand, BHA showed that definite grains considered as beta-TCP were predominantly dissolved and the grains were separated from the matrix leaving pores. In the mean time, the rest region, mainly consisting of HA, did not show any evidence of dissolution. It indicates that BHA showed rather stable grain boundaries and lack of excessive dissolution in liquid environment. PMID:17943445

  17. Evolving application of biomimetic nanostructured hydroxyapatite

    PubMed Central

    Roveri, Norberto; Iafisco, Michele

    2010-01-01

    By mimicking Nature, we can design and synthesize inorganic smart materials that are reactive to biological tissues. These smart materials can be utilized to design innovative third-generation biomaterials, which are able to not only optimize their interaction with biological tissues and environment, but also mimic biogenic materials in their functionalities. The biomedical applications involve increasing the biomimetic levels from chemical composition, structural organization, morphology, mechanical behavior, nanostructure, and bulk and surface chemical–physical properties until the surface becomes bioreactive and stimulates cellular materials. The chemical–physical characteristics of biogenic hydroxyapatites from bone and tooth have been described, in order to point out the elective sides, which are important to reproduce the design of a new biomimetic synthetic hydroxyapatite. This review outlines the evolving applications of biomimetic synthetic calcium phosphates, details the main characteristics of bone and tooth, where the calcium phosphates are present, and discusses the chemical–physical characteristics of biomimetic calcium phosphates, methods of synthesizing them, and some of their biomedical applications. PMID:24198477

  18. Biological reactivity of zirconia-hydroxyapatite composites.

    PubMed

    Silva, Viviane V; Lameiras, Fernando S; Lobato, Zélia I P

    2002-01-01

    Materials and devices intended for end-use applications as implants and medical devices must be evaluated to determine their biocompatibility potential in contact with physiological systems. The use of standard practices of biological testing provides a reasonable level of confidence concerning the response of a living organism to a given material or device, as well as guidance in selecting the proper procedures to be carried out for the screening of new or modified materials. This article presents results from cytotoxicity assays of cell culture, skin irritation, and acute toxicity by systemic and intracutaneous injections for powders, ceramic bodies, and extract liquids of hydroxyapatite (HA), calcia partially stabilized zirconia (ZO), and two types of zirconia-hydroxyapatite composites (Z4H6 and Z6H4) with potential for future use as orthopedic and dental implants. They indicate that these materials present potential for this type of application because they meet the requirements of the standard practices recommended for evaluating the biological reactivity of ATCC cell cultures (CCL1 NCTC clone 929 of mouse connective tissue and CCL 81 of monkey connective tissue) and animals (rabbit and mouse) with direct or indirect patient contact, or by the injection of specific extracts prepared from the material under test. In addition, studies involving short-term intramuscular and long-term implantation assays to estimate the reaction of living tissue to the composites studied, and investigations on long-term effects that these materials can cause on the cellular metabolism, are already in progress. PMID:12209904

  19. Improved mechanical properties of hydroxyapatite/poly(ɛ-caprolactone) scaffolds by surface modification of hydroxyapatite

    NASA Astrophysics Data System (ADS)

    Wang, Yan; Dai, Jing; Zhang, Qingchun; Xiao, Yan; Lang, Meidong

    2010-08-01

    Scaffolds comprising hydroxyapatite (HAP) or poly(ɛ-caprolactone)-grafted hydroxyapatite (g-HAP) and poly(ɛ-caprolactone) (PCL) were prepared using the thermally induced phase separation/salt leaching technique. The g-HAP nanoparticles were evaluated by Fourier Transformation Infrared Spectroscopy (FTIR) and thermal gravimetric analysis (TGA). Power X-ray Diffraction (XRD) patterns confirmed the successful grafting on the surface of HAP. The effects on mechanical strength, porosity and thermal property of scaffolds by the introduction of nanoparticles were extensively investigated. The compressive modulus of the scaffold was greatly improved by the addition of g-HAP nanoparticles. Especially the compressive modulus of the g-HAP/PCL scaffold containing 20 wt% of g-HAP was 59.4% higher than that of the corresponding HAP/PCL scaffold.

  20. Nanopowders M{sub 2}O{sub 3} (M = Y, La, Yb, Nd) with spherical particles and laser ceramics based on them

    SciTech Connect

    Bagayev, Sergei N; Kaminskii, Alexandr A; Kopylov, Yu L; Kravchenko, V B; Tolmachev, A V; Shemet, V V; Yavetskii, R P

    2013-03-31

    We have considered the problems of agglomeration of yttrium aluminium garnet (YAG) nanopowders prepared by chemical co-precipitation of precursors from aqueous solutions and subsequent calcination. To fabricate YAG and Y{sub 2}O{sub 3} laser ceramic samples with high optical transmittance and reproducible characteristics, we have developed a method for producing non-agglomerated nanopowders of pure and doped Y{sub 2}O{sub 3} by homogeneous chemical precipitation. Nanopowders Y{sub 2}O{sub 3} with La and Yb as well as mixtures of Y{sub 2}O{sub 3} : Nd and several commercial nanopowders of aluminium oxide have been compacted; optimised compacting technique have been selected; ceramic samples (Y, La, Yb){sub 2}O{sub 3} and YAG : Nd with high optical transmittance at a wavelength of 1 {mu}m have been produced by solid-phase synthesis. (extreme light fields and their applications)

  1. Effect of solution combusted TiO2 nanopowder within commercial BaTiO3 dielectric layer on the photoelectric properties for AC powder electroluminescence devices.

    PubMed

    Park, Sung; Choi, Gil Rak; Kim, Youn Cheol; Lee, Jae Chun; Lee, Ju Hyeon

    2013-05-01

    A unique synthesis method was developed, which is called solution combustion method (SCM). TiO2 nanopowder was synthesized by this method. This SCM TiO2 nanopowder (-35 nm) was added to the dielectric layer of AC powder electroluminescence (EL) device. The dielectric layer was made of commercial BaTiO3 powder (-1.2 microm) and binding polymer. 0, 5, 10 and 15 wt% of SCM TiO2 nanopowder was added to the dielectric layer during fabrication of AC powder EL device respectively. Dielectric constant of these four kinds of dielectric layers was measured. The brightness and current density of AC powder EL device were also measured. When 10 wt% of SCM TiO2 nanopowder was added, dielectric constant and brightness were increased by 30% and 101% respectively. Furthermore, the current density was decreased by 71%. This means that the brightness was double and the power consumption was one third. PMID:23858874

  2. Carbonate Hydroxyapatite and Silicon-Substituted Carbonate Hydroxyapatite: Synthesis, Mechanical Properties, and Solubility Evaluations

    PubMed Central

    Bang, L. T.; Long, B. D.; Othman, R.

    2014-01-01

    The present study investigates the chemical composition, solubility, and physical and mechanical properties of carbonate hydroxyapatite (CO3Ap) and silicon-substituted carbonate hydroxyapatite (Si-CO3Ap) which have been prepared by a simple precipitation method. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), X-ray fluorescence (XRF) spectroscopy, and inductively coupled plasma (ICP) techniques were used to characterize the formation of CO3Ap and Si-CO3Ap. The results revealed that the silicate (SiO44−) and carbonate (CO32−) ions competed to occupy the phosphate (PO43−) site and also entered simultaneously into the hydroxyapatite structure. The Si-substituted CO3Ap reduced the powder crystallinity and promoted ion release which resulted in a better solubility compared to that of Si-free CO3Ap. The mean particle size of Si-CO3Ap was much finer than that of CO3Ap. At 750°C heat-treatment temperature, the diametral tensile strengths (DTS) of Si-CO3Ap and CO3Ap were about 10.8 ± 0.3 and 11.8 ± 0.4 MPa, respectively. PMID:24723840

  3. Topography, wetting, and corrosion responses of electrodeposited hydroxyapatite and fluoridated hydroxyapatite on magnesium.

    PubMed

    Assadian, Mahtab; Jafari, Hassan; Ghaffari Shahri, Seyed Morteza; Idris, Mohd Hasbullah; Almasi, Davood

    2016-08-12

    In this study, different types of calcium-phosphate phases were coated on NaOH pre-treated pure magnesium. The coating was applied by electrodeposition method in order to provide higher corrosion resistance and improve biocompatibility for magnesium. Thickness, surface morphology and topography of the coatings were analyzed using optical, scanning electron and atomic-force microscopies, respectively. Composition and chemical bonding, crystalline structures and wettability of the coatings were characterized using energy-dispersive and attenuated total reflectance-Fourier transform infrared spectroscopies, grazing incidence X-ray diffraction and contact angle measurement, respectively. Degradation behavior of the coated specimens was also investigated by potentiodynamic polarization and immersion tests. The experiments proved the presence of a porous coating dominated by dicalcium-phosphate dehydrate on the specimens. It was also verified that the developed hydroxyapatite was crystallized by alkali post-treatment. Addition of supplemental fluoride to the coating electrolyte resulted in stable and highly crystallized structures of fluoridated hydroxyapatite. The coatings were found effective to improve biocompatibility combined with corrosion resistance of the specimens. Noticeably, the fluoride supplemented layer was efficient in lowering corrosion rate and increasing surface roughness of the specimens compared to hydroxyapatite and dicalcium-phosphate dehydrates layers. PMID:27567782

  4. [Study on an injectable biomimetic hydroxyapatite--atelocollagen composite].

    PubMed

    Maier, S S; Pelin, Irina; Bulacovschi, V

    2007-01-01

    The paper presents a procedure for preparing mineralized collagen nanofibrils, mixed with deficient nanoparticulate calcium hydroxyapatite in a ratio close to that found in living bone structures. Such a composition might represent an injectable osteoconductive constituent, used in surgical kits for bone reconstruction. The FT-IR spectra of the prepared composite reveals a weak absorption at 871.82 cm(-1), indicating the nucleation of hydroxy-apatite at the acidic atelocollagen functions. More than that, a 45 cm(-1) ipsochromic shift of carboxylic band suggest a strong ionic interaction with hydroxyapatite. The X-Ray spectra show a high resemblance between the synthetic composite and the Fluka hydroxyapatite, but only for 2theta angles higher than 30 degrees. Below that value the protein presence induce crystalline disorders. PMID:18389809

  5. Formation of pyrophosphate on hydroxyapatite with thioesters as condensing agents

    NASA Technical Reports Server (NTRS)

    Weber, A. L.

    1982-01-01

    'Energy-rich' thioesters are shown to act as condensing agents in the formation of pyrophosphate on hydroxyapatite in the presence of water at ambient temperature. The yield of pyrophosphate based on thioester ranges from 2.5% to 11.4% and depends upon the pH and concentration of reactants. Reaction of 0.130 M hydroxyapatite suspended in a solution of 0.08 M sodium phosphate and 0.20 M imidazole hydrochloride (pH 7.0) with 0.10 M N,S-diacetylcysteamine for 6 days gives the highest yield of pyrophosphate (11.4%). Pyrophosphate formation requires the presence of hydroxyapatite, sodium phosphate and the thioester, N,S-diacetylcysteamine. The related thioester, N,S-diacetylcysteine, also yields pyrophosphate in reactions on hydroxyapatite.

  6. Synthesis of mesoporous nano-hydroxyapatite by using zwitterions surfactant

    EPA Science Inventory

    Mesoporous nano-hydroxyapatite (mn-HAP) was successfully synthesized via a novel micelle-templating method using lauryl dimethylaminoacetic acid as zwitterionic surfactant. The systematic use of such a surfactant in combination with microwave energy inputenables the precise contr...

  7. Preparation and characterization of collagen-hydroxyapatite/pectin composite.

    PubMed

    Wenpo, Feng; Gaofeng, Liang; Shuying, Feng; Yuanming, Qi; Keyong, Tang

    2015-03-01

    Pectin, a kind of plant polysaccharide, was introduced into collagen-hydroxyapatite composite system, and prepared collagen-hydroxyapatite/pectin (Col-HA/pectin) composite in situ. The structure of the composite was investigated by XRD, SEM, and FT-IR. The mechanical properties, water absorption, enzyme degradation, and cytotoxicity of the composite were investigated as well. The results show that the inorganic substance in the composite materials is hydroxyapatite in relatively low crystallinity. A new interface appeared by the interaction among hydroxyapatite and collagen-pectin, and formed smooth fine particles. The mechanical properties, water absorption, enzyme degradation, and cytotoxicity indicate a potential use in bone replacement for the new composite. PMID:25485944

  8. Formation of hydroxyapatite in various aqueous solutions

    NASA Astrophysics Data System (ADS)

    Sturgeon, Jacqueline Lee

    Hydroxyapatite (HAp), Ca10(PO4)6(OH) 2, is important in the field of biomaterials as it is the mineral component of bones and teeth. Biological apatites do not maintain an exact composition and are usually calcium-deficient, represented as Ca(10- x)(HPO 4)x(PO4)(6-x)(OH)(2-x), where x ranges from 0 to 1, with various ion substitutions. Formation of calcium-deficient hydroxyapatites (CDHAp) from solid calcium phosphate precursor materials was performed at physiologic temperature (37°C) in a variety of aqueous solutions. Two cement systems were utilized in these experiments: tetralcium phosphate (TetCP) with dicalcium phosphate anhydrous (DCPA) and beta-tricalcium phosphate (beta-TCP). The kinetics, solution chemistry, phase evolution, and microstructure of the developed apatites were analyzed as appropriate. Reaction of beta-TCP in ammonium fluoride solutions formed HAp substituted with fluoride and calculated to be deficient in calcium. A new ratio of TetCP to DCPA was used with solutions of sodium bicarbonate to form a calcium-deficient carbonate hydroxyapatite. The capacity for sodium dihydrogen phosphate to buffer pH increases and enhance reaction kinetics in this system was also explored. Formation of a highly crystalline CDHAp was achieved by hydrolyzing beta-TCP in water for extended time periods. Lattice parameters were among the features characterized for this apatite. The hydrolysis of beta-TCP in phosphate buffered saline (PBS) and simulated body fluids (SBF) was also investigated; use of SBF was found to completely inhibit formation of HAp in this system while reaction in PBS was slow in comparison to water. The effects of filler materials on the mechanical properties of a calcium phosphate cement were examined using the TetCP/DCPA system. Dense aggregates were not found to decrease compressive strength in comparison to the cement alone. The use of aggregates was found to improve the compressive strength of cement formed using NaHCO3 solution as a

  9. Stable Co-Catalyst-Free Photocatalytic H2 Evolution From Oxidized Titanium Nitride Nanopowders.

    PubMed

    Zhou, Xuemei; Zolnhofer, Eva M; Nguyen, Nhat Truong; Liu, Ning; Meyer, Karsten; Schmuki, Patrik

    2015-11-01

    A simple strategy is used to thermally oxidize TiN nanopowder (∼20 nm) to an anatase phase of a TiO2:Ti(3+):N compound. In contrast to the rutile phase of such a compound, this photocatalyst provides activity for hydrogen evolution under AM1.5 conditions, without the use of any noble metal co-catalyst. Moreover the photocatalyst is active and stable over extended periods of time (tested for 4 months). Importantly, to achieve successful conversion to the active anatase polymorph, sufficiently small starting particles of TiN are needed. The key factor for catalysis is the stabilization of the co-catalytically active Ti(3+) species against oxidation by nitrogen present in the starting material. PMID:26427346

  10. Preparation and Characterization of Fine-Particle NTO and Its Formulation with Al Nanopowders

    NASA Astrophysics Data System (ADS)

    Lee, K.-Y.; Kennedy, J. E.; Asay, B. W.; Son, S. F.; Martin, E. S.

    2004-07-01

    We have initiated study of the effect of nano-aluminum on the detonation performance of NTO. A novel method for the preparation of both fine-particle NTO (UF-NTO) and its formulation with Al nanopowder has been developed. Results from small-scale sensitivity tests on both the UF-NTO and aluminized NTO composite indicated that they are insensitive to impact, friction and HESD. The performance of both UF-NTO and NTO/Al mix was evaluated by detonation-spreading floret tests. At the same pressed density, it was found that, when initiated by a 3-mm-diameter flyer plate, the aluminized NTO composite produced a shallower dent on a copper witness plate than neat UF-NTO and thus was inferior to UF-NTO in detonation spreading.

  11. The effect of calcination temperature on the crystallinity of TiO 2 nanopowders

    NASA Astrophysics Data System (ADS)

    Chen, Yung-Fang; Lee, Chi-Young; Yeng, Ming-Yu; Chiu, Hsin-Tien

    2003-01-01

    TiO 2 nanopowders have been prepared using 0.1 M titanium tetraisopropoxide (TTIP) in varied pH aqueous solution containing TMC and NP-204 surfactants. Only the powder acquired from a solution of pH=2 has a regular particle size distribution. Anatase phase powders are obtained by calcination in nitrogen in the 250-500°C temperature range. When calcined at 400°C, the diameter of the nanoparticles is approximately 10 nm with a specific surface area of 106.9 m 2/g. As the calcination temperature is increased, the particle size increases. Rutile phase powders are formed at calcination temperatures above 600°C.

  12. Acetone Sensing Properties of a Gas Sensor Composed of Carbon Nanotubes Doped With Iron Oxide Nanopowder

    PubMed Central

    Tan, Qiulin; Fang, Jiahua; Liu, Wenyi; Xiong, Jijun; Zhang, Wendong

    2015-01-01

    Iron oxide (Fe2O3) nanopowder was prepared by a precipitation method and then mixed with different proportions of carbon nanotubes. The composite materials were characterized by X-ray powder diffraction, Fourier transform infrared spectroscopy and scanning electron microscopy. A fabricated heater-type gas sensor was compared with a pure Fe2O3 gas sensor under the influence of acetone. The effects of the amount of doping, the sintering temperature, and the operating temperature on the response of the sensor and the response recovery time were analyzed. Experiments show that doping of carbon nanotubes with iron oxide effectively improves the response of the resulting gas sensors to acetone gas. It also reduces the operating temperature and shortens the response recovery time of the sensor. The response of the sensor in an acetone gas concentration of 80 ppm was enhanced, with good repeatability. PMID:26569253

  13. Modelling of laser welding of flat parts using the modifying nanopowders

    NASA Astrophysics Data System (ADS)

    Cherepanov, A. N.; Shapeev, V. P.

    2013-06-01

    A mathematical model is formulated to describe thermophysical processes at laser welding of metal plates for the case when the modifying nanoparticles of refractory compounds have been introduced in the weld pool (the nanopowder seed cultrure fermenters — NSCF). Specially prepared nanoparticles of refractory compounds serve the crystallization centers that is they are in fact the exogenous primers, on the surface of which the individual clusters are grouped. Owing to this, one can control the process of the crystallization of the alloy and the formation of its structure and, consequently, the joint weld properties. As an example, we present the results of computing the butt welding of two plates of aluminum alloy and steel. Computed and experimental data are compared.

  14. Magnetic nanopowder as effective adsorbent for the removal of Congo Red from aqueous solution.

    PubMed

    Paşka, O; Ianoş, R; Păcurariu, C; Brădeanu, A

    2014-01-01

    A magnetic iron oxide nanopowder (MnP), prepared by a simple and efficient combustion synthesis technique, was tested for the removal of the anionic dye Congo Red (CR) from aqueous solution. The influence of solution pH, adsorbent dose, temperature, contact time and initial dye concentration on the adsorption of CR onto MnP were investigated. It was shown that the CR adsorption was pH dependent and the adsorption mechanism was governed by electrostatic forces. The adsorption kinetic was best described by the pseudo-second-order model and the equilibrium data were well fitted to the Langmuir isotherm, yielding maximum adsorption capacity of 54.46 mg g(-1). The undeniable advantages of the MnP adsorbent such as inexpensive preparation method, good adsorption capacity and easy separation using an external magnetic field, recommend it as a promising candidate for the removal of anionic dyes from polluted water. PMID:24647189

  15. Effect of BaTiO3 Nanopowder Concentration on Rheological Behaviour of Ceramic Inkjet Inks

    NASA Astrophysics Data System (ADS)

    Kyrpal, R.; Dulina, I.; Ragulya, A.

    2015-04-01

    The relationship between rheological properties of ceramic inkjet inks based on BaTiO3 nanopowder and solid phase concentration has been investigated. In the ink volume takes place the formation periodic colloidal structures (PCS). The determining factor of structure formation is powder-dispersant ratio. Structural constitution of in the system with the low pigment concentration represented as PCS2, that contains solid particles in deflocculated that stabilized by the presence of adsorption-solvate layers. Dilatant structure formation for such inks explained by constrained conditions of the interaction. Samples with high BaTiO3 concentration have been classified as PKS1. Dilatant properties of the PKS1 resulted in particles rearrangement under the influence of the flow. In the region of some values powder-dispersant ratio take place conversation PKS2 to PKS1 and ink structure transformation from monodisperse to aggregate state.

  16. Acoustic Properties of Polyurethane Composition Reinforced with Carbon Nanotubes and Silicon Oxide Nano-powder

    NASA Astrophysics Data System (ADS)

    Orfali, Wasim A.

    This article demonstrates the acoustic properties of added small amount of carbon-nanotube and siliconoxide nano powder (S-type, P-Type) to the host material polyurethane composition. By adding CNT and/or nano-silica in the form of powder at different concentrations up to 2% within the PU composition to improve the sound absorption were investigated in the frequency range up to 1600 Hz. Sound transmission loss measurement of the samples were determined using large impedance tube. The tests showed that addition of 0.2 wt.% Silicon Oxide Nano-powder and 0.35 wt.% carbon nanotube to polyurethane composition improved sound transmissions loss (Sound Absorption) up to 80 dB than that of pure polyurethane foam sample.

  17. Preparation, structural and optical characterization of ZnO, ZnO: Al nanopowder

    SciTech Connect

    Mohan, R. Raj; Rajendran, K.; Sambath, K.

    2014-01-28

    In this paper, ZnO and ZnO:Al nanopowders have been synthesized by low cost hydrothermal method. Zinc nitrate, hexamethylenetetramine (HMT) and aluminium nitrate are used as precursors for ZnO and AZO with different molar ratios. The structural and optical characterization of doped and un-doped ZnO powders have been investigated by X-ray diffraction (XRD), Scanning electron microscopy (SEM), Energy dispersive X-ray spectroscopy (EDAX), photoluminescence (PL) and ultra violet visible (UV-Vis) absorption studies. The SEM results show that the hydrothermal synthesis can be used to obtain nanoparticles with different morphology. It is observed that the grain size of the AZO nanoparticles increased with increasing of Al concentration. The PL measurement of AZO shows that broad range of green emission around 550nm with high intensity. The green emission resulted mainly because of intrinsic defects.

  18. Molten salt synthesis and localized surface plasmon resonance study of vanadium dioxide nanopowders

    SciTech Connect

    Wang Fu; Liu Yun; Liu Chunyan

    2009-12-15

    Rutile-type vanadium dioxide nanopowders with four different sizes were successfully synthesized by carbothermal reducing V{sub 2}O{sub 5} in KCl-LiCl molten salt. XRD and TEM characterizations suggested that vanadium dioxide particles formed by a broken and reunited process of vanadium oxide. Molten salt and organic carbon sources are crucial to the size of final particles. In the presence of the molten salt, the organic carbon with a shorter chain length would induce smaller particles. The UV-VIS-IR spectral measurements for as-prepared vanadium dioxide announced an obvious localized surface plasmon resonance band in the near infrared region at 90 deg. C. - Graphical abstract: Schematic illustration of the formation mechanism of VO{sub 2}(M) nanoparticles in molten salt, particles size can be controlled by choosing organic carbon sources with different chain length.

  19. Green approach for the synthesis and characterization of ZrSnO4 nanopowder

    NASA Astrophysics Data System (ADS)

    Athar, Taimur; Vishwakarma, Sandeep Kumar; Bardia, Avinash; Alabass, Razzaq; Alqarlosy, Ahmed; Khan, Aleem Ahmed

    2016-06-01

    Well-defined structural framework of ZrSnO4 nanopowder has been synthesized for the fabrications of cost-effective and sensitive devices which give final reproducible result with reliability under ideal conditions. The synthesis was carried out at moderate temperature and then finally dried in the laboratory oven and then followed with calcination at 1000 °C for 4 h to get phase selective product. It was observed that gelation time depends on the concentration of reactants and temperature. The characterization of ZrSnO4 was carried out with XRD, SEM, TEM, UV, thermal analysis, DLS and FT-IR techniques. With adjustment of reaction parameters, the systematic tuning of the particle size, shape and functional properties can be controlled. It was concluded that self-assembly is an integral part for the synthesis and opens a new exciting opportunity for better understanding the formation of nanostructure framework from micro- to nanoscale along with mechanistic via wet chemical approach. ZrSnO4 has vital role in identifying its potential cytotoxicity in the biological systems. The cytotoxicity effects of ZrSnO4 nanopowder in vitro were evaluated in three different human cell types (hepatocytes, mesenchymal stem cells and neuronal cells). Acute exposure of nanoparticles was found to have greater cytotoxic effect at higher concentration (30 µg/ml). However, partial detoxification was observed during nanoparticles exposure at day 6. The study concluded that an initial stress from nanoparticles incorporates sealing or detoxification of nanoparticles which may help to recover cell viability.

  20. Physicochemical and sensory properties of milk supplemented with dispersible nanopowdered oyster shell during storage.

    PubMed

    Lee, Y K; Ahn, S I; Chang, Y H; Kwak, H S

    2015-09-01

    The current study was carried out to investigate the dispersibility of powdered oyster shell (POS), nanopowdered oyster shell (NPOS), and Zn-activated nanopowdered oyster shell (Zn-NPOS) in milk and to determine effects of adding oyster shell on the physicochemical and sensory properties of milk during storage at 4°C for 16 d. To ensure dispersibility, 10% (wt/vol) oyster shell was added to distilled water and stirred at 800 rpm for 2 h, and then the emulsifier 0.5% polyglycerol monostearate (PGMS) was added and stirred continually for 24 h. The particle sizes of POS, NPOS, and Zn-NPOS were 180μm, 389 nm, and 257 nm, respectively. The pH values of all milk samples ranged from 6.62 to 6.88 during storage, and the zeta-potential of milks with NPOS and Zn-NPOS added were more stable than that of milk with POS in low concentrations (0.5 and 1.0%, vol/vol) during storage. The L and a color values of the milks were not significantly influenced by treatment; however, the b value (yellow-blue color) significantly increased during storage after adding POS, NPOS, or Zn-NPOS. Sensory analysis revealed that sedimentation score significantly increased with POS-supplemented milk, but the NPOS- and Zn-NPOS-supplemented milks did not show sedimentation until after 8 d of storage. Based on the data obtained, we conclude that dispersible nanosized oyster shell at concentrations of 0.5 and 1.0% (vol/vol) could be supplemented to milk without significant adverse effects on physicochemical and sensory properties. PMID:26162797

  1. Combustion synthesis, characterization and Raman studies of ZnO nanopowders

    NASA Astrophysics Data System (ADS)

    Reddy, A. Jagannatha; Kokila, M. K.; Nagabhushana, H.; Rao, J. L.; Shivakumara, C.; Nagabhushana, B. M.; Chakradhar, R. P. S.

    2011-10-01

    Spherical shaped ZnO nanopowders (14-50 nm) were synthesized by a low temperature solution combustion method in a short time <5 min. Rietveld analysis show that ZnO has hexagonal wurtzite structure with lattice constants a = 3.2511(1) Å, c = 5.2076(2) Å, unit cell volume ( V) = 47.66(5) (Å) 3 and belongs to space group P63mc. SEM micrographs reveal that the particles are spherical in shape and the powders contained several voids and pores. TEM results also confirm spherical shape, with average particle size of 14-50 nm. The values are consistent with the grain sizes measured from Scherrer's method and Williamson-Hall (W-H) plots. A broad UV-vis absorption spectrum was observed at ˜375 nm which is a characteristic band for the wurtzite hexagonal pure ZnO. The optical energy band gap of 3.24 eV was observed for nanopowder which is slightly lower than that of the bulk ZnO (3.37 eV). The observed Raman peaks at 438 and 588 cm -1 were attributed to the E 2 (high) and E 1 (LO) modes respectively. The broad band at 564 cm -1 is due to disorder-activated Raman scattering for the A 1 mode. These bands are associated with the first-order Raman active modes of the ZnO phase. The weak bands observed in the range 750-1000 cm -1 are due to small defects.

  2. Novel doped hydroxyapatite thin films obtained by pulsed laser deposition

    NASA Astrophysics Data System (ADS)

    Duta, L.; Oktar, F. N.; Stan, G. E.; Popescu-Pelin, G.; Serban, N.; Luculescu, C.; Mihailescu, I. N.

    2013-01-01

    We report on the synthesis of novel ovine and bovine derived hydroxyapatite thin films on titanium substrates by pulsed laser deposition for a new generation of implants. The calcination treatment applied to produce the hydroxyapatite powders from ovine/bovine bones was intended to induce crystallization and to prohibit the transmission of diseases. The deposited films were characterized by scanning electron microscopy, X-ray diffraction, Fourier transform infrared spectroscopy, and energy dispersive X-ray spectroscopy. Pull-off adherence and profilometry measurements were also carried out. X-ray diffraction ascertained the polycrystalline hydroxyapatite nature of the powders and films. Fourier transform infrared spectroscopy evidenced the vibrational bands characteristic to a hydroxyapatite material slightly carbonated. The micrographs of the films showed a uniform distribution of spheroidal particulates with a mean diameter of ∼2 μm. Pull-off measurements demonstrated excellent bonding strength values between the hydroxyapatite films and the titanium substrates. Because of their physical-chemical properties and low cost fabrication from renewable resources, we think that these new coating materials could be considered as a prospective competitor to synthetic hydroxyapatite used for implantology applications.

  3. In situ deposition of hydroxyapatite on graphene nanosheets

    SciTech Connect

    Neelgund, Gururaj M.; Oki, Aderemi; Luo, Zhiping

    2013-02-15

    Graphical abstract: A facile chemical precipitation method is reported for effective in situ deposition of hydroxyapatite on graphene nanosheets. Prior to grafting of hydroxyapatite, chemically modified graphene nanosheets were obtained by the reduction of graphene oxide in presence of ethylenediamine. Display Omitted Highlights: ► It is a facile and effective method for deposition of HA on GR nanosheets. ► It avoids the use of harmful reducing agents like hydrazine, NaBH{sub 4} etc. ► GR nanosheets were produced using bio-compatible, ethylenediamine. ► The graphitic structure of synthesized GR nanosheets was high ordered. ► The ratio of Ca to P in HA was 1.64, which is close to ratio in natural bone. -- Abstract: Graphene nanosheets were effectively functionalized by in situ deposition of hydroxyapatite through a facile chemical precipitation method. Prior to grafting of hydroxyapatite, chemically modified graphene nanosheets were obtained by the reduction of graphene oxide in presence of ethylenediamine. The resulting hydroxyapatite functionalized graphene nanosheets were characterized by attenuated total reflection IR spectroscopy, X-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy, X-ray energy dispersive spectroscopy, Raman spectroscopy and thermogravimetric analysis. These characterization techniques revealed the successful grafting of hydroxyapatite over well exfoliated graphene nanosheets without destroying their structure.

  4. Suspension thermal spraying of hydroxyapatite: microstructure and in vitro behaviour.

    PubMed

    Bolelli, Giovanni; Bellucci, Devis; Cannillo, Valeria; Lusvarghi, Luca; Sola, Antonella; Stiegler, Nico; Müller, Philipp; Killinger, Andreas; Gadow, Rainer; Altomare, Lina; De Nardo, Luigi

    2014-01-01

    In cementless fixation of metallic prostheses, bony ingrowth onto the implant surface is often promoted by osteoconductive plasma-sprayed hydroxyapatite coatings. The present work explores the use of the innovative High Velocity Suspension Flame Spraying (HVSFS) process to coat Ti substrates with thin homogeneous hydroxyapatite coatings. The HVSFS hydroxyapatite coatings studied were dense, 27-37μm thick, with some transverse microcracks. Lamellae were sintered together and nearly unidentifiable, unlike conventional plasma-sprayed hydroxyapatite. Crystallinities of 10%-70% were obtained, depending on the deposition parameters and the use of a TiO2 bond coat. The average hardness of layers with low (<24%) and high (70%) crystallinity was ≈3.5GPa and ≈4.5GPa respectively. The distributions of hardness values, all characterised by Weibull modulus in the 5-7 range, were narrower than that of conventional plasma-sprayed hydroxyapatite, with a Weibull modulus of ≈3.3. During soaking in simulated body fluid, glassy coatings were progressively resorbed and replaced by a new, precipitated hydroxyapatite layer, whereas coatings with 70% crystallinity were stable up to 14days of immersion. The interpretation of the precipitation behaviour was also assisted by surface charge assessments, performed through Z-potential measurements. During in vitro tests, HA coatings showed no cytotoxicity towards the SAOS-2 osteoblast cell line, and surface cell proliferation was comparable with proliferation on reference polystyrene culture plates. PMID:24268261

  5. Adhesion behaviors of Escherichia coli on hydroxyapatite.

    PubMed

    Kamitakahara, Masanobu; Takahashi, Shohei; Yokoi, Taishi; Inoue, Chihiro; Ioku, Koji

    2016-04-01

    Optimum design of support materials for microorganisms is required for the construction of bioreactors. However, the effects of support materials on microorganisms are still unclear. In this study, we investigated the adhesion behavior of Escherichia coli (E. coli) on hydroxyapatite (HA), polyurethane (PU), poly(vinyl chloride) (PVC), and carbon (Carbon) to obtain basic knowledge for the design of support materials. The total metabolic activity and number of E. coli adhering on the samples followed the order of HA ≈ Carbon>PVC>PU. On the other hand, the water contact angle of the pellet surfaces followed the order of HA

  6. First principles study of hydroxyapatite surface.

    PubMed

    Slepko, Alexander; Demkov, Alexander A

    2013-07-28

    The biomineral hydroxyapatite (HA) [Ca10(PO4)6(OH)2] is the main mineral constituent of mammal bone. We report a theoretical investigation of the HA surface. We identify the low energy surface orientations and stoichiometry under a variety of chemical environments. The surface most stable in the physiologically relevant OH-rich environment is the OH-terminated (1000) surface. We calculate the work function of HA and relate it to the surface composition. For the lowest energy OH-terminated surface we find the work function of 5.1 eV, in close agreement with the experimentally reported range of 4.7 eV-5.1 eV [V. S. Bystrov, E. Paramonova, Y. Dekhtyar, A. Katashev, A. Karlov, N. Polyaka, A. V. Bystrova, A. Patmalnieks, and A. L. Kholkin, J. Phys.: Condens. Matter 23, 065302 (2011)]. PMID:23902010

  7. Novel method of preparing hydroxyapatite foams.

    PubMed

    Muthutantri, Anushini; Huang, Jie; Edirisinghe, Mohan

    2008-04-01

    Porous scaffolds are considered a key strategy in the concept of bone tissue engineering. Hydroxyapatite, which is a bioceramic has been used as a popular scaffold material due to its bioactive and osteoconductive properties. A combination of slurry-dipping and electrospraying has been used as a new foam fabrication method to produce porous and interconnected foam structures. The combined method has shown to overcome the shortcomings of the individual methods and it has produced open pores in the desired range of 100-350 microm. The porosity which was determined by calculation and microtomography was between 84% and 88%. Reduced cracks and thicker struts were observed in the microstructure, pointing to improved mechanical properties. PMID:18214644

  8. Hydroxyapatite deposition disease of the joint.

    PubMed

    Molloy, Eamonn S; McCarthy, Geraldine M

    2003-06-01

    Basic calcium phosphate (BCP) crystals include partially carbonate-substituted hydroxyapatite, octacalcium phosphate, and tricalcium phosphate. They may form deposits, which are frequently asymptomatic but may give rise to a number of clinical syndromes including calcific periarthritis, Milwaukee shoulder syndrome, and osteoarthritis, in and around joints. Recent data suggest that magnesium whitlockite, another form of BCP, may play a pathologic role in arthritis. Data from the past year have provided further understanding of the mechanisms by which BCP crystals induce inflammation and degeneration. There remains no specific treatment to modify the effects of BCP crystals. Although potential drugs are being identified as the complex pathophysiology of BCP crystals is unraveled, much work remains to be done in order to translate research advances to date into tangible clinical benefits. PMID:12744814

  9. Mechanism of incorporation of zinc into hydroxyapatite.

    PubMed

    Matsunaga, Katsuyuki; Murata, Hidenobu; Mizoguchi, Teruyasu; Nakahira, Atsushi

    2010-06-01

    The atomic level mechanism of incorporation of Zn(2+) into hydroxyapatite (HAp), which is a potential dopant to promote bone formation, was investigated, based on first principles total energy calculations and experimental X-ray absorption near edge structure (XANES) analyses. It was found that Zn(2+)-doped HAp tends to have a Ca-deficient chemical composition and substitutional Zn(2+) ions are associated with a defect complex with a Ca(2+) vacancy and two charge compensating protons. Moreover, first principles calculations demonstrated that Zn(2+) incorporation into HAp can take place by occupying the Ca(2+) vacancy of the defect complex. The Ca(2+) vacancy complex is not only the origin of the calcium deficiency in HAp, but also plays a key role in the uptake of trace elements during mineralization. PMID:19944784

  10. Effect of hydroxyapatite microcrystals on macrophage activity.

    PubMed

    Fukuchi, N; Akao, M; Sato, A

    1995-01-01

    Hydroxyapatite (HAp) microcrystals were synthesized by a neutralization reaction of Ca(OH)2 suspension and H3PO4 solution using an ultrasonic homogenizer. The in vitro interaction of HAp microcrystals with rat peritoneal macrophages was investigated by measuring the viability, acid phosphatase (ACP) activity, lactate dehydrogenase (LDH) activity and intracellular calcium content. HAp calcined at 800 degrees C and alpha-alumina particles (alumina) were used as comparative materials. Macrophages actively phagocytosed HAp microcrystals by dissolving them. However, no damage in macrophages exposed to HAp microcrystals was observed by transmission electron microscopy. Macrophages in the presence of HAp microcrystals showed less ACP and LDH activity and higher intracellular calcium content than those in the presence of calcined HAp and alumina. HAp microcrystals had excellent biocompatibility to macrophages as well as sintered HAp. PMID:8785507

  11. Thermal Diffusivity in Bone and Hydroxyapatite

    NASA Astrophysics Data System (ADS)

    Calderón, A.; Peña Rodríguez, G.; Muñoz Hernández, R. A.; Díaz Gongora, J. A. I.; Mejia Barradas, C. M.

    2004-09-01

    We report thermal diffusivity measurements in bull bone and commercial hydroxyapatite (HA), both in powder form, in order to determinate the thermal compatibility between these materials. Besides this, we report a comparison between these measured values and those of metallic samples frequently used in implants, as high purity titanium and stainless steel. Our results show a good thermal compatibility (74%) between HA and bone, both in powder form. Finally, it was obtained a one order of magnitude difference between the thermal diffusivity values of metallic samples and those corresponding values to bone and HA being this difference greater in titanium than in stainless steel, which is important to consider in some biomedical and dental applications.

  12. The Adsorption of Polyelectrolytes on Hydroxyapatite Crystals.

    PubMed

    Tsortos; Nancollas

    1999-01-01

    The adsorption of two polyelectrolytes, poly-L-Glutamate and poly-L-Aspartate, on hydroxyapatite (HAP) crystals was studied both experimentally and theoretically. Langmuir adsorption isotherms were obtained for both these molecules, with binding constants K = 6 x 10(6) and 3 x 10(6) M-1, respectively, at 37.0 degreesC, pH 7.4, and 0.15 M ionic strength. A theoretical analysis of the data, based on a model proposed by Hesselink, suggested a "train-loop" type of adsorption with non-electrostatic energy terms 3.51 and 4.76 (kT) for poly-L-Glu and poly-L-Asp, respectively. Copyright 1999 Academic Press. PMID:9878142

  13. Fluoride removal performance of glass derived hydroxyapatite

    SciTech Connect

    Liang, Wen; Zhan, Lei; Piao, Longhua; Russel, Christian

    2011-02-15

    Research highlights: {yields} Novel sodium calcium borate glass derived hydroxyapatite (G-HAP) is prepared. {yields} Micro-G-HAP adsorbs F{sup -} ions in solutions more effectively than commercial nano-HAP. {yields} The adsorption kinetics and isotherms are well fitted by a second order kinetic model and Freundlich isotherm model. -- Abstract: A novel sodium calcium borate glass derived hydroxyapatite (G-HAP) with different ranges of particle size was prepared by immersion sodium calcium borate glass in 0.1 M K{sub 2}HPO{sub 4} solution by the ratio of 50 g L{sup -1} for 7 days. The unique advantage of G-HAP for the adsorption of fluoride ions in solutions was studied. The effects of size and quantity of particles, pH value and adsorption time on adsorption performance were investigated. The maximum adsorption capacity was 17.34 mg g{sup -1} if 5 g L{sup -1}, <100 {mu}m G-HAP was added to a solution with an initial pH value of 6.72 and the adsorption time was 12 h. The results showed that the micro-G-HAP could immobilize F{sup -} in solution more effectively than commercial nano-HAP, which makes potential application of the G-HAP in removing the fluoride ions from wastewater. The adsorption kinetics and isotherms for F{sup -} could be well fitted by a second order kinetic model and Freundlich isotherm model respectively, which could be used to describe the adsorption behavior. The mechanism of G-HAP in immobilizing F{sup -} from aqueous solutions was investigated by the X-ray diffraction (XRD), infrared spectra (IR) and scanning electron microscopy (SEM).

  14. Synthesis of Spongy-Like Mesoporous Hydroxyapatite from Raw Waste Eggshells for Enhanced Dissolution of Ibuprofen Loaded via Supercritical CO2

    PubMed Central

    Ibrahim, Abdul-Rauf; Li, Xiangyun; Zhou, Yulan; Huang, Yan; Chen, Wenwen; Wang, Hongtao; Li, Jun

    2015-01-01

    The use of cheaper and recyclable biomaterials (like eggshells) to synthesize high purity hydroxyapatite (HAp) with better properties (small particle size, large surface area and pore volume) for applications (in environmental remediation, bone augmentation and replacement, and drug delivery systems) is vital since high-purity synthetic calcium sources are expensive. In this work, pure and mesoporous HAp nanopowder with large pore volume (1.4 cm3/g) and surface area (284.1 m2/g) was produced from raw eggshells at room temperature using a simple two-step procedure. The control of precursor droplets could stabilize the pH value of the reaction solution, because of the size of the needle (of the syringe pump used for precursor additions) leading to production of HAp with high surface area and pore size. The as-produced HAp revealed high ibuprofen (as a model drug) loading (1.38 g/g HAp), enhanced dissolution and controllable release of the drug via solute-saturated supercritical carbon dioxide. PMID:25860950

  15. Polymer complex solution synthesis of (Y xGd 1- x) 2O 3:Eu 3+ nanopowders

    NASA Astrophysics Data System (ADS)

    Andrić, Ž.; Dramićanin, M. D.; Mitrić, M.; Jokanović, V.; Bessière, A.; Viana, B.

    2008-03-01

    Yttrium-gadolinium-europium oxide phosphors are regarded promising for many important optical applications, for example in computed tomography medical imaging and plasma displays. In this work, we investigated procedure for (Y xGd 1- x) 2O 3:Eu 3+ ( x = 0, 0.25, 0.5, 0.75 and 1) nanopowder synthesis using polymer complex solution method (PCS) based on polyethylene glycol fuel (PEG). Structural and emission properties of nanopowders are investigated by X-ray diffraction, electron microscopy and photoluminescence measurements. We obtained particles of about 40 nm having excellent structural ordering in cubic bixbyte type of structure - space group Ia3 for all mixed oxide compositions. Luminescence emission measurements exposed characteristic transition of the trivalent europium ion incorporated into insulating host. 5D 1 and 5D 0 decay time values are measured to obtain information on different kinetic processes occurring for these two emitting levels.

  16. Application of neural network technique to planetary milling process for the production of ZnO nanopowders

    NASA Astrophysics Data System (ADS)

    Lemine, O. M.; Hiazaa, A. F.; Louly, M. A.; Al-Ahmari, A. M.

    2011-10-01

    An artificial-neural-network (ANN) model was developed to estimate the crystalline size of ZnO nanopowder as a function on the planetary milling parameters such as balls to powder ratio and rotation speed. This nanopowder was synthesized by mechanical milling and the required data for training were collected from the experimental results. The synthesized ZnO nanoparticles are characterized by X-ray diffraction (XRD). It was found that artificial neural network was very effective providing a perfect agreement between the outcomes of ANN modeling and experimental results. An optimization model is then developed to find the best milling parameters (rotation speed and balls to powder ratio) producing the minimal average crystalline size.

  17. Electrical and optical properties of SrTiO3 nanopowders: Effect of different dopants Ba and Ag

    NASA Astrophysics Data System (ADS)

    Ghasemifard, Mahdi; Ghamari, Misagh; Iziy, Meysam

    2016-05-01

    Using strontium-titanium salts precursor, nanopowders (STO-based-NPs) were successfully synthesized by controlled gel-combustion method. Citric and nitric acids in an optimum ratio were used as the fuel and oxidizer agents, respectively. After heat treatment at 850∘C, the crystalline structure of the products was investigated by X-ray diffraction. The effects of Ba and Ag dopants on particle size distribution were discussed by transmission electron microscopy (TEM). The optical and dielectric parameters such as energy band gap (Eg), real and imaginary parts of refractive index, dielectric function and energy loss function of nanopowders have been investigated by UV-Vis and FTIR spectra. The band gap of SrTiO3 increased with increasing Ba, Ag and Ba-Ag. Different atomic radii of dopants are responsible for changing optical and dielectric parameters due to the altered orbital configuration of the lattice structure.

  18. Ammonia sensing properties of V-doped ZnO:Ca nanopowders prepared by sol–gel synthesis

    SciTech Connect

    Fazio, E.; Hjiri, M.; Dhahri, R.; El Mir, L.; Sabatino, G.; Barreca, F.; Neri, F.; Leonardi, S.G.; Pistone, A.; Neri, G.

    2015-03-15

    V-doped ZnO:Ca nanopowders with different V loading were prepared by sol–gel synthesis and successive drying in ethanol under supercritical conditions. Characterization data of nanopowders annealed at 700 °C in air, revealed that they have the wurtzite structure. Raman features of V-doped ZnO:Ca samples were found to be substantially modified with respect to pure ZnO or binary ZnO:Ca samples, which indicate the substitution of vanadium ions in the ZnO lattice. The ammonia sensing properties of V-doped ZnO:Ca thick films were also investigated. The results obtained demonstrate the possibility of a fine tuning of the sensing characteristics of ZnO-based sensors by Ca and V doping. In particular, their combined effect has brought to an enhanced response towards NH{sub 3} compared to bare ZnO and binary V-ZnO and Ca-ZnO samples. Raman investigation suggested that the presence of Ca play a key role in enhancing the sensor response in these ternary composite nanomaterials. - Graphical abstract: V-doped ZnO:Ca nanopowders prepared by sol–gel synthesis possess enhanced sensing characteristics towards NH{sub 3} compared to bare ZnO. - Highlights: • V-doped ZnO:Ca nanopowders with different V loading were prepared by sol–gel synthesis. • Raman features of V-doped ZnO:Ca samples indicate the substitution of V ions in the ZnO lattice. • Combined effects of dopants have brought to an enhanced response to NH{sub 3} compared to ZnO. • Ca play a key role in enhancing the sensor response of ternary V-doped ZnO:Ca composites.

  19. Synthesis of nanostructured framework of novel ZnBaO2 nanopowder via wet chemical approach and hepatocytotoxicity response

    NASA Astrophysics Data System (ADS)

    Athar, Taimur; Vishwakarma, Sandeep Kumar; Alabass, Razzaq; Alqaralosy, Ahmed; Khan, Aleem Ahmed

    2016-08-01

    Wet synthetic process is an effective and facile method at low cost, environmentally benign process for easy scaling-up and then used for fabrication of multi-utility devices. Self-assembling of nanobrick leads to architecture framework with new functional properties which help to make its vast applications as nanodevices with their intrinsic shape, size and functional properties. The bimetallic oxide nanostructure with phase structure was characterized by FTIR, UV-visible electronic absorption, XRD, thermal studies, SEM, TEM, DLS and fluorescence. Nanocrystalline ZnBaO2 powder can be used due to its chemical stability and excellent transmission in the visible region. It was observed that the annealing rate plays an important role to redefine the structural and other physicochemical properties which finally help to change gel into crystalline functional properties with porosity. Wet chemical approach can be used for the synthesis of other metal oxide nanopowders which can be easily scale up for production level. Along with synthesis and characterization, we also assessed biological responses of human hepatocytes exposed to ZnBaO2 nanopowder. Cell membrane permeability and ammonia detoxification were investigated against various concentrations of nanoparticles on in vitro cultured hepatocytes. Our results suggest that low concentrations (<40 μg/ml) of ZnBaO2 nanopowder have no cytotoxic effect on hepatocytes viability, proliferation and detoxification, whereas concentrations above 40 μg/ml depict significant toxicity on cells.

  20. Synthesis of nanostructured framework of novel ZnBaO2 nanopowder via wet chemical approach and hepatocytotoxicity response

    NASA Astrophysics Data System (ADS)

    Athar, Taimur; Vishwakarma, Sandeep Kumar; Alabass, Razzaq; Alqaralosy, Ahmed; Khan, Aleem Ahmed

    2015-09-01

    Wet synthetic process is an effective and facile method at low cost, environmentally benign process for easy scaling-up and then used for fabrication of multi-utility devices. Self-assembling of nanobrick leads to architecture framework with new functional properties which help to make its vast applications as nanodevices with their intrinsic shape, size and functional properties. The bimetallic oxide nanostructure with phase structure was characterized by FTIR, UV-visible electronic absorption, XRD, thermal studies, SEM, TEM, DLS and fluorescence. Nanocrystalline ZnBaO2 powder can be used due to its chemical stability and excellent transmission in the visible region. It was observed that the annealing rate plays an important role to redefine the structural and other physicochemical properties which finally help to change gel into crystalline functional properties with porosity. Wet chemical approach can be used for the synthesis of other metal oxide nanopowders which can be easily scale up for production level. Along with synthesis and characterization, we also assessed biological responses of human hepatocytes exposed to ZnBaO2 nanopowder. Cell membrane permeability and ammonia detoxification were investigated against various concentrations of nanoparticles on in vitro cultured hepatocytes. Our results suggest that low concentrations (<40 μg/ml) of ZnBaO2 nanopowder have no cytotoxic effect on hepatocytes viability, proliferation and detoxification, whereas concentrations above 40 μg/ml depict significant toxicity on cells.

  1. ZnO nanopowder induced light scattering for improved visualization of emission sites in carbon nanotube films and arrays.

    PubMed

    Mesko, Marcel; Ou, Qiongrong; Matsuda, Takafumi; Ishikawa, Tomokazu; Veis, Martin; Antos, Roman; Ogino, Akihisa; Nagatsu, Masaaki

    2009-06-24

    We report on ZnO nanopowder induced light scattering for improved visualization of emission sites in carbon nanotube films and arrays. We observed a significant reduction of the internal multiple light scattering phenomena, which are characteristic for ZnO micropowders. The microsized grains of the commercially available ZnO:Zn (P 15) were reduced to the nanometre scale by pulsed laser ablation at an oxygen ambient pressure of 10 kPa. Our investigations show no crystalline change and no shift of the broad green emission peak at 500 nm for the ZnO nanopowder. For the application in field emission displays, we demonstrate the possibility of achieving cathodoluminescence with a fine pitch size of 100 microm of the patterned pixels without requiring additional electron beam focusing and without a black matrix. Moreover, the presented results show the feasibility of employing ZnO nanopowder as a detection material for the phosphorus screen method, which is able to localize emission sites of carbon nanotube films and arrays with an accuracy comparable to scanning anode field emission microscopy. PMID:19487805

  2. ZnO nanopowder induced light scattering for improved visualization of emission sites in carbon nanotube films and arrays

    NASA Astrophysics Data System (ADS)

    Meško, Marcel; Ou, Qiongrong; Matsuda, Takafumi; Ishikawa, Tomokazu; Veis, Martin; Antoš, Roman; Ogino, Akihisa; Nagatsu, Masaaki

    2009-06-01

    We report on ZnO nanopowder induced light scattering for improved visualization of emission sites in carbon nanotube films and arrays. We observed a significant reduction of the internal multiple light scattering phenomena, which are characteristic for ZnO micropowders. The microsized grains of the commercially available ZnO:Zn (P 15) were reduced to the nanometre scale by pulsed laser ablation at an oxygen ambient pressure of 10 kPa. Our investigations show no crystalline change and no shift of the broad green emission peak at 500 nm for the ZnO nanopowder. For the application in field emission displays, we demonstrate the possibility of achieving cathodoluminescence with a fine pitch size of 100 µm of the patterned pixels without requiring additional electron beam focusing and without a black matrix. Moreover, the presented results show the feasibility of employing ZnO nanopowder as a detection material for the phosphorus screen method, which is able to localize emission sites of carbon nanotube films and arrays with an accuracy comparable to scanning anode field emission microscopy.

  3. Preparation of Porous Hydroxyapatite Tablets and Porous Hydroxyapatite Coatings for Orthopaedic Use

    NASA Astrophysics Data System (ADS)

    Méndez-González, M.

    2004-09-01

    Porous hydroxyapatite tablets and coatings on metal substrates were obtained by the addition of polymeric additives and liofilization. Both tablets and coatings were characterized by scanning electron microscopy and x-ray diffraction. Coatings obtained by plasma spraying also exhibited interconnected porous of 100 μm while coatings obtained by laser ablation did not show any porosity. The diffraction patterns of the deposited HA were similar to that of the powder obtained by the precipitation method suggesting that no significant changes occurred during the coating procedure.

  4. Selective recovery of pure copper nanopowder from indium-tin-oxide etching wastewater by various wet chemical reduction process: Understanding their chemistry and comparisons of sustainable valorization processes.

    PubMed

    Swain, Basudev; Mishra, Chinmayee; Hong, Hyun Seon; Cho, Sung-Soo

    2016-05-01

    Sustainable valorization processes for selective recovery of pure copper nanopowder from Indium-Tin-Oxide (ITO) etching wastewater by various wet chemical reduction processes, their chemistry has been investigated and compared. After the indium recovery by solvent extraction from ITO etching wastewater, the same is also an environmental challenge, needs to be treated before disposal. After the indium recovery, ITO etching wastewater contains 6.11kg/m(3) of copper and 1.35kg/m(3) of aluminum, pH of the solution is very low converging to 0 and contain a significant amount of chlorine in the media. In this study, pure copper nanopowder was recovered using various reducing reagents by wet chemical reduction and characterized. Different reducing agents like a metallic, an inorganic acid and an organic acid were used to understand reduction behavior of copper in the presence of aluminum in a strong chloride medium of the ITO etching wastewater. The effect of a polymer surfactant Polyvinylpyrrolidone (PVP), which was included to prevent aggregation, to provide dispersion stability and control the size of copper nanopowder was investigated and compared. The developed copper nanopowder recovery techniques are techno-economical feasible processes for commercial production of copper nanopowder in the range of 100-500nm size from the reported facilities through a one-pot synthesis. By all the process reported pure copper nanopowder can be recovered with>99% efficiency. After the copper recovery, copper concentration in the wastewater reduced to acceptable limit recommended by WHO for wastewater disposal. The process is not only beneficial for recycling of copper, but also helps to address environment challenged posed by ITO etching wastewater. From a complex wastewater, synthesis of pure copper nanopowder using various wet chemical reduction route and their comparison is the novelty of this recovery process. PMID:26918838

  5. Electrokinetic properties of hydroxyapatite under flotation conditions.

    PubMed

    Vucinić, Dusica R; Radulović, Dragan S; Deusić, Slaven D

    2010-03-01

    The effect of calcite supernatant, calcium, and carbonate ions on the hydroxyapatite (HA) zeta potential without and in the presence of sodium oleate (1x10(-4) mol L(-1)) was examined within the pH range from 4 to 12. The interpretation of results was based on the HA surface and oleate solution chemistry, and on some floatability tests. HA, with different positive and negative surface sites formed depending on its solubility and pH, had a negative zeta potential over the whole pH range. This mineral is not naturally floatable (flotation recovery, 5%9.3. The HA surface is less negatively charged in calcite supernatant than in water from pH 6.6 to 9.2 due to the adsorption on HA negative surface active centers ([triple bond]HPO(4)(-) and [triple bond]PO(4)(2-)) of the Ca(2+), and CaOH(+) ions (present in the calcite supernatant), producing more surface sites [triple bond]HPO(4)Ca(+), [triple bond]PO(4)Ca, [triple bond]HPO(4)CaOH, and [triple bond]PO(4)(-) CaOH, and new centers [triple bond]HPO(4)CaHCO(3) and [triple bond]PO(4)(-) CaHCO(3). In the presence of 1x10(-3) mol L(-1) CaCl(2), the HA sample has positive zeta potential, the same as calcite from the same deposit, up to IEP at pH 11.25. Carbonate ions (1x10(-3) mol L(-1) Na(2)CO(3)) do not affect the HA zeta potential. However, a possible process can be the ion-exchange reaction between

  6. Osteoinductive hydroxyapatite-coated titanium implants.

    PubMed

    Ripamonti, Ugo; Roden, Laura C; Renton, Louise F

    2012-05-01

    Previous studies have shown that heterotopic induction of bone formation by calcium phosphate-based macroporous constructs is set into motion by the geometry of the implanted substrata, i.e. a sequence of repetitive concavities assembled within the macroporous spaces. The aim of this study was to construct osteoinductive titanium implants that per se, and without the exogenous application of the osteogenic soluble molecular signals of the transforming growth factor-β supergene family, would initiate the induction of bone formation. To generate intrinsically osteoinductive titanium implants for translation in clinical contexts, titanium grade Ti-6A1-4V cylinders of 15 mm in length and 3.85 mm in diameter, with or without concavities, were plasma sprayed with crystalline hydroxyapatite resulting in a uniform layer of 30 μm in thickness. Before coating, experimental titanium implants were prepared with a sequence of 36 repetitive concavities 1600 μm in diameter and 800 μm in depth, spaced a distance of 1000 μm apart. Mandibular molars and premolars were extracted to prepare edentulous mandibular ridges for later implantation. Planar and geometric hydroxyapatite-coated titanium constructs were implanted in the left and right edentulized hemi-mandibles, respectively, after a healing period of 7-8 months, 3 per hemi-mandible. Three planar and three geometric implants were implanted in the left and right tibiae, respectively; additionally, planar and geometric constructs were also inserted in the rectus abdominis muscle. Six animals were euthanized at 30 and 90 days after implantation; one animal had to be euthanized 5 days after surgery and the remaining animal was euthanized 31 months after implantation. Undecalcified longitudinal sections were precision-sawed, ground and polished to 40-60 μm; all sections were stained with a modified Goldner's trichrome. Undecalcified specimen block preparation was performed using the EXAKT precision cutting and grinding system

  7. Nanostructured nickel-free austenitic stainless steel/hydroxyapatite composites.

    PubMed

    Tulinski, Maciej; Jurczyk, Mieczyslaw

    2012-11-01

    In this work Ni-free austenitic stainless steels with nanostructure and their nanocomposites with hydroxyapatite are presented and characterized by means of X-ray diffraction and optical profiling. The samples were synthesized by mechanical alloying, heat treatment and nitriding of elemental microcrystalline powders with addition of hydroxyapatite (HA). In our work we wanted to introduce into stainless steel hydroxyapatite ceramics that have been intensively studied for bone repair and replacement applications. Such applications were chosen because of their high biocompatibility and ability to bond to bone. Since nickel-free austenitic stainless steels seem to have better mechanical properties, corrosion resistance and biocompatibility compared to 316L stainless steels, it is possible that composite made of this steel and HA could improve properties, as well. Mechanical alloying and nitriding are very effective technologies to improve the corrosion resistance of stainless steel. Similar process in case of nanocomposites of stainless steel with hydroxyapatite helps achieve even better mechanical properties and corrosion resistance. Hence nanocrystalline nickel-free stainless steels and nickel-free stainless steel/hydroxyapatite nanocomposites could be promising bionanomaterials for use as a hard tissue replacement implants, e.g., orthopedic implants. In such application, the surface roughness and more specifically the surface topography influences the proliferation of cells (e.g., osteoblasts). PMID:23421285

  8. New Bismuth-Substituted Hydroxyapatite Nanoparticles for Bone Tissue Engineering

    NASA Astrophysics Data System (ADS)

    Ciobanu, Gabriela; Bargan, Ana Maria; Luca, Constantin

    2015-11-01

    New bismuth-substituted hydroxyapatite [Ca10- x Bi x (PO4)6(OH)2 where x = 0-2.5] nanoparticles were synthesized by the co-precipitation method from aqueous solutions. The structural properties of the samples were analyzed by scanning electron microscopy coupled with x-ray analysis, x-ray powder diffraction, x-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy and Brunauer-Emmett-Teller surface area analysis. The results confirm that bismuth ions have been incorporated into the hydroxyapatite lattice. The prepared nanocrystalline powders consisted of hydroxyapatite as single phase with hexagonal structure, crystal sizes smaller than 60 nm and (Bi + Ca)/P atomic ratio of around 1.67. The hydroxyapatite samples doped with Bi have mesoporous textures with pores size of around 2 nm and specific surface area in the range of 12-25 m2/g. The Bi-substituted hydroxyapatite powders are more effective against Gram-negative Escherichia coli bacteria than Gram-positive Staphylococcus aureus bacteria.

  9. A process for the development of strontium hydroxyapatite

    NASA Astrophysics Data System (ADS)

    Zahra, N.; Fayyaz, M.; Iqbal, W.; Irfan, M.; Alam, S.

    2014-06-01

    A procedure for the preparation of Strontium Hydroxyapatite is adapted to produce high purity and better homogeneity ceramic with good Crystallinity. The strontium substituted bone cement has potential for use in orthopedic surgeries. Ionic Strontium (Sr) in humans shares the same physiological pathway as calcium and can be deposited in the mineral structure of the bone. In the present study, a novel concept of preparing Sr-contained Hydroxyapatite bone cement by using a precipitation method is proposed to get an ideal biomaterial that possesses potential degradability and more excellent pharmacological effect. Chemical analysis, Fourier Transform Infra Red analysis and Thermogravimetric/ Differential Scanning Calorimetric studies were conducted on prepared Strontium Hydroxyapatite sample to characterize the incorporation of 15% Sr2+ into the crystal lattice of Hydroxyapatite. Strontium was quantitatively incorporated into Hydroxyapatite where its substitution for calcium provoked a linear shift of the infrared absorption bands of the hydroxyl and phosphate groups. Thus, the formation of Sr-HAp was confirmed by Chemical Analysis, FT-IR and TGA/DSC results.

  10. Cobalt doped proangiogenic hydroxyapatite for bone tissue engineering application.

    PubMed

    Kulanthaivel, Senthilguru; Roy, Bibhas; Agarwal, Tarun; Giri, Supratim; Pramanik, Krishna; Pal, Kunal; Ray, Sirsendu S; Maiti, Tapas K; Banerjee, Indranil

    2016-01-01

    The present study delineates the synthesis and characterization of cobalt doped proangiogenic-osteogenic hydroxyapatite. Hydroxyapatite samples, doped with varying concentrations of bivalent cobalt (Co(2+)) were prepared by the ammoniacal precipitation method and the extent of doping was measured by ICP-OES. The crystalline structure of the doped hydroxyapatite samples was confirmed by XRD and FTIR studies. Analysis pertaining to the effect of doped hydroxyapatite on cell cycle progression and proliferation of MG-63 cells revealed that the doping of cobalt supported the cell viability and proliferation up to a threshold limit. Furthermore, such level of doping also induced differentiation of the bone cells, which was evident from the higher expression of differentiation markers (Runx2 and Osterix) and better nodule formation (SEM study). Western blot analysis in conjugation with ELISA study confirmed that the doped HAp samples significantly increased the expression of HIF-1α and VEGF in MG-63 cells. The analysis described here confirms the proangiogenic-osteogenic properties of the cobalt doped hydroxyapatite and indicates its potential application in bone tissue engineering. PMID:26478356

  11. Nano-Hydroxyapatite Thick Film Gas Sensors

    NASA Astrophysics Data System (ADS)

    Khairnar, Rajendra S.; Mene, Ravindra U.; Munde, Shivaji G.; Mahabole, Megha P.

    2011-12-01

    In the present work pure and metal ions (Co and Fe) doped hydroxyapatite (HAp) thick films have been successfully utilized to improve the structural, morphological and gas sensing properties. Nanocrystalline HAp powder is synthesized by wet chemical precipitation route, and ion exchange process is employed for addition of Co and Fe ions in HAp matrix. Moreover, swift heavy ion irradiation (SHI) technique is used to modify the surface of pure and metal ion exchanged HAp with various ion fluence. The structural investigation of pure and metal ion exchanged HAp thick films are carried out using X-ray diffraction and the presence of functional group is observed by means FTIR spectroscopy. Furthermore, surface morphology is visualized by means of SEM and AFM analysis. CO gas sensing study is carried out for, pure and metal ions doped, HAp thick films with detail investigation on operating temperature, response/recovery time and gas uptake capacity. The surface modifications of sensor matrix by SHI enhance the gas response, response/recovery and gas uptake capacity. The significant observation is here to note that, addition of Co and Fe in HAp matrix and surface modification by SHI improves the sensing properties of HAp films drastically resulting in gas sensing at relatively lower temperatures.

  12. Dual functional selenium-substituted hydroxyapatite.

    PubMed

    Wang, Yanhua; Ma, Jun; Zhou, Lei; Chen, Jin; Liu, Yonghui; Qiu, Zhiye; Zhang, Shengmin

    2012-06-01

    Hydroxyapatite (HA) doped with trace elements has attracted much attention recently owing to its excellent biological functions. Herein, we use a facile co-precipitation method to incorporate selenium into HA by adding sodium selenite during synthesis. The obtained selenium-substituted HA products are needle-like nanoparticles which have  size and crystallinity that are similar to those of the pure HA nanoparticles (HANs) when the selenium content is low. HANs are found to have the ability to induce the apoptosis of osteosarcoma cells, and the anti-tumour effects are enhanced after incorporation of selenium. Meanwhile, the nanoparticles can also support the growth of bone marrow stem cells. Furthermore, the flow cytometric results indicate that the apoptosis induction of osteosarcoma cells is caused by the increased reactive oxygen species and decreased mitochondrial membrane potential. These results show that the selenium-substituted HANs are potentially promising bone graft materials in osteosarcoma treatment due to their dual functions of supporting normal cell growth and inducing tumour cell apoptosis. PMID:23741613

  13. Nano-Hydroxyapatite Thick Film Gas Sensors

    SciTech Connect

    Khairnar, Rajendra S.; Mene, Ravindra U.; Munde, Shivaji G.; Mahabole, Megha P.

    2011-12-10

    In the present work pure and metal ions (Co and Fe) doped hydroxyapatite (HAp) thick films have been successfully utilized to improve the structural, morphological and gas sensing properties. Nanocrystalline HAp powder is synthesized by wet chemical precipitation route, and ion exchange process is employed for addition of Co and Fe ions in HAp matrix. Moreover, swift heavy ion irradiation (SHI) technique is used to modify the surface of pure and metal ion exchanged HAp with various ion fluence. The structural investigation of pure and metal ion exchanged HAp thick films are carried out using X-ray diffraction and the presence of functional group is observed by means FTIR spectroscopy. Furthermore, surface morphology is visualized by means of SEM and AFM analysis. CO gas sensing study is carried out for, pure and metal ions doped, HAp thick films with detail investigation on operating temperature, response/recovery time and gas uptake capacity. The surface modifications of sensor matrix by SHI enhance the gas response, response/recovery and gas uptake capacity. The significant observation is here to note that, addition of Co and Fe in HAp matrix and surface modification by SHI improves the sensing properties of HAp films drastically resulting in gas sensing at relatively lower temperatures.

  14. Dip coated silicon-substituted hydroxyapatite films.

    PubMed

    Hijón, Natalia; Victoria Cabañas, M; Peña, Juan; Vallet-Regí, María

    2006-09-01

    Silicon-substituted hydroxyapatites have been deposited onto Ti6Al4V substrates by sol-gel technology. The Ca(10)(PO(4))(6-x-y)(SiO(4))(x)(CO(3))(y)(OH)(2-x+y) coatings obtained, with silicon contents up to x=1 (2.8 wt.%), show a homogeneous and crack-free surface composed of particles smaller than 20 nm. The silicon enters into the apatite structure in the form of SiO(4)(4-) groups that partially substitute the PO(4)(3-) groups. The Si content and the Ca/P molar ratio of the coatings agree with those originally introduced in the sols. Layers with thicknesses around 600 nm show adhesion strengths superior to 20 MPa as determined by a pull-out test. The formation of an apatite layer onto these coatings after immersion in a simulated body fluid is enhanced by the presence of silicon. PMID:16828579

  15. Chemical characterization of some substituted hydroxyapatites

    PubMed Central

    2011-01-01

    Synthetic multi-substituted hydroxyapatite nano powders containing silicon and or carbonate prepared by a wet chemical method. The process parameters are set up to allow the simultaneous substitution of carbonate and silicon ions in the place of phosphorus. The chemical and structural characterizations of the prepared powders are determined with the aid of; XRF, ICP, XRD and FTIR. The results show that, the ion substitution in the crystal lattice of HA caused a change in the unit cell dimensions and affected the degree of crystallization of the produced powders. The apatite formation abilityy of the prepared discs from the synthesized powders is determined by immersing in SBF solution for different periods. The degree of ion release was determined in the obtained solutions. The examined surface of the immersed discs under SEM and analyzed by CDS showed a more dense HA layer than those of un-substituted ones. The HA with the substituted silicon and carbonate ions, showed the highest solubility with greater rate of ion release, compared with carbonate-free powder. All prepared powders took sodium ion from the SBF solution during immersion, which was not recorded before. PMID:22122971

  16. Elastin-like polypeptide based hydroxyapatite bionanocomposites.

    PubMed

    Wang, Eddie; Lee, Sang-Hyuk; Lee, Seung-Wuk

    2011-03-14

    In nature, organic matrix macromolecules play a critical role in enhancing the mechanical properties of biomineralized composites such as bone and teeth. Designing artificial matrix analogues is promising but challenging because relatively little is known about how natural matrix components function. Therefore, in lieu of using natural components, we created biomimetic matrices using genetically engineered elastin-like polypeptides (ELPs) and then used them to construct mechanically robust ELP-hydroxyapatite (HAP) composites. ELPs were engineered with well-defined backbone charge distributions by periodic incorporation of negative, positive, or neutral side chains or with HAP-binding octaglutamic acid motifs at one or both protein termini. ELPs exhibited sequence-specific capacities to interact with ions, bind HAP, and disperse HAP nanoparticles. HAP-binding ELPs were incorporated into calcium phosphate cements, resulting in materials with improved mechanical strength, injectability, and antiwashout properties. The results demonstrate that rational design of genetically engineered polymers is a powerful system for determining sequence-property relationships and for improving the properties of organic-inorganic composites. Our approach may be used to further develop novel, multifunctional bone cements and expanded to the design of other advanced composites. PMID:21218767

  17. Synthesis of carbonated hydroxyapatite nanospheres through nanoemulsion.

    PubMed

    Zhou, W Y; Wang, M; Cheung, W L; Guo, B C; Jia, D M

    2008-01-01

    This study investigated the nanoemulsion technique as a means to synthesize carbonated hydroxyapatite (CHAp) nanospheres which could be used to produce composite tissue engineering scaffolds. CHAp nanospheres were successfully synthesized by mixing an acetone solution of Ca(NO(3))(2).4H(2)O with an aqueous solution of (NH(4))(2)HPO(4) and NH(4)HCO(3). Four reaction temperatures, namely, 4, 25, 37 and 55 degrees C, were investigated and no surfactant was added in all nanoemulsion processes. Wet slurries of CHAp from the nanoemulsions were freeze-dried to obtain dry powders. X-ray diffraction (XRD) results showed that the as-synthesized CHAp nanoparticles were mainly in an amorphous state. After calcination at 900 degrees C, the apatite became well crystallized. Fourier transform infrared (FTIR) spectroscopy showed that the CHAp was B-type substitution. Both scanning electron microscopy (SEM) and transmission electron microscopy (TEM) revealed that the CHAp particles were spherical in shape and that their sizes were in the nanometer range. The successful synthesis of CHAp nanospheres is a critical step forward in our efforts to fabricate bone tissue engineering scaffolds using the selective laser sintering technology. PMID:17577636

  18. Osteoclasts in the interface with electrospun hydroxyapatite.

    PubMed

    Pasuri, Jenni; Holopainen, Jani; Kokkonen, Hanna; Persson, Maria; Kauppinen, Kyösti; Lehenkari, Petri; Santala, Eero; Ritala, Mikko; Tuukkanen, Juha

    2015-11-01

    Electrospinning is a method to produce lightweight, resorbable and bioinspired scaffolds for tissue engineering. Here we investigated the influence of electrospun hydroxyapatite fibers (HA) on macrophages and osteoclasts. A mouse macrophage cell line (RAW 264.7) and human bone marrow derived primary osteoclasts (hOC) were cultured with electrospun HA fibers embedded in Matrigel. Cell morphology and the secretion of pro-inflammatory cytokines (IL-6 and TNF-α) were analyzed using macrophages. Both fluorescent microscopy and scanning electron microscopy indicated that the cell morphology differed on the various materials (HA fibers on Matrigel, pure Matrigel and a glass control). Control macrophages were activated with bacterial lipopolysaccharide (LPS) but electrospun HA did not provoke an inflammatory response. Cytokine secretion detected with enzyme-linked immunosorbent assay (ELISA) also supported this observation. LPS, but not HA fibers, stimulated TNF-α and IL-6 secretion by macrophages at the 2 day time point. After 4 days in culture there was an increasing trend in cytokine secretion in the HA fiber samples. Human bone marrow myeloid precursor cells were able to fuse and differentiate on the fibrous mineral scaffold to form functional multinuclear osteoclasts that were able to resorb the HA nanofibers. This indicates that osteoclasts do not necessarily need a continuous bone surface but osteoclast ruffled border membranes can form a resorption interface with a fibrous mineral scaffold. PMID:26342323

  19. Study of thermal effects of silicate-containing hydroxyapatites

    NASA Astrophysics Data System (ADS)

    Golovanova, O. A.; Zaits, A. V.; Berdinskaya, N. V.; Mylnikova, T. S.

    2016-02-01

    The possibility of modifications of hydroxyapatite silicate ions, from the extracellular fluid prototype solution under near-physiological conditions has been studied. Formation of silicon-structured hydroxyapatite with different extent of substitution of phosphate groups in the silicate group has been established through chemical and X-ray diffraction analyses, FTIR spectroscopy and optical microscopy. The results obtained are in agreement and suggest the possibility of substitution of phosphate groups for silicate groups in the hydroxyapatite structure when introducing different sources of silica, tetraethoxysilane and sodium silicate, in the reaction mixture. Growth in the amount of silicon in Si-HA results in the increase in the thermal stability of the samples. The greatest mass loss occurs at temperatures in the range of 25-400 0C that is caused by the removal of the crystallization and adsorption water and volatile impurities. It is shown that the modified apatites are of imperfect structure and crystallize in a nanocrystalline state.

  20. Fabrication, Properties and Applications of Dense Hydroxyapatite: A Review

    PubMed Central

    Prakasam, Mythili; Locs, Janis; Salma-Ancane, Kristine; Loca, Dagnija; Largeteau, Alain; Berzina-Cimdina, Liga

    2015-01-01

    In the last five decades, there have been vast advances in the field of biomaterials, including ceramics, glasses, glass-ceramics and metal alloys. Dense and porous ceramics have been widely used for various biomedical applications. Current applications of bioceramics include bone grafts, spinal fusion, bone repairs, bone fillers, maxillofacial reconstruction, etc. Amongst the various calcium phosphate compositions, hydroxyapatite, which has a composition similar to human bone, has attracted wide interest. Much emphasis is given to tissue engineering, both in porous and dense ceramic forms. The current review focusses on the various applications of dense hydroxyapatite and other dense biomaterials on the aspects of transparency and the mechanical and electrical behavior. Prospective future applications, established along the aforesaid applications of hydroxyapatite, appear to be promising regarding bone bonding, advanced medical treatment methods, improvement of the mechanical strength of artificial bone grafts and better in vitro/in vivo methodologies to afford more particular outcomes. PMID:26703750

  1. Recent Advances in Hydroxyapatite Scaffolds Containing Mesenchymal Stem Cells

    PubMed Central

    Michel, John; Penna, Matthew; Kochen, Juan; Cheung, Herman

    2015-01-01

    Modern day tissue engineering and cellular therapies have gravitated toward using stem cells with scaffolds as a dynamic modality to aid in differentiation and tissue regeneration. Mesenchymal stem cells (MSCs) are one of the most studied stem cells used in combination with scaffolds. These cells differentiate along the osteogenic lineage when seeded on hydroxyapatite containing scaffolds and can be used as a therapeutic option to regenerate various tissues. In recent years, the combination of hydroxyapatite and natural or synthetic polymers has been studied extensively. Due to the interest in these scaffolds, this review will cover the wide range of hydroxyapatite containing scaffolds used with MSCs for in vitro and in vivo experiments. Further, in order to maintain a progressive scope of the field this review article will only focus on literature utilizing adult human derived MSCs (hMSCs) published in the last three years. PMID:26106425

  2. Fabrication, Properties and Applications of Dense Hydroxyapatite: A Review.

    PubMed

    Prakasam, Mythili; Locs, Janis; Salma-Ancane, Kristine; Loca, Dagnija; Largeteau, Alain; Berzina-Cimdina, Liga

    2015-01-01

    In the last five decades, there have been vast advances in the field of biomaterials, including ceramics, glasses, glass-ceramics and metal alloys. Dense and porous ceramics have been widely used for various biomedical applications. Current applications of bioceramics include bone grafts, spinal fusion, bone repairs, bone fillers, maxillofacial reconstruction, etc. Amongst the various calcium phosphate compositions, hydroxyapatite, which has a composition similar to human bone, has attracted wide interest. Much emphasis is given to tissue engineering, both in porous and dense ceramic forms. The current review focusses on the various applications of dense hydroxyapatite and other dense biomaterials on the aspects of transparency and the mechanical and electrical behavior. Prospective future applications, established along the aforesaid applications of hydroxyapatite, appear to be promising regarding bone bonding, advanced medical treatment methods, improvement of the mechanical strength of artificial bone grafts and better in vitro/in vivo methodologies to afford more particular outcomes. PMID:26703750

  3. Synthesis and Antimicrobial Activity of Silver-Doped Hydroxyapatite Nanoparticles

    PubMed Central

    Ciobanu, Carmen Steluta; Iconaru, Simona Liliana; Chifiriuc, Mariana Carmen; Costescu, Adrian; Le Coustumer, Philippe; Predoi, Daniela

    2013-01-01

    The synthesis of nanosized particles of Ag-doped hydroxyapatite with antibacterial properties is of great interest for the development of new biomedical applications. The aim of this study was the evaluation of Ca10−xAgx(PO4)6(OH)2 nanoparticles (Ag:HAp-NPs) for their antibacterial and antifungal activity. Resistance to antimicrobial agents by pathogenic bacteria has emerged in the recent years and became a major health problem. Here, we report a method for synthesizing Ag doped nanocrystalline hydroxyapatite. A silver-doped nanocrystalline hydroxyapatite was synthesized at 100°C in deionised water. Also, in this paper Ag:HAp-NPs are evaluated for their antimicrobial activity against Gram-positive and Gram-negative bacteria and fungal strains. The specific antimicrobial activity revealed by the qualitative assay is demonstrating that our compounds are interacting differently with the microbial targets, probably due to the differences in the microbial wall structures. PMID:23509801

  4. Investigations on hydroxyapatite powder obtained by wet precipitation

    NASA Astrophysics Data System (ADS)

    Poinescu, Aurora Anca; Ion, Rodica Mariana; van Staden, Raluca-Ioana; van Staden, Jacobus Frederick; Ghiurea, Marius

    2010-11-01

    It is well-known that hydroxyapatite have multiple applications in tissue engineering due to compositional similarities with bone tissue. In this work, hydroxyapatite powders obtained by modified chemical precipitation route, has been investigated by AMF and SEM analysis grain size, X-ray diffraction and infra-red spectroscopy. The particle size of hydroxyapatite was observed to be very fine, uniform, around 50 -60 nm. SEM observation of the HA coatings showed the presence of nano-sized needles, with a significant level of agglomeration. The infrared analysis show the characteristic peaks of absorbed water, hydroxyl, phosphate and carbonate species. The XRD pattern clearly indicated the crystallites responsible for the Bragg reflection of the (002) and (003) planes are useful for size determination by Sherrer relationship (around 68 nm).

  5. Hydroxyapatite Growth Inhibition Effect of Pellicle Statherin Peptides.

    PubMed

    Xiao, Y; Karttunen, M; Jalkanen, J; Mussi, M C M; Liao, Y; Grohe, B; Lagugné-Labarthet, F; Siqueira, W L

    2015-08-01

    In our recent studies, we have shown that in vivo-acquired enamel pellicle is a sophisticated biological structure containing a significant portion of naturally occurring salivary peptides. From a functional aspect, the identification of peptides in the acquired enamel pellicle is of interest because many salivary proteins exhibit functional domains that maintain the activities of the native protein. Among the in vivo-acquired enamel pellicle peptides that have been newly identified, 5 peptides are derived from statherin. Here, we assessed the ability of these statherin pellicle peptides to inhibit hydroxyapatite crystal growth. In addition, atomistic molecular dynamics (MD) simulations were performed to better understand the underlying physical mechanisms of hydroxyapatite growth inhibition. A microplate colorimetric assay was used to quantify hydroxyapatite growth. Statherin protein, 5 statherin-derived peptides, and a peptide lacking phosphate at residues 2 and 3 were analyzed. Statherin peptide phosphorylated on residues 2 and 3 indicated a significant inhibitory effect when compared with the 5 other peptides (P < 0.05). MD simulations showed a strong affinity and fast adsorption to hydroxyapatite for phosphopeptides, whereas unphosphorylated peptides interacted weakly with the hydroxyapatite. Our data suggest that the presence of a covalently linked phosphate group (at residues 2 and 3) in statherin peptides modulates the effect of hydroxyapatite growth inhibition. This study provides a mechanism to account for the composition and function of acquired enamel pellicle statherin peptides that will contribute as a base for the development of biologically stable and functional synthetic peptides for therapeutic use against dental caries and/or periodontal disease. PMID:26116492

  6. Proton beam effects on phenolic-based composites reinforced with nanopowders

    NASA Astrophysics Data System (ADS)

    Chhay, B.; Minamisawa, R.; Zheng, B.; Budak, S.; Ila, D.

    2007-08-01

    We have introduced various nanopowders in the precursor of glassy polymeric carbon (GPC) and studied the electrical properties as well as the chemical structure. In general the GPC ware produced at Alabama A&M University (AAMU) is used for making crucibles, heat exchangers and for prosthetic devices because of its biocompatibility and inertness. GPC ware at AAMU is synthesized from a phenolic resin solution from Georgia Pacific in a pyrolyzer system at temperatures between 100 °C and 2800 °C. The heat treatment includes several stages: gelling, curing, postcuring, precarbonization and carbonization. The fabrication of GPC is complicated because of the high production rate of gaseous products in critical temperature ranges where out-diffusion is relatively slow. Special care should be taken in temperature programming to avoid kilning faults and misshapen or porous GPC end results [H. Maleki, L.R. Holland, G.M. Jenkins, et al., Carbon 35 (1997) 227]. In this work we have introduced 1 wt% of SiC, carbon nanotubes (CNT) and Al2O3 to the precursor, pyrolyzed composites to 1000 °C and studied the effect of 1 MeV and 3 MeV proton bombardment on the final products.

  7. Irradiation creep of nano-powder sintered silicon carbide at low neutron fluences

    NASA Astrophysics Data System (ADS)

    Koyanagi, T.; Shimoda, K.; Kondo, S.; Hinoki, T.; Ozawa, K.; Katoh, Y.

    2014-12-01

    The irradiation creep behavior of nano-powder sintered silicon carbide was investigated using the bend stress relaxation method under neutron irradiation up to 1.9 dpa. The creep deformation was observed at all temperatures ranging from 380 to 1180 °C mainly from the irradiation creep but with the increasing contributions from the thermal creep at higher temperatures. The apparent stress exponent of the irradiation creep slightly exceeded unity, and instantaneous creep coefficient at 380-790 °C was estimated to be ∼1 × 10-5 [MPa-1 dpa-1] at ∼0.1 dpa and 1 × 10-7 to 1 × 10-6 [MPa-1 dpa-1] at ∼1 dpa. The irradiation creep strain appeared greater than that for the high purity SiC. Microstructural observation and data analysis indicated that the grain-boundary sliding associated with the secondary phases contributes to the irradiation creep at 380-790 °C to 0.01-0.11 dpa.

  8. TiO 2 nanopowders doped with boron and nitrogen for photocatalytic applications

    NASA Astrophysics Data System (ADS)

    Gombac, V.; De Rogatis, L.; Gasparotto, A.; Vicario, G.; Montini, T.; Barreca, D.; Balducci, G.; Fornasiero, P.; Tondello, E.; Graziani, M.

    2007-10-01

    TiO 2-based systems have attracted an increasing interest for their potential use as photocatalysts under visible-light irradiation. In this context, the present work was dedicated to the tailored synthesis of TiO 2 nanopowders doped with boron, nitrogen or both species for the photocatalytic degradation of organic dyes. In particular, the systems were synthesized by a sol-gel route starting from titanium(IV) butoxide as a Ti source and thoroughly characterized by the combined use of N 2 physisorption, X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), UV-Vis reflectance spectroscopy and temperature-programmed oxidation (TPO). Finally, the photocatalytic performances in the decomposition of the azo-dye methyl orange (MO) were investigated. The obtained results suggest that both dopants promote the photocatalytic activity with respect to pure TiO 2 systems. Nevertheless, while our surface N-doping does not appreciably modify the titania structure and texture, B incorporation inhibits the TiO 2 crystallite growth and induces an increase in the surface area. As regards the codoped systems, a remarkable reactivity improvement was observed only when B is present in excess with respect to N. A rational interpretation of the observed behaviour was attempted by calculations based on the density functional theory (DFT). We suggest that the presence of B in molar excess with respect to N generates reactive Ti(III) sites, which, in turn, might induce the formation of reactive superoxide species.

  9. Flame-driven aerosol synthesis of copper-nickel nanopowders and conductive nanoparticle films.

    PubMed

    Sharma, Munish K; Qi, Di; Buchner, Raymond D; Scharmach, William J; Papavassiliou, Vasilis; Swihart, Mark T

    2014-08-27

    We report the continuous one-step synthesis of bimetallic copper-nickel nanostructured coatings by deposition and sintering of metal nanoparticles produced as an aerosol using a flame driven high temperature reducing jet (HTRJ) process. The HTRJ process allows gas-phase (aerosol) formation of metal nanoparticles from low-cost metal salt precursors. These can be collected as discrete powders for subsequent use in formulating conductive inks or for other applications. However, direct deposition of nanoparticles to form coatings allows measurements of electrical conductivity of films of deposited nanoparticles as a function of composition and sintering temperature, without actually formulating and printing inks. This is the approach taken here for the purpose of screening nanoparticle compositions quickly. We characterized the microstructure and composition of both nanopowders and films and found that their composition consistently matched the ratio of metals in the precursor solution. The electrical conductivity was highest (∼10(4) S/m) for films with 60:40 and 40:60 copper-to-nickel mass ratios. These films maintained their conductivity during extended storage (1 month) under ambient conditions. The oxidation resistance and high conductivity observed here suggest that 60:40 and 40:60 Cu:Ni nanoparticles have promise as lower cost replacements for silver nanoparticles in conductive ink formulations. PMID:25075968

  10. Magnetic structure, magnetoelastic coupling, and thermal properties of EuCrO3 nanopowders

    NASA Astrophysics Data System (ADS)

    Taheri, M.; Razavi, F. S.; Yamani, Z.; Flacau, R.; Reuvekamp, P. G.; Schulz, A.; Kremer, R. K.

    2016-03-01

    We carried out detailed studies of the magnetic structure, magnetoelastic coupling, and thermal properties of EuCrO3 nanopowders from room temperature to liquid helium temperature. Our neutron powder diffraction and x-ray powder diffraction measurements provide precise atomic positions of all atoms in the cell, especially for the light oxygen atoms. The low-temperature neutron powder diffraction data revealed extra Bragg peaks of magnetic origin, which can be attributed to a Gx antiferromagnetic structure with an ordered moment of ˜2.4 μB consistent with the 3 d3 electronic configuration of the Cr3 + cations. Apart from previously reported antiferromagnetic and ferromagnetic transitions in EuCrO3 at low temperatures, we also observed an anomaly at about 100 K. This anomaly was observed in the temperature dependence of the sample's, lattice parameters, thermal expansion, Raman spectroscopy, permittivity, and conductance measurements. This anomaly is attributed to the magnetoelastic distortion in the EuCrO3 crystal.

  11. Structure, nanohardness and photoluminescence of ZnO ceramics based on nanopowders

    NASA Astrophysics Data System (ADS)

    Muktepavela, Faina; Grigorjeva, Larisa; Kundzins, Karlis; Gorokhova, Elena; Rodnyi, Piotr

    2015-09-01

    ZnO ceramics obtained from grained powders with different grain size by hot pressing and ceramics from tetrapods nanopowders obtained by press-less sintering have been investigated under identical conditions. Ceramics obtained by hot pressing were optically transparent but were composed of large inhomogeneous grains (d = 8-35 μm) exhibiting a substructure. Decreased values of elastic modulus within a grain and a wide defect-associated (‘green’) photoluminescence (PL) band at 2.2-2.8 eV in conjunction with a weak excitonic band indicate a high concentration of residual point defects in hot pressed ZnO ceramics. Utilization of more small-grained powders contributes to the formation of more uniform microstructure (d = 5-15 μm) and extraction of point defects. This reflects as a substantially decreased defect PL band and increased excitonic band. Ceramics obtained by press-less sintering from tetrapods had fine-grained structure (d = 1-4 μm) with no signs of a substructure. PL spectrum has a narrow excitonic band with phonon replicas (1LO_ExD0), whereas the defect ‘green’ luminescence is negligible. The effects of powders morphologies have been explained in terms of a hereditary influence of interaction processes between initial particles on the formation of a microstructure and kinetic of defect distribution on the grain growth stages during the sintering of ZnO ceramics.

  12. Temperature dependence of Er3+ ionoluminescence and photoluminescence in Gd2O3:Bi nanopowder

    NASA Astrophysics Data System (ADS)

    Boruc, Zuzanna; Gawlik, Grzegorz; Fetliński, Bartosz; Kaczkan, Marcin; Malinowski, Michał

    2014-06-01

    Ionoluminescence (IL) and photoluminescence (PL) of trivalent erbium ions (Er3+) in Gd2O3 nanopowder host activated with Bi3+ ions has been studied in order to establish the link between changes in luminescent spectra and temperature of the sample material. IL measurements have been performed with H2+ 100 keV ion beam bombarding the target material for a few seconds, while PL spectra have been collected for temperatures ranging from 20 °C to 700 °C. The PL data was used as a reference in determining the temperature corresponding to IL spectra. The collected data enabled the definition of empirical formula based on the Boltzmann distribution, which allows the temperature to be determined with a maximum sensitivity of 9.7 × 10-3 °C-1. The analysis of the Er3+ energy level structure in terms of tendency of the system to stay in thermal equilibrium, explained different behaviors of the line intensities. This work led to the conclusion that temperature changes during ion excitation can be easily defined with separately collected PL spectra. The final result, which is empirical formula describing dependence of fluorescence intensity ratio on temperature, raises the idea of an application of method in temperature control, during processes like ion implantation and some nuclear applications.

  13. When Halides Come to Lithium Niobate Nanopowders Purity and Morphology Assistance.

    PubMed

    Lamouroux, Emmanuel; Badie, Laurent; Miska, Patrice; Fort, Yves

    2016-03-01

    The preparation of pure lithium niobate nanopowders was carried out by a matrix-mediated synthesis approach. Lithium hydroxide and niobium pentachloride were used as precursors. The influence of the chemical environment was studied by adding lithium halide (LiCl or LiBr). After thermal treatment of the precursor mixture at 550 °C for 30 min, the morphology of the products was obtained from transmission electron microscopy and dynamic light scattering, whereas the crystallinity and phase purity were characterized by X-ray diffraction and UV-visible and Raman spectroscopies. Our results point out that the chemical environment during lithium niobate formation at 550 °C influences the final morphology. Moreover, direct and indirect band-gap energies have been determined from UV-visible spectroscopy. Their values for the direct-band-gap energies range from 3.97 to 4.36 eV with a slight dependence on the Li/Nb ratio, whereas for the indirect-band-gap energies, the value appears to be independent of this ratio and is 3.64 eV. No dependence of the band-gap energies on the average crystallite and nanoparticle sizes is observed. PMID:26859157

  14. One-pot synthesis and characterization of Nb2O5 nanopowder.

    PubMed

    Athar, Taimur; Hashmi, Ameed; Al-Hajry, Ali; Ansari, Z A; Ansari, S G

    2012-10-01

    Nanosized niobium oxide powders were synthesized with a yield of approximately 87% using a simple and facile soft-chemical process. Niobium pentachloride (Nb2Cl5) was used as the precursor which was first converted into niobium ethoxide and then hydrolysed with water to synthesize niobia nanopowder. The synthesized powder was calcined at 500 degrees C for phase conversion to end-centered monoclinic as confirmed by diffraction studies and elemental analysis with a chemical composition in the ratio of Nb:O as 1:2.5. The molecular framework of Nb-O-Nb stretching and asymmetric frequency was confirmed by FT-IR, UV-visible and Raman spectroscopic studies. The size, shape and surface morphology of the powders were observed by SEM and TEM which indicated particle sizes of approximately 20 nm. The surface area of 20 m2/g, pore volume of 0.0538 cm2/g and the average pore size of 6.5 nm2 for the calcined sample were obtained with the help of nitrogen adsorption/desorption method using the Barrett-Joyner-Halenda (BJH) method which indicates that the synthesized powder can be used for catalysis and other surface sensitive applications. PMID:23421157

  15. Microwave sintering of nanopowder ZnNb2O6: Densification, microstructure and microwave dielectric properties

    NASA Astrophysics Data System (ADS)

    Bafrooei, H. Barzegar; Nassaj, E. Taheri; Hu, C. F.; Huang, Q.; Ebadzadeh, T.

    2014-12-01

    High density ZnNb2O6 ceramics were successfully fabricated by microwave sintering of ZnO-Nb2O5 and ZnNb2O6 nanopowders. Phase formation, microstructure and microwave electrical properties of the microwave sintered (MS) and microwave reaction sintered (MRS) specimens were examined using X-ray diffraction, field emission scanning electron microscopy and microwave dielectric properties measurement. Specimens were sintered in a temperature range from 950 to 1075 °C for 30 min at an interval of 25 °C using a microwave furnace operated at 2.45 GHz frequency, 3 kW power. XRD pattern revealed the formation of pure columbite phase of ZnNb2O6. The SEM micrographs show grain growth and reduction in porosity of specimens with the increase in sintering temperature. Good combination of microwave dielectric properties (εr~23.6, Qf~64,300 GHz and τf~-66 ppm/°C and εr~24, Qf~75,800 GHz and τf~-64 ppm/°C) was obtained for MS- and MRS-prepared samples at 1000 °C and 1050 °C for 30 min, respectively.

  16. Plasma column and nano-powder generation from solid titanium by localized microwaves in air

    SciTech Connect

    Popescu, Simona; Jerby, Eli Meir, Yehuda; Ashkenazi, Dana; Barkay, Zahava; Mitchell, J. Brian A.; Le Garrec, Jean-Luc; Narayanan, Theyencheri

    2015-07-14

    This paper studies the effect of a plasma column ejected from solid titanium by localized microwaves in an ambient air atmosphere. Nanoparticles of titanium dioxide (titania) are found to be directly synthesized in this plasma column maintained by the microwave energy in the cavity. The process is initiated by a hotspot induced by localized microwaves, which melts the titanium substrate locally. The molten hotspot emits ionized titanium vapors continuously into the stable plasma column, which may last for more than a minute duration. The characterization of the dusty plasma obtained is performed in-situ by small-angle X-ray scattering (SAXS), optical spectroscopy, and microwave reflection analyses. The deposited titania nanoparticles are structurally and morphologically analyzed by ex-situ optical and scanning-electron microscope observations, and also by X-ray diffraction. Using the Boltzmann plot method combined with the SAXS results, the electron temperature and density in the dusty plasma are estimated as ∼0.4 eV and ∼10{sup 19 }m{sup −3}, respectively. The analysis of the plasma product reveals nanoparticles of titania in crystalline phases of anatase, brookite, and rutile. These are spatially arranged in various spherical, cubic, lamellar, and network forms. Several applications are considered for this process of titania nano-powder production.

  17. Non-isothermal oxidation of aluminum nanopowder coated by hydrocarbons and fluorohydrocarbons

    NASA Astrophysics Data System (ADS)

    Sossi, A.; Duranti, E.; Paravan, C.; DeLuca, L. T.; Vorozhtsov, A. B.; Gromov, A. A.; Pautova, Yu. I.; Lerner, M. I.; Rodkevich, N. G.

    2013-04-01

    Aluminum nanopowder (nAl) obtained by electrical explosion of wires and passivated/coated with hydrocarbons and fluorohydrocarbons is comprehensively characterized. Coatings of different natures (octadecanoic and hexadecanoic acid, (1,1,11) trihydroperfluoro-undecan-1-ol, Fluorel™ + ester from esterification of (1,1,11) trihydroperfluoro-undecan-1-ol with furan-2,5-dione) were applied on the particle surface. The powders were studied by TEM, SEM, DSC-TGA, and BET specific surface area. The active aluminum content was determined by volumetric analyses. Coated nAl particles were compared to non-coated powder by the corresponding reactivity parameters obtained from DSC-TGA. It was found that while fatty acids have a weak effect on the non-isothermal oxidation behavior, fluoroelastomers shift the oxidation onset of nAl to higher temperatures by ˜20 °C for the first oxidation stage and by ˜100 °C for the second oxidation stage.

  18. Plasticizer Effect on Rheological Behaviour of Screen Printing Pastes Based on Barium Titanate Nanopowder

    NASA Astrophysics Data System (ADS)

    Dulina, I.; Umerova, S.; Ragulya, A.

    2015-04-01

    The dependence of rheological behaviour of pastes based on BaTiO3 nanopowder vs. plasticizer content has been investigated. All pastes prepared for research can be divided into groups by structure types and viscosity. Such a grouping has been explained by different interaction between nanoparticles and binder in the pastes. Particles with molecules of binder form clusters - the representative units in the volume of paste where particles are uniformly distributed. Plasticizer adding effects on binder molecule conformation and change clusters size. Bond strength between clusters can be specified with rheopexy in the area of low shear stress and low strain rates. Rheopexy degree increasing authenticates interaction intensification between clusters. Rheopexy structure destruction leads to separate clusters formation and initiation of the pseudoplastic flow stage. The end of pseudoplastic flow corresponds to structure with clusters assembled into separated layers. Further shear stress increasing leads to inter-clusters bonds appear which can be deformed elastically and the temporary local linkage is possible. Such a phenomenon fully discloses the features of thixotropic structure destruction in plasticized pastes.

  19. Synthesis and magnetic properties of NiFe2-xSmxO4 nanopowder

    NASA Astrophysics Data System (ADS)

    Hassanzadeh-Tabrizi, S. A.; Behbahanian, Shahrzad; Amighian, Jamshid

    2016-07-01

    NiFe2-xSmxO4 (x=0.00, 0.05, 0.10 and 0.15) nanopowders were synthesized via a sol-gel combustion route. The structural studies were carried out by X-ray diffractometer, Fourier transform infrared spectroscopy, scanning electron microscopy and transmission electron microscopy. The XRD results confirmed the formation of single-phase spinel cubic structure. The crystallite size decreased with an increase of samarium ion concentration, while lattice parameter and lattice strain increased with samarium substitution. TEM micrographs showed that agglomerated nanoparticles with particle sizes ranging from 35 to 90 nm were obtained. The magnetic studies were carried out using vibrating sample magnetometer. Magnetic measurements revealed that the saturation magnetization (Ms) of NiFe2-xSmxO4 nanoparticles decreases with increasing Sm3+substitution. The reduction of saturation magnetization is attributed to the dilution of the magnetic interaction. The coercivity (Hc) of samples increases by adding samarium.

  20. Enhanced osteoblast and osteoclast responses to a thin film sputtered hydroxyapatite coating.

    PubMed

    Hao, J; Kuroda, S; Ohya, K; Bartakova, S; Aoki, H; Kasugai, S

    2011-06-01

    A sputtering technique followed by a low temperature hydrothermal treatment has been demonstrated to produce a dense-and-bioactive hydroxyapatite thin film coating. The purpose of the present study was to investigate osteoblast and osteoclast responses to the hydroxyapatite coated plates and titanium plates with similar roughness. Rat bone marrow stromal cells were cultured on these plates to induce osteoblasts. The cells showed a significantly enhanced proliferation on the hydroxyapatite surface, accompanied by increase of osteoblastic phenotypes. The co-cultured osteoclasts exhibited the significantly different cell number and morphology between the hydroxyapatite and the titanium surfaces. A series of osteoclast marker genes were more stimulated on the hydroxyapatite and thirty two percent of the hydroxyapatite surface area could be resorbed by osteoclasts. The thin film sputtered hydroxyapatite could provide a favorable surface for both osteoblast and osteoclast formation and their function, indicating its good osteoconductivity and biodegradability. PMID:21567286

  1. Aminosilane as an effective binder for hydroxyapatite-gelatin nanocomposites.

    PubMed

    Luo, Tzy-Jiun M; Ko, Ching-Chang; Chiu, Chi-Kai; Llyod, Jacob; Huh, Uk

    2010-02-01

    Aminosilane has been explored as an alternative chemical linker to facilitate the binding and solidification of hydroxyapatite-gelatin nanocomposite at room temperature, which was synthesized using co-precipitation method in the presence of gelatin. This aminosilane treatment was found effective at low concentration (~25 μL/mL) and the solidification and dehydration of hydroxyapatite-gelatin slurry completes within hours depending on the amount of aminosilane. The resulting sample exhibits compressive strength of 133 MPa, about 40% higher than glutaraldehyde treated samples, and shows good biocompatibility based on cell adhesion, proliferation, alkaline phosphate synthesis, and mineralization studies. PMID:23833395

  2. Aminosilane as an effective binder for hydroxyapatite-gelatin nanocomposites

    PubMed Central

    Luo, Tzy-Jiun M.; Ko, Ching-Chang; Chiu, Chi-Kai; Llyod, Jacob; Huh, Uk

    2013-01-01

    Aminosilane has been explored as an alternative chemical linker to facilitate the binding and solidification of hydroxyapatite-gelatin nanocomposite at room temperature, which was synthesized using co-precipitation method in the presence of gelatin. This aminosilane treatment was found effective at low concentration (~25 μL/mL) and the solidification and dehydration of hydroxyapatite-gelatin slurry completes within hours depending on the amount of aminosilane. The resulting sample exhibits compressive strength of 133 MPa, about 40% higher than glutaraldehyde treated samples, and shows good biocompatibility based on cell adhesion, proliferation, alkaline phosphate synthesis, and mineralization studies. PMID:23833395

  3. Femur bone repair in ovariectomized rats under the local action of alendronate, hydroxyapatite and the association of alendronate and hydroxyapatite

    PubMed Central

    Canettieri, Antonio Carlos Victor; Colombo, Carlos Eduardo Dias; Chin, Chung Man; Faig-Leite, Horácio

    2009-01-01

    An evaluation was made of the local action of alendronate sodium (A), hydroxyapatite (HA) and the association of both substances (A + HA), in different molar concentrations, on the femur bone repair of ovariectomized rats. Ninety-eight animals were divided into seven groups: control (C), starch (S), alendronate 1 mol (A1), alendronate 2 mols (A2), hydroxyapatite 1 mol (HA1), hydroxyapatite 2 mols (HA2) and the association of alendronate + hydroxyapatite (A + HA). Rats weighing about 250 g were ovariectomized and 2.5-mm diameter bone defects were made on the left femur 30 days later. Each experimental group had defects filled with appropriate material, except for group C (control). The animals were killed 7 and 21 days after surgery. Histological, histomorphometric and statistical analyses of bone neoformation in the bone defect site were performed. From the histological standpoint, the major differences occurred after 21 days. All specimens in groups C, S, HA1 and HA2 presented linear closure of the bone defect, and most animals in groups A1, A2 and A + HA showed no bone neoformation in the central area of the defect. No statistically significant difference was found among the experimental groups after 7 days; after 21 days, group HA2 presented the highest amount of neoformed bone. There was no significant difference among groups A1, A2 and A + HA in the two study periods. It was concluded that alendronate, either isolated or in association with hydroxyapatite, had an adverse effect on bone repair in this experimental model. Moreover, the hydroxyapatite used here proved to be biocompatible and osteoconductive, with group HA2 showing the best results. PMID:19765106

  4. Luminous and tunable white-light upconversion for YAG (Yb3Al5O12) and (Yb,Y)2O3 nanopowders.

    PubMed

    Wang, Jiwei; Hao, Jian Hua; Tanner, Peter A

    2010-12-01

    We report on multiphoton white-light upconversion in vacuum for Pechini synthesis Yb(3)Al(5)O(12) (YbAG) and combustion synthesis (Yb,Y(2))O(3) nanopowders under IR excitation. Their intense white-light upconversion is attributed to charge transfer luminescence superimposed upon a broadband emission. Unlike common nanoscale phosphors, which show low luminescence efficiency, the intensity of white-light upconversion for nanopowders is similar to that of their bulk counterparts. The luminary efficacy of the upconversion is estimated to be 10-15 lm W(-1), and the Commission Internationale d'Eclairage (CIE) coordinates can be widely tuned by the excitation power, pressure, and codoping ratio. The nano-YbAG sample exhibits a longer buildup time for emission, a higher excitation threshold, and a wider CIE range than the oxide nanopowders. PMID:21124566

  5. Inhibition of hydroxyapatite formation by osteopontin phosphopeptides.

    PubMed Central

    Pampena, David A; Robertson, Karen A; Litvinova, Olga; Lajoie, Gilles; Goldberg, Harvey A; Hunter, Graeme K

    2004-01-01

    Osteopontin (OPN) is an acidic phosphoglycoprotein that is believed to function in the prevention of soft tissue calcification. In vitro studies have shown that OPN can inhibit the formation of hydroxyapatite (HA) and other biologically relevant crystal phases, and that this inhibitory activity requires phosphorylation of the protein; however, it is not known which phosphorylated residues are involved. We have synthesized peptides corresponding to four phosphoserine-containing sequences in rat OPN: OPN7-17, containing phosphoserines 10 and 11; OPN41-52, containing phosphoserines 46 and 47; OPN248-264, containing phosphoserines 250, 257 and 262; and OPN290-301, containing phosphoserines 295-297. The abilities of these peptides to inhibit de novo HA formation were determined using a constant-composition autotitration assay. All four OPN phosphopeptides caused a dose-dependent increase in nucleation lag time, but did not significantly affect subsequent formation of the crystals. However, OPN41-52 (inhibitory constant 73.5 min/microM) and OPN290-301 (72.2 min/microM) were approx. 4 times more potent inhibitors than OPN7-17 (19.7 min/microM) and OPN247-264 (16.3 min/microM). 'Scrambling' the amino acid sequence of OPN290-301 resulted in decreased potency (45.6 min/microM), whereas omission of the phosphate groups from this peptide caused a greater decrease (5.20 min/microM). These findings have identified phosphorylated sequences that are important for the ability of rat bone OPN to inhibit HA crystal formation, and suggest that negative-charge density is an important factor in this activity. PMID:14678013

  6. Biomechanical analysis of hydroxyapatite cement cranioplasty.

    PubMed

    Matic, Damir B; Manson, Paul N

    2004-05-01

    A recent review of the authors' experience with hydroxyapatite (HA) cement cranioplasties revealed a high infection rate. During removal of these implants, all were loose and fractured. Forty percent of these patients had a history of minor trauma at the site of cranioplasty before experiencing infection. Minor trauma may fracture HA cranioplasties and result in infection. The purpose of this study is to determine the force to fracture full- and partial-thickness cranial defects reconstructed with HA cement and to compare peak loads of differing HA cement cranioplasty techniques. Standardized craniotomy defects were created in five fresh cadaver heads. Full-thickness defects were reconstructed with either rigid or flexible titanium mesh and then covered with HA cement. Partial-thickness defects were reconstructed with HA alone. After setting, a uniaxial impact was delivered to each of the defects. Peak loads were recorded, and defects were examined for evidence of fracture.Predictable fractures of the HA cranioplasties occurred at 1200 N in all full-thickness defects reconstructed with mesh and a thin layer of HA. Implant loosening and chipping was similar to what was seen clinically in the authors' patients with infections. Full-thickness defects in which titanium mesh was shaped like a cup and filled with a thick layer of HA resist fracture at 1200 N. Partial-thickness defects reconstructed with HA alone also do not fracture at this peak load. Patient selection, defect characteristics, and reconstructive techniques are factors that need to be considered before using HA cement for cranioplasty purposes. PMID:15111799

  7. Structural study and phase transition investigation in a simple synthesis of porous architected-ZnO nanopowder

    SciTech Connect

    Shang, C.; Barnabé, A.

    2013-12-15

    In this work, zinc oxide powder with a rectangular-shaped porous architecture, made of numerous spherical nanometric particles, was obtained. A simple precipitation/decomposition procedure was used comprising a zinc oxalate intermediate, obtained from zinc sulfate and oxalic acid without any additives. Detailed studies on zinc oxalate dehydration, decomposition and zinc oxide formation, were carried out using in-situ temperature X-ray diffraction and thermogravimetric analysis. During the investigation, the temperature dependence of particle sizes, lattice parameters and crystal structures of ZnC{sub 2}O{sub 4}·2H{sub 2}O, ZnC{sub 2}O{sub 4} and ZnO nanopowders were analyzed from room temperature to 450 °C. Structural transitions were also discussed. The structure and morphology of the as-prepared ZnO nanopowder were investigated by electron microscopy and compared to the crystalline rectangular shape of ZnC{sub 2}O{sub 4}·2H{sub 2}O. The calcination temperature, counter ion and precipitate agent were found to be related to the product's shape and diameter. Spherical ZnO nanoparticles with diameters of less than 20 nm and a maximum specific surface of 53 m{sup 2}/g were obtained using this method. Highlights: • ZnO nanopowders with porous architecture were synthesized by a simple method. • Spherical ZnO nanoparticles confined in submicronic rectangular shape are obtained. • Crystal structures are determined temperature in-situ XRD up to 450 °C. • Structural transitions were analyzed.

  8. Facilitated transport of copper with hydroxyapatite nanoparticles in saturated sand

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Saturated packed column experiments were conducted to investigate the facilitated transport of Cu with hydroxyapatite nanoparticles (nHAP) at different pore water velocities (0.22-2.2 cm min–1), solution pH (6.2-9.0), and fraction of Fe oxide coating on grain surfaces (', 0-0.36). The facilitated tr...

  9. Peculiarities of hydroxyapatite/nanodiamond composites as novel implants

    NASA Astrophysics Data System (ADS)

    Pramatarova, L.; Dimitrova, R.; Pecheva, E.; Spassov, T.; Dimitrova, M.

    2007-12-01

    Hydroxyapatite/detonation nanodiamond composites are created on silica glass and cover glass by simple soaking process in an open deposition type set-up. The supersaturated solution (simulated body fluid, SBF) is prepared in a way to resemble the composition of human blood plasma. The composite growth is carried out through the addition of detonation nanodiamond particles to the SBF. Scanning electron microscopy, X-ray diffraction and FTIR spectroscopy are used to determine the surface morphology and the structure of the hydroxyapatite /detonation nanodiamond composite layers. The applied methods provide evidence that the nanodiamond surface functional groups interact strongly with the biological solution. The detonation nanodiamond surface is chemically multifunctional (surface OH, C-O-H, C = C, C-O-C and C = O groups exist), so that the hydroxyapatite is grown both by physical adsorption and chemical interaction. The OH- groups are regarded to play an important role in the hydroxyapatite growth on a diamond's surface from SBF, as they charge it negatively and attract Ca2+ ions, which in turn attract PO43- ions, thus forming apatite nuclei.

  10. Electrophoretic deposition of zinc-substituted hydroxyapatite coatings.

    PubMed

    Sun, Guangfei; Ma, Jun; Zhang, Shengmin

    2014-06-01

    Zinc-substituted hydroxyapatite nanoparticles synthesized by the co-precipitation method were used to coat stainless steel plates by electrophoretic deposition in n-butanol with triethanolamine as a dispersant. The effect of zinc concentration in the synthesis on the morphology and microstructure of coatings was investigated. It is found that the deposition current densities significantly increase with the increasing zinc concentration. The zinc-substituted hydroxyapatite coatings were analyzed by X-ray diffraction, scanning electron microscopy and Fourier transform infrared spectroscopy. It is inferred that hydroxyapatite and triethanolamine predominate in the chemical composition of coatings. With the increasing Zn/Ca ratios, the contents of triethanolamine decrease in the final products. The triethanolamine can be burnt out by heat treatment. The tests of adhesive strength have confirmed good adhesion between the coatings and substrates. The formation of new apatite layer on the coatings has been observed after 7days of immersion in a simulated body fluid. In summary, the results show that dense, uniform zinc-substituted hydroxyapatite coatings are obtained by electrophoretic deposition when the Zn/Ca ratio reaches 5%. PMID:24863199

  11. Accelerated Nucleation of Hydroxyapatite Using an Engineered Hydrophobin Fusion Protein.

    PubMed

    Melcher, Melanie; Facey, Sandra J; Henkes, Thorsten M; Subkowski, Thomas; Hauer, Bernhard

    2016-05-01

    Calcium phosphate mineralization is of particular interest in dental repair. A biomimetic approach using proteins or peptides is a highly promising way to reconstruct eroded teeth. In this study, the screening of several proteins is described for their binding and nucleating activities toward hydroxyapatite. Out of 27 tested candidates, only two hydrophobin fusion proteins showed binding abilities to hydroxyapatite in a mouthwash formulation and an increased nucleation in artificial saliva. Using a semirational approach, one of the two candidates (DEWA_5), a fusion protein consisting of a truncated section of the Bacillus subtilis synthase YaaD, the Aspergillus nidulans hydrophobin DEWA, and the rationally designed peptide P11-4 described in the literature, could be further engineered toward a faster mineral formation. The variants DEWA_5a (40aaYaaD-SDSDSD-DEWA) and DEWA_5b (40aaYaaD-RDRDRD-DEWA) were able to enhance the nucleation activity without losing the ability to form hydroxyapatite. In the case of variant DEWA_5b, an additional increase in the binding toward hydroxyapatite could be achieved. Especially with the variant DEWA_5a, the protein engineering of the rationally designed peptide sequence resulted in a resemblance of an amino acid motif that is found in nature. The engineered peptide resembles the amino acid motif in dentin phosphoprotein, one of the major proteins involved in dentinogenesis. PMID:27010648

  12. Periodontal regeneration with stem cells-seeded collagen-hydroxyapatite scaffold.

    PubMed

    Liu, Zeping; Yin, Xing; Ye, Qingsong; He, Wulin; Ge, Mengke; Zhou, Xiaofu; Hu, Jing; Zou, Shujuan

    2016-07-01

    Re-establishing compromised periodontium to its original structure, properties and function is demanding, but also challenging, for successful orthodontic treatment. In this study, the periodontal regeneration capability of collagen-hydroxyapatite scaffolds, seeded with bone marrow stem cells, was investigated in a canine labial alveolar bone defect model. Bone marrow stem cells were isolated, expanded and characterized. Porous collagen-hydroxyapatite scaffold and cross-linked collagen-hydroxyapatite scaffold were prepared. Attachment, migration, proliferation and morphology of bone marrow stem cells, co-cultured with porous collagen-hydroxyapatite or cross-linked collagen-hydroxyapatite, were evaluated in vitro. The periodontal regeneration capability of collagen-hydroxyapatite scaffold with or without bone marrow stem cells was tested in six beagle dogs, with each dog carrying one sham-operated site as healthy control, and three labial alveolar bone defects untreated to allow natural healing, treated with bone marrow stem cells - collagen-hydroxyapatite scaffold implant or collagen-hydroxyapatite scaffold implant, respectively. Animals were euthanized at 3 and 6 months (3 animals per group) after implantation and the resected maxillary and mandibular segments were examined using micro-computed tomography scan, H&E staining, Masson's staining and histometric evaluation. Bone marrow stem cells were successfully isolated and demonstrated self-renewal and multi-potency in vitro. The porous collagen-hydroxyapatite and cross-linked collagen-hydroxyapatite had average pore sizes of 415 ± 20 µm and 203 ± 18 µm and porosity of 69 ± 0.5% and 50 ± 0.2%, respectively. The attachment, proliferation and migration of bone marrow stem cells were satisfactory on both porous collagen-hydroxyapatite and cross-linked collagen-hydroxyapatite scaffolds. Implantation of bone marrow stem cells - collagen-hydroxyapatite or collagen-hydroxyapatite scaffold in

  13. Specific features of nonlinear optical properties of Eu3+ doped BiFeO3 nanopowders near antiferromagnetic transition

    NASA Astrophysics Data System (ADS)

    El Bahraoui, T.; Sekkati, M.; Taibi, M.; Abd-Lefdil, M.; El-Naggar, A. M.; AlZayed, N. S.; Albassam, A. A.; Kityk, I. V.; Maciag, A.

    2016-01-01

    The monitoring of the Eu3+ doped BiFeO3 nanopowders was performed near the antiferromagnetic transformation by photoinduced optical second harmonic generation. As photoinduced laser beams we have used bicolor coherent excitations of the Er:glass laser emitting at 1540 nm with frequency repetition about 15 ns. The studies of the photoinduced SHG were performed versus temperature including the temperature range of ferromagnetic-ferroelectric transition (350 °C…390 °C). The optimal light polarization and intensity ratio were chosen; the sensitivity of the photoinduced SHG to the multiferroic phase transitions was explored.

  14. X-Ray Diffraction Microstructural Analysis of Bimodal-Size-Distribution MgO Nanopowders

    NASA Astrophysics Data System (ADS)

    Pratapa, Suminar; Hartono, Budi

    2010-01-01

    Investigation on the characteristics of x-ray diffraction data for MgO powdered mixture of nano and sub-nano particles has been carried out to reveal the crystallite-size-related microstructural information. The MgO powders were prepared by co-precipitation method followed by heat treatment at 500, 800 and 1200° C for 1 hour, being the difference in the temperature was to obtain two powders with distinct crystallite size and size-distribution. The powders were then carefully blended in air to give the presumably strain-free, bimodal-size-distribution MgO nanopowder. High-quality laboratory X-ray diffraction data for the powders were collected and then analysed using Rietveld-based MAUD software using the lognormal size distribution. Results show that the single-mode powders exhibit spherical crystallite size (Dv) of 29(1) nm, 36(1) and 185(0) nm for the 500, 800 and 1200° C data respectively with the nanometric powder displays slightly narrower crystallite size distribution character, indicated by lognormal dispersion parameter (σ) of 0.22 as compared to 0.18 for the sub-nanometric 1200° C powder. The mixture exhibits relatively more asymmetric peak broadening. By analysing the x-ray diffraction data of the latter specimen by using the single phase approach the results obtained was not according to experimental finding. Introducing two phase models for the `double-phase' 500-1200 mixture to accommodate the bimodal-size-distribution characteristics give Dv = 34(2) and σ = 0.10 for the `nanometric phase' and Dv = 363(0) and σ = 1.38 for the `sub-nanometric phase'.

  15. Physicochemical, microbial, and sensory properties of nanopowdered eggshell-supplemented yogurt during storage.

    PubMed

    Al Mijan, Mohammad; Choi, Kyung-Hoon; Kwak, Hae-Soo

    2014-01-01

    This study was carried out to investigate the possibility of adding nanopowdered eggshell (NPES) into yogurt to improve the functionality of yogurt and the effects of adding NPES on the physicochemical, microbial, and sensory properties of the products during storage. The pH and mean lactic acid bacteria counts of NPES-added (0.15-0.45%, wt/vol) yogurt ranged from 4.31 to 4.66 and from 6.56 × 10(8) to 8.56 × 10(8)cfu/mL, respectively, whereas these values ranged from 4.13 to 4.44 and 8.46 × 10(8) to 1.39 × 10(9), respectively, for the control samples during storage at 5 °C for 16d, which indicates a prolonged shelf-life with NPES-supplemented yogurt. Color analysis showed that the lightness (L*) and position between red and green (a*) values were not significantly influenced by the addition of NPES. However, the position between yellow and blue (b*) value significantly increased with the addition of the concentration (0.45%, wt/vol) of NPES at d 16 of storage. Sensory evaluation revealed that NPES-added yogurts showed a notably less sourness score and a higher astringency score than the control. An earthy flavor was higher in 0.45% NPES-supplemented yogurt compared with the control. Based on the results obtained from the current study, the concentration (0.15 to 0.30%, wt/vol) of NPES can be used to formulate NPES-supplemented yogurt without any significant adverse effects on the physicochemical, microbial, and sensory properties. PMID:24746127

  16. Magnetic field-enhanced sedimentation of nanopowder magnetite in water flow.

    PubMed

    Bakhteeva, Iu; Medvedeva, I; Byzov, I; Zhakov, S; Yermakov, A; Uimin, M; Shchegoleva, N

    2015-01-01

    Sedimentation dynamics of magnetite (γ-Fe3O4) nanopowder (10-20 nm) in water in a gradient magnetic field Bmax=0.3 T, (dB/dz)max=0.13 T/cm was studied for different water flow speeds and starting particle concentrations (0.1 and 1.0 g/l). The aggregates formation in water was monitored under the same conditions. In cyclical water flow, the velocity of particle sedimentation increases significantly in comparison to its rate in still water, which corresponds to the intensified aggregate formation. However, at a water flow speed more than 0.1 cm/s sedimentation velocity slows down, which might be connected to aggregate destruction in a faster water flow. Correlation between sedimentation time and the nanoparticle concentration in water does not follow the trend expected for spherical superparamagnetic particles. In our case sedimentation time is shorter for c=0.1 g/l in comparison with that for c=1 g/l. We submit that such a feature is caused by particle self-organization in water into complex structures of fractal type. This effect is unexplained in the framework of existing theoretical models of colloids systems, so far. Provisional recommendations are suggested for the design of a magnetic separator on the permanent magnets base. The main device parameters are magnetic field intensity B≥0.1 T, magnetic field gradient (dB/dz)max≈(0.1-0.2) T/cm, and water flow speed V<0.15 cm/s. For particle concentration c=1 g/l, purification of water from magnetite down to ecological and hygienic standards is reached in 80 min, for c=0.1 g/l the time is reduced down to 50 min. PMID:25650300

  17. Anode-supported microtubular cells fabricated with gadolinia-doped ceria nanopowders

    NASA Astrophysics Data System (ADS)

    Gil, V.; Gurauskis, J.; Campana, R.; Merino, R. I.; Larrea, A.; Orera, V. M.

    Anode-supported microtubular SOFCs based on ceria 3 ± 0.2 mm diameter and about 100 mm in length have been prepared using gadolinia-doped ceria (GDC) nanopowders. Nanometric Ce 0.9Gd 0.1O 1.95 (GDC) powders were deposited on NiO-Ce 0.9Gd 0.1O 1.95 (NiO-GDC) anode supports by dip-coating technique. Fabrication conditions to obtain dense and gas tight electrolyte layers on porous microtubular supports were studied. Three different dispersing agents: commercial Beycostat C213 (CECA, France) and short chain monomer (≤4 carbon atoms) with alcohol or carboxylic acid functional groups were evaluated. By optimizing colloidal dispersion parameters and sintering process, gas tight and dense GDC layers were obtained. Significantly lower sintering temperatures than reported previously (≤1300 °C) were employed to reach ≥98% values of theoretical density within electrolyte layers of ∼10 μm in thickness. A composite cathode, LSCF-GDC 50 wt.% with about 50 μm thickness was dip coated on the co-fired half-cell and then sintered at 1050 °C for 1 h. The electrochemical performance of these cells has been tested. In spite of electronic conduction due to partial reduction of the thin-electrolyte layer, the I- V measurements show power densities of 66 mW cm -2 at 0.45 V at temperatures as low as 450 °C (using 100% H 2 as fuel in the anodic compartment and air in the cathodic chamber).

  18. EVALUATION OF LEAKAGE FROM FUME HOODS USING TRACER GAS, TRACER NANOPARTICLES AND NANOPOWDER HANDLING TEST METHODOLOGIES

    PubMed Central

    Dunn, Kevin H.; Tsai, Candace Su-Jung; Woskie, Susan R.; Bennett, James S.; Garcia, Alberto; Ellenbecker, Michael J.

    2015-01-01

    The most commonly reported control used to minimize workplace exposures to nanomaterials is the chemical fume hood. Studies have shown, however, that significant releases of nanoparticles can occur when materials are handled inside fume hoods. This study evaluated the performance of a new commercially available nano fume hood using three different test protocols. Tracer gas, tracer nanoparticle, and nanopowder handling protocols were used to evaluate the hood. A static test procedure using tracer gas (sulfur hexafluoride) and nanoparticles as well as an active test using an operator handling nanoalumina were conducted. A commercially available particle generator was used to produce sodium chloride tracer nanoparticles. Containment effectiveness was evaluated by sampling both in the breathing zone (BZ) of a mannequin and operator as well as across the hood opening. These containment tests were conducted across a range of hood face velocities (60, 80, and 100 feet/minute) and with the room ventilation system turned off and on. For the tracer gas and tracer nanoparticle tests, leakage was much more prominent on the left side of the hood (closest to the room supply air diffuser) although some leakage was noted on the right side and in the BZ sample locations. During the tracer gas and tracer nanoparticle tests, leakage was primarily noted when the room air conditioner was on for both the low and medium hood exhaust air flows. When the room air conditioner was turned off, the static tracer gas tests showed good containment across most test conditions. The tracer gas and nanoparticle test results were well correlated showing hood leakage under the same conditions and at the same sample locations. The impact of a room air conditioner was demonstrated with containment being adversely impacted during the use of room air ventilation. The tracer nanoparticle approach is a simple method requiring minimal setup and instrumentation. However, the method requires the reduction in

  19. Ultrasound assisted dispersal of a copper nanopowder for electroless copper activation.

    PubMed

    Graves, John E; Sugden, Mark; Litchfield, Robert E; Hutt, David A; Mason, Timothy J; Cobley, Andrew J

    2016-03-01

    This paper describes the ultrasound assisted dispersal of a low wt./vol.% copper nanopowder mixture and determines the optimum conditions for de-agglomeration. A commercially available powder was added to propan-2-ol and dispersed using a magnetic stirrer, a high frequency 850 kHz ultrasonic cell, a standard 40 kHz bath and a 20 kHz ultrasonic probe. The particle size of the powder was characterized using dynamic light scattering (DLS). Z-Average diameters (mean cluster size based on the intensity of scattered light) and intensity, volume and number size distributions were monitored as a function of time and energy input. Low frequency ultrasound was found to be more effective than high frequency ultrasound at de-agglomerating the powder and dispersion with a 20 kHz ultrasonic probe was found to be very effective at breaking apart large agglomerates containing weakly bound clusters of nanoparticles. In general, the breakage of nanoclusters was found to be a factor of ultrasonic intensity, the higher the intensity the greater the de-agglomeration and typically micron sized clusters were reduced to sub 100 nm particles in less than 30 min using optimum conditions. However, there came a point at which the forces generated by ultrasonic cavitation were either insufficient to overcome the cohesive bonds between smaller aggregates or at very high intensities decoupling between the tip and solution occurred. Absorption spectroscopy indicated a copper core structure with a thin oxide shell and the catalytic performance of this dispersion was demonstrated by drop coating onto substrates and subsequent electroless copper metallization. This relatively inexpensive catalytic suspension has the potential to replace precious metal based colloids used in electronics manufacturing. PMID:26585024

  20. The inhibition of lamellar hydroxyapatite and lamellar magnetic hydroxyapatite on the migration and adhesion of breast cancer cells.

    PubMed

    Jin, Jun; Zuo, Guifu; Xiong, Guangyao; Luo, Honglin; Li, Qiuping; Ma, Chunying; Li, Deying; Gu, Feng; Ma, Yongjie; Wan, Yizao

    2014-04-01

    Hydroxyapatite nanoparticles have been reported to exhibit potent anti-tumor effects in some cancer cells. In our previous study, we have successfully synthesized two types of hydroxyapatite nanoparticles, laminated hydroxyapatite (L-HAp) and laminated magnetic hydroxyapatite (LM-HAp). In this study, we wanted to investigate the effects of L-HAp and LM-HAp with various concentrations on human breast cancer MDA-MB-231 cells. Cell proliferation was assessed with a MTT colorimetric assay. Scratch and adhesion assays were used to detect the effects of these two materials on migration and adhesion. The expressions of integrin β1 and Akt were measured by Western blotting. Our results showed that L-HAp and LM-HAp had little cell cytotoxicity and significantly reduced cell mobility and adhesion. LM-HAp showed greater inhibitor ability on migration and adhesion of MDA-MB-231 cells. Moreover, results from western blotting showed that L-HAp and LM-HAp impacted the phosphorylation of integrin β1, but showed no regular impact on Akt. This study suggests that L-HAp and LM-HAp may be potential anti-tumor and delivery system for breast cancer therapy. PMID:24363068

  1. Synthesis of TiO2 nano-powders prepared from purified sulphate leach liquor of red mud.

    PubMed

    Tsakiridis, P E; Oustadakis, P; Katsiapi, A; Perraki, M; Agatzini-Leonardou, S

    2011-10-30

    The research work presented in this paper is focused on the development of a purification process of red mud sulphate leach liquor for the recovery of titanium oxide (TiO(2)) nano-powders in the form of anatase. Initially, titanium was extracted over iron and aluminium from the leach liquor by solvent extraction using Cyanex 272 in toluene, at pH: 0.3 and T: 25°C, with 40% extractant concentration. Stripping of the loaded, with titanium, organic phase was carried out by diluted HCl (3 mol/L) at ambient temperature. Finally, the recovery of titanium nano-powder, in the form of anatase, was performed by chemical precipitation at pH: 6 and T: 95°C, using 10 wt% MgO pulp as neutralizing agent. The produced precipitates were characterized by X-ray diffraction analysis (XRD), Fourier transform infrared spectroscopy (FT-IR) and thermogravimetric/differential thermal analysis (TGA/DTA). Their morphological characteristics and microstructure were studied by scanning electron microscopy (SEM). High grade titanium white precipitate, in the form of anatase, was obtained. Iron concentration in the precipitate did not exceed 0.3%, whereas no aluminium was detected. PMID:21868153

  2. In vitro fabrication of dental filling nanopowder by green route and its antibacterial activity against dental pathogens.

    PubMed

    Lee, Jeong-Ho; Velmurugan, Palanivel; Park, Jung-Hee; Lee, Kui-Jae; Jin, Jong-Sik; Park, Yool-Jin; Bang, Keuk-Soo; Oh, Byung-Taek

    2016-06-01

    The aim of this study was to introduce novel Sn, Cu, Hg, and Ag nanopowders (NPs) and a composite nanopowder (NP) synthesized using Salvia miltiorrhiza Bunge (SM) root extract as a reducing and capping agent to improve the antibacterial property of dental filling materials. All of the NPs obtained were characterized using a scanning transmission electron microscope (STEM), and energy dispersive X-ray (EDX) spectrum imaging was performed to map the elemental distributions of the NP composite. Fourier transform infrared (FTIR) spectroscopy was performed to identify the role of various functional groups in all of the obtained NPs and the phyto-compound responsible for the reduction of various metal ions. The X-ray diffraction (XRD) patterns clearly illustrated the crystalline phase of the synthesized NP. The antibacterial properties of the synthesized Sn, Cu, Hg, Ag, composite NP, SM root extract, and commercial amalgam powder were evaluated. The Cu, composite NP, SM root extract and Ag NP displayed excellent antibacterial activity against dental bacteria Streptococcus mutans and Lactobacillus acidophilus. The results of this study require further evaluation for signs of metal toxicity in appropriate animal models. However, the results are encouraging for the application of metal NPs as suitable alternatives for antibiotics and disinfectants, especially in dental filling materials. PMID:27085055

  3. Effect of Mg content on the bioactivity and biocompatibility of Mg-substituted fluorapatite nanopowders fabricated via mechanical activation.

    PubMed

    Kheradmandfard, M; Fathi, M H; Ansari, F; Ahmadi, T

    2016-11-01

    The aim of this work was preparation, characterization, bioactivity and biocompatibility evaluation of Mg-substituted fluorapatite (Mg-FA) nanopowders. Mg-FA nanopowders with a chemical composition of Ca10-xMgx(PO4)6F2, with x=0, 0.5, 1, and 2 were prepared by mechanically activated method. The in vitro bioactivity was investigated by soaking the powders in simulated body fluid (SBF) for various time periods to analyze the nucleation and growth of bone-like apatite on the surface of the samples. Cell viability and cell attachment were studied by MTT assay. Results indicated that the bioactivity of all of samples with different Mg content was improved compared with the pure FA. However, the mechanism of bioactivity is different and depends on the amount of Mg substitution. Finally, cell culture suggested that the addition of Mg(2+) has no adverse effect and Mg-FA samples have good biocompatibility. The Mg-FA material shows potential in satisfying the requirements of biomedical applications. PMID:27524005

  4. Effects of Calcination on Structural, Photocatalytic Properties of TiO2 Nanopowders Via TiCl4 Hydrolysis

    NASA Astrophysics Data System (ADS)

    Khalid, N. R.; Ahmed, E.; Ikram, M.; Ahmad, M.; Phoenix, D. A.; Elhissi, A.; Ahmed, W.; Jackson, M. J.

    2013-02-01

    Photocatalytic degradation of methyl orange (MO) in water was examined using TiO2 nanopowders under solar irradiation. These photocatalysts were successfully synthesized by hydrolysis of titanium tetra chloride (TiCl4) in the temperature range of 70-95 °C and calcined at higher temperatures of between 400 and 900 °C. The samples prepared were characterized using x-ray powder diffraction, scanning electron microscope (SEM) and Fourier transform infrared spectrophotometer (FTIR). UV-Vis spectrometer was used for analyzing the concentration of MO in solution at different time intervals during the photodegradation experiment. Parameters affecting the photodegradation rate such as catalyst crystallinity, concentration of the catalyst, MO concentration, and pH of the solution have been investigated. The results indicate that TiO2 nanopowder was antase at low calcination temperatures in the range of 400-500 °C. The sample calcined at 600 °C is composed of both anatase and rutile phase. Further increase in the temperature enhanced the intensities of diffraction peaks of the rutile phase. The size of the crystallites for all the samples prepared were found to be in the 6-13 nm range and from SEM micrographs it was in the range of 19-43 nm. The mixture of both phases exhibited a higher photoactivity in comparison with pure anatase or rutile catalysts.

  5. Photocatalytic removal of Cu ions from aqueous Cu-EDTA solution using solution combusted zinc oxide nanopowder.

    PubMed

    Lee, Jae Chun; Kim, Hong-Sick; Lee, Ju-Hyeon; Park, Sung

    2008-10-01

    Nano-sized ZnO powder was prepared by "solution-combustion method (SCM)." The ZnO powder using Zn(OH)2 and glycine as an oxidant and a fuel (F/O = 0.8), showed good powder characteristics, such as average grain size of 30 nm and the specific surface area of 120 m2/g. and it was used as a semiconductor photocatalyst to remove Cu ions from aqueous Cu-EDTA solution. The result was then compared with other semiconductor photocatalyst powders such as titanium dioxide (TiO2) powder (P25, Degussa) and TiO2 powder prepared by homogeneous precipitation process at low temperature (HPPLT). The SCM ZnO nanopowder showed excellent photocatalytic properties. The Cu++ ions were completely removed from the solution within 90 min. However, for the other two powders, no complete removal of the ions was observed within the reaction time of 180 min. The ZnO powder synthesized at the fuel/oxidant ratio of 0.8, showed higher PL intensity at UV region than the other photocatalytic powders. The superior photoreduction ability of SCM ZnO nanopowder might be due to its excellent UV absorption capacity. PMID:19198439

  6. Enhancement in the antibacterial efficiency of ZnO nanopowders by tuning the shape of the nanograins through fluorine doping

    NASA Astrophysics Data System (ADS)

    Ravichandran, K.; Snega, S.; Jabena Begum, N.; Swaminathan, K.; Sakthivel, B.; Rene Christena, L.; Chandramohan, G.; Ochiai, Shizuyasu

    2014-05-01

    Fluorine doped ZnO nanopowders were synthesized from starting solutions having different doping levels of F (0, 5, … , 20 at.%) using a simple soft chemical route and the effects of the doping level on the structural, optical, surface morphological and antibacterial properties were investigated. The XRD studies reveal that all the products have preferential orientation along the (1 0 1) plane. The PL studies show that all the samples exhibit strong visible emission with a peak at 425 nm. The enhancement in the visible emission indicates an increasing number of surface defects caused by the doping of F. The obtained FTIR spectra confirm the incorporation of F into ZnO lattice. From the SEM studies, it is observed that the ZnO nanowires formed at 10 at.% of F doping level exhibit excellent antibacterial activities. Antibacterial activity of F doped ZnO nanopowders against Staphylococcus aureus was found to be significantly higher than that against the Escherichia coli and Pseudomonas aeruginosa micro-organisms. All the physical properties were corroborated well with the findings related to antibacterial activity. Finally, we conclude that, the analysis of all the results shows that F doping level of 10 at.% is optimal in all respects and is suitable for antibacterial applications.

  7. Synthesis of 8YSZ-LSGM Composite Thick Film Ceramics for Solid Electrolyte From Nanopowder Utilizing Local Zircon Prepared Using Sol Gel Process

    SciTech Connect

    Syarif, Dani Gustaman; Soepriyanto, Syoni; Korda, Akhmad; Ismunandar

    2010-10-24

    Thick film ceramics of 8% mol Y{sub 2}O{sub 3} doped-ZrO{sub 2}(8YSZ)-La{sub 0.8}Sr{sub 0.2}Ga{sub 0.2}Mg{sub 0.8}O{sub 3}(LSGM) composite for solid electrolyte have been synthesized from nanopowder. Concentration of LSGM was 0 and 10% weight. A paste for the thick films was made from 8YSZ nanopowder prepared using sol gel method and LSGM powder prepared by solid state reaction. Precursors for the 8YSZ nanopowder preparation were ZrOCl{sub 2{center_dot}}8H{sub 2}O derived from local zircon as byproduct of Tin processing at Bangka Island using caustic fusion method, and Y(NO{sub 3}){sub 3}. The thick films were produced by screen printing technique on alumina substrates. The films were sintered at 1500 deg. C for 2 hours in air. X-ray diffraction (XRD) data showed that the nanopowder of 8YSZ was well produced with broad peaks. The particle size of the 8YSZ powder was about 12 nm as calculated using Debye Scherrer method. The thick films of 8YSZ and 8YSZ-LSGM (90:10 in weight %) composite could be produced, however, the films still contain voids. The ionic conductance of the YSZ-10LSGM films was smaller than that of the YSZ films.

  8. Preparation of Carbon-Doped TiO2 Nanopowder Synthesized by Droplet Injection of Solution Precursor in a DC-RF Hybrid Plasma Flow System

    NASA Astrophysics Data System (ADS)

    Jang, Juyong; Takana, Hidemasa; Ando, Yasutaka; Solonenko, Oleg P.; Nishiyama, Hideya

    2013-08-01

    Carbon-doped titanium dioxide nanopowder has received much attention because of its higher photocatalytic performance, which is practically activated not only by UV, but also by visible light irradiation. In the present study, C-TiO2 nanopowder was synthesized by droplet injection of solution precursor in a DC-RF hybrid plasma flow system, resulting in higher photocatalytic performance even under visible light irradiation. In-flight C-TiO2 nanoparticles reacted with the high concentration of carbon in plasma flow and were then deposited on the surfaces of two quartz tubes in the upstream and downstream regions of this system. The collected C-TiO2 nanopowder contained anatase-rutile mixed-phase TiO2 and TiC, the contents of which depended on the location of the powder collection, the temperature, and the duration of plasma treatment. Highly functional C-TiO2 nanopowder collected in the downstream region exhibited a higher degradation rate of methylene blue than that of single-phase anatase TiO2, even under visible light irradiation, in spite of being TiC.

  9. Preparation of Y2O3:Eu3+, Tb3+ nanopowders with tunable luminescence by ammonium bicarbonate co-precipitation method

    NASA Astrophysics Data System (ADS)

    Shi, Hui; Zhang, Xi-Yan; Wang, Neng-Li; Dong, Wei-Li; Mi, Xiao-Yun

    2015-09-01

    Y2O3:Eu3+, Tb3+ nanopowders were prepared by co-precipitation method with NH4HCO3 as precipitant. The nanopowders with different calcined temperatures and Eu3+/Tb3+ doped ratio were characterized by X-ray Diffraction (XRD), scanning electron microscopy (SEM) and fluorescence spectrophotometer. The results showed that the nanopowders calcined at 1100°C for 2 h had a uniform distribution, high purity and good dispersibility. The particle size was in the range of 60-80 nm. The excitation spectra of Eu3+/Tb3+ co-doped phosphors were wide. The phosphors could emit the green light at the peak of 543 nm and the red light at the peak of 611 nm simultaneously under 276 nm or 300 nm excited. Because of the energy transfer between Tb3+ and Eu3+, the 543 nm emission of Tb3+ ion was weakened while the 611 nm emission of Eu3+ enhanced. The emissive colors of Y2O3:Eu3+, Tb3+ nanopowders could be adjusted from yellow-green to orange-red by changing the Eu3+/Tb3+ doping ratio.

  10. Effects of size-controlled TiO2 nanopowders synthesized by chemical vapor condensation process on conversion efficiency of dye-sensitized solar cells.

    PubMed

    Kim, Woo-Byoung; Lee, Jai-Sung

    2013-07-01

    To investigate the microstructural effects of the synthesized TiO2 nanopowders such as particle size, specific surface area, pore size and pore distributions for the application of an anode material of dye-sensitized solar cells (DSSC), size-controlled and well-dispersed TiO2 nanopowders were synthesized by chemical vapor condensation (CVC) process in the range of 800-1000 degreesC under a pressure of 50 mbar. The average particle size of synthesized TiO2 nanopowders was increased with increasing temperature from 13 nm for 800 degreesC, 15 nm for 900 degreesC and 26 nm. The specific surface area of synthesized nanoparticles were measured as 119.1 m2/g for 800 degreesC, 104.7 m2/g for 900 degreesC and 59.5 m2/g for 1000 degreesC, respectively. The conversion efficiency values (eta%) of DSSC with the synthesized TiO2 nanopowders at 800 degreesC, 900 degreesC, and 1000 degreesC were 2.59%, 5.96% and 3.66%, respectively. The highest conversion efficiency obtained in the 900 degreesC (5.96%) sample is thought to be attributable to homogeneous particle size and pore distributions, large specific surface area, and high transmittance in regions of dye absorption wavelength. PMID:23901483

  11. Outcomes following ossicular chain reconstruction with composite prostheses: hydroxyapatite-polyethylene vs. hydroxyapatite-titanium.

    PubMed

    Hahn, Yoav; Bojrab, Dennis I

    2013-06-01

    We conducted a retrospective study to compare the results of ossicular chain reconstruction (OCR) with two types of composite prosthesis: a hydroxyapatite-polyethylene (HAPEX) implant and a hydroxyapatite-titanium (HATi) prosthesis. We reviewed the records of 222 patients-104 males and 118 females, aged 8 to 79 years (mean: 39.7)-who had undergone OCR for ossicular chain dysfunction and who met our eligibility criteria. In addition to demographic data and the type of prosthesis, we compiled information on pre- and postoperative audiometric findings, the underlying diagnosis, the timing of surgery (primary, planned, or revision), the type of surgery (tympanoplasty alone, tympanoplasty with antrotomy, intact-canal-wall tympanomastoidectomy, or canal-wall-down tympanomastoidectomy), the extent of reconstruction (partial or total), the use of the malleus, the use of a tragal cartilage graft, and evidence of extrusion. Of the 222 patients, 46 had undergone insertion of either a partial (n = 36) or total (n = 10) ossicular replacement prosthesis (PORP and TORP, respectively) made with HAPEX, and 176 had received a PORP (n = 101) or TORP (n = 75) made with HATi. Postoperatively, the mean air-bone gap (ABG) was 14.0 dB in the HAPEX group and 14.7 dB in the HATi group, which was not a significant difference (p = 0.61). Postoperative success (ABG ≤20 dB) with PORP was obtained in 30 of the 36 patients in the HAPEX group (83.3%) and in 87 of the 101 patients in the HATi group (86.1%), while success with TORP was achieved in 7 of 10 HAPEX patients (70.0%) and 56 of 75 HATi patients (74.7%); there was no significant difference in either PORP or TORP success rates between the HAPEX and HATi groups (p = 0.32). A significantly better hearing result was obtained when the malleus was used in reconstruction (p = 0.035), but the use of tragal cartilage led to a significantly worse outcome (p = 0.026). Revision surgery was associated with a significantly worse postoperative result (p

  12. Production and thermal stability of pure and Cr3+ -doped hydroxyapatite

    NASA Astrophysics Data System (ADS)

    de Araujo, T. S.; de Souza, S. O.; de Sousa, E. M. B.; Araújo, M. S.

    2010-11-01

    Hydroxyapatite (HAP) have been used as starting material for biomedical applications. The pure and Cr3+ -doped hydroxyapatite were prepared by chemical precipitation reactions at 100, 500 e 800 °C in order to investigate the thermal stability of these materials. The characterization of the thermal behavior of this phosphate, especially on the structural changes with heating, is very important for production of sunscreens The powders were characterized using chemical analysis: X-ray diffraction (XRD) and thermal analysis. The present study was successful in the preparation of pure hydroxyapatite and chromium substituted hydroxyapatites with good thermal stability and nanoparticles formation.

  13. Structure of Biocompatible Coatings Produced from Hydroxyapatite Nanoparticles by Detonation Spraying

    NASA Astrophysics Data System (ADS)

    Nosenko, Valentyna; Strutynska, Nataliia; Vorona, Igor; Zatovsky, Igor; Dzhagan, Volodymyr; Lemishko, Sergiy; Epple, Matthias; Prymak, Oleg; Baran, Nikolai; Ishchenko, Stanislav; Slobodyanik, Nikolai; Prylutskyy, Yuriy; Klyui, Nickolai; Temchenko, Volodymyr

    2015-12-01

    Detonation-produced hydroxyapatite coatings were studied by scanning electron microscopy (SEM), X-ray powder diffraction (XRD), Raman spectroscopy, and electron paramagnetic resonance (EPR) spectroscopy. The source material for detonation spraying was a B-type carbonated hydroxyapatite powder. The coatings consisted of tetracalcium phosphate and apatite. The ratio depended slightly on the degree of crystallinity of the initial powder and processing parameters of the coating preparation. The tetracalcium phosphate phase was homogeneous; the apatite phase contained defects localized on the sixfold axis and consisted of hydroxyapatite and oxyapatite. Technological factors contributing to the transformation of hydroxyapatite powder structure during coating formation by detonation spraying are discussed.

  14. Development of lattice-inserted 5-Fluorouracil-hydroxyapatite nanoparticles as a chemotherapeutic delivery system.

    PubMed

    Tseng, Ching-Li; Chen, Jung-Chih; Wu, Yu-Chun; Fang, Hsu-Wei; Lin, Feng-Huei; Tang, Tzu-Piao

    2015-10-01

    Developing an effective vehicle for cancer treatment, hydroxyapatite nanoparticles were fabricated for drug delivery. When 5-Fluorouracil, a major chemoagent, is combined with hydroxyapatite nanocarriers by interclay insertion, the modified hydroxyapatite nanoparticles have superior lysosomal degradation profiles, which could be leveraged as controlled drug release. The decomposition of the hydroxyapatite nanocarriers facilitates the release of 5-Fluorouracil into the cytoplasm causing cell death. Hydroxyapatite nanoparticles with/without 5-Fluorouracil were synthesized and analyzed in this study. Their crystallization properties and chemical composition were examined by X-ray diffraction and Fourier transforms infrared spectroscopy. The 5-Fluorouracil release rate was determined by UV spectroscopy. The biocompatibility of hydroxyapatite-5-Fluorouracil extraction solution was assessed using 3T3 cells via a WST-8 assay. The effect of hydroxyapatite-5-Fluorouracil particles which directly work on the human lung adenocarcinoma (A549) cells was evaluated by a lactate dehydrogenase assay via contact cultivation. A 5-Fluorouracil-absorbed hydroxyapatite particles were also tested. Overall, hydroxyapatite-5-Fluorouracils were prepared using a co-precipitation method wherein 5-Fluorouracil was intercalated in the hydroxyapatite lattice as determined by X-ray diffraction. Energy dispersive scanning examination showed the 5-Fluorouracil content was higher in hydroxyapatite-5-Fluorouracil than in a prepared absorption formulation. With 5-Fluorouracil insertion in the lattice, the widths of the a and c axial constants of the hydroxyapatite crystal increased. The extraction solution of hydroxyapatite-5-Fluorouracil was nontoxic to 3T3 cells, in which 5-Fluorouracil was not released in a neutral phosphate buffer solution. In contrast, at a lower pH value (2.5), 5-Fluorouracil was released by the acidic decomposition of hydroxyapatite. Finally, the results of the lactate

  15. Structure of Biocompatible Coatings Produced from Hydroxyapatite Nanoparticles by Detonation Spraying.

    PubMed

    Nosenko, Valentyna; Strutynska, Nataliia; Vorona, Igor; Zatovsky, Igor; Dzhagan, Volodymyr; Lemishko, Sergiy; Epple, Matthias; Prymak, Oleg; Baran, Nikolai; Ishchenko, Stanislav; Slobodyanik, Nikolai; Prylutskyy, Yuriy; Klyui, Nickolai; Temchenko, Volodymyr

    2015-12-01

    Detonation-produced hydroxyapatite coatings were studied by scanning electron microscopy (SEM), X-ray powder diffraction (XRD), Raman spectroscopy, and electron paramagnetic resonance (EPR) spectroscopy. The source material for detonation spraying was a B-type carbonated hydroxyapatite powder. The coatings consisted of tetracalcium phosphate and apatite. The ratio depended slightly on the degree of crystallinity of the initial powder and processing parameters of the coating preparation. The tetracalcium phosphate phase was homogeneous; the apatite phase contained defects localized on the sixfold axis and consisted of hydroxyapatite and oxyapatite. Technological factors contributing to the transformation of hydroxyapatite powder structure during coating formation by detonation spraying are discussed. PMID:26625888

  16. On the assessment of hydroxyapatite fluoridation by means of Raman scattering

    SciTech Connect

    Campillo, M.; Valiente, M.; Lacharmoise, P. D.; Reparaz, J. S.; Goni, A. R.

    2010-06-28

    Hydroxyapatite is the main mineral component of bones and teeth. Fluorapatite, a bioceramic that can be obtained from hydroxyapatite by chemical substitution of the hydroxide ions with fluoride, exhibits lower mineral solubility and larger mechanical strength. Despite the widespread use of fluoride against caries, a reliable technique for unambiguous assessment of fluoridation in in vitro tests is still lacking. Here we present a method to probe fluorapatite formation in fluoridated hydroxyapatite by combining Raman scattering with thermal annealing. In synthetic minerals, we found that effectively fluoride substituted hydroxyapatite transforms into fluorapatite only after heat treatment, due to the high activation energy for this first order phase transition.

  17. Hydroxyapatite/poly(epsilon-caprolactone) double coating on magnesium for enhanced corrosion resistance and coating flexibility.

    PubMed

    Jo, Ji-Hoon; Li, Yuanlong; Kim, Sae-Mi; Kim, Hyoun-Ee; Koh, Young-Hag

    2013-11-01

    Hydroxyapatite was deposited on pure magnesium (Mg) with a flexible poly(ε-caprolactone) interlayer to reduce the corrosion rate of Mg and enhance coating flexibility. The poly(ε-caprolactone) interlayer was uniformly coated on Mg by a spraying method, followed by hydroxyapatite deposition on the poly(ε-caprolactone) using an aerosol deposition method. In scanning electron microscopy observations, inorganic/organic composite-like structure was observed between the hydroxyapatite and poly(ε-caprolactone) layers, resulting from the collisions of hydroxyapatite particles into the poly(ε-caprolactone) matrix at the initial stage of the aerosol deposition. The corrosion resistance of the coated Mg was examined using potentiodynamic polarization tests. The hydroxyapatite/poly(ε-caprolactone) double coating remarkably improved the corrosion resistance of Mg in Hank's solution. In the in vitro cell tests, the coated Mg showed better cell adhesion compared with the bare Mg due to the reduced corrosion rate and enhanced biocompatibility. The stability and flexibility of hydroxyapatite/poly(ε-caprolactone) double coating was investigated by scanning electron microscopy inspections after the coated Mg was deformed. The hydroxyapatite coating on the poly(ε-caprolactone) interlayer revealed enhanced coating stability and flexibility without cracking or delamination during bending and stretching compared with the hydroxyapatite single coating. These results demonstrated that the hydroxyapatite/poly(ε-caprolactone) double coating significantly improved the surface corrosion resistance of Mg and enhanced coating flexibility for use of Mg as a biodegradable implant. PMID:23241964

  18. On the assessment of hydroxyapatite fluoridation by means of Raman scattering

    NASA Astrophysics Data System (ADS)

    Campillo, M.; Lacharmoise, P. D.; Reparaz, J. S.; Goñi, A. R.; Valiente, M.

    2010-06-01

    Hydroxyapatite is the main mineral component of bones and teeth. Fluorapatite, a bioceramic that can be obtained from hydroxyapatite by chemical substitution of the hydroxide ions with fluoride, exhibits lower mineral solubility and larger mechanical strength. Despite the widespread use of fluoride against caries, a reliable technique for unambiguous assessment of fluoridation in in vitro tests is still lacking. Here we present a method to probe fluorapatite formation in fluoridated hydroxyapatite by combining Raman scattering with thermal annealing. In synthetic minerals, we found that effectively fluoride substituted hydroxyapatite transforms into fluorapatite only after heat treatment, due to the high activation energy for this first order phase transition.

  19. [FTIR and XRD analysis of hydroxyapatite from fossil human and animal teeth in Jinsha Relict, Chengdu].

    PubMed

    Huang, Cheng-min; Zhang, Qing; Bai, Song; Wang, Cheng-shan

    2007-12-01

    Diagenetic effect during burial on the hydroxyapatite in enamel and dentin from fossil human and animal teeth was examined, using X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR). For the enamel and dentin of all fossil teeth, XRD patterns exhibit bulge line and overlap between major reflections of hydroxyapatite, and the crystallinity of hydroxyapatite is low. For each infrared spectrum, H2O and OH(-) have distinct peaks of absorbance, and PO4(3-) and CO3(2-) ions have intensive infrared vibration modes at the fundamental wave numbers. The component of hydroxyapatite of all fossil teeth is similar to the modern biological hydroxyapatite. Furthermore, the index (PCI) which reflects the hydroxyapatite crystallinity of each sample ranges from 2.4 to 4.0 while the index (BPI) reflecting the amount of type B carbonate to phosphate indicates that the values of CO3(2-) content in hydroxyapatite are rather high, accordingly the crystallinity of all fossil hydroxyapatites are poor. It could be concluded that little alteration of hydroxyapatites from fossil human and animal teeth occurred in the process of diagenesis in Jinsha Relict, Chengdu, China. PMID:18330282

  20. X-ray photoelectron spectroscopy analysis for the chemical impact of solvent addition rate on electromagnetic shielding effectiveness of HCl-doped polyaniline nanopowders

    SciTech Connect

    Tantawy, Hesham Ramzy; Aston, D. Eric; Kengne, Blaise-Alexis F.; McIlroy, David N.; Qiang, You; Nguyen, Tai; Heo, Deukhyoun

    2015-11-07

    An in-depth analysis of the chemical functionality in HCl-doped polyaniline (PANI) nanopowders is discussed through interpretations of x-ray photoelectron spectra. The distinctions between three PANI sample types, produced under varied synthesis conditions, are compared on the basis correlations between newly collected electron spectra for chemical analysis (or also x-ray photoelectron spectroscopy) and electromagnetic (EM) shielding effectiveness (SE) within two frequency bands (100–1500 MHz and ∼2–14 GHz). The findings are discussed with reference to previous data analysis of electrical conductivities and Raman and UV-vis spectra analyzed from replicates of the same PANI nanopowders, where only the 8–12 GHz range for SE was tested. They further corroborate previous results for limited-solvent conditions that enhance EM shielding. The three nanopowder types show distinctive differences in polaron, bipolaron, and polar lattice contributions. The collective findings describe the chemical connections between controlling and, most importantly, limiting the available solvent for polymerization with simultaneously doping and how it is that the newly developed solvent-limited approach for HCl-PANI nanopowders provides better shielding than traditionally solvent-rich methods by having more extended and perhaps even faster polaron delocalization than other PANI-based products. The maximum oxidation (50%) and doping (49%) levels obtained in the solvent-free nanopowders also produced the highest SE values of 37.3 ± 3.7 dB (MHz band) and 68.6 ± 4.6 dB (GHz band)

  1. X-ray photoelectron spectroscopy analysis for the chemical impact of solvent addition rate on electromagnetic shielding effectiveness of HCl-doped polyaniline nanopowders

    NASA Astrophysics Data System (ADS)

    Tantawy, Hesham Ramzy; Kengne, Blaise-Alexis F.; McIlroy, David N.; Nguyen, Tai; Heo, Deukhyoun; Qiang, You; Aston, D. Eric

    2015-11-01

    An in-depth analysis of the chemical functionality in HCl-doped polyaniline (PANI) nanopowders is discussed through interpretations of x-ray photoelectron spectra. The distinctions between three PANI sample types, produced under varied synthesis conditions, are compared on the basis correlations between newly collected electron spectra for chemical analysis (or also x-ray photoelectron spectroscopy) and electromagnetic (EM) shielding effectiveness (SE) within two frequency bands (100-1500 MHz and ˜2-14 GHz). The findings are discussed with reference to previous data analysis of electrical conductivities and Raman and UV-vis spectra analyzed from replicates of the same PANI nanopowders, where only the 8-12 GHz range for SE was tested. They further corroborate previous results for limited-solvent conditions that enhance EM shielding. The three nanopowder types show distinctive differences in polaron, bipolaron, and polar lattice contributions. The collective findings describe the chemical connections between controlling and, most importantly, limiting the available solvent for polymerization with simultaneously doping and how it is that the newly developed solvent-limited approach for HCl-PANI nanopowders provides better shielding than traditionally solvent-rich methods by having more extended and perhaps even faster polaron delocalization than other PANI-based products. The maximum oxidation (50%) and doping (49%) levels obtained in the solvent-free nanopowders also produced the highest SE values of 37.3 ± 3.7 dB (MHz band) and 68.6 ± 4.6 dB (GHz band).

  2. Osteogenesis with hematopoiesis simulating infection in a hydroxyapatite orbital implant.

    PubMed

    Jordan, David R; Belliveau, Michel J; Brownstein, Seymour; Padmore, Ruth F

    2009-01-01

    A 28-year-old woman underwent secondary orbital implant surgery with placement of a hydroxyapatite implant. Over the next 7 years she underwent 3 drilling procedures. She began having copious discharge 1 year after the last drilling procedure. She was seen on numerous occasions with socket discharge, unresponsive to a variety of topical and oral antibiotics. Clinically, with the conjunctiva diffusely inflamed, the implant tender to touch, and the presence of a pyogenic granuloma, implant infection was suspected and the implant subsequently removed. Histopathologic assessment revealed widespread lamellar bone formation, including focal areas of marrow with active extramedullary hematopoiesis. There was no evidence of an inflammatory process or infection. Postoperatively the patient's symptoms and signs resolved. Extramedullary hematopoiesis within hydroxyapatite implants is rare. Porous orbital implant infection is also rare. Osteogenesis with extramedullary hematopoiesis simulating implant infection has not previously been reported. PMID:19273939

  3. Influence of Barium Hexaferrite on Magnetic Properties of Hydroxyapatite Ceramics.

    PubMed

    Jarupoom, P; Jaita, P

    2015-11-01

    Hydroxyapatite (HA) powders was derived from natural bovine bone by sequence of thermal processes. The barium hexaferrite (BF) find magnetic powders were added into HA powders in ratio of 1-3 vol.%. The HA-BF ceramics were prepared by a solid state reaction method and sintered at 1250 degrees C for 2 h. Effects of BF additive on structural, physical and magnetic properties of HA ceramics were investigated. X-ray diffraction revealed that all HA-BF samples showed a main phase of high purity hydroxyapatite [Ca10(PO4)6(OH)2] with calcium and phosphate molar ratio of 1.67. The addition of BF into HA inhibited grain growth and caused an improvement of mechanical properties. The M-H hysteresis loops also showed an improvement in magnetic behavior for higher content of BF. Moreover, in vitro bioactivity test indicated that the 2-3 vol.% sample may be suitable for biological applications. PMID:26726671

  4. Nanocrystalline hydroxyapatite prepared under various pH conditions

    NASA Astrophysics Data System (ADS)

    Palanivelu, R.; Mary Saral, A.; Ruban Kumar, A.

    2014-10-01

    Hydroxyapatite (HAP) has sovereign biomedical application due to its excellent biocompatibility, chemical and crystallographic similitude with natural human bone. In this present work, we discussed about the role of pH in the synthesis of calcium phosphate compound using calcium nitrate tetrahydrate and di-ammonium hydrogen phosphate as starting materials by chemical precipitation method assisted with ultrasonic irradiation technique. 5% polyethylene glycol (PEG600) is added along with the precursors under various pH condition of 7, 9 and 11 respectively. The functional group analysis, crystallized size and fraction of crystallized size are confirmed using Fourier Transformation Infra-Red spectroscopy and X-ray diffraction pattern. Morphological observations are done by scanning electron microscope. The results revealed the presence of nanocrystalline hydroxyapatite at pH above 9.

  5. Dissolution rates of carbonated hydroxyapatite in hydrochloric acid.

    PubMed

    Hankermeyer, Christine R; Ohashi, Kevin L; Delaney, David C; Ross, John; Constantz, Brent R

    2002-02-01

    Osteoclasts have been shown to dissolve efficiently and effectively the mineral phase of bone by locally controlling the environment surrounding the cell. Although this mineral phase has been identified and well characterized as carbonated hydroxyapatite, there is little understanding of the factors that affect the dissolution properties of this mineral phase. Mimicking the mechanism by which osteoclasts dissolve the mineral phase of bone may provide insight into methods for the decalcification of atherosclerotic mineral deposits in the vascular system. Accordingly, a detailed characterization of the effects of various chemical and mechanical parameters on the dissolution of carbonated hydroxyapatite mineral was investigated in this study. Increases in the mineral dissolution rate (2-10 times) were associated with increases in dissolving solution [H+], osmolality, temperature, and flow rate. Mineral dissolution rate increases (5-8 times) were associated with greater surface area of the mineral and mechanical agitation of the dissolving solution. PMID:11771694

  6. Antimicrobial and cytotoxicity evaluation of aliovalent substituted hydroxyapatite

    NASA Astrophysics Data System (ADS)

    Shanmugam, Sumathi; Gopal, Buvaneswari

    2014-06-01

    Aliovalent ion substituted hydroxyapatite of formulae BiNaCa3(PO4)3OH, Bi0.5M0.5Ca4(PO4)3OH (M = K, Ag) were synthesized and characterized. Antimicrobial properties of these synthesized materials were studied quantitatively by spread plate method against the microorganisms Escherichia coli (gram negative bacteria), Staphylococcus aureus (gram positive bacteria) and Candida albicans (yeast). Among the substituted hydroxyapatite compounds bismuth and silver substituted compound of formula Bi0.5Ag0.5Ca4(PO4)3OH shown excellent activity against all the three organisms. Cytotoxicity study was carried out against mouse fibroblast NIH-3T3 cell line in two different concentrations 10 μg/mL and 20 μg/mL by MTT assay method.

  7. Electrohydrodynamic coating of metal with nano-sized hydroxyapatite.

    PubMed

    Li, Xiang; Huang, Jie; Ahmad, Zeeshan; Edirisinghe, Mohan

    2007-01-01

    Electrohydrodynamic spray deposition of a hydroxyapatite (HA) suspension consisting of nano-particles has been used to create a hydroxyapatite coating comprising of nanostructured surface topography. Preliminary coating experiments were carried out on an Al substrate and 30 s was found to be the most appropriate coating time. HA coating on titanium for this duration was found to be well-bonded to the substrate after heat-treatment. A thickness of 2 mum was achieved in 30 s and formation of a bone-like apatite on the surface was detected after incubation of the heat-treated coated Ti in simulated body fluid. Therefore, we have uncovered a new procedure by which nano-biomaterials can be deposited on real orthopedic substrates to prepare bioactive thin coatings in a simple and easy manner. PMID:18032815

  8. Hydroxyapatite: Vibrational spectra and monoclinic to hexagonal phase transition

    NASA Astrophysics Data System (ADS)

    Slepko, Alexander; Demkov, Alexander A.

    2015-02-01

    Fundamental studies of biomaterials are necessary to deepen our understanding of their degradation and to develop cure for related illnesses. Biomineral hydroxyapatite Ca10(PO4)6(OH)2 is the main mineral constituent of mammal bone, and its synthetic analogues are used in biomedical applications. The mineral can be found in either hexagonal or monoclinic form. The transformation between these two phases is poorly understood, but knowing its mechanism may be critical to reversing processes in bone related to aging. Using density functional theory, we investigate the mechanisms of the phase transformation and estimate the transition temperature to be 680 K in fair agreement with the experimental temperature of 470 K. We also report the heat capacity of hydroxyapatite and a peculiarity in its phonon dispersion that might allow for non-destructive measurements of the crystal composition with applications in preventive medical screening for bone mineral loss.

  9. Gradient porous hydroxyapatite ceramics fabricated by freeze casting method

    NASA Astrophysics Data System (ADS)

    Zuo, Kai-hui; zhang, Yuan; Jiang, Dongliang; Zeng, Yu-Ping

    2011-04-01

    By controlling the cooling rates and the composition of slurries, the gradient porous hydroxyapatite ceramics are fabricated by the freeze casting method. According to the different cooling rate, the pores of HAP ceramics fabricated by gradient freeze casting are divided into three parts: one is lamellar pores, another is column pore and the last one is fine round pores. The laminated freeze casting is in favour of obtaining the gradient porous ceramics composed of different materials and the ceramics have unclear interfaces.

  10. Growth of one-dimensional single-crystalline hydroxyapatite nanorods

    NASA Astrophysics Data System (ADS)

    Ren, Fuzeng; Ding, Yonghui; Ge, Xiang; Lu, Xiong; Wang, Kefeng; Leng, Yang

    2012-06-01

    A facile, effective and template/surfactant-free hydrothermal route in the presence of sodium bicarbonate was developed to synthesize highly uniform single-crystalline hydroxyapatite (HA) nanorods with the lengths of several hundred nanometers and aspect ratio up to ˜20. One dimensional (1-D) growth and aspect ratio could be controlled by hydrothermal reaction time and temperature. The longitudinal axis, also the growth direction of the nanorods, is parallel to the [001] direction of HA hexagonal crystal structure.

  11. Advanced Microstructural Study of Suspension Plasma Sprayed Hydroxyapatite Coatings

    NASA Astrophysics Data System (ADS)

    Podlesak, Harry; Pawlowski, Lech; D'Haese, Romain; Laureyns, Jacky; Lampke, Thomas; Bellayer, Severine

    2010-03-01

    Fine, home-synthesized, hydroxyapatite powder was formulated with water and alcohol to obtain a suspension used to plasma spray coatings onto a titanium substrate. The deposition process was optimized using statistical design of 2 n experiments with two variables: spray distance and electric power input to plasma. X-ray diffraction (XRD) was used to determine quantitatively the phase composition of obtained deposits. Raman microscopy and electron probe microanalysis (EPMA) enabled localization of the phases in different positions of the coating cross sections. Transmission electron microscopic (TEM) study associated with energy-dispersive x-ray spectroscopy (EDS) enabled visualization and analysis of a two-zone microstructure. One zone contained crystals of hydroxyapatite, tetracalcium phosphate, and a phase rich in calcium oxide. This zone included lamellas, usually observed in thermally sprayed coatings. The other zone contained fine hydroxyapatite grains that correspond to nanometric and submicrometric solids from the suspension that were agglomerated and sintered in the cold regions of plasma jet and on the substrate.

  12. XANES Data on Trace Quantities of Iron in Hydroxyapatite Structures

    NASA Astrophysics Data System (ADS)

    Tabor-Morris, A.; Schaefer, B.

    2003-03-01

    Trace elements such as iron are of interest in both biologically and geologically formed apatites. They are thought to occupy substitutional sites at the concentration of about 200 ppm. Most likely metal atoms replace the calcium atom in one of two non-equivalent calcium sites. The inorganic mineral structure hydroxyapatite (which comprises 30% of human and animal bone) consists of Ca_5(OH)(PO_4)3 in a hexagonal crystal structure designated in Herman-Maugin crystallography notation as P63/m or as Number 176 in the International Tables of Crystallography (ITC). Hydroxyapatite formed under geological conditions has the same crystal structure. Hydroxyapatite can also be fabricated synthetically, but has limitations in terms of crystal growth size. The experimental technique of X-ray Absorption Near Edge Structure (XANES) and X-ray Absorption Fine-structure Spectroscopy (XAFS) were used to evaluate the oxidation state of iron. Data was taken at the X-9B line at the National Synchrotron Light Source at Brookhaven National Laboratory.

  13. XANES Data on Metal Ions in Hydroxyapatite Structures

    NASA Astrophysics Data System (ADS)

    Schaefer, Beth; Tabor-Morris, Anne; Simons, Adrian

    2004-03-01

    The experimental technique of X-ray Absorption Near Edge Structure (XANES) was used to compare the absorption edges of different oxidation states of iron, strontium, lead, copper and zinc in the inorganic mineral structure hydroxyapatite and fluoroapatite. Trace elements such as iron, copper, zinc, lead and strontium are of interest in both biologically and geologically formed apatites. They are thought to occupy substitutional sites at the concentration of about 200 ppm. These metal atoms replace the calcium atom in one of two non-equivalent calcium sites. Hydroxyapatite consists of Ca _5 (OH)(PO_4)3 in a hexagonal crystal structure. Hydroxyapatite formed under geological conditions has the same crystal structure. Data was taken at the X-9B line at the National Synchrotron Light Source at Brookhaven National Laboratory. Samples were obtained from Dr. Susan G. Sheridan, at the University of Notre Dame, Dr. Catherine Skinner from Yale University, Dr. John Rakovan at Miami University in Ohio, Dr. Richard Riman at Rutgers University.

  14. Calcium Deficient Hydroxyapatite for Medical Application Prepared by Hydrothermal Method

    NASA Astrophysics Data System (ADS)

    Ioku, Koji; Kamitakahara, Masanobu; Ikeda, Tohru

    2010-11-01

    Hydrothermal processing plays a key role in the synthesis of biomaterials with excellent biocompatibility in the physiological environment. Especially, calcium phosphates are paid to much attention for the regenerative medicine. Two kinds of porous materials of hydroxyapatite with 70% porosity were prepared. One of them is a newly developed calcium-deficient hydroxyapatite composed of rod-shaped particles of about 20 μm in length synthesized hydrothermally (HHA) and the other one is the stoichiometric hydroxyapatite (SHA) prepared by the conventional sintering method. These materials were used for animal implantation tests to compare these biological responses. In the rabbit femur, implanted HHA was slowly resorbed and then most of the implanted HHA was resorbed after 72 weeks. The implanted SHA was unresorbed throughout the experimental period. The volume of newly formed bone and the number of osteoclasts in the implanted region were significantly larger in HHA than in SHA after 24 weeks. Results in the present research suggested that the activity of osteoclasts correlated to the bone forming activity of osteoblasts. The method to synthesize biodegradable pure calcium-deficient HA is expected to provide adequate biodegradability and bone replaceability.

  15. Multifunctional hydroxyapatite nanofibers and microbelts as drug carriers.

    PubMed

    Hou, Zhiyao; Yang, Piaoping; Lian, Hongzhou; Wang, Lili; Zhang, Cuimiao; Li, Chunxia; Chai, Ruitao; Cheng, Ziyong; Lin, Jun

    2009-07-13

    Luminescent, mesoporous, and bioactive europium-doped hydroxyapatite (HAp:Eu(3+)) nanofibers and microbelts have been prepared by a combination of sol-gel and electrospinning processes with a cationic surfactant as template. The obtained multifunctional hydroxyapatite nanofibers and microbelts, which have mesoporous structure and red luminescence, were tested as drug carriers by investigating their drug-storage/release properties with ibuprofen (IBU) as model drug. X-ray diffraction, scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution (HR) TEM, FTIR spectroscopy, N(2) adsorption/desorption, photoluminescence (PL) spectra, and UV/Vis spectroscopy were used to characterize the structural, morphological, textural, and optical properties of the resulting samples. The results reveal that the multifunctional hydroxyapatites exhibit irregular mesostructure, and have fiberlike and beltlike morphologies with sizes of several hundred nanometers in width and several millimeters in length. The IBU-loaded HAp:Eu(3+) system shows red luminescence of Eu(3+) ((5)D(0)-(7)F(0,1,2)) under UV irradiation and controlled release of IBU. In addition, the emission intensity of Eu(3+) in the drug carrier system varies with the released amount of IBU, and thus drug release can be easily tracked and monitored by the change in luminescence intensity. PMID:19496099

  16. Controlled synthesis and thermal stability of hydroxyapatite hierarchical microstructures

    SciTech Connect

    Sun, Ruixue; Chen, Kezheng; Liao, Zhongmiao; Meng, Nan

    2013-03-15

    Highlights: ► Hydroxyapatite hierarchical microstructures have been synthesized by a facile method. ► The morphology and size of the building units of 3D structures can be controlled. ► The hydroxyapatite with 3D structure is morphologically and structurally stable up to 800 °C. - Abstract: Hydroxyapatite (HAp) hierarchical microstructures with novel 3D morphology were prepared through a template- and surfactant-free hydrothermal homogeneous precipitation method. Field emission scanning electron microscopy (FESEM), high-resolution transmission electron microscopy (HRTEM), and X-ray diffraction (XRD) were used to characterize the morphology and composition of the synthesized products. Interestingly, the obtained HAp with 3D structure is composed of one-dimensional (1D) nanorods or two-dimensional (2D) nanoribbons, and the length and morphology of these building blocks can be controlled through controlling the pH of the reaction. The building blocks are single crystalline and have different preferential orientation growth under different pH conditions. At low pH values, octacalcium phosphate (OCP) phase formed first and then transformed into HAp phase due to the increased pH value caused by the decomposition of urea. The investigation on the thermal stability reveals that the prepared HAp hierarchical microstructures are morphologically and structurally stable up to 800 °C.

  17. Synthesis of fluorapatite–hydroxyapatite nanoparticles and toxicity investigations

    PubMed Central

    Montazeri, N; Jahandideh, R; Biazar, Esmaeil

    2011-01-01

    In this study, calcium phosphate nanoparticles with two phases, fluorapatite (FA; Ca10(PO4)6F2) and hydroxyapatite (HA; Ca10(PO4)6(OH)2), were prepared using the solgel method. Ethyl phosphate, hydrated calcium nitrate, and ammonium fluoride were used, respectively, as P, Ca, and F precursors with a Ca:P ratio of 1:72. Powders obtained from the sol-gel process were studied after they were dried at 80°C and heat treated at 550°C. The degree of crystallinity, particle and crystallite size, powder morphology, chemical structure, and phase analysis were investigated by scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and Zetasizer experiments. The results of XRD analysis and FTIR showed the presence of hydroxyapatite and fluorapatite phases. The sizes of the crystallites estimated from XRD patterns using the Scherrer equation and the crystallinity of the hydroxyapatite phase were about 20 nm and 70%, respectively. Transmission electron microscope and SEM images and Zetasizer experiments showed an average size of 100 nm. The in vitro behavior of powder was investigated with mouse fibroblast cells. The results of these experiments indicated that the powders were biocompatibile and would not cause toxic reactions. These compounds could be applied for hard-tissue engineering. PMID:21499417

  18. Synthesis of fluorapatite-hydroxyapatite nanoparticles and toxicity investigations.

    PubMed

    Montazeri, N; Jahandideh, R; Biazar, Esmaeil

    2011-01-01

    In this study, calcium phosphate nanoparticles with two phases, fluorapatite (FA; Ca(10)(PO(4))(6)F(2)) and hydroxyapatite (HA; Ca(10)(PO(4))(6)(OH)(2)), were prepared using the solgel method. Ethyl phosphate, hydrated calcium nitrate, and ammonium fluoride were used, respectively, as P, Ca, and F precursors with a Ca:P ratio of 1:72. Powders obtained from the sol-gel process were studied after they were dried at 80°C and heat treated at 550°C. The degree of crystallinity, particle and crystallite size, powder morphology, chemical structure, and phase analysis were investigated by scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and Zetasizer experiments. The results of XRD analysis and FTIR showed the presence of hydroxyapatite and fluorapatite phases. The sizes of the crystallites estimated from XRD patterns using the Scherrer equation and the crystallinity of the hydroxyapatite phase were about 20 nm and 70%, respectively. Transmission electron microscope and SEM images and Zetasizer experiments showed an average size of 100 nm. The in vitro behavior of powder was investigated with mouse fibroblast cells. The results of these experiments indicated that the powders were biocompatible and would not cause toxic reactions. These compounds could be applied for hard-tissue engineering. PMID:21499417

  19. Comparison of the Weibull characteristics of hydroxyapatite and strontium doped hydroxyapatite.

    PubMed

    Yatongchai, Chokchai; Wren, Anthony W; Curran, Declan J; Hornez, Jean-Christophe; Mark R, Towler

    2013-05-01

    The effects of two strontium (Sr) additions, 5% and 10% of the total calcium (Ca) content, on the phase assemblage and Weibull statistics of hydroxyapatite (HA) are investigated and compared to those of undoped HA. Sintering was carried out in the range of 900-1200 °C in steps of 1000 °C in a conventional furnace. Sr content had little effect on the mean particulate size. Decomposition of the HA phase occurred with Sr incorporation, while β-TCP stabilization was shown to occur with 10% Sr additions. Porosity in both sets of doped samples was at a comparable level to porosity in the undoped HA samples, however the 5% Sr-HA samples displayed the greatest reduction in porosity with increasing temperature while the porosity of the 10% Sr-HA samples remain relatively constant over the full sintering temperature range. The undoped HA samples displayed the greatest Weibull strengths and the porosity was determined to be the major controlling factor. However, with the introduction of decompositional phases in the Sr-HA samples, the dependence of strength on porosity is reduced and the phase assemblage becomes the more dominant factor for Weibull strength. The Weibull modulus is relatively independent of the porosity in the undoped HA samples. The 5% Sr-HA samples experience a slight increase in Weibull modulus with porosity, indicating a possible relationship between the parameters. However the 10% Sr-HA samples show the highest Weibull modulus with a value of approximately 15 across all sintering temperatures. It is postulated that this is due to the increased amount of surface and lattice diffusion that these samples undergo, which effectively smooths out flaws in the microstructure, due to a saturation of Sr content occurring in grain boundary movement. PMID:23524073

  20. Characterization and inhibitive study of gel-grown hydroxyapatite crystals at physiological temperature

    NASA Astrophysics Data System (ADS)

    Parekh, Bharat; Joshi, Mihir; Vaidya, Ashok

    2008-04-01

    Hydroxyapatite is very useful for various biomedical applications, due to its chemical similarity with mineralized bone of human. Hydroxyapatite is also responsible for arthropathy (joint disease). In the present study, the growth of hydroxyapatite crystals was carried out by using single-diffusion gel growth technique in silica hydro gel media, at physiological temperature. The growth of hydroxyapatite crystals under slow and controlled environment in gel medium can be simulated in a simple manner to the growth in human body. The crystals, formed in the Liesegang rings, were characterized by powder XRD, FTIR and dielectric study. The diffusion study is also carried out for the hydroxyapatite crystals using the moving boundary model. The inhibitive influence of various Ayurvedic medicinal plant extracts such as Boswellia serrata gum resin , Tribulus terrestris fruits, Rotula aquatica roots, Boerhaavia diffusa roots and Commiphora wightii, on the growth of hydroxyapatite was studied. Roots of R. aquatica and B. diffusa show some inhibition of the hydroxyapatite crystals in vitro. This preclinical study will be helpful to design the therapy for prevention of hydroxyapatite-based ailments.

  1. Containment of uranium in the proposed Egyptian geologic repository for radioactive waste using hydroxyapatite.

    SciTech Connect

    Moore, Robert Charles; Hasan, Ahmed Ali Mohamed; Headley, Thomas Jeffrey; Sanchez, Charles Anthony; Zhao, Hongting; Salas, Fred Manuel; Hasan, Mahmoud A.; Holt, Kathleen Caroline

    2003-08-01

    Currently, the Egyptian Atomic Energy Authority is designing a shallow-land disposal facility for low-level radioactive waste. To insure containment and prevent migration of radionuclides from the site, the use of a reactive backfill material is being considered. One material under consideration is hydroxyapatite, Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2}, which has a high affinity for the sorption of many radionuclides. Hydroxyapatite has many properties that make it an ideal material for use as a backfill including low water solubility (K{sub sp} > 10{sup -40}), high stability under reducing and oxidizing conditions over a wide temperature range, availability, and low cost. However, there is often considerable variation in the properties of apatites depending on source and method of preparation. In this work, we characterized and compared a synthetic hydroxyapatite with hydroxyapatites prepared from cattle bone calcined at 500 C, 700 C, 900 C and 1100 C. The analysis indicated the synthetic hydroxyapatite was similar in morphology to 500 C prepared cattle hydroxyapatite. With increasing calcination temperature the crystallinity and crystal size of the hydroxyapatites increased and the BET surface area and carbonate concentration decreased. Batch sorption experiments were performed to determine the effectiveness of each material to sorb uranium. Sorption of U was strong regardless of apatite type indicating all apatite materials evaluated. Sixty day desorption experiments indicated desorption of uranium for each hydroxyapatite was negligible.

  2. Containment of uranium in the proposed Egyptian geologic repository for radioactive waste using hydroxyapatite.

    SciTech Connect

    Moore, Robert Charles; Hasan, Ahmed Ali Mohamed; Headley, Thomas Jeffrey; Sanchez, Charles Anthony; Zhao, Hongting; Salas, Fred Manuel; Hasan, Mahmoud A.; Holt, Kathleen Caroline

    2004-04-01

    Currently, the Egyptian Atomic Energy Authority is designing a shallow-land disposal facility for low-level radioactive waste. To insure containment and prevent migration of radionuclides from the site, the use of a reactive backfill material is being considered. One material under consideration is hydroxyapatite, Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2}, which has a high affinity for the sorption of many radionuclides. Hydroxyapatite has many properties that make it an ideal material for use as a backfill including low water solubility (K{sub sp}>10{sup -40}), high stability under reducing and oxidizing conditions over a wide temperature range, availability, and low cost. However, there is often considerable variation in the properties of apatites depending on source and method of preparation. In this work, we characterized and compared a synthetic hydroxyapatite with hydroxyapatites prepared from cattle bone calcined at 500 C, 700 C, 900 C and 1100 C. The analysis indicated the synthetic hydroxyapatite was similar in morphology to 500 C prepared cattle hydroxyapatite. With increasing calcination temperature the crystallinity and crystal size of the hydroxyapatites increased and the BET surface area and carbonate concentration decreased. Batch sorption experiments were performed to determine the effectiveness of each material to sorb uranium. Sorption of U was strong regardless of apatite type indicating all apatite materials evaluated. Sixty day desorption experiments indicated desorption of uranium for each hydroxyapatite was negligible.

  3. FORMATION OF CHLOROPYROMORPHITE IN A LEAD-CONTAMINATED SOIL AMENDED WITH HYDROXYAPATITE

    EPA Science Inventory

    To evaluate conversion of soil Pb to pyromorphite, a Pb contaminated soil collected adjacent to a historical smelter was reacted with hydroxyapatite in a traditional incubation experiment and in a dialysis system in which the soil and hydroxyapatite solids were separated by a dia...

  4. Synthesis and release of trace elements from hollow and porous hydroxyapatite spheres

    NASA Astrophysics Data System (ADS)

    Xia, Wei; Grandfield, Kathryn; Schwenke, Almut; Engqvist, Håkan

    2011-07-01

    It is known that organic species regulate fabrication of hierarchical biological forms via solution methods. However, in this study, we observed that the presence of inorganic ions plays an important role in the formation and regulation of biological spherical hydroxyapatite formation. We present a mineralization method to prepare ion-doped hydroxyapatite spheres with a hierarchical structure that is free of organic surfactants and biological additives. Porous and hollow strontium-doped hydroxyapatite spheres were synthesized via controlling the concentration of strontium ions in a calcium and phosphate buffer solution. Similarly, fluoride and silicon-doped hydroxyapatite spheres were synthesized. While spherical particle formation was attainable at low and high temperature for Sr-doped hydroxyapatite, it was only possible at high temperature in the F/Si-doped system. The presence of inorganic ions not only plays an important role in the formation and regulation of biological spherical hydroxyapatite, but also could introduce pharmaceutical effects as a result of trace element release. Such ion release results showed a sustained release with pH responsive behavior, and significantly influenced the hydroxyapatite re-precipitation. These ion-doped hydroxyapatite spheres with hollow and porous structure could have promising applications as bone/tooth materials, drug delivery systems, and chromatography supports.

  5. Ho:YAG transparent ceramics based on nanopowders produced by laser ablation method: Fabrication, optical properties, and laser performance

    NASA Astrophysics Data System (ADS)

    Bagayev, S. N.; Osipov, V. V.; Vatnik, S. M.; Shitov, V. A.; Vedin, I. A.; Platonov, V. V.; Steinberg, I. Sh.; Maksimov, R. N.

    2015-12-01

    We fabricate Ho:YAG transparent ceramics based on nanopowders produced by laser ablation method via two approaches. Higher transmittance (82% in the infrared region) is achieved in ceramics prepared with an additional round of pre-calcining before sintering. We evaluate the average volume of the scattering centers in the ceramics and their distribution along the sample depth by the direct count method using an optical microscope and by the novel method of collinear two-photon interband photoexcitation, respectively. The laser characteristics of the 1% Ho:YAG ceramics are investigated using an intracavity pumping scheme. The slope efficiency is ∼40% relative to the absorbed pumping power at 1.85 μm.

  6. Preparation and spectroscopy characterization of Eu:MgAl2O4 nanopowder prepared by modified Pechini method.

    PubMed

    Wiglusz, R J; Grzyb, T; Lis, S; Strek, W

    2009-10-01

    In the present work, a modified Pechini method was employed to prepare nanostructured MgAl2O4 spinel powders doped with Eu3+ ions. The XRD analyses demonstrated that the powders were single-phase spinel nanopowders with high crystallite dispersion. The average spinel particle size was determined to be approximately 15 nm for calcination at 700 degrees C, and approximately 20 at 1000 degrees C. The emission and excitation spectra measured for the samples calcinated at 700 and 1000 degrees C demonstrated characteristic spectra of Eu3+ ions as well as were measured the emission spectra of Eu2+ ions for the samples calcinated at 700 degrees C. The effect of MgAl2O4 grain sizes on luminescence properties was noticed. To explain these differences a detailed analysis of luminescence spectra by the Judd-Ofelt theory has been performed. PMID:19908456

  7. X-ray diffraction analysis of the effect of annealing temperature on the microstructure of magnesium oxide nanopowder

    NASA Astrophysics Data System (ADS)

    Soleimanian, V.; Aghdaee, S. R.

    2015-06-01

    In this study, nanocrystalline MgO powders were prepared using the sol-gel method and annealed in air over a temperature range of [400-700] °C. Various microstructural characteristics were determined using three different X-ray diffraction analysis approaches, i.e., modified Williamson-Hall, modified Warren-Averbach, and variance methods. The transmission electron microscopy micrographs were used to measure the size distributions of the MgO samples. The results obtained using the three different methods were in good agreement. At all temperatures, the main source of dislocation was edge type but as the annealing temperature increased, the crystallite size and dislocation density increased and decreased, respectively, thereby indicating that the crystal quality of the nanopowders was improved.

  8. Synthesis and structural characterization of Co2+ ions doped ZnO nanopowders by solid state reaction through sonication

    NASA Astrophysics Data System (ADS)

    Babu, B.; Rama Krishna, Ch.; Venkata Reddy, Ch.; Pushpa Manjari, V.; Ravikumar, R. V. S. S. N.

    2013-05-01

    Cobalt ions doped zinc oxide nanopowder was prepared at room temperature by a novel and simple one step solid-state reaction method through sonication in the presence of a suitable surfactant Sodium Lauryl Sulphate (SLS). The prepared powder was characterized by various spectroscopic techniques. Powder XRD data revealed that the crystal structure belongs to hexagonal and its average crystallite size was evaluated. From optical absorption data, crystal fields (Dq), inter-electronic repulsion parameters (B, C) were evaluated. By correlating optical and EPR spectral data, the site symmetry of Co2+ ion in the host lattice was determined as octahedral. Photoluminescence spectra exhibited the emission bands in ultraviolet and blue regions. The CIE chromaticity coordinates are also evaluated from the emission spectrum. FT-IR spectra showed the characteristic vibrational bands of Znsbnd O.

  9. Effect of different dopants Ba and Ag on the properties of SrTiO3 nanopowders

    NASA Astrophysics Data System (ADS)

    Ghasemifard, M.; Abrishami, M. E.; Iziy, M.

    Undoped and Ba and Ag-doped SrTiO3-based nanopowders (NPs) were successfully grown by a modified auto-combustion method. An optimum ratio of citric acid and nitric acid was used as the polymerization agent and fuel. The X-ray diffraction (XRD) results revealed that the products were crystalline with cubic and tetragonal structures. The particle aggregation state, nanoparticles size distribution, morphology and electrical properties were characterized by transmission electron microscopy (TEM), dynamic light scattering (DLS), atomic force microscopy (AFM) and ultraviolet-visible (UV-vis) were studied, respectively. Using the X-ray peak broadening and size-strain plot (SSP) method the crystallite sizes and lattice strain of the samples were investigated. The UV-vis absorption spectra revealed that the band gap of the STO-based has a strong absorption peak which lies in the UV region.

  10. Nanostructured MgTiO3 thick films obtained by electrophoretic deposition from nanopowders prepared by solar PVD

    NASA Astrophysics Data System (ADS)

    Apostol, Irina; Mahajan, Amit; Monty, Claude J. A.; Venkata Saravanan, K.

    2015-12-01

    A novel combination of solar physical vapor deposition (SPVD) and electrophoretic deposition (EPD) that was developed to grow MgTiO3 nanostructured thick films is presented. Obtaining nanostructured MgTiO3 thick films, which can replace bulk ceramic components, a major trend in electronic industry, is the main objective of this work. The advantage of SPVD is direct synthesis of nanopowders, while EPD is simple, fast and inexpensive technique for preparing thick films. SPVD technique was developed at CNRS-PROMES Laboratory, Odeillo-Font Romeu, France, while the EPD was performed at University of Aveiro - DeMAC/CICECO, Portugal. The nanopowders with an average crystallite size of about 30 nm prepared by SPVD were dispersed in 50 ml of acetone in basic media with addition of triethanolamine. The obtained well-dispersed and stable suspensions were used for carrying out EPD on 25 μm thick platinum foils. After deposition, films with thickness of about 22-25 μm were sintered in air for 15 min at 800, 900 and 1000 °C. The structural and microstructural characterization of the sintered thick films was carried out using XRD and SEM, respectively. The thickness of the sintered samples were about 18-20 μm, which was determined by cross-sectional SEM. Films sintered at 900 °C exhibit a dielectric constant, ɛr ∼18.3 and dielectric loss, tan δ ∼0.0012 at 1 MHz. The effects of processing techniques (SPVD and EPD) on the structure, microstructure and dielectric properties are reported in detail. The obtained results indicate that the thick films obtained in the present study can be promising for low loss materials for microwave and millimeter wave applications.

  11. Influence of Starting Powders on Hydroxyapatite Coatings Fabricated by Room Temperature Spraying Method.

    PubMed

    Seo, Dong Seok; Lee, Jong Kook; Hwang, Kyu Hong; Hahn, Byung Dong; Yoon, Seog Young

    2015-08-01

    Three types of raw materials were used for the fabrication of hydroxyapatite coatings by using the room temperature spraying method and their influence on the microstructure and in vitro characteristics were investigated. Starting hydroxyapatite powders for coatings on titanium substrate were prepared by a heat treatment at 1100 °C for 2 h of bovine bone, bone ash, and commercial hydroxyapatite powders. The phase compositions and Ca/P ratios of the three hydroxyapatite coatings were similar to those of the raw materials without decomposition or formation of a new phase. All hydroxyapatite coatings showed a honeycomb structure, but their surface microstructures revealed different features in regards to surface morphology and roughness, based on the staring materials. All coatings consisted of nano-sized grains and had dense microstructure. Inferred from in vitro experiments in pure water, all coatings have a good dissolution-resistance and biostability in water. PMID:26369193

  12. [In Situ Polymerization and Characterization of Hydroxyapatite/polyurethane Implanted Material].

    PubMed

    Gu, Muqing; Xiao, Fengjuan; Liang, Ye; Yue, Lin; Li, Song; Li, Lanlan; Feng, Feifei

    2015-08-01

    In order to improve the interfacial bonding strength of hydroxyapatite/polyurethane implanted material and dispersion of hydroxyapatite in the polyurethane matrix, we in the present study synthesized nano-hydroxyapatite/polyurethane composites by in situ polymerization. We then characterized and analyzed the fracture morphology, thermal stability, glass transition temperature and mechanical properties. We seeded MG63 cells on composites to evaluate the cytocompatibility of the composites. In situ polymerization could improve the interfacial bonding strength, ameliorate dispersion of hydroxyapatite in the properties of the composites. After adding 20 wt% hydroxyapatite into the polyurethane, the thermal stability was improved and the glass transition temperatures were increased. The tensile strength and maximum elongation were 6.83 MPa and 861.17%, respectively. Compared with those of pure polyurethane the tensile strength and maximum elongation increased by 236.45% and 143.30%, respectively. The composites were helpful for cell adhesion and proliferation in cultivation. PMID:26710455

  13. [Using Metronidazole and Hydroxyapatite for preventing dry socket after extraction of impacted mandibular 3rd molar

    PubMed

    Xue, Z X; Mao, T Q

    1993-03-01

    Dry socket is one of the most frequent complications after teeth extraction,especially in impacted mandibular third molars.The etilogy and prevention is not clear.This study id based on principles of clinical epidemiology.Randomized double-blind method was carried out in 549 patients to test the value of the prophylactic use of Hydroxyapatite,to test the value of the prophylactic use of Hydroxyapatite and Metronidazole,placed in the sockets of extracted impacted mandibular third molars.The results of the incidence of DS was 7.1% of Metronidazole treated sockets,and 2.1% of Hydroxyapatite treated sockets,It is concluded that Hydroxyapatite is an effective preventive factor for dry socket,The possible mechanism of Hydroxyapatite and the dry socket etiology were discussed. PMID:15159869

  14. Surface free energy predominates in cell adhesion to hydroxyapatite through wettability.

    PubMed

    Nakamura, Miho; Hori, Naoko; Ando, Hiroshi; Namba, Saki; Toyama, Takeshi; Nishimiya, Nobuyuki; Yamashita, Kimihiro

    2016-05-01

    The initial adhesion of cells to biomaterials is critical in the regulation of subsequent cell behaviors. The purpose of this study was to investigate a mechanism through which the surface wettability of biomaterials can be improved and determine the effects of biomaterial surface characteristics on cellular behaviors. We investigated the surface characteristics of various types of hydroxyapatite after sintering in different atmospheres and examined the effects of various surface characteristics on cell adhesion to study cell-biomaterial interactions. Sintering atmosphere affects the polarization capacity of hydroxyapatite by changing hydroxide ion content and grain size. Compared with hydroxyapatite sintered in air, hydroxyapatite sintered in saturated water vapor had a higher polarization capacity that increased surface free energy and improved wettability, which in turn accelerated cell adhesion. We determined the optimal conditions of hydroxyapatite polarization for the improvement of surface wettability and acceleration of cell adhesion. PMID:26952425

  15. Is hydroxyapatite a reliable fixation option in unicompartmental knee arthroplasty? A 5- to 13-year experience with the hydroxyapatite-coated unix prosthesis.

    PubMed

    Epinette, Jean-Alain; Manley, Michael T

    2008-10-01

    Hydroxyapatite-coated unicompartmental knee arthroplasty (UKA) is a debatable approach to unicompartmental knee arthritis because UKA isoften viewed as a short-term solution, at best, fora condition that will eventually require a total knee arthroplasty (TKA). Unicompartmental knee arthroplasty is a more technically demanding procedure than TKA, and appropriate patient selection, careful surgical technique, and correct choice of implant geometry are all critical components to its success. A fundamental issue surrounding UKA is whether hydroxyapatite-coated unicompartmental components can provide a long-term solution to unicondylar arthritis. We address this issue in the current study, which is based on a prospective series of 125 hydroxyapatite-coated Unix knee prostheses implanted consecutively between 1994 and 2002, with a 5-year minimum follow-up and a 13-year maximum follow-up. The results of our study indicate that uncemented hydroxyapatite-coated UKA can be successful in the long term. PMID:18979933

  16. Size-controlled hydroxyapatite nanoparticles as self-organized organic-inorganic composite materials.

    PubMed

    Rusu, Viorel Marin; Ng, Chuen-How; Wilke, Max; Tiersch, Brigitte; Fratzl, Peter; Peter, Martin G

    2005-09-01

    This paper presents some results concerning the size-controlled hydroxyapatite nanoparticles obtained in aqueous media in a biopolymer matrix from soluble precursors salts. Taking the inspiration from nature, where composite materials made of a polymer matrix and inorganic fillers are often found, e.g. bone, shell of crustaceans, shell of eggs, etc., the feasibility on making composite materials containing chitosan and nanosized hydroxyapatite was investigated. A stepwise co-precipitation approach was used to obtain different types of composites by means of different ratio between components. The synthesis of hydroxyapatite was carried out in the chitosan matrix from calcium chloride and sodium dihydrogenphosphate in alkaline solutions at moderate pH of 10-11 for 24 h. Our research is focused on studying and understanding the structure of this class of composites, aiming at the development of novel materials, controlled at the nanolevel scale. The X-ray diffraction technique was employed in order to study the kinetic of hydroxyapatite formation in the chitosan matrix as well as to determine the HAp crystallite sizes in the composite samples. The hydroxyapatite synthesized using this route was found to be nano-sized (15-50 nm). Moreover, applying an original approach to analyze the (002) XRD diffraction peak profile of hydroxyapatite by using a sum of two Gauss functions, the bimodal distribution of nanosized hydroxyapatite within the chitosan matrix was revealed. Two types of size distribution domains such as cluster-like (between 200 and 400 nm), which are the habitat of ''small'' hydroxyapatite nanocrystallites and scattered-like, which are the habitat of ''large'' hydroxyapatite nanocrystallites was probed by TEM and CSLM. The structural features of composites suggest that self-assembly processes might be involved. The composites contain nanosized hydroxyapatite with structural features close to those of biological apatites that make them attractive for bone

  17. Corrosion stability and bioactivity in simulated body fluid of silver/hydroxyapatite and silver/hydroxyapatite/lignin coatings on titanium obtained by electrophoretic deposition.

    PubMed

    Eraković, Sanja; Janković, Ana; Veljović, Djordje; Palcevskis, Eriks; Mitrić, Miodrag; Stevanović, Tatjana; Janaćković, Djordje; Mišković-Stanković, Vesna

    2013-02-14

    Hydroxyapatite is the most suitable biocompatible material for bone implant coatings. However, its brittleness is a major obstacle, and that is why, recently, research focused on creating composites with various biopolymers. In this study, hydroxyapatite coatings were modified with lignin in order to attain corrosion stability and surface porosity that enables osteogenesis. Incorporating silver, well known for its antimicrobial properties, seemed the best strategy for avoiding possible infections. The silver/hydroxyapatite (Ag/HAP) and silver/hydroxyapatite/lignin (Ag/HAP/Lig) coatings were cathaphoretically deposited on titanium from ethanol suspensions, sintered at 900 °C in Ar, and characterized by X-ray diffraction, scanning electron microscopy, field emission scanning electron microscopy, attenuated total reflection Fourier transform infrared, and X-ray photoelectron spectroscopy. The corrosion stability of electrodeposited coatings was evaluated in vitro in Kokubo's simulated body fluid (SBF) at 37 °C using electrochemical impedance spectroscopy. Bioactivity was estimated by immersion in SBF to evaluate the formation of hydroxyapatite on the coating surface. A microcrystalline structure of newly formed plate-shaped carbonate-hydroxyapatite was detected after only 7 days, indicating enhanced bioactive behavior. Both coatings had good corrosion stability during a prolonged immersion time. Among the two, the Ag/HAP/Lig coating had a homogeneous surface, less roughness, and low values of contact angle. PMID:22991920

  18. [Morphological studies of hydroxyapatite crystals exposed to disodium pamidronate].

    PubMed

    Hein, L E; Grassi, R L; Roldán, E J; Gregori, D; Varela, M E; Piccinni, E P

    1997-01-01

    "In vitro" effects of disodium pamidronate on hydroxyapatite crystals morphology, and some "in vivo" data from bone powder of tibia and vertebrae from treated young and mature rabbits are here reported. Hydroxyapatite, synthesized following Rigoli et al method, and bone powder from rabbits were studied with X-ray, infrared and raman emission techniques for crystallographic analysis. Adsorption studies were also performed with a balanced solution of hydroxyapatite exposed to different times, 48, 120 and 168 hours and concentrations 1 x 10(-5) M, 3 x 10(-5) M, 8 x 10(-5) M y 1 x 10(-4) M of pamidronate. Infrared and raman spectrometry were not conclusive due to technical bias, but X-ray difractograms showed pure hydroxyapatite crystals in an hexagonal system. At constant time, pamidronate concentrations were varied, showing after 48 hours of exposition, a slight growth in the 002 plane, an aleatoric behavior in 213 and a marked increase in 004. After 120 hours, 002 plane is steady with a net growth in 004 and 213. After 168 hours, the 3 mentioned planes grow in proportion to pamidronate concentrations, tending to enlarge the crystal shape. Plane 13 markedly grow with pamidronate 8 x 10(-5) M a 1 x 10(-4) M, which are biologically high concentrations. Potentiometric assessments, in the 1 x 10(-5) to 1 x 10(-4) M range of concentrations show that bisphosphonate was completely adsorbed to the crystals. Additional "in vivo" observations showed changes in bone powder crystals isolated from pamidronate treated young animals, involving a growing of planes 002 and 211, in samples from both epiphysis and diaphysis, regarding untreated samples. Changes were more evident at epiphysis. In mature rabbits, it was shown a decrease in basal plane 002 and growing at 210, 211 and 310 with a trend to enlarge the crystal shape in diaphysis and to shorten it in vertebrate spongiosa. The "in vivo" doses are equivalent to those used by Ferretti et al. in intact rats with pamidronate low

  19. Influence of technology of nanopowder production on the microstructure of the sintered by spark-plasma material on the example of aluminum oxide

    NASA Astrophysics Data System (ADS)

    Zholnin, A. G.; Melekhov, A. P.; Hafizov, R. S.; Vakulenko, S. A.; Rubinkovskiy, N. A.; Samokhin, A. V.; Alekseev, N. V.; Grigoryev, E. G.

    2016-04-01

    A comparative study of the results of spark-plasma sintering (SPS) of two-types of aluminum oxide nanopowders, obtained by the method of conductor explosion and plasma synthesis. When the parameters of both powders are similar (spherical form of the particles, size, phase composition) as well as SPS modes the properties of the resulting compacts are significantly different both in mechanical properties and microstructure. The reason of differences in the properties of the obtained compacts is in technological impurities in powders, obtained by different methods. Artificial addition of impurities, contained in the nanopowder, obtained by electro explosion of conductor, into the powder, made by synthesis in plasma and not containing these impurities, allowed to reveal their effect on the formation of the microstructure and properties of the sintered by SPS method sample.

  20. Factorial design analysis for sorption of zinc on hydroxyapatite.

    PubMed

    Meski, S; Ziani, S; Khireddine, H; Boudboub, S; Zaidi, S

    2011-02-28

    A factorial design was employed to evaluate the quantitative removal of zinc from aqueous solutions on synthesized hydroxyapatite. The experimental factors and their respective levels studied were the initial zinc concentration in solution (35≤C(Zn)≤85 mg/L), adsorbent dosage (4.5≤C(susp)≤9.5 g/L), Ca/P molar ratio (1.667≤Ca/P≤2) and calcination temperature of hydroxyapatite (600≤T(Cal)≤800 °C). The adsorption parameters were analysed statistically by means of variance analysis by using the STATISTICA software. The experimental results and statistical analysis show that increasing in the calcination temperature from 600 to 800 °C decrease the zinc adsorption whereas the increase of adsorbent dosage increases it. Based on the analysis of variance and the factorial design of experiments, adsorbent dosage has a positive effect on the removal of zinc, whereas zinc concentration, Ca/P molar ratio and calcination temperature have a negative effect on this process. The factorial results also demonstrate the existence of statistically significant binary interactions of the experimental factors. The experimental results were fitted to the Langmuir and Freundlich equations to find out adsorption capacities. In most cases, the results indicate that the sorption data fits well in the Freundlich isotherm model. The results of XRD analysis, pH(PZC) and pH(Final) values indicated that ion exchange and dissolution/precipitation mechanisms predominate for the sorption of zinc on our hydroxyapatite. PMID:21159426

  1. Induction suspension plasma sprayed biological-like hydroxyapatite coatings.

    PubMed

    Loszach, Max; Gitzhofer, François

    2015-04-01

    Substituted hydroxyapatite coatings with different ions (Mg, Na, K, Cl, F) have been developed by the induction suspension plasma spray process. Suspensions were prepared with sol-gel. The main objective of this study was to demonstrate that induction suspension plasma spray technology possesses high material composition flexibility that allows as-sprayed coatings to closely mimic natural bone composition. Long-term in vitro behaviour of as-sprayed substituted coatings was evaluated with simulated body fluid. Data on the suspensions showed the formation of a pure hydroxyapatite phase. Transmission electron microscopy characterized various preparation stages of the suspensions. As-sprayed samples were distinguished by X-ray diffraction and scanning electron microscopy. Substituted elements were quantified by neutron activation. A well-crystallized hydroxyapatite phase was produced with concentration in various substitutions very close to natural bone composition. Ca/P and (Ca + Mg + Na + K)/P ratios provided evidence of the introduction of different cations into apatite structures. The immersion of samples into simulated body fluid led to the nucleation and growth of a flake-like octacalcium phosphate crystal layer at the surface of as-sprayed coatings after one week. Proof of octacalcium phosphate transformation and its partial dissolution and direct re-precipitation into apatite was disclosed by local energy dispersive spectroscopy and microstructure observation. Formation of a Ca/P ratio gradient from the precipitated layer surface to the as-sprayed coatings interface was observed after four weeks once the octacalcium phosphate crystals reached a critical size, resulting in the formation of a rich apatite layer at the interface after six weeks. A set of mechanisms has been proposed to explain these findings. PMID:25586411

  2. Nucleation and Growth of Hydroxyapatite on Hierarchically Ordered Polymer Nanofibers

    NASA Astrophysics Data System (ADS)

    Chen, Xi; Dong, Bin; Wang, Bingbing; Li, Christopher

    2011-03-01

    The hierarchically ordered polymer nanofibers, named as nanofiber shish kebabs (NFSKs), were constructed via combination of electrospinning polycaprolactone (PCL) (shish polymer) and controlled crystallization of polycaprolactone-b-poly acrylic acid (PCL-b-PAA) (kebab polymer). These NFSKs were then employed as a template to control the nucleation and growth of hydroxypatite nanocrystals. Electron microscopy and diffraction technique were used to characterize this novel hybrid structure. The growth of minerals starts on the surface of single crystal kebabs and eventually covers the surface of NFSKs. The formation mechanism of hydroxyapatite on NFSKs is of great interest because of the NFSKs' potential application as bone scaffold materials.

  3. Polyether sulfone/hydroxyapatite mixed matrix membranes for protein purification

    NASA Astrophysics Data System (ADS)

    Sun, Junfen; Wu, Lishun

    2014-07-01

    This work proposes a novel approach for protein purification from solution using mixed matrix membranes (MMMs) comprising of hydroxyapatite (HAP) inside polyether sulfone (PES) matrix. The influence of HAP particle loading on membrane morphology is studied. The MMMs are further characterized concerning permeability and adsorption capacity. The MMMs show purification of protein via both diffusion as well as adsorption, and show the potential of using MMMs for improvements in protein purification techniques. The bovine serum albumin (BSA) was used as a model protein. The properties and structures of MMMs prepared by immersion phase separation process were characterized by pure water flux, BSA adsorption and scanning electron microscopy (SEM).

  4. Hydroxyapatite-binding peptides for bone growth and inhibition

    DOEpatents

    Bertozzi, Carolyn R.; Song, Jie; Lee, Seung-Wuk

    2011-09-20

    Hydroxyapatite (HA)-binding peptides are selected using combinatorial phage library display. Pseudo-repetitive consensus amino acid sequences possessing periodic hydroxyl side chains in every two or three amino acid sequences are obtained. These sequences resemble the (Gly-Pro-Hyp).sub.x repeat of human type I collagen, a major component of extracellular matrices of natural bone. A consistent presence of basic amino acid residues is also observed. The peptides are synthesized by the solid-phase synthetic method and then used for template-driven HA-mineralization. Microscopy reveal that the peptides template the growth of polycrystalline HA crystals .about.40 nm in size.

  5. Novel multiform morphologies of hydroxyapatite: Synthesis and growth mechanism

    NASA Astrophysics Data System (ADS)

    Mary, I. Reeta; Sonia, S.; Viji, S.; Mangalaraj, D.; Viswanathan, C.; Ponpandian, N.

    2016-01-01

    Morphological evolution of materials becomes a prodigious challenge due to their key role in defining their functional properties and desired applications. Herein, we report the synthesis of hydroxyapatite (HAp) microstructures with multiform morphologies, such as spheres, cubes, hexagonal rods and nested bundles constructed from their respective nanoscale building blocks via a simple cost effective hydro/solvothermal method. A possible formation mechanism of diverse morphologies of HAp has been presented. Structural analysis based on X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy confirms the purity of the HAp microstructures. The multiform morphologies of HAp were corroborated by using Field emission scanning electron microscope (FESEM).

  6. Collagen hydrolysate based collagen/hydroxyapatite composite materials

    NASA Astrophysics Data System (ADS)

    Ficai, Anton; Albu, Madalina Georgiana; Birsan, Mihaela; Sonmez, Maria; Ficai, Denisa; Trandafir, Viorica; Andronescu, Ecaterina

    2013-04-01

    The aim of this study was to study the influence of collagen hydrolysate (HAS) on the formation of ternary collagen-hydrolysate/hydroxyapatite composite materials (COLL-HAS/HA). During the precipitation process of HA, a large amount of brushite is resulted at pH = 7 but, practically pure HA is obtained at pH ⩾ 8. The FTIR data reveal the duplication of the most important collagen absorption bands due to the presence of the collagen hydrolysate. The presence of collagen hydrolysate is beneficial for the management of bone and joint disorders such as osteoarthritis and osteoporosis.

  7. Ion-exchange properties of strontium hydroxyapatite under acidic conditions

    SciTech Connect

    Sugiyama, Shigeru; Nishioka, Hitoshi; Moriga, Toshihiro; Hayashi, Hiromu; Moffat, J.B.

    1998-09-01

    The ion exchange of strontium hydroxyapatite (SrHAp) with Pb{sup 2+} has been investigated under acidic conditions at 293 K. The addition of various acids to the exchanging solution enhanced the exchange capacity in the order HCl > HBr > HF > HNO{sub 3} > no acid, corresponding to the formation of halogen apatites with the former three acids or hydrogen phosphate with HNO{sub 3}. Since the ion-exchange capacity of SrHAp under nonacidic conditions is higher than that of chlorapatite, the aforementioned observations can be attributed to the participation of the protons introduced by the acids.z

  8. Pyroelectric, piezoelectric, and photoeffects in hydroxyapatite thin films on silicon

    NASA Astrophysics Data System (ADS)

    Lang, S. B.; Tofail, S. A. M.; Gandhi, A. A.; Gregor, M.; Wolf-Brandstetter, C.; Kost, J.; Bauer, S.; Krause, M.

    2011-03-01

    Hydroxyapatite (HA) is the major component of bone and is used in artificial form in many biomedical applications. It was once believed to have a centrosymmetric crystal structure. In theoretical and experimental studies published in 2005, it was shown to have a monoclinic P21 structure. In the work reported here, 500 nm films of HA were spin-coated on silicon wafers. The materials were not poled. They had a nonuniform polarization distribution and exhibited pyroelectricity, piezoelectricity, and photoeffects. Structures of this type may have a number of technological applications.

  9. Characterization of processed tooth hydroxyapatite for potential biomedical implant applications.

    PubMed

    Oktar, F N; Kesenci, K; Pişkin, E

    1999-07-01

    In this study hydroxyapatite (HA) (100-150 microns) derived from freshly-extracted human teeth in laboratory conditions was investigated. Scanning electron microscope (SEM), energy dispersive x-ray spectroscopy (EDXS), wet chemical, ion chromatographic peak method (ICP), atomic absorption, x-ray diffraction and infra-red (IR) were performed separately for HA obtained from dentine and enamel. This naturally derived HA did not differ from synthetic ones. Its production was simple when compared with other methods. Processed tooth HA could safely be used in animal subjects prior to human studies as a graft material after biocompatibility studies fully conducted. PMID:10427420

  10. Microstructural characterization of glass-reinforced hydroxyapatite composites.

    PubMed

    Santos, J D; Knowles, J C; Reis, R L; Monteiro, F J; Hastings, G W

    1994-01-01

    The influence of phosphate-based glasses and a bioactive silica glass on the sintering mechanism of hydroxyapatite was studied over a wide range of temperatures. The composites were microstructurally characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). Small additions of phosphate-based glasses proved to be beneficial to the sintering process and fully dense materials were obtained. A significant improvement in mechanical properties was achieved. beta-TCP and alpha-TCP were found in the microstructure depending on the sintering temperature. Additions of bioactive glass led to the development of calcium phosphate silicate. PMID:8161658

  11. 188Re-labeled hydroxyapatite particles for radiation synovectomy.

    PubMed

    Kothari, K; Suresh, S; Sarma, H D; Meera, V; Pillai, M R A

    2003-04-01

    A new procedure for labeling hydroxyapatite (HA) particles with 188Re for radiation synovectomy is described and standardized. The particles were labeled with 188Re in high yields (99%) in acidic medium. HA particle size remained unaffected by reaction conditions as checked by laser diffraction particle analyzer. 188Re-HA was found to be stable retaining 99% radiochemical purity after 4 days when stored in ascorbic acid solution (10mg/ml, pH 5). Intra-articular injection in rats revealed approximately 98% retention of 188Re-HA in the knee after 48-h pi. PMID:12672625

  12. Temperature-mediated phase transformation, pore geometry and pore hysteresis transformation of borohydride derived in-born porous zirconium hydroxide nanopowders

    PubMed Central

    Nayak, Nadiya B.; Nayak, Bibhuti B.

    2016-01-01

    Development of in-born porous nature of zirconium hydroxide nanopowders through a facile hydrogen (H2) gas-bubbles assisted borohydride synthesis route using sodium borohydride (NaBH4) and novel information on the temperature-mediated phase transformation, pore geometry as well as pore hysteresis transformation of in-born porous zirconium hydroxide nanopowders with the help of X-ray diffraction (XRD), Brunauer–Emmett–Teller (BET) isotherm and Transmission Electron Microscopy (TEM) images are the main theme of this research work. Without any surfactants or pore forming agents, the borohydride derived amorphous nature of porous powders was stable up to 500 °C and then the seed crystals start to develop within the loose amorphous matrix and trapping the inter-particulate voids, which led to develop the porous nature of tetragonal zirconium oxide at 600 °C and further sustain this porous nature as well as tetragonal phase of zirconium oxide up to 800 °C. The novel hydrogen (H2) gas-bubbles assisted borohydride synthesis route led to develop thermally stable porous zirconium hydroxide/oxide nanopowders with an adequate pore size, pore volume, and surface area and thus these porous materials are further suggested for promising use in different areas of applications. PMID:27198738

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

    SciTech Connect

    Czosnek, Cezary; Bućko, Mirosław M.; Janik, Jerzy F.; Olejniczak, Zbigniew; Bystrzejewski, Michał; Łabędź, Olga; Huczko, Andrzej

    2015-03-15

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

  14. Temperature-mediated phase transformation, pore geometry and pore hysteresis transformation of borohydride derived in-born porous zirconium hydroxide nanopowders

    NASA Astrophysics Data System (ADS)

    Nayak, Nadiya B.; Nayak, Bibhuti B.

    2016-05-01

    Development of in-born porous nature of zirconium hydroxide nanopowders through a facile hydrogen (H2) gas-bubbles assisted borohydride synthesis route using sodium borohydride (NaBH4) and novel information on the temperature-mediated phase transformation, pore geometry as well as pore hysteresis transformation of in-born porous zirconium hydroxide nanopowders with the help of X-ray diffraction (XRD), Brunauer–Emmett–Teller (BET) isotherm and Transmission Electron Microscopy (TEM) images are the main theme of this research work. Without any surfactants or pore forming agents, the borohydride derived amorphous nature of porous powders was stable up to 500 °C and then the seed crystals start to develop within the loose amorphous matrix and trapping the inter-particulate voids, which led to develop the porous nature of tetragonal zirconium oxide at 600 °C and further sustain this porous nature as well as tetragonal phase of zirconium oxide up to 800 °C. The novel hydrogen (H2) gas-bubbles assisted borohydride synthesis route led to develop thermally stable porous zirconium hydroxide/oxide nanopowders with an adequate pore size, pore volume, and surface area and thus these porous materials are further suggested for promising use in different areas of applications.

  15. Temperature-mediated phase transformation, pore geometry and pore hysteresis transformation of borohydride derived in-born porous zirconium hydroxide nanopowders.

    PubMed

    Nayak, Nadiya B; Nayak, Bibhuti B

    2016-01-01

    Development of in-born porous nature of zirconium hydroxide nanopowders through a facile hydrogen (H2) gas-bubbles assisted borohydride synthesis route using sodium borohydride (NaBH4) and novel information on the temperature-mediated phase transformation, pore geometry as well as pore hysteresis transformation of in-born porous zirconium hydroxide nanopowders with the help of X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET) isotherm and Transmission Electron Microscopy (TEM) images are the main theme of this research work. Without any surfactants or pore forming agents, the borohydride derived amorphous nature of porous powders was stable up to 500 °C and then the seed crystals start to develop within the loose amorphous matrix and trapping the inter-particulate voids, which led to develop the porous nature of tetragonal zirconium oxide at 600 °C and further sustain this porous nature as well as tetragonal phase of zirconium oxide up to 800 °C. The novel hydrogen (H2) gas-bubbles assisted borohydride synthesis route led to develop thermally stable porous zirconium hydroxide/oxide nanopowders with an adequate pore size, pore volume, and surface area and thus these porous materials are further suggested for promising use in different areas of applications. PMID:27198738

  16. The Fate of Porous Hydroxyapatite Granules Used in Facial Skeletal Augmentation

    PubMed Central

    Jacobson, Steve R.; Lavoipierre, Alain M.; Huggins, Richard J.

    2010-01-01

    Facial appearance is largely determined by the morphology of the underlying skeleton. Hydroxyapatite is one of several materials available to enhance projection of the facial skeleton. This study evaluated the long-term maintenance of augmented bony projection when porous hydroxyapatite granules are used on the facial skeleton. Ten female patients aged 28–58 years were studied following aesthetic augmentation of the facial skeleton at 24 sites using porous hydroxyapatite granules. Postoperative CT scans at 3 months served as the baseline measurement and compared with scans taken at 1 and 2 years, with the thickness of the hydroxyapatite measured in axial and coronal planes. Thickness of original bone plus overlay of hydroxyapatite, thickness of the overlying soft tissue, and the overall projection (bone plus soft tissue) were recorded. It was found that 99.7% of the hydroxyapatite was maintained at 2 years, with no statistical difference (t test) from the baseline measurement. The overall projection (bony and soft tissue) was maintained as there was no evidence of native bone resorption or soft tissue atrophy. Radiographic results confirmed that the use of porous hydroxyapatite granules for enhancement of the facial skeleton is not only a predictable procedure, but maintains full bony projection at 2 years. PMID:20186415

  17. Relative contributions of chemistry and topography to the osseointegration of hydroxyapatite coatings.

    PubMed

    Hacking, S A; Tanzer, M; Harvey, E J; Krygier, J J; Bobyn, J D

    2002-12-01

    The purpose of the current study was to ascertain the relative contributions of surface chemistry and topography to the osseointegration of hydroxyapatite-coated implants. A canine femoral intramedullary implant model was used to compare the osseous response to commercially pure titanium implants that were either polished, grit-blasted, plasma-sprayed with hydroxyapatite, or plasma-sprayed with hydroxyapatite and masked with a very thin layer of titanium using physical vapor deposition (titanium mask). The titanium mask isolated the chemistry of the underlying hydroxyapatite layer without functionally changing its surface topography and morphologic features. At 12 weeks, the bone-implant specimens were prepared for undecalcified thin section histologic evaluation and serial transverse sections were quantified with backscattered scanning electron microscopy for the percentage of bone apposition to the implant surface. Bone apposition averaged 3% for the polished implants and 23% for the grit-blasted implants. Bone apposition to the hydroxyapatite-coated implants averaged 74% whereas bone apposition to the titanium mask implants averaged 59%. Although there was significantly greater osseointegration with the hydroxyapatite-coated implants, 80% of the maximum bone forming response to the implant surfaces developed with the titanium mask implants. This simple, controlled experiment revealed that topography is the dominant factor governing bone apposition to hydroxyapatite-coated implants. PMID:12461353

  18. An improved biofunction of titanium for keratoprosthesis by hydroxyapatite-coating.

    PubMed

    Dong, Ying; Yang, Jingxin; Wang, Liqiang; Ma, Xiao; Huang, Yifei; Qiu, Zhiye; Cui, Fuzhai

    2014-03-01

    Titanium framework keratoprosthesis has been commonly used in the severe corneal blindness, but the tissue melting occurred frequently around titanium. Since hydroxyapatite has been approved to possess a good tissue integration characteristic, nanostructured hydroxyapatite was coated on the surface of titanium through the aerosol deposition method. In this study, nanostructured hydroxyapatite coating was characterized by X-ray diffraction, scanning electron microscopy, atomic force microscopy, and auger electronic spectrometer. Biological evaluations were performed with rabbit cornea fibroblast in vitro and an animal model in vivo. The outcomes showed the coating had a grain-like surface topography and a good atomic mixed area with substrate. The rabbit cornea fibroblasts appeared a good adhesion on the surface of nanostructured hydroxyapatite in vitro. In the animal model, nanostructured hydroxyapatite-titanium implants were stably retained in the rabbit cornea, and by contrast, the corneal stroma became thinner anterior to the implants in the control. Therefore, our findings proved that nanostructured hydroxyapatite-titanium could not only provide an improved bond for substrate but also enhance the tissue integration with implants in host. As a promising material, nanostructured hydroxyapatite-titanium-based keratoprosthesis prepared by the aerosol deposition method could be utilized for the corneal blindness treatment. PMID:23749719

  19. The affect of densification and dehydroxylation on the mechanical properties of stoichiometric hydroxyapatite bioceramics

    SciTech Connect

    Laasri, S.; Taha, M.; Laghzizil, A.; Hlil, E.K.; Chevalier, J.

    2010-10-15

    This paper reports the effects of processing densification on the mechanical properties of hydroxyapatite bioceramics. Densification of synthetic hydroxyapatite is conducted in the range 1000-1300 {sup o}C. X-ray diffraction and SEM microscopy are used to check the microstructure transformations. Vickers hardness, toughness and Young's modulus are analyzed versus the density and grain size. The sintering temperature and the particle size influence strongly the densification and the resulting mechanical properties. In addition, the critical sintering temperature appears around 1200 {sup o}C and the declined strength at the temperature up to 1200 {sup o}C is found sensitive to the dehydroxylation process of hydroxyapatite.

  20. Effect of osteogenesis imperfecta mutations in tropocollagen molecule on strength of biomimetic tropocollagen-hydroxyapatite nanocomposites

    NASA Astrophysics Data System (ADS)

    Dubey, Devendra K.; Tomar, Vikas

    2010-01-01

    Osteogenesis Imperfecta (OI) is a genetic disorder that affects cellular synthesis of Type-I collagen fibrils and causes extreme bone fragility. This study reports the effects of OI mutations in Tropocollagen (TC) molecules on strength of model Tropocollagen-Hydroxyapatite biomaterials with two different mineral [hydroxyapatite (HAP)] distributions using three dimensional atomistic simulations. Results show that the effect of TC mutations on the strength of TC-HAP biomaterials is insignificant. Instead, change in mineral distribution showed significant impact on the overall strength of TC-HAP biomaterials. Study suggests that TC mutations manifest themselves by changing the mineral distribution during hydroxyapatite growth and nucleation period.

  1. Osteocalcin enhances bone remodeling around hydroxyapatite/collagen composites.

    PubMed

    Rammelt, Stefan; Neumann, Mirjam; Hanisch, Uwe; Reinstorf, Antje; Pompe, Wolfgang; Zwipp, Hans; Biewener, Achim

    2005-06-01

    The effect of osteocalcin (OC), an extracellular bone matrix protein, on bone healing around hydroxyapatite/collagen composites was investigated. Cylindrical nanocrystalline hydroxyapatite implants of 2.5-mm diameter containing 2.5% biomimetically mineralized collagen type I were inserted press-fit into the tibial head of adult Wistar rats. To one implant group, 10 mug/g OC was added. Six specimens per group were analyzed at 2, 7, 14, 28, and 56 days. After 14 days, newly formed woven bone had reached the implant surface of the OC implants whereas a broad fibrous interface could still be observed around controls. Woven bone was formed directly around both implant groups after 28 days and had been replaced partially by lamellar bone around the OC implants only. No significant differences in total bone contact were seen between both groups after 56 days. The higher number of phagocytosing cells and osteoclasts characterized immunohistochemically with ED1, cathepsin D, and tartate-resistant alkaline phosphatase around the OC implants at the early stages of bone healing suggests an earlier onset of bone remodeling. The earlier and increased expression of bone-specific matrix proteins and multifunctional adhesion proteins (osteopontin, bone sialoprotein, CD44) at the interface around the OC implants indicates that OC may accelerate bone formation and regeneration. This study supports the observations from in vitro studies that OC activates both osteoclasts and osteoblasts during early bone formation. PMID:15800855

  2. Novel selenium-doped hydroxyapatite coatings for biomedical applications.

    PubMed

    Rodríguez-Valencia, C; López-Álvarez, M; Cochón-Cores, B; Pereiro, I; Serra, J; González, P

    2013-03-01

    Nowadays there is a short-term need of investigating in orthopedic implants with a greater functionality, including an improved osseointegration and also antibacterial properties. The coating of metallic implants with hydroxyapatite (HA) remains to be the main proposal, but superior quality HA coatings with compositions closer to natural bone apatites, including carbonates, trace elements are required. Selenium is an essential nutrient in biological tissues and, at the same time, it also presents antibacterial properties. A pioneering study on the fabrication of selenium-doped carbonated hydroxyapatite (iHA:Se) coatings by Pulsed Laser Deposition (PLD) is presented. Different proportions of selenium were incorporated to obtain the iHA:Se coatings. Their physicochemical characterization, performed by SEM/EDS, FTIR, FT-Raman, Interferometric Profilometry and XPS, revealed typical columnar growth of HA in globular aggregates and the efficient incorporation of selenium into the HA coatings by the, most probably, substitution of SeO(3)(2-) groups in the CO(3)(2-) sites. Biological evaluation illustrated the absence of cytotoxicity when an amount of 0.6 at.% of Se was added to the iHA:Se coatings and excellent proliferation of the MC3T3-E1 preosteoblasts. Antibacterial properties were also proved with the inhibition of P. aeruginosa and S. aureus from establishing bacterial biofilms. PMID:22968925

  3. Intrinsic magnetism and hyperthermia in bioactive Fe-doped hydroxyapatite.

    PubMed

    Tampieri, Anna; D'Alessandro, Teresa; Sandri, Monica; Sprio, Simone; Landi, Elena; Bertinetti, Luca; Panseri, Silvia; Pepponi, Giancarlo; Goettlicher, Joerg; Bañobre-López, Manuel; Rivas, Jose

    2012-02-01

    The use of magnetic activation has been proposed to answer the growing need for assisted bone and vascular remodeling during template/scaffold regeneration. With this in mind, a synthesis procedure was developed to prepare bioactive (Fe2+/Fe3+)-doped hydroxyapatite (Fe-HA), endowed with superparamagnetic-like properties. This new class of magnetic hydroxyapatites can be potentially employed to develop new magnetic ceramic scaffolds with enhanced regenerative properties for bone surgery; in addition, magnetic Fe-HA can find application in anticancer therapies, to replace the widely used magnetic iron oxide nanoparticles, whose long-term cytotoxicity was recently found to reach harmful levels. An extensive physicochemical, microstructural and magnetic characterization was performed on the obtained Fe-HA powders, and demonstrated that the simultaneous addition of Fe2+ and Fe3+ ions during apatite nucleation under controlled synthesis conditions induces intrinsic magnetization in the final product, minimizing the formation of magnetite as secondary phase. This result potentially opens new perspectives for biodevices aimed at bone regeneration and for anti-cancer therapies based on hyperthermia. PMID:22005331

  4. Quantification of bone ingrowth into porous block hydroxyapatite in humans.

    PubMed

    Ayers, R A; Wolford, L M; Bateman, T A; Ferguson, V L; Simske, S J

    1999-10-01

    This study sought to quantify bone ingrowth from a single bone-implant surface into porous block hydroxyapatite used in maxillofacial applications. Seventeen maxillary hydroxyapatite implants (implant time of 4-138 months, 39-month mean) were harvested for analysis from 14 patients. The implants had been placed into the lateral maxillary wall during orthognathic surgery, juxtapositioned to the maxillary sinus. Ingrowth was measured in 100-microm increments from a bone-implant interface to a depth of 1500 microm. Bone ingrowth averaged over the 14 patients (0-1100 microm depth) is described by the equation % ingrowth - 20% * (depth in millimeters) + 41.25% (R2 = 0.98, n = 10 incremental depths). Beyond 1100 microm, the average ingrowth remained constant at 15.0 +/- 0.7%. The duration of implantation also showed as affect on the percent ingrowth into the implants at the incremental depths, and the percent ingrowth asymptotically approached a maximum. Overall, the composite average data from all depths is best described by the logarithmic function % ingrowth = 15% * ln(implantation time in months) - 24.0% (R2 = 0.71, n = 14 patients). Several factors may come into play in determining bone ingrowth including the mechanical environment, the osteoconductivity of the implant material, and the osteogenic capability of the tissues in the pore spaces. Measurements of bone ingrowth are most influenced by the depth into the implant and the time the implant was in the body; the age of the patient had little affect on bone ingrowth. PMID:10400880

  5. Properties of pulsed laser deposited fluorinated hydroxyapatite films on titanium

    SciTech Connect

    Rau, J.V.; Smirnov, V.V.; Laureti, S.; Generosi, A.; Varvaro, G.; Fosca, M.; Ferro, D.; Cesaro, S. Nunziante; Albertini, V. Rossi; Barinov, S.M.

    2010-09-15

    Fluorinated hydroxyapatite coated titanium was investigated for application as implant coating for bone substitute materials in orthopaedics and dentistry. Pulsed laser deposition technique was used for films preparation. Fluorinated hydroxyapatite target composition, Ca{sub 10}(PO{sub 4}){sub 6}F{sub 1.37}(OH){sub 0.63}, was maintained at 2 J/cm{sup 2} of laser fluence and 500-600 {sup o}C of the substrate temperature. Prepared films had a compact microstructure, composed of spherical micrometric-size aggregates. The average surface roughness resulted to be of 3 nm for the film grown at 500 {sup o}C and of 10 nm for that grown at 600 {sup o}C, showing that the temperature increase did not favour the growth of a more fine granulated surface. The films were polycrystalline with no preferential growth orientation. The films grown at 500-600 {sup o}C were about 8 {mu}m thick and possessed a hardness of 12-13 GPa. Lower or higher substrate temperature provides the possibility to obtain coatings with different fine texture and roughness, thus tayloring them for various applications.

  6. Hydroxyapatite-titanium bulk composites for bone tissue engineering applications.

    PubMed

    Kumar, Alok; Biswas, Krishanu; Basu, Bikramjit

    2015-02-01

    The research work on bulk hydroxyapatite (HA)-based composites are driven by the need to develop biomaterials with better mechanical properties without compromising its bioactivity and biocompatibility properties. Despite several years of research, the mechanical properties of the HA-based composites still need to be enhanced to match the properties of natural cortical bone. In this regard, the scope of this review on the HA-based bulk biomaterials is limited to the processing and the mechanical as well as biocompatibility properties for bone tissue engineering applications of a model system that is hydroxyapatite-titanium (HA-Ti) bulk composites. It will be discussed in this review how HA-Ti based bulk composites can be processed to have better fracture toughness and strength without compromising biocompatibility. The advantages of the functionally gradient materials to integrate the mechanical and biocompatibility properties is a promising approach in hard tissue engineering and has been emphasized here in reference to the limited literature reports. On the biomaterials fabrication aspect, the recent results are discussed to demonstrate that advanced manufacturing techniques, like spark plasma sintering can be adopted as a processing route to restrict the sintering reactions, while enhancing the mechanical properties. Various toughening mechanisms related to careful tailoring of microstructure are discussed. The in vitro cytocompatibilty, cell fate processes as well as in vivo biocompatibility results are also reviewed and the use of flow cytometry to quantify in vitro cell fate processes is being emphasized. PMID:24737723

  7. Alkoxide route for preparing hydroxyapatite and its coatings.

    PubMed

    Weng, W; Baptista, J L

    1998-01-01

    The preparation of hydroxyapatite using n-butanol or ethanol solutions of P2O5 and Ca glycoxide as precursors of P and Ca was investigated by nuclear magnetic resonance (NMR), X-Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM). Stable mixed solutions of the precursors could be obtained in the presence of acetic acid (HOAC). For the mixed solution of Ca glycoxide with the ethanol solution of P2O5, a lower HOAC/Ca ratio was needed since the ethanol solution of P2O5 contained a lower concentration of H3PO4, a species that easily forms precipitates in the presence of the Ca containing species. An amorphous powder was obtained by heating the stable solution of Ca glycoxide and PO(OH)x(OEt)3-x with an HOAC/Ca ratio of 4 in a hot plate at approximately 150 degrees C. Hydroxyapatite (HAP) was directly formed after calcining the amorphous powder at 500 degrees C. The stable mixed solutions of Ca glycoxide and the alcoholic solutions of P2O5 were used to prepare HAP coatings on alumina substrates using a dip-coating method. The resulting ceramic coatings have a rough surface and an adhesion strength of about 10 MPa. The morphology of the coatings is dependent on the preparation chemistry. PMID:9678859

  8. Bioactive glass/hydroxyapatite composites: mechanical properties and biological evaluation.

    PubMed

    Bellucci, Devis; Sola, Antonella; Anesi, Alexandre; Salvatori, Roberta; Chiarini, Luigi; Cannillo, Valeria

    2015-06-01

    Bioactive glass/hydroxyapatite composites for bone tissue repair and regeneration have been produced and discussed. The use of a recently developed glass, namely BG_Ca/Mix, with its low tendency to crystallize, allowed one to sinter the samples at a relatively low temperature thus avoiding several adverse effects usually reported in the literature, such as extensive crystallization of the glassy phase, hydroxyapatite (HA) decomposition and reaction between HA and glass. The mechanical properties of the composites with 80wt.% BG_Ca/Mix and 20wt.% HA are sensibly higher than those of Bioglass® 45S5 reference samples due to the presence of HA (mechanically stronger than the 45S5 glass) and to the thermal behaviour of the BG_Ca/Mix, which is able to favour the sintering process of the composites. Biocompatibility tests, performed with murine fibroblasts BALB/3T3 and osteocites MLO-Y4 throughout a multi-parametrical approach, allow one to look with optimism to the produced composites, since both the samples themselves and their extracts do not induce negative effects in cell viability and do not cause inhibition in cell growth. PMID:25842126

  9. Strontium and zoledronate hydroxyapatites graded composite coatings for bone prostheses.

    PubMed

    Boanini, Elisa; Torricelli, Paola; Sima, Felix; Axente, Emanuel; Fini, Milena; Mihailescu, Ion N; Bigi, Adriana

    2015-06-15

    Both strontium and zoledronate (ZOL) are known to be useful for the treatment of bone diseases associated to the loss of bone substance. In this work, we applied an innovative technique, Combinatorial Matrix-Assisted Pulsed Laser Evaporation (C-MAPLE), to deposit gradient thin films with variable compositions of Sr-substituted hydroxyapatite (SrHA) and ZOL modified hydroxyapatite (ZOLHA) on Titanium substrates. Compositional gradients were obtained by simultaneous laser vaporization of the two distinct material targets. The coatings display good crystallinity and granular morphology, which do not vary with composition. Osteoblast-like MG63 cells and human osteoclasts were co-cultured on the thin films up to 21 days. The results show that Sr counteracts the negative effect of relatively high concentration of ZOL on osteoblast viability, whereas both Sr and ZOL enhance extracellular matrix deposition. In particular, ZOL promotes type I collagen production, whereas Sr increases the production of alkaline phosphatase. Moreover, ZOL exerts a greater effect than Sr on osteoprotegerin/RANKL ratio and, as a consequence, on the reduction of osteoclast proliferation and activity. The deposition method allows to modulate the composition of the thin films and hence the promotion of bone growth and the inhibition of bone resorption. PMID:25706198

  10. Titanium--hydroxyapatite porous structures for endosseous applications.

    PubMed

    Popa, C; Simon, V; Vida-Simiti, I; Batin, G; Candea, V; Simon, S

    2005-12-01

    Materials for uncemented endosseous implants have to assure an as short as possible osseointegration time. Thus, a material with both surface bioactivity and a porous outer structure can become a preferred choice for this type of applications. This paper presents a class of titanium-base PM composites, reinforced with particulate hydroxyapatite. Raw materials were titanium powder, obtained through hydriding--milling--dehydriding, with the grain size of 63-100 microm, and sol-gel hydroxyapatite (HA) powder, produced by the reaction between Ca(NO3)2 x 4H2O and (NH4)2HPO4. Blends with 5 to 50% HA were prepared and pressed in a rigid die, producing single composition or gradual composition samples. The applied pressure was of 400, 500 or 600 MPa. Sintering was performed in vacuum, at 1160 ( composite function)C. All samples, although well sintered, displayed swelling during sintering, due to diffusion into the matrix. The increase in volume is more severe for higher amounts of HA in the green compacts and for higher applied compaction pressure. Compacts with a gradual increase of the HA content are recommended from the functional and mechanical point of view, but the increase should be slow, not to produce interlayer cracks. The outer surface shows interconnected pores, suitable for the ingrowth of vital new bone. PMID:16362217

  11. Hydroxyapatite substituted by transition metals: experiment and theory.

    PubMed

    Zilm, M E; Chen, L; Sharma, V; McDannald, A; Jain, M; Ramprasad, R; Wei, M

    2016-06-28

    Bioceramics are versatile materials for hard tissue engineering. Hydroxyapatite (HA) is a widely studied biomaterial for bone grafting and tissue engineering applications. The crystal structure of HA allows for a wide range of substitutions, which allows for tailoring materials properties. Transition metals and lanthanides are of interest since substitution in HA can result in magnetic properties. In this study, experimental results were compared to theoretical calculations of HA substituted with a transition metal. Calculation of a 10 atomic percent substitution of a transition metal ion Mn(2+), Fe(2+), and Co(2+) substituted HA samples lead to magnetic moments of 5, 4, and 3 Bohr magnetons, respectively. Hydroxyapatite substituted by transition metals (MHA) was fabricated through an ion exchange procedure and characterized with X-ray diffraction, Fourier transform infra-red spectroscopy (FTIR), X-ray photoelectron spectroscopy, and vibrating sample magnetometer, and results were compared to theoretical calculations. All the substitutions resulted in phase-pure M(2+)HA with lattice parameters and FTIR spectra in good agreement with calculations. Magnetic measurements revealed that the substitution of Mn(2+) has the greatest effect on the magnetic properties of HA followed by the substitution of Fe(2+) and then Co(2+). The present work underlines the power of synergistic theoretical-experimental work in guiding the rational design of materials. PMID:27264723

  12. Gallium increases bone calcium and crystallite perfection of hydroxyapatite.

    PubMed

    Bockman, R S; Boskey, A L; Blumenthal, N C; Alcock, N W; Warrell, R P

    1986-12-01

    Gallium, a group IIIa metal, is known to interact with hydroxyapatite as well as the cellular components of bone. In recent studies we have found gallium to be a potent inhibitor of bone resorption that is clinically effective in controlling cancer-related hypercalcemia as well as the accelerated bone resorption associated with bone metastases. To begin to elucidate gallium's mechanism of action we have examined its effects on bone mineral properties. After short-term (14 days) administration to rats, gallium nitrate produced measurable changes in bone mineral properties. Using atomic absorption spectroscopy, low levels of gallium were noted to preferentially accumulate in regions of active bone formation, 0.54 +/- .07 microgram/mg bone in the metaphyses versus 0.21 +/- .03 microgram/mg bone in the diaphyses, P less than 0.001. The bones of treated animals had increased calcium content measured spectrophotometrically. Rats injected with radiolabeled calcium during gallium treatment had greater 45-calcium content compared to control animals. By wide-angle X-ray analyses, larger and/or more perfect hydroxyapatite was observed. The combined effects of gallium on bone cell function and bone mineral may explain its clinical efficacy in blocking accelerated bone resorption. PMID:3026592

  13. Alendronate functionalized mesoporous hydroxyapatite nanoparticles for drug delivery

    SciTech Connect

    Li, Dongdong; Zhu, Yuntao; Liang, Zhiqiang

    2013-06-01

    Highlights: ► The synthesized mesoporous hydroxyapatite has nanostructure and bioactivity. ► The materials have high surface area and amino group. ► The materials show higher drug loading and slower release rate than pure HAP. - Abstract: Mesoporous nanosized hydroxyapatite (HAP) functionalized by alendronate (ALN) was synthesized using cationic surfactant CTAB as template. The structural, morphological and textural properties were fully characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) and N{sub 2} adsorption/desorption. Then the obtained materials were performed as drug delivery carriers using ibuprofen (IBU) as a model drug to investigate their drug storage/release properties in simulated body fluid (SBF). The materials showed relatively slower release rate compared with HAP due to the ionic interaction between -NH{sub 3}{sup +} on the matrix and -COO{sup −}belongs to IBU. The system provides a new concept for improving the drug loading or slowing down the release rate.

  14. Effect of hydroxyapatite-based biomaterials on human osteoblast phenotype.

    PubMed

    Trombelli, L; Penolazzi, L; Torreggiani, E; Farina, R; Lambertini, E; Vecchiatini, R; Piva, R

    2010-03-01

    The present study evaluated human primary osteoblasts and two different osteoblast-like cell lines behaviour when cultured in presence of different hydroxyapatite-based (HA) biomaterials (SINTlife-FIN-CERAMICA S.p.a., Faenza, Italy; Bio-Oss, Geistlich Biomaterials, Woulhusen, Switzerland; Biostite-GABA Vebas, San Giuliano Milanese, MI, Italy), focusing attention on the effect of HA/Biostite in terms of modulation of osteoblastic differentiation. Analysis were about adhesion, proliferation and mineralization activity. Runt-related transcription factor 2 (Runx2), Estrogen Receptor alpha (ERalfa) expression and alkaline phosphatase activity (ALP) were measured as osteoblastic differentiation markers. Determination of viable cells was done with MTT colorimetric assay. Scanning electron microscopy (SEM) analysis was performed on biomaterial-treated cells. All hydroxyapatite-based biomaterials didn't affect cells morphology and viability, whereas only presence of HA/Biostite improved cells adhesion, growth and differentiation. Adhesion and spreading of the primary cells on HA/Biostite were the same showed by two different osteoblast-like cell lines. These results have important implications for both tissue-engineered bone grafts and enhancement of HA implants performance, to develop new teeth's supporting structure therapies and replacement. PMID:20357737

  15. Antibacterial coatings of fluoridated hydroxyapatite for percutaneous implants.

    PubMed

    Ge, Xiang; Leng, Yang; Bao, Chongyun; Xu, Sherry Li; Wang, Renke; Ren, Fuzeng

    2010-11-01

    Percutaneous orthopedic and dental implants require not only good adhesion with bone but also the ability to attach and form seals with connective tissues and the skin. To solve the skin-seal problem of such implants, an electrochemical deposition method was used to modify the surfaces of metallic implants to improve their antibacterial ability and skin seals around them. A dense and uniform fluoridated calcium phosphate coating with a thickness of about 200 nm was deposited on an acid-etched pure titanium substrate by controlling the current density and reaction duration of the electrochemical process. The as-deposited amorphous fluoridated calcium phosphate transformed to fluoridated hydroxyapatite (FHA) after heat treatment at 600°C in a water vapor environment for 3 h. Both single crystal diffraction patterns and high-resolution transmission electron microscope (HRTEM) images confirmed the phase of the fluoridated calcium phosphate after the heat treatment. The antibacterial activities of FHA coatings were tested against Staphylococcus aureus (S. aureus), Escherichia coli (E. coli), and Porphyromonas gingivalis (P. gingivalis) with the film attachment method. The antibacterial activity of FHA coating is much higher than that of pure hydroxyapatite (HA) coating and acid-etched pure titanium surface. The promising features of FHA coating make it suitable for orthopedic and dental applications. PMID:20725973

  16. Hydroxyapatite electrodeposition on anodized titanium nanotubes for orthopedic applications

    NASA Astrophysics Data System (ADS)

    Parcharoen, Yardnapar; Kajitvichyanukul, Puangrat; Sirivisoot, Sirinrath; Termsuksawad, Preecha

    2014-08-01

    Nanotubes modification for orthopedic implants has shown interesting biological performances (such as improving cell adhesion, cell differentiation, and enhancing osseointegration). The purpose of this study is to investigate effect of titanium dioxide (TiO2) nanotube feature on performance of hydroxyapatite-coated titanium (Ti) bone implants. TiO2 nanotubes were prepared by anodization using ammonium fluoride electrolyte (NH4F) with and without modifiers (PEG400 and Glycerol) at various potential forms, and times. After anodization, the nanotubes were subsequently annealed. TiO2 nanotubes were characterized by scanning electron microscope and X-ray diffractometer. The amorphous to anatase transformation due to annealing was observed. Smooth and highly organized TiO2 nanotubes were found when high viscous electrolyte, NH4F in glycerol, was used. Negative voltage (-4 V) during anodization was confirmed to increase nanotube thickness. Length of the TiO2 nanotubes was significantly increased by times. The TiO2 nanotube was electrodeposited with hydroxyapatite (HA) and its adhesion was estimated by adhesive tape test. The result showed that nanotubes with the tube length of 560 nm showed excellent adhesion. The coated HA were tested for biological test by live/dead cell straining. HA coated on TiO2 nanotubes showed higher cells density, higher live cells, and more spreading of MC3T3-E1 cells than that growing on titanium plate surface.

  17. Biopolymers for Medical Applications: Polyglycerol Sebacate (PGS) doped Hydroxyapatite (HA)

    NASA Astrophysics Data System (ADS)

    Teruel, Maria; Kuthirummal, Narayanan; Levi, Nicole; Wake College Team

    2011-04-01

    In the investigation to engineer the ideal scaffolding device for cleft palate repair, polyglycerol sebacate (PGS) doped with hydroxyapatite (HA) were chosen for their elastomeric and biodegradable properties, as well as their cost-effective synthesis. Hydroxyapatite was integrated into the PGS to form a composite with high porosity and improved mechanical properties yielding a good substrate for cell attachment during the repair process. FT-IR scans were performed to characterize the composite polymer. Differential Scanning Calorimetry (DSC) was utilized to identify an acceptable glass transition temperature (Tg), between -18 and - 21°C. At this Tg, it was determined that the material was sufficiently polymerized to a point where it was durable yet pliable enough to use for cleft palate devices. In the synthesis of PGS 3% and 5% HA, a Tg of - 20.10°C and - 21.72°C, respectively, was achieved and further analytical tests were then performed on the polymers. Methods of analysis included X-Ray Diffraction and Tensile Strength Testing. Acknowledgements to the Research Department of Plastic and Reconstructive Surgery, Wake Forest University and College of Charleston.

  18. Phosphate reduction in a hydroxyapatite fluoride removal system

    NASA Astrophysics Data System (ADS)

    Egner, A.

    2012-12-01

    Fluorosis is a widespread disease that occurs as a result of excess fluoride consumption and can cause severe tooth and bone deformations. To combat fluorosis, several previous studies have examined the potential to replace traditional bone char filters with synthetic hydroxyapatite. Calcite particles with a synthetic hydroxyapatite coating have been shown to effectively removed fluoride, yet the low-cost method for forming these particles leaves high amounts of phosphate both in synthesis waste-water and in filter effluent. High phosphate in filter effluent is problematic because consumption of extremely high phosphate can leach calcium from bones, further exacerbating the fluoride effect. This study examines ways of reducing and reusing waste. In particular, a method of fluoride removal is explored in which fluorapatite coatings may be formed directly. In preliminary studies, batches of 4.1g of Florida limestone (<710 μm) were equilibrated with 100 mL of 10ppm fluoride. In a control batch containing lime but no added phosphate, 14% treatment was achieved, but with added phosphate, 100% treatment was achieved in all batches. Batches with lower levels of phosphate took longer to reach 100% treatment, ranging from less than 24 hours in the highest phosphate batches to approximately 42 hours in the lowest batches. The lower levels tested were well within reasonable levels for drinking water and reached 0ppm fluoride in 42 hours or less.

  19. Molecular Recognition at the Protein-Hydroxyapatite Interface

    SciTech Connect

    Stayton, Partick S.; Drobny, G. P.; Shaw, Wendy J.; Long, Joanna R.; Gilbert, Michelle R.

    2003-09-01

    Proteins found in mineralized tissues act as nature's crystal engineers, where they play a key role in promoting or inhibiting the growth of minerals, such as hydroxyapitite (bones/teeth) and calcium oxalate (kidney stones). Despite their importance in hard-tissue formation and remodeling, and in pathological processes such as stone formation and arterial calcification, there is little known of the protein structure-function relationships that govern hard-tissue engineering. Here we review early studies that have utilized solid-state NMR (ssNMR) techniques to provide in situ secondary-structure determination of statherin and statherin peptides on their biologically relevant hydroxyapatite (HAP) surfaces. In addition to direct structural study, molecular dynamics studies have provided considerable insight into the protein-binding footprint on hydroxyapatite. The molecular insight provided by these studies has also led to the design of biomimetic fusion peptides that utilize nature's crystal-recognition mechanism to display accessible and dynamic bioactive sequences from the HAP surface. These peptides selectively engage adhesion receptors and direct specific outside-in signaling pathway activation in osteoblast-like cells.

  20. Synthesis, characterization and cell behavior of fluoridated hydroxyapatite

    NASA Astrophysics Data System (ADS)

    Qu, Haibo

    Fluorine-containing hydroxyapatite (Ca5(PO4) 3(OH)1-xFx FHA), where F- partially replaces OH- in hydroxyapatite (HA), is recognized as a possible biomaterial for bone and tooth implants and gaining attention in the last several years as a possible alternative to HA. In this study, FHA powders were synthesized through a pH-cycling method. It was discovered that fluorine incorporation increased with the fluorine content in the initial solution and the number of pH cycles employed. A relatively low fluorine incorporation efficiency, ˜60%, was attained for most of the FHA samples. The short time of stay at each pH cycle and the limited number of cycles used are believed to be the main reasons of the low fluorine incorporation into the apatite structure. It was also revealed that the FHA particles produced by the pH-cycling method were inhomogeneous. They were a mixture of hydroxyapatite and F-rich apatite (or FA) particles. The mechanisms of incorporation of fluorine ions into hydroxyapatite by a pH cyclicing method were studied using TEM, XRD and fluorine measurement. Instead of forming laminated structures as reported by other research groups, a mixture of nano-sized F-rich apatite (FHA) and hydroxyapatite (HA) particles were obtained using the pH-cyclicing method. After calcination, these FHA particles were homogenized and became single phased FHA. The effect of fluorine content, preparing method, and sintering temperature on both the bulk density and biaxial flexural strength of sintered FHA was studied. Both uniaxially pressed un-milled (UPU) and cold isostatically pressed milled (IPM) FHA discs were sintered at temperatures between 1200˜400°C at an interval of 100°C. It was found that the fluorine content had a significant impact on the sintering behavior, densification, and mechanical properties of FHA discs. A close correlation between the sintered density and biaxial flexural strength of the specimens was revealed, where the biaxial flexural strength

  1. Optical emission spectroscopy of microwave-plasmas at atmospheric pressure applied to the growth of organosilicon and organotitanium nanopowders

    NASA Astrophysics Data System (ADS)

    Kilicaslan, A.; Levasseur, O.; Roy-Garofano, V.; Profili, J.; Moisan, M.; Côté, C.; Sarkissian, A.; Stafford, L.

    2014-03-01

    An atmospheric-pressure plasma sustained by an electromagnetic surface wave (SW) in the microwave regime combined with a bubbler/flash evaporator for the injection of liquid precursors was used to produce organosilicon and organotitanium nanopowders. Following the addition of hexamethyldisiloxane (HMDSO) vapors in the nominally pure argon plasma, optical emission spectra revealed the apparition of strong C2 molecular bands along with Si and Balmer H emission lines. Such features were not observed in our atmospheric-pressure Ar/HMDSO discharges controlled by dielectric barriers, indicating that microwave plasmas are characterized by much higher fragmentation levels of the precursors due to much higher electron densities. Emission spectra from the Ar/HMDSO SW plasma further showed a high-intensity continuum, the intensity of which decreased with time as powders started to form on the discharge tube walls. In presence of titanium isopropoxide (TTIP) vapors in the nominally pure Ar plasma, the emission was dominated by Ar and Ti lines, with no trace of carbon and no continuum. Fourier-Transform Infrared (FTIR) Spectroscopy of the powders formed in Ar/HMDSO plasmas showed very strong Si-(CH3)x and O-Si-(CH3)x bands, which is consistent with the formation of silicon oxycarbide. Transmission Electron Microscopy (TEM) further showed tube and sheet-like nanofeatures as well as larger structures consisting of agglomerated primary clusters. On the other hand, introduction of O2 in Ar/HMDSO plasmas produced only round-like nanoparticles with strong Si-O-Si bands and no trace of carbon, consistent with the formation of SiOx. The average size of the silica nanoparticles was 50 nm. FTIR spectra of powders formed in Ar/TTIP plasmas showed strong Ti-O signals, even without the addition of O2 in the gas phase. Corresponding TEM analysis showed nano- and agglomerated features comparable to those obtained in Ar/HMDSO although the average size of the titanate nanoparticles was smaller

  2. Optical emission spectroscopy of microwave-plasmas at atmospheric pressure applied to the growth of organosilicon and organotitanium nanopowders

    SciTech Connect

    Kilicaslan, A.; Levasseur, O.; Roy-Garofano, V.; Profili, J.; Moisan, M.; Stafford, L.; Côté, C.; Sarkissian, A.

    2014-03-21

    An atmospheric-pressure plasma sustained by an electromagnetic surface wave (SW) in the microwave regime combined with a bubbler/flash evaporator for the injection of liquid precursors was used to produce organosilicon and organotitanium nanopowders. Following the addition of hexamethyldisiloxane (HMDSO) vapors in the nominally pure argon plasma, optical emission spectra revealed the apparition of strong C{sub 2} molecular bands along with Si and Balmer H emission lines. Such features were not observed in our atmospheric-pressure Ar/HMDSO discharges controlled by dielectric barriers, indicating that microwave plasmas are characterized by much higher fragmentation levels of the precursors due to much higher electron densities. Emission spectra from the Ar/HMDSO SW plasma further showed a high-intensity continuum, the intensity of which decreased with time as powders started to form on the discharge tube walls. In presence of titanium isopropoxide (TTIP) vapors in the nominally pure Ar plasma, the emission was dominated by Ar and Ti lines, with no trace of carbon and no continuum. Fourier-Transform Infrared (FTIR) Spectroscopy of the powders formed in Ar/HMDSO plasmas showed very strong Si-(CH{sub 3}){sub x} and O-Si-(CH{sub 3}){sub x} bands, which is consistent with the formation of silicon oxycarbide. Transmission Electron Microscopy (TEM) further showed tube and sheet-like nanofeatures as well as larger structures consisting of agglomerated primary clusters. On the other hand, introduction of O{sub 2} in Ar/HMDSO plasmas produced only round-like nanoparticles with strong Si-O-Si bands and no trace of carbon, consistent with the formation of SiO{sub x}. The average size of the silica nanoparticles was 50 nm. FTIR spectra of powders formed in Ar/TTIP plasmas showed strong Ti-O signals, even without the addition of O{sub 2} in the gas phase. Corresponding TEM analysis showed nano- and agglomerated features comparable to those obtained in Ar/HMDSO although the

  3. Mechanosynthesis of nanopowders of the proton-conducting electrolyte material Ba(Zr, Y)O{sub 3-{delta}}

    SciTech Connect

    Antunes, I.; Brandao, A.; Figueiredo, F.M.; Frade, J.R.; Gracio, J.; Fagg, D.P.

    2009-08-15

    The formation of perovskite nanopowders of the common proton-conducting, electrolyte material Ba(Zr{sub 1-x}Y{sub x})O{sub 3-{delta}} is demonstrated by room temperature mechanosynthesis for the compositional range x=0, 0.058 and 0.148. This is achieved with a planetary ball mill at 650 rpm in zirconia vials, starting from BaO{sub 2} with ZrO{sub 2}, (ZrO{sub 2}){sub 0.97}(Y{sub 2}O{sub 3}){sub 0.03} or (ZrO{sub 2}){sub 0.92}(Y{sub 2}O{sub 3}){sub 0.08} precursors, respectively. Powder X-ray diffraction (XRD) reveals the formation of the perovskite phase in the early stages of milling with phase purity being achieved after milling times of 240 min for composition x=0.058 whereas 420 min is necessary for composition x=0.148. In contrast, traces of ZrO{sub 2} are apparent in composition x=0 even after milling times of 420 min. The use of BaCO{sub 3} as precursor does not allow the formation of the perovskite phase for any composition. The perovskite crystallites are spherical in shape with an average size determined from XRD of ca. 30 nm in agreement with transmission electron microscopy observations. FTIR spectra demonstrate that contamination levels of BaCO{sub 3} in the mechanosynthesized powders are very low. The spherical shape and nanoscale of the crystallites allow densification levels that are highly competitive when compared to BaZrO{sub 3}-based materials formed by alternative synthesis techniques documented in the literature. - Graphical abstract: The formation of perovskite nanopowders of the common proton-conducting, electrolyte, material Ba(Zr{sub 1-x}Y{sub x})O{sub 3-{delta}} is demonstrated by room temperature mechanosynthesis, starting from BaO{sub 2} with ZrO{sub 2}, (ZrO{sub 2}){sub 0.97}(Y{sub 2}O{sub 3}){sub 0.03} or (ZrO{sub 2}){sub 0.92}(Y{sub 2}O{sub 3}){sub 0.08} precursors.

  4. Characterization of Sr-substituted hydroxyapatite thin film by sputtering technique from mixture targets of hydroxyapatite and strontium apatite.

    PubMed

    Ozeki, K; Goto, T; Aoki, H; Masuzawa, T

    2014-01-01

    Sr-substituted hydroxyapatite thin films were prepared by sputtering technique from mixture targets of hydroxyapatite (HA) and strontium apatite (SrAp). The HA and SrAp powders were mixed at 0-100% Sr/(Sr+Ca) target ratios. The coated films were recrystallized by a hydrothermal treatment to reduce film dissolution. The films were then characterized by X-ray diffractometry (XRD), scanning electron microscopy (SEM) and inductively coupled plasma atomic emission spectrometry (ICP). The osteocompatiblity of the films was also evaluated by the size of the bone formation area in osteoblast cells.In the XRD patterns, peaks shifted to lower 2θ values with increasing Sr/(Sr+Ca) target ratios, which indicated Sr incorporation into the HA lattice. In the SEM observation of the hydrothermally treated films, the surface was covered with globular particles, and the size of the globular particles increased from Sr0 to Sr40, and then the size decreased from Sr60 to Sr100. The ICP analysis showed that the Sr/(Sr+Ca) film ratios were almost the same as the target ratios. In the cell culture, the bone formation area on the Sr-substituted HA films increased with increasing Sr concentration, and saturated at Sr60. PMID:24642972

  5. Effect of Ni doping on structural and optical properties of Zn{sub 1−x}Ni{sub x}O nanopowder synthesized via low cost sono-chemical method

    SciTech Connect

    Singh, Budhendra; Kaushal, Ajay; Bdikin, Igor; Venkata Saravanan, K.; Ferreira, J.M.F.

    2015-10-15

    Highlights: • Pure and Ni doped ZnO nanopowders were synthesized by low cost sonochemical method. • The optical properties of Zn{sub 1−x}Ni{sub x}O nanopowders can be tuned by varying Ni content. • The results reveal the solubility limit of Ni into ZnO matrix as below 8%. - Abstract: Zn{sub 1−x}Ni{sub x}O nanopowders with different Ni contents of x = 0.0, 0.04 and 0.08 were synthesized via cost effective sonochemical reaction method. X-ray diffraction (XRD) pattern reveals pure wurtzite phase of prepared nanostructures with no additional impurity peaks. The morphology and dimensions of nanoparticles were investigated using scanning electron microscope (SEM). A sharp and strong peak for first order optical mode for wurtzite zinc oxide (ZnO) structure was observed at ∼438 cm{sup −1} in Raman spectra. The calculated optical band gap (E{sub g}) from UV–vis transmission data was found to decrease with increase in Ni content. The observed red shift in E{sub g} with increasing Ni content in ZnO nanopowders were in agreement with band gap behaviours found in their photoluminescence (PL) spectra. The synthesised ZnO nanopowders with controlled band gap on Ni doping reveals their potential for use in various electronic and optical device applications. The results were discussed in detail.

  6. Organically modified porous hydroxyapatites: A comparison between alkylphosphonate grafting and citrate chelation

    SciTech Connect

    El-Hammari, L.; Marroun, H.; Laghzizil, A.; Saoiabi, A.; Roux, C.; Livage, J.; Coradin, T.

    2008-04-15

    Two alternative methods to prepare organically modified porous hydroxyapatites following a 'one pot' approach were compared. The partial substitution of inorganic phosphates by alkylphosphonates leads to mesoporous materials with high specific surface area (>200 m{sup 2} g{sup -1}). The incorporation of the organic moieties within the hydroxyapatite structure is confirmed by Infra-red and solid-state NMR spectroscopy and depends on the nature of the alkyl chain. However, it induces a significant loss of the material crystallinity. In contrast, the introduction of citrate, a calcium-chelating agent, to the precursor solution does not improve the material specific surface area but allows a better control of the hydroxyapatite structure, both in terms of crystallinity and pore size distribution. - Graphical abstract: Evolution of pore size distribution of hydroxyapatite (HAp) after alkylphosphonate grafting (20% TPOH) or citrate addition (c-HAp) demonstrates the formation of organically modified mesoporous materials.

  7. Micro- and nano-hydroxyapatite as active reinforcement for soft biocomposites.

    PubMed

    Munarin, F; Petrini, P; Gentilini, R; Pillai, R S; Dirè, S; Tanzi, M C; Sglavo, V M

    2015-01-01

    Pectin-based biocomposite hydrogels were produced by internal gelation, using different hydroxyapatite (HA) powders from commercial source or synthesized by the wet chemical method. HA possesses the double functionality of cross-linking agent and inorganic reinforcement. The mineralogical composition, grain size, specific surface area and microstructure of the hydroxyapatite powders are shown to strongly influence the properties of the biocomposites. Specifically, the grain size and specific surface area of the HA powders are strictly correlated to the gelling time and rheological properties of the hydrogels at room temperature. Pectin pH is also significant for the formation of ionic cross-links and therefore for the hydrogels stability at higher temperatures. The obtained results point out that micrometric-size hydroxyapatite can be proposed for applications which require rapid gelling kinetics and improved mechanical properties; conversely the nanometric hydroxyapatite synthesized in the present work seems the best choice to obtain homogeneous hydrogels with more easily controlled gelling kinetics. PMID:25109458

  8. Template-directed synthesis and selective adsorption of oligoadenylates in hydroxyapatite

    NASA Technical Reports Server (NTRS)

    Gibbs, D.; Lohrmann, R.; Orgel, L. E.

    1980-01-01

    Polyuridylic acid is adsorbed completely from aqueous solution by hydroxyapatite under conditions that permit template-directed synthesis of oligoadenylates in free solution. The yield of oligoadenylates is enhanced to almost the same extent by poly(U) in the presence or the absence of hydroxyapatite. Under very similar conditions small quantities of hydroxyapatite adsorb higher-molecular-weight oligoadenylates selectively from a mixture of oligomers. On the basis of these results a mechanism for prebiotic oligonucleotide formation is proposed in which selective adsorption on hydroxyapatite or some other immobilized anion-exchanging material plays a major role. Monomers are released from the surface for reactivation, while oligomers are retained in a protected environment by adsorption to the apatite surface.

  9. Crystalline hydroxyapatite coatings synthesized under hydrothermal conditions on modified titanium substrates.

    PubMed

    Suchanek, Katarzyna; Bartkowiak, Amanda; Gdowik, Agnieszka; Perzanowski, Marcin; Kąc, Sławomir; Szaraniec, Barbara; Suchanek, Mateusz; Marszałek, Marta

    2015-06-01

    Hydroxyapatite coatings were successfully produced on modified titanium substrates via hydrothermal synthesis in a Ca(EDTA)(2-) and (NH4)2HPO4 solution. The morphology of modified titanium substrates as well as hydroxyapatite coatings was studied using scanning electron microcopy and phase identification by X-ray diffraction, and Raman and FTIR spectroscopy. The results show that the nucleation and growth of hydroxyapatite needle-like crystals with hexagonal symmetry occurred only on titanium substrates both chemically and thermally treated. No hydroxyapatite phase was detected on only acid etched Ti metal. This finding demonstrates that only a particular titanium surface treatment can effectively induce the apatite nucleation under hydrothermal conditions. PMID:25842108

  10. Bio resorbability of the modified hydroxyapatite in Tris-HCL buffer

    NASA Astrophysics Data System (ADS)

    Golovanova, O. A.; Izmailov, R. R.; Ghyngazov, S. A.

    2016-02-01

    The solubility of carbonated hydroxyapatite powders and granulated carbonated hydroxyapatite produced from the synovial biofluid model solution has been studied. The kinetic characteristics of dissolution were determined. It was found that the solubility of carbonated hydroxyapatite is higher as compared to that of hydroxyapatite. The impact of the organic matrix on the rate of sample dissolution was revealed. For HA-gelatin composites, as the gelatin concentration grows, the dissolution rate becomes greater, and a sample of 6.0 g / L concentration has higher resorbability. The results of the research can be used to study the kinetics of dissolution and the biocompatibility of ceramic materials for medicine, namely for reconstructive surgery, dentistry, and development of drug delivery systems.

  11. Preparation and characterization of an iron oxide-hydroxyapatite nanocomposite for potential bone cancer therapy

    PubMed Central

    Sneha, Murugesan; Sundaram, Nachiappan Meenakshi

    2015-01-01

    Recently, multifunctional magnetic nanostructures have been found to have potential applications in biomedical and tissue engineering. Iron oxide nanoparticles are biocompatible and have distinctive magnetic properties that allow their use in vivo for drug delivery and hyperthermia, and as T2 contrast agents for magnetic resonance imaging. Hydroxyapatite is used frequently due to its well-known biocompatibility, bioactivity, and lack of toxicity, so a combination of iron oxide and hydroxyapatite materials could be useful because hydroxyapatite has better bone-bonding ability. In this study, we prepared nanocomposites of iron oxide and hydroxyapatite and analyzed their physicochemical properties. The results suggest that these composites have superparamagnetic as well as biocompatible properties. This type of material architecture would be well suited for bone cancer therapy and other biomedical applications. PMID:26491311

  12. Simple and Rapid Synthesis of Magnetite/Hydroxyapatite Composites for Hyperthermia Treatments via a Mechanochemical Route

    PubMed Central

    Iwasaki, Tomohiro; Nakatsuka, Ryo; Murase, Kenya; Takata, Hiroshige; Nakamura, Hideya; Watano, Satoru

    2013-01-01

    This paper presents a simple method for the rapid synthesis of magnetite/hydroxyapatite composite particles. In this method, superparamagnetic magnetite nanoparticles are first synthesized by coprecipitation using ferrous chloride and ferric chloride. Immediately following the synthesis, carbonate-substituted (B-type) hydroxyapatite particles are mechanochemically synthesized by wet milling dicalcium phosphate dihydrate and calcium carbonate in a dispersed suspension of magnetite nanoparticles, during which the magnetite nanoparticles are incorporated into the hydroxyapatite matrix. We observed that the resultant magnetite/hydroxyapatite composites possessed a homogeneous dispersion of magnetite nanoparticles, characterized by an absence of large aggregates. When this material was subjected to an alternating magnetic field, the heat generated increased with increasing magnetite concentration. For a magnetite concentration of 30 mass%, a temperature increase greater than 20 K was achieved in less than 50 s. These results suggest that our composites exhibit good hyperthermia properties and are promising candidates for hyperthermia treatments. PMID:23629669

  13. Sol-gel processing and characterization of potassium niobate nano-powders by an EDTA/citrate complexing method

    NASA Astrophysics Data System (ADS)

    Cao, Yang; Zhu, Kongjun; Qiu, Jinhao; Pang, Xuming; Ji, Hongli

    2012-05-01

    The present research describes a modified sol-gel technique used to obtain nano-crystalline potassium niobate (KNbO3) powders by using ethylene diamine tetraacetic acid (EDTA)/citrate as a complexing agent. The metal ions chemically interact with EDTA in the precursor sol. The aging treatments lead to the formation of a precursor-polymeric gel network. The effects of the amounts of citric acid and EDTA on the stability of the precursor sol are investigated. The influence of excess K on the formation of pure-phase KNbO3 powders is also studied. The obtained gels and powders are characterized by thermogravimetric-differential scanning calorimetry, X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. The results indicate that a stable precursor sol is formed when n(CA):n(Mn+) = 3:1 and n(EDTA) :n(NH4OH) = 1:3.5. The xerogel is calcined at 700-850 °C to prepare the KNbO3 nano-powder. The smallest grain size of the sample obtained at 850 °C is about 60 nm when the K/Nb molar ratio equals 1.2.

  14. Shape tailored green synthesis of CeO2:Ho3+ nanopowders, its structural, photoluminescence and gamma radiation sensing properties

    NASA Astrophysics Data System (ADS)

    Malleshappa, J.; Nagabhushana, H.; Kavyashree, D.; Prashantha, S. C.; Sharma, S. C.; Premkumar, H. B.; Shivakumara, C.

    2015-06-01

    CeO2:Ho3+ (1-9 mol%) nanopowders have been prepared by efficient and environmental friendly green combustion method using Aloe vera gel as fuel for the first time. The final products are well characterized by powder X-ray diffraction (PXRD), scanning electron microscopy (SEM), fourier transform infrared (FTIR). Bell, urchin, core shell and flower like morphologies are observed with different concentrations of the A. vera gel. It is apparent that by adjusting the concentration of the gel, considerable changes in the formation of CeO2:Ho3+ nano structures can be achieved. Photoluminescence (PL) studies show green (543, 548 nm) and red (645, 732 nm) emissions upon excited at 400 nm wavelength. The emission peaks at ∼526, 548, 655 and 732 nm are associated with the transitions of 5F3 → 5I8, 5S2 → 5I8, 5F5 → 5I8 and 5S2 → 5I7, respectively. Three TL glow peaks are observed at 118, 267 and 204 °C for all the γ irradiated samples which specify the surface and deeper traps. Linear TL response in the range 0.1-2 kGy shows that phosphor is fairly useful as γ radiation dosimeter. Kinetic parameters associated with the glow peaks are estimated using Chen's half width method. The CIE coordinate values show that phosphor is quite useful for the possible applications in WLEDs as orange red phosphor.

  15. Application of the soluble salt-assisted route to scalable synthesis of ZnO nanopowder with repeated photocatalytic activity.

    PubMed

    Lv, Yingying; Yu, Leshu; Huang, Heyong; Feng, Yuying; Chen, Dongzhen; Xie, Xin

    2012-02-17

    In this paper, the soluble salt-assisted route has been extended to the low-cost and scalable preparation of ZnO nanostructures via the simple oxidation of Zn-Na2SO4 mixture followed by washing with water. The as-prepared ZnO nanopowders are of nanoscaled size, hexagonal phase, and pure, without being stained by Na2SO4. Their optical band gap is 3.22 eV, exhibiting a red-shift of 0.15 eV in comparison with pure ZnO bulk, and their optical absorbance is strong in the region of 200-400 nm, suggesting their full utilization of most of the UV light in sunlight. The product shows evident photocatalytic activity in degradation of RhB under solar light irradiation, and then its solar light degradation efficiency is close to that under UV irradiation, indicating that there is a possibility of practical application. More importantly, the obtained ZnO nanoparticles, because of the quick precipitation by themselves in solution with no stirring, could be easily recycled without any accessorial means such as high-speed centrifuge. The low-cost and scalable preparation, high photocatalytic activity, and convenient recycling of this ZnO nanomaterial gives it potential in purifying waste water. Hence the interesting results in this study indicate the wide range of the soluble salt-assisted route for the industrial preparation of many other advanced nanomaterials. PMID:22248758

  16. Preparation and Scintillating Properties of Sol-Gel Eu3+, Tb3+ Co-Doped Lu2O3 Nanopowders

    PubMed Central

    de Jesús Morales Ramírez, Ángel; Murillo, Antonieta García; de Jesús Carrillo Romo, Felipe; Hernández, Margarita García; Palmerin, Joel Moreno; Guerrero, Rosario Ruiz

    2011-01-01

    Nanocrystalline Eu3+, Tb3+ co-doped Lu2O3 powders with a maximum size of 25.5 nm were prepared by the sol-gel process, using lutetium, europium and terbium nitrates as precursors, and ethanol as a solvent. Differential thermal analysis (DTA) and infrared spectroscopy (IR) were used to study the chemical changes during the xerogel annealing. After the sol evaporation at 100 °C, the formed gel was annealed from 300 to 900 °C for 30 min under a rich O2 atmosphere, and the yielded product was analyzed by X-ray diffraction (XRD) to characterize the microstructural behavior and confirm the crystalline structure. The results showed that Lu2O3 nanopowders start to crystallize at 400 °C and that the crystallite size increases along with the annealing temperature. A transmission electron microscopy (TEM) study of samples annealed at 700 and 900 °C was carried out in order to analyze the microstructure, as well as the size, of crystallites. Finally, in regard to scintillating properties, Eu3+ dopant (5 mol%), Tb3+ codoped Lu2O3 exhibited a typical red emission at 611 nm (D°→7F2), furthermore, the effect of Tb3+ molar content (0.01, 0.015 and 0.02% mol) on the Eu3+ radioluminiscence was analyzed and it was found that the higher emission intensity corresponds to the lower Tb3+ content. PMID:22016655

  17. The effect of Tb 3+ doping on the structure and spectroscopic properties of MgAl 2O 4 nanopowders

    NASA Astrophysics Data System (ADS)

    Wiglusz, R. J.; Grzyb, T.

    2011-08-01

    In this paper, a modified sol-gel method was employed to prepare nanostructured MgAl 2O 4 spinel powders doped with Tb 3+ ions and thermally treated at 700 and 1000 °C for 3 h. The structural properties of the prepared at 700 and 1000 °C powders where characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). According to obtained XRD patterns the formation of single-phase spinels after calcination was confirmed. The XRD analyses demonstrated that the powders were single-phase spinel nanopowders with high crystallite dispersion. The Rietveld method was applied to calculate lattice parameters. The averaged spinel particle size was determined to be ˜10 nm for calcination at 700 °C and ˜20 nm at 1000 °C. The emission and excitation spectra measured at room and low temperature (77 K) for the samples calcined at 700 and 1000 °C demonstrated characteristic spectra of Tb 3+ ions. The effect of MgAl 2O 4:Tb 3+ grain sizes on luminescence properties was noticed.

  18. Variations in Physicochemical Properties of a Traditional Mercury-Based Nanopowder Formulation: Need for Standard Manufacturing Practices

    PubMed Central

    Kamath, S. U.; Pemiah, B.; Rajan, K. S.; Krishnaswamy, S.; Sethuraman, S.; Krishnan, U. M.

    2014-01-01

    Rasasindura is a mercury-based nanopowder synthesized using natural products through mechanothermal processing. It has been used in the Ayurvedic system of medicine since time immemorial for various therapeutic purposes such as rejuvenation, treatment of syphilis and in genital disorders. Rasasindura is said to be composed of mercury, sulphur and organic moieties derived from the decoction of plant extracts used during its synthesis. There is little scientific understanding of the preparation process so far. Though metallic mercury is incorporated deliberately for therapeutic purposes, it certainly raises toxicity concerns. The lack of gold standards in manufacturing of such drugs leads to a variation in the chemical composition of the final product. The objective of the present study was to assess the physicochemical properties of Rasasindura samples of different batches purchased from different manufacturers and assess the extent of deviation and gauge its impact on human health. Modern characterization techniques were employed to analyze particle size and morphology, surface area, zeta potential, elemental composition, crystallinity, thermal stability and degradation. Average particle size of the samples observed through scanning electron microscope ranged from 5-100 nm. Mercury content was found to be between 84 and 89% from elemental analysis. Despite batch-to-batch and manufacturer-to-manufacturer variations in the physicochemical properties, all the samples contained mercury in the form of HgS. These differences in the physicochemical properties may ultimately impact its biological outcome. PMID:25593382

  19. Role of paramagnetic defects in light emission processes in Y-doped ZrO2 nanopowders

    NASA Astrophysics Data System (ADS)

    Korsunska, N.; Baran, M.; Zhuk, A.; Polishchuk, Yu; Stara, T.; Kladko, V.; Bacherikov, Yu; Venger, Ye; Konstantinova, T.; Khomenkova, L.

    2014-12-01

    Luminescence and structural properties of pure and Y-doped ZrO2 nanopowders with different Y content synthesized by co-precipitation of Zr and Y salts were investigated by x-ray diffraction, transmission electron microscopy, electron paramagnetic resonance (EPR) and photoluminescence (PL) methods. It was found that at constant calcination temperature (700 °С), the increase of Y content stimulates the transformation of crystalline phase from monoclinic through the tetragonal to the cubic one. Generally, room temperature PL emission was found to be similar for the samples with different Y content, demonstrating the same overlapped PL components in visible spectral range under extrinsic excitation. The relative contribution of each PL component was found to be affected by calcination time. In EPR spectra of as-prepared samples no signals were observed. The annealing in N2 or H2 flow results in the appearance of the signal from surface Zr3+ defects. In the latter the signal assigned to F-center also arises. The anti-correlation observed between the PL intensity and the value of the Zr3+ EPR signal allows us to conclude that the Zr3+ center is the center of fast non-radiative recombination. At the same time, interrelation between the intensity of the EPR signal assigned to F-centers and observed PL bands was not found.

  20. Influence of Cr on structural and optical properties of TiO 2:Cr nanopowders prepared by flame spray synthesis

    NASA Astrophysics Data System (ADS)

    Trenczek-Zajac, A.; Radecka, M.; Jasinski, M.; Michalow, K. A.; Rekas, M.; Kusior, E.; Zakrzewska, K.; Heel, A.; Graule, T.; Kowalski, K.

    Influence of chromium incorporation on structural and optical properties of titanium dioxide nanopowders obtained by flame spray synthesis, FSS is studied by means of: X-ray diffraction, XRD; Raman spectroscopy; transmission electron spectroscopy, TEM; photoelectron spectroscopy, XPS and optical spectrophotometry over the ultraviolet, UV and visible range of the light spectrum from 250 nm to 2200 nm. The specific surface area, SSA, of the powders has been adjusted from 48 m 2/g for TiO 2 + 0.1at.% Cr to 177 m 2/g for TiO 2 + 15 at.% Cr which is accompanied by a decrease in the anatase grain size from 21 nm to 5 nm. The anatase-to-rutile ratio changes with Cr 3+ concentration but there is no evidence of precipitation of chromium oxides or chromium titanates. Incorporation of Cr 3+ into TiO 2 lattice, as proved by XPS, is found to affect the electronic structure of TiO 2, as indicated by the optical spectrophotometry. The impurity band is formed within the forbidden band gap of titanium dioxide which results in the additional absorption within the visible range of the light spectrum. The general aim of this work is to improve the visible light absorption and hence the efficiency of photocatalytic decomposition of organic contaminants.

  1. Diffusion Processes in Water on Oxide Surfaces: Quasielastic Neutron Scattering Study of Hydration Water in Rutile Nano-Powder

    SciTech Connect

    Chu, Xiang-Qiang; Ehlers, Georg; Mamontov, Eugene; Podlesnyak, Andrey A; Wang, Wei; Wesolowski, David J

    2011-01-01

    Quasielastic neutron scattering (QENS) was used to investigate the diffusion dynamics of hydration water on the surface of rutile (TiO{sub 2}) nanopowder. The dynamics measurements utilizing two inelastic instruments, a backscattering spectrometer and a disk chopper spectrometer, probed the fast, intermediate, and slow motions of the water molecules on the time scale of picoseconds to more than a nanosecond. We employed a model-independent analysis of the data collected at each value of the scattering momentum transfer to investigate the temperature dependence of several diffusion components. All of the probed components were present in the studied temperature range of 230-320 K, providing, at a first sight, no evidence of discontinuity in the hydration water dynamics. However, a qualitative change in the elastic scattering between 240 and 250 K suggested a surface freezing-melting transition, when the motions that were localized at lower temperatures became delocalized at higher temperatures. On the basis of our previous molecular dynamics simulations of this system, we argue that interpretation of QENS data from such a complex interfacial system requires at least qualitative input from simulations, particularly when comparing results from spectrometers with very different energy resolutions and dynamic ranges.

  2. Al-Mg co-doping effect on optical and magnetic properties of ZnO nanopowders

    NASA Astrophysics Data System (ADS)

    Si, Xiaodong; Liu, Yongsheng; Wu, Xinfang; Lei, Wei; Lin, Jia; Gao, Tian; Zheng, Li

    2015-07-01

    Zn0.97 - xMgxAl0.03O (x = 0 , 0.01 , 0.03 and 0.05) nanoparticles were prepared by hydrothermal growth, and their optical and magnetic properties were systematically studied by the X-ray diffraction (XRD), the UV-visible spectrophotometer, the infrared spectrometer and the physical properties measurement system (PPMS). These results showed that all the nanopowders had hexagonal wurtzite structures. With increasing the content of Mg, the strength of the (110) intensity peak increased. When Mg atoms were not incorporated into the Zn0.97Al0.03O lattice, the infrared light transmittance was higher than that of other groups of samples. In the UV range, the absorption decreased with the increase of the concentration of Mg. Mg doping weakened the magnetic property of the nanoparticles at room temperature. The zero-field-cooled (ZFC) and field-cooled (FC) magnetization curves were separated with the decrease of temperature due to the pinning effect between the ferromagnetic domain and antiferromagnetic domain.

  3. Crystallization and microstructure of 8YSZ nanopowders synthesized by ball-mill assisted constant pH route

    NASA Astrophysics Data System (ADS)

    Mohanty, Subrat K.; Nayak, Bibhuti B.

    2013-06-01

    8 mol% Y2O3 stabilized ZrO2 (8YSZ) nanopowders were prepared by two ways of precipitation technique namely conventional precipitation (i.e. stepwise increase of pH) and constant pH precipitation (i.e. precipitation at constant pH). The crystallization, microstructure and density of both the powders were studied with and without ball milling. The ball milled powders prepared in conventional method were found to be sintered upto 92% of the theoretical density, whereas the powders prepared in constant pH precipitation method after ball milling showed 97% of the theoretical density, at 1600°C. The presence of fine and uniformly distributed pores were observed, for the 8YSZ pellets synthesized via conventional precipitation method, whereas a relatively dense microstructure was observed for that synthesized via constant pH precipitation method, from the SEM micrographs. Constant pH route shows better results as compared to conventional route and seems to be effective way of synthesis to prepare 8YSZ for electrolyte in solid oxide fuel cell (SOFC) application.

  4. Application of 8YSZ Nanopowder Synthesized by the Modified Solvothermal Process for Anode Supported Solid Oxide Fuel Cells.

    PubMed

    Meepho, Malinee; Wattanasiriwech, Suthee; Angkavatana, Pavadee; Wattanasiriwech, Darunee

    2015-03-01

    Thin electrolyte yttria-stabilized zirconia (8YSZ) films were coated on the porous solid oxide fuel cell (SOFC) anode substrates for the use at an intermediate temperature range. Nano-8YSZ powder with a particle size of about 5 nm was synthesized using the modified solvothermal process. The electrolyte suspension was prepared by dispersion the synthesized 8YSZ nanopowder in ethanol, with PVB and 1,3-propanediol as a binder and a charging agent respectively. The 8YSZ suspension was subsequently deposited on the pre-sintered NiO-YSZ porous substrates by the electrophoretic deposition (EPD) technique. In order to obtain high quality electrolyte films, preparation process was optimized through two strategic approaches; (i) adjustment of suspension's rheological property and (ii) compatibility of anode-electrolyte sintering shrinkage. Rheological property of the suspension was improved with an addition of 1,3-propanediol. The zeta potential of this suspension was increased and reached the value of +24 mV so the well-dispersed slurry was finally obtained. The second approach was achieved by using a proper composite anode powders. Dense and uniform 8YSZ electrolyte films with a thickness of about 1 thickness successfully be formed on the NiO-YSZ porous substrates after co-sintering at 1400 °C for 2 h. PMID:26413707

  5. Preparation and scintillating properties of Sol-Gel Eu(3+), TB(3+) co-doped Lu(2)O(3) nanopowders.

    PubMed

    de Jesús Morales Ramírez, Angel; Murillo, Antonieta García; de Jesús Carrillo Romo, Felipe; Hernández, Margarita García; Palmerin, Joel Moreno; Guerrero, Rosario Ruiz

    2011-01-01

    Nanocrystalline Eu(3+), Tb(3+) co-doped Lu(2)O(3) powders with a maximum size of 25.5 nm were prepared by the sol-gel process, using lutetium, europium and terbium nitrates as precursors, and ethanol as a solvent. Differential thermal analysis (DTA) and infrared spectroscopy (IR) were used to study the chemical changes during the xerogel annealing. After the sol evaporation at 100 °C, the formed gel was annealed from 300 to 900 °C for 30 min under a rich O(2) atmosphere, and the yielded product was analyzed by X-ray diffraction (XRD) to characterize the microstructural behavior and confirm the crystalline structure. The results showed that Lu(2)O(3) nanopowders start to crystallize at 400 °C and that the crystallite size increases along with the annealing temperature. A transmission electron microscopy (TEM) study of samples annealed at 700 and 900 °C was carried out in order to analyze the microstructure, as well as the size, of crystallites. Finally, in regard to scintillating properties, Eu(3+) dopant (5 mol%), Tb(3+) codoped Lu(2)O(3) exhibited a typical red emission at 611 nm (D(°)→(7)F(2)), furthermore, the effect of Tb(3+) molar content (0.01, 0.015 and 0.02% mol) on the Eu(3+) radioluminiscence was analyzed and it was found that the higher emission intensity corresponds to the lower Tb(3+) content. PMID:22016655

  6. Improved compaction of ZnO nano-powder triggered by the presence of acetate and its effect on sintering

    NASA Astrophysics Data System (ADS)

    Dargatz, Benjamin; Gonzalez-Julian, Jesus; Guillon, Olivier

    2015-04-01

    The retention of nanocrystallinity in dense ceramic materials is still a challenge, even with the application of external pressure during sintering. The compaction behavior of high purity and acetate enriched zinc oxide (ZnO) nano-powders was investigated. It was found that acetate in combination with water plays a key role during the compaction into green bodies at moderate temperatures. Application of constant pressure resulted in a homogeneous green body with superior packing density (86% of theoretical value) at moderate temperature (85 °C) in the presence of water. In contrast, no improvement in density could be achieved if pure ZnO powder was used. This compaction behavior offers superior packing of the particles, resulting in a high relative density of the consolidated compact with negligible coarsening. Dissolution accompanying creep diffusion based matter transport is suggested to strongly support reorientation of ZnO particles towards densities beyond the theoretical limit for packing of ideal monosized spheres. Finally, the sintering trajectory reveals that grain growth is retarded compared to conventional processing up to 90% of theoretical density. Moreover, nearly no radial shrinkage was observed after sinter-forging for bodies performed with this advanced processing method.

  7. Surface modification for titanium implants by hydroxyapatite nanocomposite

    PubMed Central

    Family, Roxana; Solati-Hashjin, Mehran; Namjoy Nik, Shahram; Nemati, Ali

    2012-01-01

    Background: Titanium (Ti) implants are commonly coated with hydroxyapatite (HA). However, HA has some disadvantages such as brittleness, low tensile strength and fracture toughness. It is desirable to combine the excellent mechanical properties of ZrO2 and the chemical inertness of Al2O3 with respect to the purpose of this project which was coating Ti implants with HA-ZrO2-Al2O3 to modify the surface of these implants by adding ZrO2 and Al2O3 to HA. The purpose of this study was to evaluate the efficacy of hydroxyapatite coating nonocomposite. Methods: From September 2009 to January2011, functionally graded HA-Al2O3-ZrO2 and HA coatings were applied on Ti samples. HA-Al2O3-ZrO2 and HA sols were orderly dip coated on the substrates and calcined. Scanning electron microscopy and EDS were used to estimate the particle size of the surfaces and for morphological analysis. The morphology of non-coated HA-coated HA-Al2O3-ZrO2 (composite-coated) and double-layer composite coated samples were compared with one other. Mechanical test (heat & quench) was also done for comparing single-phase (HA), composite and double-layer composite samples. Results: The morphology of HA-Al2O3-ZrO2 coating is more homogenous than HA-coated and uncoated samples. Furthermore, single-layer coating is more homogenous than double-layer coating. EDS analysis was done on HA-coated sample and showed that the Ca/P ratio in the film was similar to the theoretical value 1.67 in HA. Conclusion: Surface modification of Ti implants can be done by coating them with single-layer of HA-Al2O3-ZrO2. Single-layer hydroxyapatite-alumina-zirconia coated sample has the most homogenous morphology on the surface. PMID:24009915

  8. Preparation and characterization of hydroxyapatite/sodium alginate biocomposites for bone implant application

    NASA Astrophysics Data System (ADS)

    Kanasan, Nanthini; Adzila, Sharifah; Suid, Mohd Syafiq; Gurubaran, P.

    2016-07-01

    In biomedical fields, synthetic scaffolds are being improved by using the ceramics, polymers and composites materials to avoid the limitations of allograft. Ceramic-polymer composites are appearing to be the most successful bone graft substitute in human body. The natural bones itself are well-known as composite of collagen and hydroxyapatite. In this research, precipitation method was used to synthesis hydroxyapatite (HA)/sodium alginate (SA) in various parameters. This paper describes the hydroxyapatite/sodium alginate biocomposite which suitable for use in bone defects or regeneration of bone through the characterizations which include FTIR, FESEM, EDS and DTA. In FTIR, the characteristi peaks of PO4-3 and OH- groups which corresponding to hydroxyapatite are existed in the mixing powders. The needle-size particle of hydroxyapatite/ alginate (HA/SA) are observed in FESEM in the range of 15.8nm-38.2nm.EDS confirmed the existence of HA/SA composition in the mixing powders. There is an endothermic peak which corresponds to the dehydration and the loss of physically adsorbed water molecules of the hydroxyapatite (HA)/sodium alginate (SA) powder which are described in DTA.

  9. Preparation of hollow hydroxyapatite microspheres by the conversion of borate glass at near room temperature

    SciTech Connect

    Yao, Aihua; Ai, Fanrong; Liu, Xin; Wang, Deping; Huang, Wenhai; Xu, Wei

    2010-01-15

    Hollow hydroxyapatite microspheres, consisting of a hollow core and a porous shell, were prepared by converting Li{sub 2}O-CaO-B{sub 2}O{sub 3} glass microspheres in dilute phosphate solution at 37 {sup o}C. The results confirmed that Li{sub 2}O-CaO-B{sub 2}O{sub 3} glass was transformed to hydroxyapatite without changing the external shape and dimension of the original glass object. Scanning electron microscopy images showed the shell wall of the microsphere was built from hydroxyapatite particles, and these particles spontaneously align with one another to form a porous sphere with an interior cavity. Increase in phosphate concentration resulted in an increase in the reaction rate, which in turn had an effect on shell wall structure of the hollow hydroxyapatite microsphere. For the Li{sub 2}O-CaO-B{sub 2}O{sub 3} glass microspheres reacted in low-concentration K{sub 2}HPO{sub 4} solution, lower reaction rate and a multilayered microstructure were observed. On the other hand, the glass microspheres reacted in higher phosphate solution converted more rapidly and produced a single hydroxyapatite layer. Furthermore, the mechanism of forming hydroxyapatite hollow microsphere was described.

  10. In situ synthesis of hydroxyapatite nanocomposites using iron oxide nanofluids at ambient conditions.

    PubMed

    Sheikh, Lubna; Mahto, Neha; Nayar, Suprabha

    2015-01-01

    This paper describes a simple method for the room temperature synthesis of magnetite/hydroxyapatite composite nanocomposites using ferrofluids. The in situ synthesis of magnetic-hydroxyapatite results in a homogenous distribution of the two phases as seen both in transmission electron micrographs and assembled to a micron range in the confocal micrographs. The selected area diffraction pattern analysis shows the presence of both phases of iron oxide and hydroxyapatite. To the dialyzed ferrofluid, the constituents of hydroxyapatite synthesis was added, the presence of the superparamagnetic iron oxide particles imparts directionality to the hydroxyapatite crystal growth. Electron probe microanalysis confirms the co-existence of both iron and calcium atoms. Vibrating Sample magnetometer data shows magnetization three times more than the parent ferrofluid, the local concentration of iron oxide nanoparticles affects the strength of dipolar interparticle interactions changing the energy barrier for determining the collective magnetic behavior of the sample. The limitations inherent to the use of external magnetic fields which can be circumvented by the introduction of internal magnets located in the proximity of the target by a minimal surgery or by using a superparamagnetic scaffold under the influence of externally applied magnetic field inspires us to increase the magnetization of our samples. The composite in addition shows anti-bacterial properties against the two gram (-ve) bacteria tested. This work is significant as magnetite-hydroxyapatite composites are attracting a lot of attention as adsorbents, catalysts, hyperthermia agents and even as regenerative medicine. PMID:25589209

  11. Nanosized hydroxyapatite powder synthesized from eggshell and phosphoric acid.

    PubMed

    Lee, Sang-Jin; Yoon, Young-Soo; Lee, Myung-Hyun; Oh, Nam-Sik

    2007-11-01

    The present research describes synthesis of highly sinterable, nano-sized hydroxyapatite (HAp) powders using a wet chemical route with recycled eggshell and phosphoric acid as calcium and phosphorous sources. The raw eggshell was easily turned to CaO by the calcining process, and phosphoric acid was mixed with the calcined eggshell by the wet, ball-milling method. The crystalline development and microstructures of the synthesized powders and sintered samples were examined by X-ray diffractometry and scanning electron microscopy, respectively. The observed phases on the powder synthesis process were dependent on the mixing ratio (wt%) of the calcined eggshell to phosphoric acid and the heating temperature. The ball-milled, nano-sized HAp powder, which has an average particle size of 70 nm, was fully densified at 1300 degrees C for 1h. The Ca/P ratio for stoichiometric composition of HAp was controlled by adjustment of the mixing ratio. PMID:18047119

  12. Retrospective dosimetry using synthesized nano-structure hydroxyapatite.

    PubMed

    Ziaie, F; Hajiloo, N; Alipour, A; Amraei, R; Mehtieva, S I

    2011-06-01

    Micro and nano-structure hydroxyapatite samples were synthesized via several different methods. The samples were characterised utilising the Fourier transmission infra-red, scanning electron microscope and X-ray diffraction methods, to find out the structure most similar to human tooth enamel, and the best method was found. The electron paramagnetic resonance (EPR) signals of the gamma-irradiated samples were measured using an EPR spectrometer system. A calibration curve was established by irradiation of the samples at four doses of 50-500 mGy. The parameters of the calibration curve, slope and intercept with dose axis are determined by linear regression analysis. This calibration curve can be used for human tooth enamel for retrospective dosimetry purposes. PMID:21131666

  13. Low temperature synthesis and characterization of carbonated hydroxyapatite nanocrystals

    NASA Astrophysics Data System (ADS)

    Anwar, Aneela; Asghar, Muhammad Nadeem; Kanwal, Qudsia; Kazmi, Mohsin; Sadiqa, Ayesha

    2016-08-01

    Carbonate substituted hydroxyapatite (CHA) nanorods were synthesized via coprecipitation method from aqueous solution of calcium nitrate tetrahydrate and diammonium hydrogen phosphate (with urea as carbonate ion source) in the presence of ammonium hydroxide solution at 70 °C at the conditions of pH 11. The obtained powders were physically characterized using transmission electron microscopy (TEM), X-ray powder diffraction analysis (XRD), and FTIR and Raman spectroscopy. The particle size was evaluated by Dynamic light scattering (DLS). The chemical structural analysis of as prepared sample was performed using X-ray photoelectron spectroscopy (XPS). After ageing for 12 h, and heat treatment at 1000 °C for 1 h, the product was obtained as highly crystalline nanorods of CHA.

  14. Dielectric relaxation in monoclinic hydroxyapatite: Observation of hydroxide ion dipoles

    NASA Astrophysics Data System (ADS)

    Horiuchi, N.; Wada, N.; Nozaki, K.; Nakamura, M.; Nagai, A.; Yamashita, K.

    2016-02-01

    We prepared monoclinic hydroxyapatite (HAp) ceramics and measured their dielectric properties. The dielectric dispersion that was observed in the monoclinic HAp consisted of two different relaxations and could be expressed by a summation of two Debye-like relaxations. One relaxation was ascribed to the reorientational motions of OH- ions. The temperature dependence of the relaxation time obeyed the Arrhenius equation. The relaxation time decreased with temperature but decreased discontinuously at 483 K, the monoclinic-hexagonal phase transition temperature of HAp. Correspondingly, the activation energy changed from 0.74 eV for the monoclinic phase to 0.43 eV for the hexagonal phase. The results suggest that the mobility of the OH- ions increases discontinuously with the phase transition to hexagonal HAp. However, critical phenomena, such as critical slowing down, were not observed.

  15. Thermoluminescence properties of gamma-irradiated nano-structure hydroxyapatite.

    PubMed

    Shafaei, M; Ziaie, F; Sardari, D; Larijani, M M

    2016-02-01

    The suitability of nano-structured hydroxyapatite (HAP) for use as a thermoluminescence dosimeter was investigated. HAP samples were synthesized using a hydrolysis method. The formation of nanoparticles was confirmed by X-ray diffraction and average particle size was estimated to be ~30 nm. The glow curve exhibited a peak centered at around 200 °C. The additive dose method was applied and this showed that the thermoluminescence (TL) glow curves follow first-order kinetics due to the non-shifting nature of Tm after different doses. The numbers of overlapping peaks and related kinetic parameters were identified from Tm -Tstop through computerized glow curve deconvolution methods. The dependence of the TL responses on radiation dose was studied and a linear dose response up to 1000 Gy was observed for the samples. PMID:26015169

  16. Biomimetic hydroxyapatite as a new consolidating agent for archaeological bone

    NASA Astrophysics Data System (ADS)

    North, Alexis E.

    Recent studies on calcareous stone and plaster consolidation have demonstrated considerable potential by bio-mimicking the growth of hydroxyapatite (HAP), the main mineralogical constituent of teeth and bone matrix. These initial conservation applications, together with significant fundamental research on the precipitation of HAP for bioengineering and biomedical applications, offer great promise in the use of HAP as a consolidating agent for archaeological bone and other similar materials such as archaeological teeth, ivory, and antler. Experimental research via the controlled application of diammonium phosphate (DAP) precursors to bone flour, modern bone samples, and archaeological bones, indicated the in situ formation of HAP with a simultaneous increase in the cohesiveness of friable bone material, while preserving the bone's physiochemical properties. These preliminary results point towards a promising new method in archaeological conservation.

  17. Hydroxyapatite whisker-reinforced polyetherketoneketone bone ingrowth scaffolds.

    PubMed

    Converse, Gabriel L; Conrad, Timothy L; Merrill, Christina H; Roeder, Ryan K

    2010-03-01

    Hydroxyapatite (HA) whisker-reinforced polyetherketoneketone (PEKK) bone ingrowth scaffolds were prepared and characterized. High levels of porosity (75-90%) and HA whisker reinforcement (0-40 vol.%) were attained using a powder processing approach to mix the HA whiskers, PEKK powder and a NaCl porogen, followed by compression molding at 350-375 degrees Celsius and particle leaching to remove the porogen. The scaffold architecture and microstructure exhibited characteristics known to be favorable for osteointegration. Scaffold porosity was interconnected with a mean pore size in the range 200-300 microm as measured by micro-computed tomography. HA whiskers were embedded within and exposed on the surface of scaffold struts, producing a microscale surface topography, shown by von Kossa staining and scanning electron microscopy. Therefore, HA whisker-reinforced PEKK bone ingrowth scaffolds may be advantageous for orthopedic implant fixation, including interbody spinal fusion. PMID:19665061

  18. Polarization-induced surface charges in hydroxyapatite ceramics

    NASA Astrophysics Data System (ADS)

    Horiuchi, N.; Nakaguki, S.; Wada, N.; Nozaki, K.; Nakamura, M.; Nagai, A.; Katayama, K.; Yamashita, K.

    2014-07-01

    Calcium hydroxyapatite (HAp; Ca10(PO4)6(OH)2) is a well-known biomaterial that is the main inorganic component of bones and teeth. Control over the surface charge on HAp would be a key advance in the development of the material for tissue engineering. We demonstrate here that surface charge can be induced by an electrical poling process using the Kelvin method. Positive and negative charges were induced on the HAp surface in response to the applied electric field in the poling process. The surface charging is attributed to dipole polarization that is homogeneously distributed in HAp. Additionally, the surface charging is considered to originate from the organization of OH- ions into a polar phase in the structure.

  19. Problem of hydroxyapatite dispersion in polymer matrices: a review.

    PubMed

    Supová, Monika

    2009-06-01

    This review summarizes recent work on manufacturing biocomposites suitable for bone tissue engineering. There is a great need to engineer multi-phase (i.e. composite) materials that combine the advantages exhibited by each component of the material, with a structure and composition similar to that of natural bone. The discussion concentrates on the preparation of nanocomposites containing hydroxyapatite particles (one of the most widely used bioceramics materials) with polymer matrices. Special attention is paid to the preparation of nanocomposites with individual (non-aggregated) nanoparticles because this is a key problem in nanotechnology industrialization. Controlling the mixing between so two dissimilar phases is a critical challenge in the design of these inorganic-organic systems. Several approaches that may be applied to overcome this problem will be described in this review. PMID:19225871

  20. Preparation and Comprehensive Characterization of a Calcium Hydroxyapatite Reference Material

    PubMed Central

    Markovic, Milenko; Fowler, Bruce O.; Tung, Ming S.

    2004-01-01

    Numerous biological and chemical studies involve the use of calcium hydroxyapatite (HA), Ca10(PO4)6(OH)2. In this study detailed physicochemical characterization of HA, prepared from an aqueous solution, was carried out employing different methods and techniques: chemical and thermal analyses, x-ray diffraction, infrared and Raman spectroscopies, scanning and transmission microscopies, and Brunauer, Emmett, and Teller (BET) surface-area method. The contents of calcium (Ca2+), phosphate (PO43−), hydroxide (OH−), hydrogenphosphate (HPO42−), water (H2O), carbonate (CO32−), and trace constituents, the Ca/P molar ratio, crystal size and morphology, surface area, unit-cell parameters, crystallinity, and solubility of this HA were determined. This highly pure, homogeneous, and highly crystalline HA is certified as a National Institute of Standards and Technology (NIST) standard reference material, SRM 2910. PMID:27366634

  1. Bone protein extraction without demineralization utilizing principles from hydroxyapatite chromatography

    PubMed Central

    Cleland, Timothy P.; Vashishth, Deepak

    2014-01-01

    Historically, extraction of bone proteins has relied on the use of demineralization to better retrieve proteins from the extracellular matrix; however, demineralization can be a slow process that restricts subsequent analysis of the samples. Here, we developed a novel protein extraction method that does not use demineralization, but utilizes a methodology from hydroxyapatite chromatography where high concentrations of ammonium phosphate and ammonium bicarbonate are used to extract bone proteins. We report that this method has a higher yield than previously published small-scale extant bone extractions, with and without demineralization. Furthermore, after digestion with trypsin and subsequent HPLC-MS/MS analysis, we were able to detect several extracellular matrix and vascular proteins in addition to collagen I and osteocalcin. Our new method has the potential to isolate proteins in a short period (4 hrs) and provide information about bone proteins that may be lost during demineralization or with the use of denaturing agents. PMID:25535955

  2. Nanocrystalline Hydroxyapatite/Si Coating by Mechanical Alloying Technique

    PubMed Central

    Hannora, Ahmed E.; Mukasyan, Alexander S.; Mansurov, Zulkhair A.

    2012-01-01

    A novel approach for depositing hydroxyapatite (HA) films on titanium substrates by using mechanical alloying (MA) technique has been developed. However, it was shown that one-hour heat treatment at 800°C of such mechanically coated HA layer leads to partial transformation of desired HA phase to beta-tri-calcium phosphate (β-TCP) phase. It appears that the grain boundary and interface defects formed during MA promote this transformation. It was discovered that doping HA by silicon results in hindering this phase transformation process. The Si-doped HA does not show phase transition to β-TCP or decomposition after heat treatment even at 900°C. PMID:22312324

  3. Hydroxyapatite/metal composite coatings formed by electrocodeposition.

    PubMed

    Dasarathy, H; Riley, C; Coble, H D; Lacefield, W R; Maybee, G

    1996-05-01

    Early bone infusion by cementless fixation of composite orthopedic and dental implants consisting of metallic substrates and bioceramics is well documented. Calcium phosphate ceramics in general and hydroxyapatite (HA) in particular have been the most popular of the bioceramics used for coating metals. Here, a non-line of sight coating procedure by electrocodeposition is reported for mechanically fixing HA particles in a metal matrix. Analyses of the coating showed excellent adhesion to the substrate and no structural transformation in either crystallinity or stoichiometry. Adhesion and surface coverage of HA depended upon the particle size. As a demonstration of the coating procedure's non-line of sight applicability, it was successfully used to coat titanium rods sintered with small titanium spheres. PMID:8731152

  4. Sulfobetaine as a zwitterionic mediator for 3D hydroxyapatite mineralization

    PubMed Central

    Liu, Pingsheng; Song, Jie

    2013-01-01

    Both positively and negatively charged residues play pivotal roles in recruiting precursor ions or ion clusters, and lowering interfacial energy in natural biomineralization process. Synergistic utilization of opposite charges, however, has rarely been implemented in the design of cytocompatible synthetic scaffolds promoting hydroxyapatite (HA)-mineralization and osteointegration. We report the use of cytocompatible zwitterionic sulfobetaine ligands to enable 3-dimensional in vitro mineralization of HA across covalently crosslinked hydrogels. The overall charge-neutral zwitterionic hydrogel effectively recruited oppositely charged precursor ions while overcame excessive swelling exhibited by anionic and cationic hydrogels under physiological conditions, resulting in denser and structurally well-integrated mineralized composites. Further controls over the size, content, and spatial distribution of the mineral domains within the zwitterionic hydrogel are accomplished by facile adjustments of hydrogel crosslinking densities and the supersaturation rate governing heterogeneous mineral nucleation and growth. These findings should inspire many creative uses of zwitterionic polymers and polymer coatings for skeletal tissue repair and regeneration. PMID:23332320

  5. Nano hydroxyapatite-coated implants improve bone nanomechanical properties.

    PubMed

    Jimbo, R; Coelho, P G; Bryington, M; Baldassarri, M; Tovar, N; Currie, F; Hayashi, M; Janal, M N; Andersson, M; Ono, D; Vandeweghe, S; Wennerberg, A

    2012-12-01

    Nanostructure modification of dental implants has long been sought as a means to improve osseointegration through enhanced biomimicry of host structures. Several methods have been proposed and demonstrated for creating nanotopographic features; here we describe a nanoscale hydroxyapatite (HA)-coated implant surface and hypothesize that it will hasten osseointegration and improve its quality relative to that of non-coated implants. Twenty threaded titanium alloy implants, half prepared with a stable HA nanoparticle surface and half grit-blasted, acid-etched, and heat-treated (HT), were inserted into rabbit femurs. Pre-operatively, the implants were morphologically and topographically characterized. After 3 weeks of healing, the samples were retrieved for histomorphometry. The nanomechanical properties of the surrounding bone were evaluated by nanoindentation. While both implants revealed similar bone-to-implant contact, the nanoindentation demonstrated that the tissue quality was significantly enhanced around the HA-coated implants, validating the postulated hypothesis. PMID:23045363

  6. Dynamics of CTAB in hybrid CTAB-hydroxyapatite system

    NASA Astrophysics Data System (ADS)

    Dubey, P.; Sharma, V. K.; Mitra, S.; Verma, G.; Hassan, P. A.; Johnson, M.; Mukhopadhyay, R.

    2016-05-01

    Synthetic hydroxyapatite (HAp) is an important material in biomedical engineering due to its excellent biocompatibility and bioactivity. Here we report dynamics of cetyltrimethylammonium bromide (CTAB) in HAp composite, prepared by co-precipitation method, as studied by quasielastic neutron scattering (QENS) technique. It is found that the observed dynamics involved two time scales associated with fast torsional motion and segmental motion of the CTAB monomers. In addition to segmental motion of the hydrogen atoms, few undergo torsional motion as well. Torsional dynamics was described by a 2-fold jump diffusion model. The segmental dynamics of CTAB has been described assumimg the hydrogen atoms undergoing diffusion inside a sphere of confined volume. While the diffusivity is found to increase with temperature, the spherical volumes within which the hydrogen atoms are undergoing diffusion remain almost unchanged.

  7. Hydroxyapatite nanocrystals: simple preparation, characterization and formation mechanism.

    PubMed

    Mohandes, Fatemeh; Salavati-Niasari, Masoud; Fathi, Mohammadhossein; Fereshteh, Zeinab

    2014-12-01

    Crystalline hydroxyapatite (HAP) nanoparticles and nanorods have been successfully synthesized via a simple precipitation method. To control the shape and particle size of HAP nanocrystals, coordination ligands derived from 2-hydroxy-1-naphthaldehyde were first prepared, characterized by Fourier transform infrared (FT-IR) and proton nuclear magnetic resonance ((1)H-NMR) spectroscopies, and finally applied in the synthesis process of HAP. On the other hand, the HAP nanocrystals were also characterized by several techniques including powder X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). According to the FE-SEM and TEM micrographs, it was found that the morphology and crystallinity of the HAP powders depended on the coordination mode of the ligands. PMID:25491798

  8. Hydroxyapatite-phosphonoformic acid hybrid compounds prepared by hydrothermal method

    NASA Astrophysics Data System (ADS)

    Turki, Thouraya; Othmani, Masseoud; Bantignies, Jean-Louis; Bouzouita, Khaled

    2014-01-01

    Hydroxyapatites were prepared in the presence of different amounts of phosphonoformic acid (PFA) via the hydrothermal method. The obtained powders were characterized through chemical analysis, XRD, IR, 31P MAS-NMR, TEM, and TG-TDA. The XRD showed that the PFA did not affect the apatite composition. Indeed, only a reduction of the crystallite size was noted. After grafting of PFA, the IR spectroscopy revealed the appearance of new bands belonging to HPO42- and carboxylate groups of the apatite and organic moiety, respectively. Moreover, the 31P MAS-NMR spectra exhibited a peak with a low intensity assigned to the terminal phosphonate group of the organic moiety in addition to that of the apatite. Based on these results, a reaction mechanism involving the surface hydroxyl groups (tbnd Casbnd OH) of the apatite and the carboxyl group of the acid was proposed.

  9. Spheroidized Hydroxyapatite (HA) Powders Plasma Spraying of Combustion Flame

    NASA Astrophysics Data System (ADS)

    Khor, K. A.; Wang, Y.; Cheang, P.

    1998-06-01

    Tailoring powder characteristics to suit the plasma spray process can alleviate difficulties associated with the preparation of hydroxyapatite (HA) coatings. Commercial HA feedstock normally exhibit an angular morphology and a wide particle size range that present difficulties in powder transport from the powder hopper to the plasma spray gun and in nonuniform melting of the powders in the plasma flame. Hence, combustion flame spheroidized hydroxyapatite (SHA) was used as the feedstock for plasma spraying. Spherical particles within a narrow particle size range are found to be more effective for the plasma spray processes. Results show coatings generated from spheroidized HA powders have unique surface and microstructure characteristics. Scanning electron microscope (SEM) observation of the coating surface revealed well-formed splats that spread and flatten into disc configurations with no disintegration, reflecting adequate melting of the HA in the plasma and subsequent deposition consistency. The surface topography is generally flat with good overlapping of subsequent spreading droplets. Porosity in the form of macropores is substantially reduced. The cross-section microstructure reveals a dense coating comprised of randomly stacked lamellae. The tensile bond strengths of the SHA coatings, phase composition, and characteristics of the coatings generated with different particle sizes (125 to 75 µm, 45 to 75 µm, 20 to 45 µm, and 5 to 20 µm) showed that a high bond strength of ˜16 MPa can be obtained with SHA in the size range from 20 to 45 µm. This can be improved further by a postspray treatment by hot isostatic pressing (HIP). However, larger particle size ranges exhibited higher degrees of crystallinity and relatively higher HA content among the various calcium phosphate phases found in the coatings.

  10. Mechanisms of uranium interactions with hydroxyapatite: Implications for groundwater remediation

    USGS Publications Warehouse

    Fuller, C.C.; Bargar, J.R.; Davis, J.A.; Piana, M.J.

    2002-01-01

    The speciation of U(VI) sorbed to synthetic hydroxyapatite was investigated using a combination of U LIII-edge XAS, synchrotron XRD, batch uptake measurements, and SEM-EDS. The mechanisms of U(VI) removal by apatite were determined in order to evaluate the feasibility of apatitebased in-situ permeable reactive barriers (PRBs). In batch U(VI) uptake experiments with synthetic hydroxyapatite (HA), near complete removal of dissolved uranium (>99.5%) to <0.05 ??M was observed over a range of total U(VI) concentrations up to equimolar of the total P in the suspension. XRD and XAS analyses of U(VI)-reacted HA at sorbed concentrations ???4700 ppm U(VI) suggested that uranium(VI) phosphate, hydroxide, and carbonate solids were not present at these concentrations. Fits to EXAFS spectra indicate the presence of Ca neighbors at 3.81 A??. U-Ca separation, suggesting that U(VI) adsorbs to the HA surfaces as an inner-sphere complex. Uranium(VI) phosphate solid phases were not detected in HA with 4700 ppm sorbed U(VI) by backscatter SEM or EDS, in agreement with the surface complexation process. In contrast, U(VI) speciation in samples that exceeded 7000 ppm sorbed U(VI) included a crystalline uranium(VI) phosphate solid phase, identified as chernikovite by XRD. At these higher concentrations, a secondary, uranium(VI) phosphate solid was detected by SEM-EDS, consistent with chernikovite precipitation. Autunite formation occurred at total U:P molar ratios ???0.2. Our findings provide a basis for evaluating U(VI) sorption mechanisms by commercially available natural apatites for use in development of PRBs for groundwater U(VI) remediation.

  11. Photodegradation of pharmaceutical persistent pollutants using hydroxyapatite-based materials.

    PubMed

    Márquez Brazón, E; Piccirillo, C; Moreira, I S; Castro, P M L

    2016-11-01

    Pharmaceutical persistent pollutants pose a serious threat to the environment. The aim of this study was to use, for the first time, hydroxyapatite-based biomaterials as photocatalysts to degrade micropollutants. Diclofenac and fluoxetine were selected for these initial tests. Hydroxyapatite (Ca10(PO4)(OH)2, HAp) is one of the most commonly used biomaterials/bioceramics, being a major constituent of bone. In this work sustainable HAp-based materials of marine origin, obtained from cod fish bones, were used; these photocatalysts were previously fully studied and characterised. Both single-phase HAp and HAp-titania multicomponent materials (1 wt% TiO2) were employed as UV light photocatalysts, the latter showing better performance, indicated by higher degradation rates of both compounds. The HAp-titania photocatalyst showed excellent degradation of both persistent pollutants, the maximum degradation performance being 100% for fluoxetine and 92% for diclofenac, with pollutant and photocatalyst concentrations of 2 ppm and 4 g/L, respectively. Variations in features such as pollutant and photocatalyst concentrations were investigated, and results showed that generally fluoxetine was degraded more easily than diclofenac. The photocatalyst's crystallinity was not affected by the photodegradation reaction; indeed the material exhibited good photostability, as the degradation rate did not decrease when the material was reused. Tests were also performed using actual treated wastewater; the photocatalyst was still effective, even if with lower efficiency (-20% and -4% for diclofenac and fluoxetine, respectively). TOC analysis showed high but incomplete mineralisation of the pollutants (maximum 60% and 80% for DCF and FXT, respectively). PMID:27526086

  12. The influence of hydroxyapatite particles on osteoclast cell activities.

    PubMed

    Sun, J S; Lin, F H; Hung, T Y; Tsuang, Y H; Chang, W H; Liu, H C

    1999-06-15

    Aseptic loosening after total joint arthroplasty is a major problem in orthopedic surgery. Small particles from material wear have been reported as the main cause of implant failure. For this reason, investigation into possible wear particles from the materials used in the implant may lead to longevity after arthroplasty. Hydroxyapatite (HA) has been extensively investigated and reported as an excellent biomaterial with excellent biocompatibility. In this study, we used an in vitro osteoblast/osteoclast model to test the biocompatibility of various-sized HA particles. Primary osteoclasts/osteoblasts were co-cultured with different-sized HA particles (0.5-3.0 microm, 37-53 microm, 177-205 microm, and 420-841 microm) for 3 h, 1 day, 3 days, and 7 days. Cellular responses to the HA particles were evaluated by changes in cell counts and the secretion of transforming growth factor (TGF-beta1), alkaline phosphatase (ALP), tumor necrosis factor (TNF-alpha), prostaglandin (PGE2), and lactate dehydrogenase (LDH) in the supernatant of the culture media. The results showed that osteoblasts/osteoclasts co-cultured with HA particles smaller than 53 microm undergo the most significant changes. Cellular counts significantly decreased, and the changes were more obvious in the osteoblast population. There also was a significant decrease in TGF-beta1 concentration and a significant increase in PGE2 and LDH concentration, but there were no changes in the TNF-alpha or ALP titer. It can be concluded that larger HA particles may be quite compatible with bone cells while smaller-sized HA particles can both activate the osteoclasts and decrease the cell population of the osteoblasts. Justification for the additional expense incurred with the use of hydroxyapatite in primary total hip arthroplasty should be further evaluated. PMID:10321703

  13. Microwave assisted synthesis of nano sized sulphate doped hydroxyapatite

    SciTech Connect

    Alshemary, Ammar Z.; Goh, Yi-Fan; Akram, Muhammad; Razali, Ili Rabihah; Abdul Kadir, Mohammed Rafiq; Hussain, Rafaqat

    2013-06-01

    Highlights: ► Phase pure nano-sized sulphur doped hydroxyapatite has been synthesized. ► TEM analysis confirmed formation of needle shaped structure. ► Lattice parameters and cell volume increased with increase in sulphate doping. ► Crystallite size decreased as sulphate content inside the structure increased. ► Degree of crystallinity decreased with increase in sulphate substitution. - Abstract: Inorganic sulphate is required by all mammalian cells to function properly, it is the fourth most abundant anion in the human plasma. Sulphate ions are the major source of sulphur which is considered an important element for sustenance of life as it is present in the essential amino and is required by cells to function properly. In this study we have successfully substituted sulphate ions (SO{sub 4}{sup 2−}) into hydroxyapatite (Ca{sub 10}(PO{sub 4}){sub 6−x}(SO{sub 4}){sub x}(OH){sub 2−x}) lattice via ion exchange process with phosphate group. Concentration of SO{sub 4}{sup 2−} ions was varied between X = 0.05–0.5, using (Ca (NO{sub 3}){sub 2}·4H{sub 2}O), ((NH{sub 4}){sub 2}HPO{sub 4}) and (Na{sub 2}SO{sub 4}) as starting materials. X-ray diffraction (XRD), Fourier transform IR spectroscopy (FTIR), showed that the substitution of SO{sub 4}{sup 2−} ions into the lattice resulted in peak broadening and reduced peak height due to the amorphous nature and reduced crystallinity of the resulting HA powder. Transmission electron microscopy (TEM) and field emission electron microscopy (FESEM) analysis confirmed the formation of needle shaped particles of 41 nm size with homogenous and uniform distribution of element within the HA structure.

  14. Corrosion behavior of plasma sprayed hydroxyapatite and hydroxyapatite-silicon oxide coatings on AISI 304 for biomedical application

    NASA Astrophysics Data System (ADS)

    Singh, Gurpreet; Singh, Hazoor; Sidhu, Buta Singh

    2013-11-01

    The objective of this study is to evaluate corrosion resistance of plasma sprayed hydroxyapatite (HA) and HAsbnd silicon oxide (SiO2) coated AISI 304 substrates. In HAsbnd SiO2 coatings, 10 wt% SiO2 and 20 wt% SiO2 was mixed with HA. The feedstock and coatings were characterized by X-ray diffraction and scanning electron microscopy/energy dispersive X-ray spectroscopy. The corrosion resistance was determined for the uncoated and coated samples. The corrosion resistance of the AISI 304 was found more after the deposition of the HAsbnd SiO2 coatings rather than HA coating and uncoated. All the coatings were crack free after 24 h dipping in Ringer's solution for electrochemical corrosion testing.

  15. Design of polymer-biopolymer-hydroxyapatite biomaterials for bone tissue engineering: Through molecular control of interfaces

    NASA Astrophysics Data System (ADS)

    Verma, Devendra

    In this dissertation, novel biomaterials are designed for bone biomaterials and bone tissue engineering applications. Novel biomaterials of hydroxyapatite with synthetic and natural polymers have been fabricated using a combination of processing routes. Initially, we investigated hydroxyapatite-polycaprolactone-polyacrylic acid composites and observed that minimal interfacial interactions between polymer and mineral led to inadequate improvement in the mechanical properties. Bioactivity experiments on these composites showed that the presence of functional groups, such as carboxylate groups, influence bioactivity of the composites. We have developed and investigated composites of hydroxyapatite with chitosan and polygalacturonic acid (PgA). Chitosan and PgA are biocompatible, biodegradable, and also electrostatically complementary to each other. This strategy led to significant improvement in mechanical properties of new composites. The nanostructure analysis using atomic force microscopy revealed a multilevel organization in these composites. Enhancement in mechanical response was attributed to stronger interfaces due to strong electrostatic interaction between oppositely charged chitosan and PgA. Further analysis using the Rietveld method showed that biopolymers have marked impact on hydroxyapatite crystal growth and also on its crystal structure. Significant changes were observed in the lattice parameters of hydroxyapatite synthesized by following biomineralization method (organics mediated mineralization). For scaffold preparation, chitosan and PgA were mixed first, and then, nano-hydroxyapatite was added. Oppositely charged polyelectrolytes, such as chitosan and PgA, spontaneously form complex upon mixing. The poly-electrolyte complex exists as nano-sized particles. Chitosan/PgA scaffolds with and without hydroxyapatite were prepared by the freeze drying method. By controlling the rate of cooling and concentration, we have produced both fibrous and sheet

  16. Comparison of structural and luminescence properties of Dy{sub 2}O{sub 3} nanopowders synthesized by co-precipitation and green combustion routes

    SciTech Connect

    Chandrasekhar, M.; Nagabhushana, H.; Sudheerkumar, K.H.; Dhananjaya, N.; Sharma, S.C.; Kavyashree, D.; Shivakumara, C.; Nagabhushana, B.M.

    2014-07-01

    Highlights: • Dy{sub 2}O{sub 3} nanopowders were prepared by co-precipitation and eco-friendly green combustion route using plant latex. • Both the products show excellent chromaticity coordinates in the white region, which were quite useful for white LED’s. • Thermoluminescence response of the Dy{sub 2}O{sub 3} product prepared by green synthesis was higher when compared to co-precipitation route. • Structural parameters of Dy{sub 2}O{sub 3} were estimated using Rietveld refinement. • The development of nanosize materials using eco-friendly resources was an attractive non-hazardous chemical route. - Abstract: Dysprosium oxide (Dy{sub 2}O{sub 3}) nanopowders were prepared by co-precipitation (CP) and eco-friendly green combustion (GC) routes. SEM micrographs prepared by CP route show smooth rods with various lengths and diameters while, GC route show porous, agglomerated particles. The results were further confirmed by TEM. Thermoluminescence (TL) responses of the nanopowder prepared by both the routes were studied using γ-rays. A well resolved glow peak at 353 °C along with less intense peak at 183 °C was observed in GC route while, in CP a single glow peak at 364 °C was observed. The kinetic parameters were estimated using Chen’s glow peak route. Photoluminescence (PL) of Dy{sub 2}O{sub 3} shows peaks at 481, 577, 666 and 756 nm which were attributed to Dy{sup 3+} transitions of {sup 4}F{sub 9/2}⟶{sup 6}H{sub 15/2}, {sup 6}H{sub 13/2}, {sup 6}H{sub 11/2} and {sup 6}H{sub 9/2}, respectively. Color co-ordinate values were located in the white region as a result the product may be useful for the fabrication of WLED’S.

  17. Production of Y{sub 3}Al{sub 5}O{sub 12} and Y{sub 2}O{sub 3} nanopowders for optical ceramics

    SciTech Connect

    Baumer, V. N.; Deineka, T. G.; Korshikova, T. A.; Vovk, E. A.; Kosmyna, M. B.; Nazarenko, B. P.; Puzikov, V. M.; Sergienko, Z. P.; Tkachenko, V. F.; Tolmachev, A. V.; Shekhovtsov, A. N.

    2008-12-15

    The physical and technical conditions for reproducible production of nanodispersed yttrium aluminum garnet (Y{sub 3}Al{sub 5}O{sub 12}, YAG) and yttrium oxide (Y{sub 2}O{sub 3}) powders by chemical coprecipitation have been investigated. It is established that the obtained YAG nanopowders have enhanced reactivity, which significantly decreases the temperature range of interaction in the Y{sub 2}O{sub 3}-Al{sub 2}O{sub 3} system in comparison with ceramic synthesis. It is shown that vacuum heat treatment may lead to reversible transformation of the YAG crystal structure from cubic to tetragonal.

  18. [Preparation and spectroscopy properties of Eu2 (CA)3 (phen)2 doped Eu3+/TiO2 nano-powders].

    PubMed

    Zhao, Si-qin; Guo, Min; Zhang, Mei; Wang, Xi-gui; Chang, Shan

    2010-08-01

    The 1% Eu3+ doped Eu3+ /TiO2 nano-powders were prepared via sol-gel method by using Eu(NO3)3 and Eu2 (CA)3 (phen)2 (CA: camphoric acid; phen: 1, 10-phenanthroline) as precursors respectively, and the samples were characterized by thermal analyses (TG-DTA), X-ray powder diffraction(XRD), scanning electron microscope(SEM), Fourier transform infrared spectroscopy (FTIR), UV-Vis absorption spectra and fluorescence spectra for their microstructure, morphology and spectroscopy properties. The results of TG-DTA and XRD indicate that the increasing trend of particle size and the conversion temperature of crystalline phase of the as prepared samples was restrained when using organic complexes Eu2(CA)3 (phen)2 as the do pant. The particle size was decreased from 9 to 7 nm, and the name powders were still anatase TiO2 when the calcination temperature was increased up to 500 degrees C. The absorption peak at about 370 nm in UV-Vis spectra was red-shifted when doping with organic complexes Eu2 (CA)3 (phen)2, namely the doped TiO2 nano powders have the ability of visible light responding. The characteristic absorption peaks of organic complex did not appear in FTIR spectrum, indicating that the Eu3+ has little impact on the formation process of TiO2 crystal when using Eu2(CA)3 (phen)2 as precursor. The result of fluorescence spectrum indicates that the characteristic transition of Eu3+ at 578 nm (corresponding to (5)D0---(7)F0), 590 nm((5)D0-(7)F1) and 612 nm ((5)D0-(7)F2) appeared in both samples, in which the peak at 612 nm was the characteristic red transmutation peak. When doping Eu3+ with the same content, the nano-powders using Eu2 (CA)3 (phen)2 as precursor obtain higher luminescence intensity. Therefore, by using a simple approach, the authors prepared the light-emitting rare earth inorganic nano-powders with better luminescence property and high stability, and such inorganic nano-powders might have potential applications in many fields. PMID:20939336

  19. Effect of heat treatment on the structural parameters and magnetic properties of copper ferrite nanopowders obtained by the sol-gel combustion

    NASA Astrophysics Data System (ADS)

    Zhuravlev, V. A.; Naiden, E. P.; Minin, R. V.; Itin, V. I.; Ufimtsev, M. R.

    2016-02-01

    Phase composition, structure parameters and basic magnetic characteristics obtained by the sol-gel combustion nanopowders of ferrospinel CuFe2O4 are investigated. A comparison of the properties of synthesized materials: first sample - immediately after the combustion of the gel and second sample - after annealing at 1073 K for 4 hours are performed. Annealing leads to an increase in the concentration of the phase with tetragonal crystal structure. Particle sizes and the value of anisotropy field of this phase also increased.

  20. Dynamics and structure of hydration water on rutile and cassiterite nanopowders studied by quasielastic neutron scattering and molecular dynamics simulations.

    SciTech Connect

    Mamontov, Eugene; Vlcek, Lukas; Wesolowski, David J

    2007-03-01

    Quasielastic neutron scattering (QENS) experiments carried out using time-of-flight and backscattering neutron spectrometers with widely different energy resolution and dynamic range revealed the diffusion dynamics of hydration water in nanopowder rutile (TiO{sub 2}) and cassiterite (SnO{sub 2}) that possess the rutile crystal structure with the (110) crystal face predominant on the surface. These isostructural oxides differ in their bulk dielectric constants, metal atom electronegativities, and lattice spacings, which may all contribute to differences in the structure and dynamics of sorbed water. When hydrated under ambient conditions, the nanopowders had similar levels of hydration: about 3.5 (OH/H{sub 2}O) molecules per Ti{sub 2}O{sub 4} surface structural unit of TiO{sub 2} and about 4.0 (OH/H{sub 2}O) molecules per Sn{sub 2}O{sub 4} surface unit of SnO{sub 2}. Ab initio optimized classical molecular dynamics (MD) simulations of the (110) surfaces in contact with SPC/E water at these levels of hydration indicate three structurally distinct sorbed water layers L{sub 1}, L{sub 2}, and L{sub 3}, where the L{sub 1} species are either associated water molecules or dissociated hydroxyl groups in direct contact with the surface, L{sub 2} water molecules are hydrogen bonded to L{sub 1} and structural oxygen atoms at the surface, and L{sub 3} water molecules are more weakly bound. At the hydration levels studied, L{sub 3} is incomplete compared with axial oxygen density profiles of bulk SPC/E water in contact with these surfaces, but the structure and dynamics of L{sub 1}-L{sub 3} species are remarkably similar at full and reduced water coverage. Three hydration water diffusion components, on the time scale of a picosecond, tens of picoseconds, and a nanosecond could be extracted from the QENS spectra of both oxides. However, the spectral weight of the faster components was significantly lower for SnO{sub 2} compared to TiO{sub 2}. In TiO{sub 2} hydration water, the

  1. Effect of Hydroxyapatite on Bone Integration in a Rabbit Tibial Defect Model

    PubMed Central

    Sohn, Sung-Keun; Kim, Kyung-Taek; Kim, Chul-Hong; Ahn, Hee-Bae; Rho, Mee-Sook; Jeong, Min-Ho; Sun, Sang-Kyu

    2010-01-01

    Background The aim of the present study was to prepare hydroxyapatite (HA) and then characterize its effect on bone integration in a rabbit tibial defect model. The bone formation with different designs of HA was compared and the bony integration of several graft materials was investigated qualitatively by radiologic and histologic study. Methods Ten rabbits were included in this study; two holes were drilled bilaterally across the near cortex and the four holes in each rabbit were divided into four treatment groups (HAP, hydroxyapatite powder; HAC, hydroxyapatite cylinder; HA/TCP, hydroxyapatite/tri-calcium phosphate cylinder, and titanium cylinder). The volume of bone ingrowth and the change of bone mineral density were statistically calculated by computed tomography five times for each treatment group at 0, 2, 4, 6, and 8 weeks after grafting. Histologic analysis was performed at 8 weeks after grafting. Results The HAP group showed the most pronounced effect on the bone ingrowth surface area, which seen at 4, 6, and 8 weeks after graft (p < 0.05). On comparing the change of bone mineral density the bone ingrowth surface area among the 4 groups, there were no statistically significant differences among the groups found for any period (p > 0.05). On histological examination, the HAP group revealed well-recovered cortical bone, but the bone was irregularly thickened and haphazardly admixed with powder. The HAC group showed similar histological features to those of the HA/TCP group; the cortical surface of the newly developed bone was smooth and the bone matrix on the surface of the cylinder was regularly arranged. Conclusions We concluded that both the hydroxyapatite powder and cylinder models investigated in our study may be suitable as a bone substitute in the rabbit tibial defect model, but their characteristic properties are quite different. In contrast to hydroxyapatite powder, which showed better results for the bone ingrowth surface, the hydroxyapatite

  2. Development of dental composites with reactive fillers that promote precipitation of antibacterial-hydroxyapatite layers.

    PubMed

    Aljabo, Anas; Abou Neel, Ensanya A; Knowles, Jonathan C; Young, Anne M

    2016-03-01

    The study aim was to develop light-curable, high strength dental composites that would release calcium phosphate and chlorhexidine (CHX) but additionally promote surface hydroxyapatite/CHX co-precipitation in simulated body fluid (SBF). 80 wt.% urethane dimethacrylate based liquid was mixed with glass fillers containing 10 wt.% CHX and 0, 10, 20 or 40 wt.% reactive mono- and tricalcium phosphate (CaP). Surface hydroxyapatite layer thickness/coverage from SEM images, Ca/Si ratio from EDX and hydroxyapatite Raman peak intensities were all proportional to both time in SBF and CaP wt.% in the filler. Hydroxyapatite was, however, difficult to detect by XRD until 4 weeks. XRD peak width and SEM images suggested this was due to the very small size (~10 nm) of the hydroxyapatite crystallites. Precipitate mass at 12 weeks was 22 wt.% of the sample CaP total mass irrespective of CaP wt.% and up to 7 wt.% of the specimen. Early diffusion controlled CHX release, assessed by UV spectrometry, was proportional to CaP and twice as fast in water compared with SBF. After 1 week, CHX continued to diffuse into water but in SBF, became entrapped within the precipitating hydroxyapatite layer. At 12 weeks CHX formed 5 to 15% of the HA layer with 10 to 40 wt.% CaP respectively. Despite linear decline of strength and modulus in 4 weeks from 160 to 101 MPa and 4 to 2.4 GPa, respectively, upon raising CaP content, all values were still within the range expected for commercial composites. The high strength, hydroxyapatite precipitation and surface antibacterial accumulation should reduce tooth restoration failure due to fracture, aid demineralised dentine repair and prevent subsurface carious disease respectively. PMID:26706532

  3. Binding strength-associated toxicity reduction by birnessite and hydroxyapatite in Pb and Cd contaminated sediments.

    PubMed

    Lee, Seungbae; An, Jinsung; Kim, Young-Jin; Nam, Kyoungphile

    2011-02-28

    In situ stabilization of sediment-bound heavy metals has been proposed as an alternative to ex situ treatment due to the concerns on ecosystem disturbance and remediation cost. The present study was conducted to test the performance of birnessite, hydroxyapatite, and zeolite as stabilizing agents for Pb and Cd in sediment. The heavy metal binding capacity and strength of the stabilizing agents were determined by analyzing Langmuir model parameters. The three agents showed the similar binding capacity (i.e., maximum monolayer sorption constant, K(a)) ranging from 1.13 to 3.62×10(5) mg/kg for Pb and 1.07 to 1.33×10(5) mg/kg for Cd. In contrast, binding strength (i.e., binding energy constant, b) of birnessite and hydroxyapatite was about one order higher than that of zeolite. This is further supported by five-step sequential extraction data: more than 99 and 70% of freshly spiked Pb and Cd were present as not-readily extractable fractions in birnessite and hydroxyapatite, respectively while the fractions were 17.9 and 14.1% in zeolite. Toxicity Characteristic Leaching Procedure (TCLP) test was also conducted to verify the effectiveness of the heavy metal-stabilizing ability of birnessite and hydroxyapatite. Birnessite successfully retained both Pb and Cd against the leaching solution, satisfying the TCLP extract concentration limits (i.e., 5 and 1 mg/L, respectively). However, hydroxyapatite released about 223.7 mg/L of Cd into the solution, which greatly exceeded the limit. The toxicity test with Hyalella azteca showed that their survival rate increased by 92.5-100% when birnessite or hydroxyapatite was added to Pb- or Cd-spiked sediment as a stabilizing agent. Our data demonstrate the potential use of birnessite and hydroxyapatite as an effective in situ remediation means for heavy metal-contaminated sediment with minimal risk to the aquatic ecosystem. PMID:21255927

  4. Formation of Chloropyromorphite in a Lead-Contaminated Soil Amended with Hydroxyapatite

    SciTech Connect

    RYAN,JAMES A.; ZHANG,PENGCHU; HESTERBERG,DEAN; ZHOU,WEIQING; SAYERS,DALE E.

    2000-07-14

    To confirm conversion of soil Pb to pyromorphite [Pb{sub 5}(PO{sub 4}){sub 3}Cl], a Pb contaminated soil collected adjacent to a historical smelter was reacted with hydroxyapatite in slurries of soil and hydroxyapatite separated by a dialysis membrane and incubated. A crystalline precipitate formed on the dialysis membrane in the slurry systems was identified as chloropyromorphite. Soluble species measured in the soil slurry indicated that dissolution of solid-phase soil Pb was the rate-limiting step for pyromorphite formation. Additionally samples reacted with hydroxyapatite were incubated at field-capacity moisture content. The sequential chemical extraction used to identify species in the field-moist soil incubation experiment showed that hydroxyapatite treatment reduced the first four fractions of extractable Pb and correspondingly increased the recalcitrant extraction residue fraction by 35% of total Pb at 0 d incubation and by 45% after 240 d incubation. the increase in the extraction residue fraction in the 240 d incubation as compared to the 0 d incubation implies that the reaction occurs in the soil but the increase in the hydroxyapatite amended 0 d incubated soil as compared to the control soil illustrates the chemical extraction procedure caused changes in the extractability. Thus, the chemical extraction procedure cannot easily be utilized to confirm changes occurring in the soil as a result of incubation. Extended x-ray absorption fine structure (EXAFS) spectroscopy indicated that the 240 d incubated hydroxyapatite treatment caused a change in the average, local molecular bonding environment of soil Pb. Low-temperature EXAFS spectra (chi data and radial structure functions - RSFs) showed a high degree of similarity between the chemical extraction residue and synthetic pyromorphite. Thus, confirming that the change of soil Pb to pyromorphite is possible by simple amendments of hydroxyapatite to soil.

  5. Reassigning the most stable surface of hydroxyapatite to the water resistant hydroxyl terminated (010) surface

    NASA Astrophysics Data System (ADS)

    Zeglinski, Jacek; Nolan, Michael; Thompson, Damien; Tofail, Syed A. M.

    2014-05-01

    Understanding the surface stability and crystal growth morphology of hydroxyapatite is important to comprehend bone growth and repair processes and to engineer protein adsorption, cellular adhesion and biomineralization on calcium phosphate based bone grafts and implant coatings. It has generally been assumed from electronic structure calculations that the most stable hydroxyapatite surface is the (001) surface, terminated just above hydroxyl ions perpendicular to the {001} crystal plane. However, this is inconsistent with the known preferential growth direction of hydroxyapatite crystals and previous experimental work which indicates that, contrary to currently accepted theoretical predictions, it is actually the (010) surface that is preferentially exposed. The surface structure of the (010) face is still debated and needs reconciliation. In this work, we use a large set of density functional theory calculations to model the interaction of water with hydroxyapatite surfaces and probe the surface stability and resistance to hydrolytic remodeling of a range of surface faces including the (001) surface and the phosphate-exposed, calcium-exposed, and hydroxyl-exposed terminations of the (010) surface. For the (001) surface and the phosphate-exposed (010) surface, dissociative water adsorption is favorable. In contrast, the hydroxyl-terminated (010) surface will not split water and only molecular adsorption of water is possible. Our calculations show, overall, that the hydroxyl-terminated (010) surface is the most stable and thus should be the predominant form of the hydroxyapatite surface exposed in experiments. This finding reconciles discrepancies between the currently proposed surface terminations of hydroxyapatite and the experimentally observed crystal growth direction and surface stability, which may aid efforts to accelerate biomineralization and better control bone-repair processes on hydroxyapatite surfaces.

  6. Synthesis and magnetization studies of nanopowder Fe₇₀Ni₂₀Cr₁₀ alloys prepared by high energy milling

    SciTech Connect

    Chater, R.; Bououdina, M.; Chaanbi, D.; Abbas, H.

    2013-05-01

    Nanocrystalline Fe{sub 1–x–y}NixCry (x=20, y=10% in Wt)) alloy samples were prepared by mechanical alloying process. Fe, Ni and Cr elemental powders have been ball milled in a planetary mill for various periods of time, up to 27 h. XRD analysis allowed the determination of the structure of the mixture, the average crystallite size and the lattice parameter as a function of milling time. The complete formation of FeNiCr is observed after 27 h milling. With increasing milling time from 0 to 27 h, it is observed that the lattice parameter increases from 0.3515 to 0.3593 nm as well as an increase of microstrain from 0.15 to 0.40%, whereas the grain size decreases from 48 to 13 nm. Grain morphology of the powders at different formation stages was examined using SEM. Saturation magnetization and coercive fields derived from the hysteresis curves are discussed as a function of milling time. - Graphical abstract: Fe₇₀Ni₂₀Cr₁₀ nanopowders were prepared using a planetary ball mill. The structure and microstructure vary with milling time; thereby important modifications of the magnetic properties were observed and discussed. Highlights: • Nanocrystalline Fe₇₀Ni₂₀Cr₁₀ alloy were prepared by the mechanical alloying process. • The complete formation of Fe₇₀Ni₂₀Cr₁₀ is observed after 24 h milling. • With increasing milling time, the grain size decreases, while the strain increases. • The SEM images allowed following the morphology of the materials at different stages. • Ms and HC derived from the hysteresis are discussed as a function of milling time.

  7. Formation of hydroxyapatite by hydrolysis of alpha-tricalcium phosphate

    NASA Astrophysics Data System (ADS)

    Durucan, Caner

    Low-temperature cement-type formation of hydroxyapatite [Ca10(PO4)6(OH)2 or HAp) has value in terms of developing synthetic compounds similar in compositions to those formed by natural mineralization of bone. Understanding the in vitro kinetics of formation of the synthetic composition could produce insights into developing hard tissue analogs. The kinetics and chemistry of cement-type formation of HAp by hydrolysis of particulate alpha-tricalcium phosphate (alpha-Ca 3(PO4)2 or alpha-TCP) were examined. In particular, the effects of reaction temperature, synthesis route, inorganic salt additives and presence of biodegradable polymers (poly(alpha-hydroxyl acids) on the hydrolysis rate and microstructural/mechanical properties of HAp were determined using the following analytical techniques: isothermal calorimetry, x-ray diffraction, scanning electron microscsopy (SEM), fourier transform infrared spectroscopy (FTIR), solution chemistry, diametrical compression and 3-point bending tests. For the phase-pure alpha-TCP/water system the complete reaction times and morphologies of the resultant HAp were found to be strongly dependent on reaction temperature over a range of 37°C to 56°C. Isothermal calorimetry analyses revealed a thermally activated hydrolysis mechanism, leading to higher reaction rates with an increase in hydrolysis temperature. The microstructure of the resultant HAp typically had entangled, flake-like morphology, with HAp formed at 37°C having a smaller crystalline size than that formed at 45°C and 56°C. The cement hardening contributed to entanglement at the microstructural level. In all cases the hydrated product was phase pure calcium-deficient hydroxyapatite [Ca10-x(HPO4) x(PO4)6-x(OH)2-x], and no other intermediates or by-products were formed through the complete transformation. According to the proposed kinetic model, a two-step mechanism was found to control the overall hydrolysis reaction and thereby HAp formation at 37°C. During the first

  8. EFFECTS OF AQUEOUS AL, CD, CU, FE(II), NI, AND ZN ON PB IMMOBILIZATION BY HYDROXYAPATITE

    EPA Science Inventory

    The effects of aqueous Al, Cd, Cu, Fe(II), Ni, or Zn on Pb immobilization by hydroxyapatite (Ca10(PO4),(OH)2) were studied. ead was removed mainly via hydroxyapatite dissolution and hydroxypyromorphite (Pb10(PO4)6(OH)2) precipitation in the presence of these metals with a Pb remo...

  9. Highly efficient one-pot three-component synthesis of naphthopyran derivatives in water catalyzed by hydroxyapatite

    EPA Science Inventory

    An expeditious and efficient protocol for the synthesis of naphthopyrans has been developed that proceeds via one-pot three-component sequential reaction in water catalyzed by hydroxyapatite or sodium-modified-hydroxyapatite. The title compounds have been obtained in high yield a...

  10. Novel synthesis strategy for composite hydrogel of collagen/hydroxyapatite-microsphere originating from conversion of CaCO3 templates

    NASA Astrophysics Data System (ADS)

    Wei, Qingrong; Lu, Jian; Wang, Qiaoying; Fan, Hongsong; Zhang, Xingdong

    2015-03-01

    Inspired by coralline-derived hydroxyapatite, we designed a methodological route to synthesize carbonated-hydroxyapatite microspheres from the conversion of CaCO3 spherulite templates within a collagen matrix under mild conditions and thus constructed the composite hydrogel of collagen/hydroxyapatite-microspheres. Fourier transform infrared spectroscopy (FTIR) and x-ray diffraction (XRD) were employed to confirm the successful generation of the carbonated hydroxyapatite phase originating from CaCO3, and the ratios of calcium to phosphate were tracked over time. Variations in the weight portion of the components in the hybrid gels before and after the phase transformation of the CaCO3 templates were identified via thermogravimetric analysis (TGA). Scanning electron microscopy (SEM) shows these composite hydrogels have a unique multiscale microstructure consisting of a collagen nanofibril network and hydroxyapatite microspheres. The relationship between the hydroxyapatite nanocrystals and the collagen fibrils was revealed by transmission electron microscopy (TEM) in detail, and the selected area electron diffraction (SAED) pattern further confirmed the results of the XRD analyses which show the typical low crystallinity of the generated hydroxyapatite. This smart synthesis strategy achieved the simultaneous construction of microscale hydroxyapatite particles and collagen fibrillar hydrogel, and appears to provide a novel route to explore an advanced functional hydrogel materials with promising potentials for applications in bone tissue engineering and reconstruction medicine.

  11. Biomimetic hydroxyapatite coating on pore walls improves osteointegration of poly(L-lactic acid) scaffolds.

    PubMed

    Deplaine, H; Lebourg, M; Ripalda, P; Vidaurre, A; Sanz-Ramos, P; Mora, G; Prósper, F; Ochoa, I; Doblaré, M; Gómez Ribelles, J L; Izal-Azcárate, I; Gallego Ferrer, G

    2013-01-01

    Polymer-ceramic composites obtained as the result of a mineralization process hold great promise for the future of tissue engineering. Simulated body fluids (SBFs) are widely used for the mineralization of polymer scaffolds. In this work an exhaustive study with the aim of optimizing the mineralization process on a poly(L-lactic acid) (PLLA) macroporous scaffold has been performed. We observed that when an air plasma treatment is applied to the PLLA scaffold its hydroxyapatite nucleation ability is considerably improved. However, plasma treatment only allows apatite deposition on the surface of the scaffold but not in its interior. When a 5 wt % of synthetic hydroxyapatite (HAp) nanoparticles is mixed with PLLA a more abundant biomimetic hydroxyapatite layer grows inside the scaffold in SBF. The morphology, amount, and composition of the generated biomimetic hydroxyapatite layer on the pores' surface have been analyzed. Large mineralization times are harmful to pure PLLA as it rapidly degrades and its elastic compression modulus significantly decreases. Degradation is retarded in the composite scaffolds because of the faster and extensive biomimetic apatite deposition and the role of HAp to control the pH. Mineralized scaffolds, covered by an apatite layer in SBF, were implanted in osteochondral lesions performed in the medial femoral condyle of healthy sheep. We observed that the presence of biomimetic hydroxyapatite on the pore's surface of the composite scaffold produces a better integration in the subchondral bone, in comparison to bare PLLA scaffolds. PMID:23152082

  12. Fabrication and in vitro biological evaluation of photopolymerisable hydroxyapatite hydrogel composites for bone regeneration.

    PubMed

    Killion, John A; Geever, Luke M; Devine, Declan M; Higginbotham, Clement L

    2014-04-01

    The aim of this study was to improve the bioactive and compressive properties of photopolymerisable polyethylene glycol hydrogels with the incorporation of hydroxyapatite at different loadings. The synthesis of pure hydroxyapatite was verified through Fourier transform infrared spectroscopy (FTIR) analysis by the complete reaction of all constituents. The formation of a bioactive layer of the hydrogel based composites was confirmed through the formation of carbonate hydroxyapatite after soaking the samples in simulated body fluid. The incorporation of hydroxyapatite into the system resulted in an increase in Young's modulus from 4.36 to 12.73 MPa and an increase in the stress at limit value from 1.20 to 4.42 MPa. This was due to the hydroxyapatite absorbing the compressive load, the polymer matrix distributing the load, a reduction in swelling and the presence of physical crosslinking between both components. Drug dissolution testing showed that the release rate of a drug from the hydrogels was dependent on the molecular weight of the polymer and the type of drug used. PMID:24114559

  13. Synthesis and properties of hybrid hydroxyapatite-ferrite (Fe3O4) particles for hyperthermia applications

    NASA Astrophysics Data System (ADS)

    Tkachenko, M. V.; Kamzin, A. S.

    2016-04-01

    Hybrid ceramics consisting of hydroxyapatite Ca10(PO4)6(OH)2 and ferrite Fe3O4 were synthesized using a two-stage procedure. The first stage included the synthesis of Fe3O4 ferrite particles by co-precipitation and the synthesis of hydroxyapatite. In the second stage, the magnetic hybrid hydroxyapatite-ferrite bioceramics were synthesized by a thorough mixing of the obtained powders of carbonated hydroxyapatite and Fe3O4 ferrite taken in a certain proportion, pressing into tablets, and annealing in a carbon dioxide atmosphere for 30 min at a temperature of 1200°C. The properties of the components and hybrid particles were investigated using X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and Mössbauer spectroscopy. The saturation magnetization of the hybrid ceramic composite containing 20 wt % Fe3O4 was found to be 12 emu/g. The hybrid hydroxyapatite (Ca10(PO4)6(OH)2)-ferrite Fe3O4 ceramics, which are promising for the use in magnetotransport and hyperthermia treatment, were synthesized and investigated for the first time.

  14. Comparison of the x-ray attenuation properties of breast calcifications, aluminium, hydroxyapatite and calcium oxalate

    NASA Astrophysics Data System (ADS)

    Warren, L. M.; Mackenzie, A.; Dance, D. R.; Young, K. C.

    2013-04-01

    Aluminium is often used as a substitute material for calcifications in phantom measurements in mammography. Additionally, calcium oxalate, hydroxyapatite and aluminium are used in simulation studies. This assumes that these materials have similar attenuation properties to calcification, and this assumption is examined in this work. Sliced mastectomy samples containing calcification were imaged at ×5 magnification using a digital specimen cabinet. Images of the individual calcifications were extracted, and the diameter and contrast of each calculated. The thicknesses of aluminium required to achieve the same contrast as each calcification when imaged under the same conditions were calculated using measurements of the contrast of aluminium foils. As hydroxyapatite and calcium oxalate are also used to simulate calcifications, the equivalent aluminium thicknesses of these materials were also calculated using tabulated attenuation coefficients. On average the equivalent aluminium thickness was 0.85 times the calcification diameter. For calcium oxalate and hydroxyapatite, the equivalent aluminium thicknesses were 1.01 and 2.19 times the thickness of these materials respectively. Aluminium and calcium oxalate are suitable substitute materials for calcifications. Hydroxyapatite is much more attenuating than the calcifications and aluminium. Using solid hydroxyapatite as a substitute for calcification of the same size would lead to excessive contrast in the mammographic image.

  15. Comparison of the x-ray attenuation properties of breast calcifications, aluminium, hydroxyapatite and calcium oxalate.

    PubMed

    Warren, L M; Mackenzie, A; Dance, D R; Young, K C

    2013-04-01

    Aluminium is often used as a substitute material for calcifications in phantom measurements in mammography. Additionally, calcium oxalate, hydroxyapatite and aluminium are used in simulation studies. This assumes that these materials have similar attenuation properties to calcification, and this assumption is examined in this work. Sliced mastectomy samples containing calcification were imaged at ×5 magnification using a digital specimen cabinet. Images of the individual calcifications were extracted, and the diameter and contrast of each calculated. The thicknesses of aluminium required to achieve the same contrast as each calcification when imaged under the same conditions were calculated using measurements of the contrast of aluminium foils. As hydroxyapatite and calcium oxalate are also used to simulate calcifications, the equivalent aluminium thicknesses of these materials were also calculated using tabulated attenuation coefficients. On average the equivalent aluminium thickness was 0.85 times the calcification diameter. For calcium oxalate and hydroxyapatite, the equivalent aluminium thicknesses were 1.01 and 2.19 times the thickness of these materials respectively. Aluminium and calcium oxalate are suitable substitute materials for calcifications. Hydroxyapatite is much more attenuating than the calcifications and aluminium. Using solid hydroxyapatite as a substitute for calcification of the same size would lead to excessive contrast in the mammographic image. PMID:23470559

  16. Open-Porous Hydroxyapatite Scaffolds for Three-Dimensional Culture of Human Adult Liver Cells

    PubMed Central

    Schmelzer, Eva; Over, Patrick; Nettleship, Ian; Gerlach, Joerg C.

    2016-01-01

    Liver cell culture within three-dimensional structures provides an improved culture system for various applications in basic research, pharmacological screening, and implantable or extracorporeal liver support. Biodegradable calcium-based scaffolds in such systems could enhance liver cell functionality by providing endothelial and hepatic cell support through locally elevated calcium levels, increased surface area for cell attachment, and allowing three-dimensional tissue restructuring. Open-porous hydroxyapatite scaffolds were fabricated and seeded with primary adult human liver cells, which were embedded within or without gels of extracellular matrix protein collagen-1 or hyaluronan. Metabolic functions were assessed after 5, 15, and 28 days. Longer-term cultures exhibited highest cell numbers and liver specific gene expression when cultured on hydroxyapatite scaffolds in collagen-1. Endothelial gene expression was induced in cells cultured on scaffolds without extracellular matrix proteins. Hydroxyapatite induced gene expression for cytokeratin-19 when cells were cultured in collagen-1 gel while culture in hyaluronan increased cytokeratin-19 gene expression independent of the use of scaffold in long-term culture. The implementation of hydroxyapatite composites with extracellular matrices affected liver cell cultures and cell differentiation depending on the type of matrix protein and the presence of a scaffold. The hydroxyapatite scaffolds enable scale-up of hepatic three-dimensional culture models for regenerative medicine applications. PMID:27403430

  17. Fabrication and Microstructure of Hydroxyapatite Coatings on Zirconia by Room Temperature Spray Process.

    PubMed

    Seo, Dong Seok; Chae, Hak Cheol; Lee, Jong Kook

    2015-08-01

    Hydroxyapatite coatings were fabricated on zirconia substrates by a room temperature spray process and were investigated with regards to their microstructure, composition and dissolution in water. An initial hydroxyapatite powder was prepared by heat treatment of bovine-bone derived powder at 1100 °C for 2 h, while dense zirconia substrates were fabricated by pressing 3Y-TZP powder and sintering it at 1350 °C for 2 h. Room temperature spray coating was performed using a slit nozzle in a low pressure-chamber with a controlled coating time. The phase composition of the resultant hydroxyapatite coatings was similar to that of the starting powder, however, the grain size of the hydroxyapatite particles was reduced to about 100 nm due to their formation by particle impaction and fracture. All areas of the coating had a similar morphology, consisting of reticulated structure with a high surface roughness. The hydroxyapatite coating layer exhibited biostability in a stimulated body fluid, with no severe dissolution being observed during in vitro experimentation. PMID:26369194

  18. Nanocrystalline hydroxyapatite enriched in selenite and manganese ions: physicochemical and antibacterial properties.

    PubMed

    Kolmas, Joanna; Groszyk, Ewa; Piotrowska, Urszula

    2015-12-01

    In this work, we used the co-precipitation method to synthesize hydroxyapatite (Mn-SeO3-HA) containing both selenium IV (approximately 3.60 wt.%) and manganese II (approximately 0.29 wt.%). Pure hydroxyapatite (HA), hydroxyapatite-containing manganese (II) ions (Mn-HA), and hydroxyapatite-containing selenite ions alone (SeO3-HA), prepared with the same method, were used as reference materials. The structures and physicochemical properties of all the obtained samples were investigated. PXRD studies showed that the obtained materials were homogeneous and consisted of apatite phase. Introducing selenites into the hydroxyapatite crystals considerably affects the size and degree of ordering. Experiments with transmission electron microscopy (TEM) showed that Mn-SeO3-HA crystals are very small, needle-like, and tend to form agglomerates. Fourier transform infrared spectroscopy (FT-IR) and solid-state nuclear magnetic resonance (ssNMR) were used to analyze the structure of the obtained material. Preliminary microbiological tests showed that the material demonstrated antibacterial activity against Staphylococcus aureus, yet such properties were not confirmed regarding Escherichia coli. PACS codes: 61, 76, 81. PMID:26138453

  19. Nanocrystalline hydroxyapatite enriched in selenite and manganese ions: physicochemical and antibacterial properties

    NASA Astrophysics Data System (ADS)

    Kolmas, Joanna; Groszyk, Ewa; Piotrowska, Urszula

    2015-07-01

    In this work, we used the co-precipitation method to synthesize hydroxyapatite (Mn-SeO3-HA) containing both selenium IV (approximately 3.60 wt.%) and manganese II (approximately 0.29 wt.%). Pure hydroxyapatite (HA), hydroxyapatite-containing manganese (II) ions (Mn-HA), and hydroxyapatite-containing selenite ions alone (SeO3-HA), prepared with the same method, were used as reference materials. The structures and physicochemical properties of all the obtained samples were investigated. PXRD studies showed that the obtained materials were homogeneous and consisted of apatite phase. Introducing selenites into the hydroxyapatite crystals considerably affects the size and degree of ordering. Experiments with transmission electron microscopy (TEM) showed that Mn-SeO3-HA crystals are very small, needle-like, and tend to form agglomerates. Fourier transform infrared spectroscopy (FT-IR) and solid-state nuclear magnetic resonance (ssNMR) were used to analyze the structure of the obtained material. Preliminary microbiological tests showed that the material demonstrated antibacterial activity against Staphylococcus aureus, yet such properties were not confirmed regarding Escherichia coli. PACS codes: 61, 76, 81

  20. About the use of stoichiometric hydroxyapatite in compression - incidence of manufacturing process on compressibility.

    PubMed

    Pontier, C; Viana, M; Champion, E; Bernache-Assollant, D; Chulia, D

    2001-05-01

    Literature concerning calcium phosphates in pharmacy exhibits the chemical diversity of the compounds available. Some excipient manufacturers offer hydroxyapatite as a direct compression excipient, but the chemical analysis of this compound usually shows a variability of the composition: the so-called materials can be hydroxyapatite or other calcium phosphates, uncalcined (i.e. with a low crystallinity) or calcined and well-crystallized hydroxyapatite. This study points out the incidence of the crystallinity of one compound (i.e. hydroxyapatite) on the mechanical properties. Stoichiometric hydroxyapatite is synthesized and compounds differing in their crystallinity, manufacturing process and particle size are manufactured. X-Ray diffraction analysis is used to investigate the chemical nature of the compounds. The mechanical study (study of the compression, diametral compressive strength, Heckel plots) highlights the negative effect of calcination on the mechanical properties. Porosity and specific surface area measurements show the effect of calcination on compaction. Uncalcined materials show bulk and mechanical properties in accordance with their use as direct compression excipients. PMID:11343890

  1. Nano-hydroxyapatite and its applications in preventive, restorative and regenerative dentistry: a review of literature

    PubMed Central

    Pepla, Erlind; Besharat, Lait Kostantinos; Palaia, Gaspare; Tenore, Gianluca; Migliau, Guido

    2014-01-01

    Summary This study aims to critically summarize the literature about nano-hydroxyapatite. The purpose of this work is to analyze the benefits of using nano-hydroxyapatite in dentistry, especially for its preventive, restorative and regenerative applications. We also provide an overview of new dental materials, still experimental, which contain the nano-hydroxyapatite in its nano-crystalline form. Hydroxyapatite is one of the most studied biomaterials in the medical field for its proven biocompatibility and for being the main constituent of the mineral part of bone and teeth. In terms of restorative and preventive dentistry, nano-hydroxyapatite has significant remineralizing effects on initial enamel lesions, certainly superior to conventional fluoride, and good results on the sensitivity of the teeth. The nano-HA has also been used as an additive material, in order to improve already existing and widely used dental materials, in the restorative field (experimental addition to conventional glass ionomer cements, that has led to significant improvements in their mechanical properties). Because of its unique properties, such as the ability to chemically bond to bone, to not induce toxicity or inflammation and to stimulate bone growth through a direct action on osteoblasts, nano-HA has been widely used in periodontology and in oral and maxillofacial surgery. Its use in oral implantology, however, is a widely used practice established for years, as this substance has excellent osteoinductive capacity and improves bone-to-implant integration. PMID:25506416

  2. Large-scale synthesis of water-soluble luminescent hydroxyapatite nanorods for security printing.

    PubMed

    Chen, Xiaohu; Jin, Xiaoying; Tan, Junjun; Li, Wei; Chen, Minfang; Yao, Lan; Yang, Haitao

    2016-04-15

    Luminescent hydroxyapatite nanoparticles, which have excellent biocompatibility, excellent photostability, and strong fluorescence, have received increasing attention as bioprobes in cell imaging. However, they are also excellent candidates for use in ink-jet security printing. Successful products for related applications usually require highly crystalline, mono-dispersible hydroxyapatite nanorods with good colloidal stability and high fluorescence in aqueous media. These requirements are hard to simultaneously satisfy using most synthetic methods. In this paper, we report a simple and versatile hydrothermal method that incorporates the use of sodium citrate to prepare water-dispersible Eu(3+)-doped hydroxyapatite nanorods. The hydroxyapatite nanorods obtained using this method are highly crystalline rod-shaped particles with an average length of 50-80 nm and an average diameter of 15-30 nm. Dispersions of these hydroxyapatite nanorods, which are transparent with a slightly milky color under natural light and a bright red color when excited with 241 nm UV light, display zeta potentials of -35 mV and hydrodynamic diameters of 120 nm. These dispersions remain colloidally stable for a few months. Dispersions with these properties could be easily applied to security printing for confidential information storage and anti-counterfeiting technologies. PMID:26852354

  3. BMP2-loaded hollow hydroxyapatite microspheres exhibit enhanced osteoinduction and osteogenicity in large bone defects

    PubMed Central

    Xiong, Long; Zeng, Jianhua; Yao, Aihua; Tu, Qiquan; Li, Jingtang; Yan, Liang; Tang, Zhiming

    2015-01-01

    The regeneration of large bone defects is an osteoinductive, osteoconductive, and osteogenic process that often requires a bone graft for support. Limitations associated with naturally autogenic or allogenic bone grafts have demonstrated the need for synthetic substitutes. The present study investigates the feasibility of using novel hollow hydroxyapatite microspheres as an osteoconductive matrix and a carrier for controlled local delivery of bone morphogenetic protein 2 (BMP2), a potent osteogenic inducer of bone regeneration. Hollow hydroxyapatite microspheres (100±25 μm) with a core (60±18 μm) and a mesoporous shell (180±42 m2/g surface area) were prepared by a glass conversion technique and loaded with recombinant human BMP2 (1 μg/mg). There was a gentle burst release of BMP2 from microspheres into the surrounding phosphate-buffered saline in vitro within the initial 48 hours, and continued at a low rate for over 40 days. In comparison with hollow hydroxyapatite microspheres without BMP2 or soluble BMP2 without a carrier, BMP2-loaded hollow hydroxyapatite microspheres had a significantly enhanced capacity to reconstitute radial bone defects in rabbit, as shown by increased serum alkaline phosphatase; quick and complete new bone formation within 12 weeks; and great biomechanical flexural strength. These results indicate that BMP2-loaded hollow hydroxyapatite microspheres could be a potential new option for bone graft substitutes in bone regeneration. PMID:25609957

  4. Hydrothermal synthesis, characterization, photocatalytic activity and dye-sensitized solar cell performance of mesoporous anatase TiO{sub 2} nanopowders

    SciTech Connect

    Pavasupree, Sorapong; Jitputti, Jaturong; Ngamsinlapasathian, Supachai; Yoshikawa, Susumu

    2008-01-08

    Mesoporous anatase TiO{sub 2} nanopowder was synthesized by hydrothermal method at 130 deg. C for 12 h. The samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected-area electron diffraction (SAED), HRTEM, and Brunauer-Emmett-Teller (BET) surface area. The as-synthesized sample with narrow pore size distribution had average pore diameter about 3-4 nm. The specific BET surface area of the as-synthesized sample was about 193 m{sup 2}/g. Mesoporous anatase TiO{sub 2} nanopowders (prepared by this study) showed higher photocatalytic activity than the nanorods TiO{sub 2}, nanofibers TiO{sub 2} mesoporous TiO{sub 2}, and commercial TiO{sub 2} nanoparticles (P-25, JRC-01, and JRC-03). The solar energy conversion efficiency ({eta}) of the cell using the mesoporous anatase TiO{sub 2} was about 6.30% with the short-circuit current density (Jsc) of 13.28 mA/cm{sup 2}, the open-circuit voltage (Voc) of 0.702 V and the fill factor (ff) of 0.676; while {eta} of the cell using P-25 reached 5.82% with Jsc of 12.74 mA/cm{sup 2}, Voc of 0.704 V and ff of 0.649.

  5. Direct solid sampling system for electrothermal vaporization and its application to the determination of chlorine in nanopowder samples by inductively coupled plasma optical emission spectroscopy.

    PubMed

    Nakata, Kenichi; Hashimoto, Bunji; Uchihara, Hiroshi; Okamoto, Yasuaki; Ishizaka, Syoji; Fujiwara, Terufumi

    2015-06-01

    An electrothermal vaporization (ETV) system using a tungsten boat furnace (TBF) sample cuvette was designed for the direct determination of chlorine in metallic nanopowders and fine powder samples with detection by inductively coupled plasma optical emission spectroscopy (ICP-OES). A portion of a powder or particle sample was placed into a small tungsten sample cuvette and weighed accurately. A modifier solution of aqueous or alcoholic potassium hydroxide was added to it. Then, the cuvette was positioned on the TBF incorporated into the ETV apparatus. The analyte was vaporized and introduced into the ICP optical emission spectrometer with a carrier gas stream of argon and hydrogen. The metal samples were analyzed by using an external calibration curve prepared from aqueous standard solutions. Few chemical species including analyte and some chlorine-free species were introduced into the ICP, because the analyte has been separated from the matrix before introduction. Under such dry plasma conditions, the energy of plasma discharge was focused on the excitation of chlorine atoms, and as a result, lower detection limits were achieved. A detection limit of 170 ng g(-1) of chlorine in solid metal samples was established when 60 mg sample was used. The relative standard deviation for 16 replicate measurements obtained with 100 ng chlorine was 8.7%. Approximately 30 batches could be vaporized per hour. The analytical results for various nanopowders (iron (III) oxide, copper, silver, and gold) and metallic fine powder samples (silver and gold) are described. PMID:25863402

  6. Preparation of UO2, ThO2 and (Th,U)O2 pellets from photochemically-prepared nano-powders

    NASA Astrophysics Data System (ADS)

    Pavelková, Tereza; Čuba, Václav; de Visser-Týnová, Eva; Ekberg, Christian; Persson, Ingmar

    2016-02-01

    Photochemically-induced preparation of nano-powders of crystalline uranium and/or thorium oxides and their subsequent pelletizing has been investigated. The preparative method was based on the photochemically induced formation of amorphous solid precursors in aqueous solution containing uranyl and/or thorium nitrate and ammonium formate. The EXAFS analyses of the precursors shown that photon irradiation of thorium containing solutions yields a compound with little long-range order but likely "ThO2 like" and the irradiation of uranium containing solutions yields the mixture of U(IV) and U(VI) compounds. The U-containing precursors were carbon free, thus allowing direct heat treatment in reducing atmosphere without pre-treatment in the air. Subsequent heat treatment of amorphous solid precursors at 300-550 °C yielded nano-crystalline UO2, ThO2 or solid (Th,U)O2 solutions with high purity, well-developed crystals with linear crystallite size <15 nm. The prepared nano-powders of crystalline oxides were pelletized without any binder (pressure 500 MPa), the green pellets were subsequently sintered at 1300 °C under an Ar:H2 (20:1) mixture (UO2 and (Th,U)O2 pellets) or at 1600 °C in ambient air (ThO2 pellets). The theoretical density of the sintered pellets varied from 91 to 97%.

  7. Dual responsive dysprosium-doped hydroxyapatite particles and toxicity reduction after functionalization with folic and glucuronic acids.

    PubMed

    Sánchez Lafarga, Ana Karen; Pacheco Moisés, Fermín P; Gurinov, Andrey; Ortiz, Genaro Gabriel; Carbajal Arízaga, Gregorio Guadalupe

    2015-03-01

    The development of probes for biomedical applications demands materials with low toxicity levels besides fluorescence or magnetic properties to be detected by confocal microscopes or MRI resonators. Several drug delivery systems or other biomedical materials prepared with hydroxyapatite have been proposed, however, toxicity effects might arise when the size of particles is nanometric. In this study, hydroxyapatite functionalized with glucuronic or folic acids presented lower oxidative stress, measured from lipoperoxides and nitric oxide indicators in rats than pure hydroxyapatite. In separated experiments, hydroxyapatite was doped with dysprosium cations by coprecipitation producing a single crystal phase with fluorescent properties easily visualized by confocal microscopy when excited at 488nm. These particles also presented the ability to modify the proton relaxation time in T1 maps collected by magnetic resonance imaging. These modified hydroxyapatite nanoparticles could be candidates to design bimodal probes with low toxicity. PMID:25579955

  8. La{sub 0.7}Sr{sub 0.3}MnO{sub 3} nanopowders: Synthesis of different powders structures and real magnetic properties of nanomanganites

    SciTech Connect

    Danilenko, Igor Konstantinova, Tetyana; Volkova, Galina; Glazunova, Valentina

    2013-08-15

    The difference in the magnetic properties between two lanthanum manganite nanopowders with identical phase and chemical composition is discussed in terms of the influence of nanopowder synthesis conditions on their properties. The aim of this investigation was to show the influence of precursor type and structure on the structure and properties of final La{sub 0.7}Sr{sub 0.3}MnO{sub 3} nanopowders obtained by precipitation technique. The forming of a complex structure of precursor materials during drying and inheritance at firing stage led to the formation of bimodal particle size distribution and magnetic properties typical of coarse powders. The correct choice of precursor material and the technological conditions of the drying and firing stage were allowed for the creation of a uniform powder structure with special magnetic properties. We showed that the magnetic properties of nanopowders were not always determined by chemical or phase composition and mean particle size of synthesized powders. The difference in precipitation process can lead to unpredictable and catastrophic results, and masked the effect of nanoparticles on the magnetic properties of the material. - Highlights: • Precursor’s structure has a strong influence on LSM nanoparticles structure. • Amorphous precursor structure led to uniform LSM nanoparticles formation. • Crystal precursors led to the formation of bimodal LSM particles distribution. • Decrease the single-domain LSM NP size led to decrease the powder’s magnetization.

  9. Effects of ethanol on the osteogenesis around porous hydroxyapatite implants.

    PubMed

    Lima, C C; Silva, T D; Santos, L; Nakagaki, W R; Loyola, Y C S; Resck, M C C; Camilli, J A; Soares, E A; Garcia, J A D

    2011-02-01

    Alcohol consumption compromises bone tissue, and thus may either impair or stop the fixation and maintenance of osseointegrated implants. To evaluate the effects of 5% and 15% ethanol on bone neoformation around porous hydroxiapatite implants. Fifteen rats were separated into 3 groups of 5 animals each: control (CT); 5% alcohol (A); and 15% alcohol (AA). After four weeks of ethanol consumption, the rats received porous hydroxiapatite implants into surgically made cavities in the femur. After surgery, the animals continued to consume ethanol until day 90 of the experiment, when they were euthanised and their femurs removed for histological processing. Bone tissue was found around the ceramic specimens of all the animals. The largest volume of neoformed bone around ceramic specimens occurred in the CT group, and the smallest in the AA group, followed by the A group. It was concluded that ethanol consumption produced a negative effect on osteogenesis around hydroxyapatite implants. Even small doses, such as the 5% ethanol dilution can interfere with bone repair. PMID:21437407

  10. Biomimetic synthesis of oriented hydroxyapatite mediated by nonionic surfactants

    NASA Astrophysics Data System (ADS)

    Ye, Feng; Guo, Haifeng; Zhang, Haijiao

    2008-06-01

    Highly oriented organization of hydroxyapatite (HAP) nanorods was achieved through a simple reflux method using mixtures of triblock copolymer pluronic P123 and tween-60 as the mediated agents. Raft-like organized complexes were prepared when the nanorods were only directed by the mixed surfactants. Bundles of nanorod-like HAP crystals were obtained when urea was used as the cosurfactant. These HAP nanorods with a large amount of uniform 4 nm worm-like mesopores were arranged in parallel to each other along the c axis of HAP. The raft-like complexes might be mediated by the reverse lamellar micelles. And the added urea transformed the reverse lamellar micelles into hexagonal ones due to its association with the surfactant molecules by hydrogen bonds, resulting in the formation of bundles of nanorod-like HAP crystals. The regulation of the oriented HAP complexes in morphology extends the understanding of biomineralization and permits controllable design of biomimetic materials. In addition, the c-axis oriented raft-like HAP complex has great potential in selective bio-absorption and separation.

  11. Biomimetic synthesis of oriented hydroxyapatite mediated by nonionic surfactants.

    PubMed

    Ye, Feng; Guo, Haifeng; Zhang, Haijiao

    2008-06-18

    Highly oriented organization of hydroxyapatite (HAP) nanorods was achieved through a simple reflux method using mixtures of triblock copolymer pluronic P123 and tween-60 as the mediated agents. Raft-like organized complexes were prepared when the nanorods were only directed by the mixed surfactants. Bundles of nanorod-like HAP crystals were obtained when urea was used as the cosurfactant. These HAP nanorods with a large amount of uniform 4 nm worm-like mesopores were arranged in parallel to each other along the c axis of HAP. The raft-like complexes might be mediated by the reverse lamellar micelles. And the added urea transformed the reverse lamellar micelles into hexagonal ones due to its association with the surfactant molecules by hydrogen bonds, resulting in the formation of bundles of nanorod-like HAP crystals. The regulation of the oriented HAP complexes in morphology extends the understanding of biomineralization and permits controllable design of biomimetic materials. In addition, the c-axis oriented raft-like HAP complex has great potential in selective bio-absorption and separation. PMID:21825817

  12. Analysis of retrieved hydroxyapatite-coated hip prostheses

    NASA Astrophysics Data System (ADS)

    Gross, K. A.; Walsh, W.; Swarts, E.

    2004-06-01

    Hydroxyapatite (HAp) coatings are used extensively on orthopaedic devices to improve the adhesion of bone to the prosthesis. This approach increases the integrity and longevity of the implanted prosthesis. Four HAp-coated hip components recovered from patients during revision surgery were investigated for bone attachment and coating modification after storage in ethanol or formaldehyde. Orthopedic components displayed preferable bone attachment on microtextured areas and little bone on smoother areas. The coating microstructure differed between three coatings that remained on the prosthesis surface, ranging from completely crystalline coatings made by vacuum plasma spraying to less crystalline coatings manufactured by air plasma spraying. Coating failure for the lower crystallinity coatings was observed by a crack at the interface that was possibly caused by the dissolution of an amorphous phase. While higher crystallinity coatings degraded by coating delamination, the lower crystallinity coating produced loose particulate on the outer coating surface. Coating morphology as observed by scanning electron microscopy (SEM) displayed lamellae fracture, chemical dissolution, osteoclastic resorption, and precipitation in agreement with previously identified in-vitro events. The coating longevity appeared to be extended in those areas subject to lower levels of stress and more bone coverage.

  13. Nanocrystalline hydroxyapatite coatings on titanium: a new fast biomimetic method.

    PubMed

    Bigi, Adriana; Boanini, Elisa; Bracci, Barbara; Facchini, Alessandro; Panzavolta, Silvia; Segatti, Francesco; Sturba, Luigina

    2005-07-01

    We obtained a fast biomimetic deposition of hydroxyapatite (HA) coatings on Ti6Al4V substrates using a slightly supersaturated Ca/P solution, with an ionic composition simpler than that of simulated body fluid (SBF). At variance with other fast deposition methods, which produce amorphous calcium phosphate coatings, the new proposed composition allows one to obtain nanocrystalline HA. Soaking in supersaturated Ca/P solution results in the deposition of a uniform coating in a few hours, whereas SBF, or even 1.5SBF, requires 14 days to deposit a homogeneous coating on the same substrates. The coating consists of HA globular aggregates, which exhibit a finer lamellar structure than those deposited from SBF. The extent of deposition increases on increasing the immersion time. Transmission electron microscope (TEM) images recorded on the material detached from the coating show that the deposition is constituted of thin nanocrystals. Electron diffraction (ED) patterns recorded from most of the crystals exhibit the presence of rings, which can be indexed as reflections characteristic of HA. Furthermore, several HA single-crystal spot ED images were obtained from individual crystals. PMID:15664635

  14. Freeze-cast hydroxyapatite scaffolds for bone tissue engineering applications.

    PubMed

    Fu, Qiang; Rahaman, Mohamed N; Dogan, Fatih; Bal, B Sonny

    2008-06-01

    Freeze casting of aqueous suspensions was investigated as a method for preparing porous hydroxyapatite (HA) scaffolds for eventual application to bone tissue engineering. Suspensions of HA particles (10-20 volume percent) were frozen unidirectionally in a cylindrical mold placed on a cold steel substrate (-20 degrees C). After sublimation of the ice, sintering for 3 h at 1350 degrees C produced constructs with dense HA lamellae, with porosity of approximately 50%, and inter-lamellar pore widths of 5-30 microm. These constructs had compressive strengths of 12 +/- 1 MPa and 5 +/- 1 MPa in the directions parallel and perpendicular to the freezing direction, respectively. Manipulation of the microstructure was achieved by modifying the solvent composition of the suspension used for freeze casting. The use of water-glycerol mixtures (20 wt% glycerol) resulted in the production of constructs with finer pores (1-10 microm) and a larger number of dendritic growth connecting the HA lamellae, and higher strength. On the other hand, the use of water-dioxane mixtures (60 wt% dioxane) resulted in a cellular-type microstructure with larger pores (90-110 microm). The mechanical response showed high strain tolerance (5-10% at the maximum stress), high strain for failure (>20%) and sensitivity to the loading rate. The favorable mechanical behavior of the porous constructs, coupled with the ability to modify their microstructure, indicates the potential of the present freeze casting route for the production of porous scaffolds for bone tissue engineering. PMID:18458369

  15. Enhanced initial bone regeneration with inorganic polyphosphate-adsorbed hydroxyapatite.

    PubMed

    Morita, K; Doi, K; Kubo, T; Takeshita, R; Kato, S; Shiba, T; Akagawa, Y

    2010-07-01

    Inorganic polyphosphate (poly(P)) can promote binding between fibroblast growth factors and their receptors and enhance osteoblastic cell differentiation and calcification. This study evaluated the possibilities for poly(P) adsorbed onto interconnected porous calcium hydroxyapatite (IP-CHA) as a new bone regeneration material. Prepared 1%, 5%, 25% and 50% poly(P)/IP-CHA composites showed the elution peak of poly(P) between 15 and 20 min, respectively, with the highest value from 50% poly(P)/IP-CHA in vitro. Histologically, at 1 week of placement into the femur of rabbits, granulation tissue had penetrated into the pores in all composites and IP-CHA as a control. In contrast, at 2 weeks of placement, newly formed lamellar bone was found in all groups, although a higher amount of bone regeneration was obviously formed in the 25% and 50% poly(P)/IP-CHA with a significantly higher value of bone regeneration ratio of 50% poly(P)/IP-CHA. These results indicate that 25% and 50% poly(P)/IP-CHA composites may enhance initial bone regeneration. PMID:20056175

  16. Template synthesis and characterization of highly ordered lamellar hydroxyapatite

    NASA Astrophysics Data System (ADS)

    Liu, Chao; Ji, Xiujie; Cheng, Guoxiang

    2007-06-01

    Surfactant template synthesis attracts great attention in the fields of biomaterials and functional materials. In this study, highly ordered lamellar hydroxyapatite (Lα-HA) powder was synthesized by a surfactant templating method in water-ethanol. Ca(NO 3) 2 and (NH 4) 2HPO 4 were used as calcium and phosphorus sources, respectively. Sodium dodecyl sulphonate (SDS, C 12H 25SO 3Na) acted as the template. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) analyses showed that HA is the only crystal phase in Lα-HA. Transmission electron microscope (TEM) observation further proved this regular lamellar structure detected by XRD. The repeat periodicity of the structure is about 3.6 nm observed by TEM, which is in well accordance with the XRD data (3.16 nm). The selected area electron diffraction (SAED) results indicated that Lα-HA was a polycrystalline structure. The formation of Lα-HA could be explained by a surfactant template.

  17. A functionally graded titanium/hydroxyapatite film obtained by sputtering.

    PubMed

    Ozeki, Kazuhide; Yuhta, Toshio; Fukui, Yasuhiro; Aoki, Hideki; Nishimura, Ikuya

    2002-03-01

    A functionally graded film of titanium/hydroxyapatite (HA) was prepared on a titanium substrate using a radio frequency magnetron sputtering. The ratio of titanium to HA was controlled by moving the target shutter. The film was composed of five layers, with overall film thickness of 1 microm. The HA was concentrated close to the surface, while the titanium concentration increased with proximity to the substrate. The bonding strength between the film and the substrate was 15.2 MPa in a pull-out test and the critical load from a scratch test was 58.85 mN. The corresponding values of a pure HA sputtered film were 8.0 MPa and 38.47 mN, respectively. The bonding strength of a pure HA plasma spray coating was 10.4 MPa in the pull-out test. The graded film and the pure HA film were sputter-coated to a thickness of 1 microm on titanium columns (10 mm in length and 4 mm in diameter). These columns were implanted in diaphyses of the femora of six adult dogs and a push-out test was carried out after 2, 4, and 12 weeks. After 12 weeks, the push-out strengths of the graded film, the pure HA film and the non-coated columns were 3.7, 3.5, and 1.0 MPa. PMID:15348621

  18. Control of hydroxyapatite crystallinity by mechanical grinding method.

    PubMed

    Nakano, T; Tokumura, A; Umakoshi, Y; Imazato, S; Ehara, A; Ebisu, S

    2001-08-01

    Crystallinity of hydroxyapatite reflecting crystal size and crystal elastic strain was controlled by the mechanical grinding (MG) technique using a set of container and balls made of SUS304 stainless steel or agate. Variation in the crystallinity through MG was monitored by the XRD method and represented by the broadening of the diffraction peak. Effect of changes in crystallite size and strain on the crystallinity was also examined using the Hall-plot method. Crystallinity rapidly decreased with milling time. Significant crystallographic diffraction peaks disappeared and a broad diffraction around 2theta=32 degrees was observed after MG for 72 h. The broadening was dominantly due to an increase in crystal strain in addition to fine crystallite size. Contamination from the container and balls during MG was more suppressed using agate than SUS304 stainless steel. The recovery process of crystallinity during heating between 300 degrees C and 1200 degrees C was examined focusing on the decrease in residual elastic strain. Low crystallinity was maintained at annealing temperatures below 800 degrees C but lattice defects were recovered above 1000 degrees C. PMID:15348242

  19. Sol-gel hydroxyapatite coatings on stainless steel substrates.

    PubMed

    Liu, Dean-Mo; Yang, Quanzu; Troczynski, Tom

    2002-02-01

    Thin film hydroxyapatite deposits onto sandblasted 316L stainless steel substrates were prepared using water-based sol-gel technique recently developed in our lab. The coatings were annealed in air at 375 degrees C, 400 degrees C, and 500 degrees C. Phase formation, surface morphology, interfacial microstructure, and interfacial bonding strength of the coatings were investigated. Apatitic structure developed within the coatings while annealing at temperatures > or = 400 degrees C, while those heat-treated at 375 degrees C showed poor crystallinity. The coatings were dense and firmly attached to the underlying substrates, reaching an average bonding strength (as determined through the pull-out test) of 44 MPa. Nano-porous structure was found for the coatings annealed at 500 degrees C, believed to result from grain growth, and causing a slight decrease in the bonding strength. Surface microcracking, although not extensive, occurred after annealing at temperatures > or = 400 degrees C, and was linked to non-uniform thickness of the coating due to roughness of the substrate. A contraction of the coatings as a result of sintering, and phase transition from amorphous (or poor crystalline) to reasonably good crystalline apatite, may be responsible for the loss of structural integrity of the thicker sections of the coatings. It seems quite promising that a dense and adhesive apatite coating can be achieved through water-based sol gel technology after short-term annealing at around 400 degrees C in air. PMID:11771689

  20. Electronic Structure of Ti substituted hydroxyapatite: TiHap

    NASA Astrophysics Data System (ADS)

    Yin, Shuxia; Ellis, Donald

    2009-03-01

    Hydroxyapatite (Hap), with the chemical formula Ca10(PO4)6(OH)2, is the main mineral constituent of mammal tooth enamel and bone and has become an important biomaterial with medical applications. Hap also attracts increasing interest for use in environmental adsorbents and catalysts due to its porous nature and highly active ion-exchange character. Ti-modified Hap (TiHap) has been proved to possess high affinity to organic molecules and bacteria as well as high photocatalytic activity for their oxidative decomposition. The concentration of Ti^4+ is a key factor controlling TiHap crystallinity and catalytic efficiency. Here we studied the sorption mechanism of Ti^4+ on Hap using Density Functional Theory within periodic slab models. Ti^4+ or (Ti(OH)2)^2+, as the most likely ion exchange species with Ca^2+, were first considered in bulk Hap. A second charge compensated model considered includes both surface Ca ion vacancies and substitutional Ti^4+. To obtain insight of the energetic stability and microscopic crystal structure of TiHap, Ti substitution on different Ca sites and distributions at different atomic ratios are investigated in both bulk and surface models.

  1. Dissolution behavior of plasma-sprayed hydroxyapatite coatings.

    PubMed

    Fazan, F; Marquis, P M

    2000-12-01

    The long-term stability of plasma-sprayed hydroxyapatite coatings is influenced by the dissolution behavior of the coating in in vivo conditions. Plasma-spraying generates a mixture of phases and this study has focused on how the balance of phases affects the in vitro dissolution behavior of the coatings in double distilled-deionized water and in tris-buffer solutions. The pH changes in double distilled-deionized water were monitored, whilst the pH value was maintained at 7.25 for the tris-buffer solution at 37 degrees C with 5% CO2 atmosphere. The phosphate and calcium ions released were measured using UV-Visible Spectrophotometer and Atomic Absorption Spectroscopy respectively. Changes in crystal and surface topology were also studied. The results indicate that the dissolution behavior of the coatings depends on several factors. The rate of release of phosphate ions was found to increase significantly for the tris-buffer solution compared to the deionized water, indicating that the presence of electrolyte constituents affects the dissolution behavior of the coatings. The Ca/P ratio in the tris-buffer solution is approximately three. Increases in the level of crystallinity of the coatings significantly decreased the dissolution rate and hence, the amount of phosphate ions released. The higher the percentage of crystallinity, the higher the stability of the coating under in vitro conditions. PMID:15348061

  2. Computational study of hydroxyapatite structures, properties and defects

    NASA Astrophysics Data System (ADS)

    Bystrov, V. S.; Coutinho, J.; Bystrova, A. V.; Dekhtyar, Yu D.; Pullar, R. C.; Poronin, A.; Palcevskis, E.; Dindune, A.; Alkan, B.; Durucan, C.; Paramonova, E. V.

    2015-03-01

    Hydroxyapatite (HAp) was studied from a first principle approach using the local density approximation (LDA) method in AIMPRO code, in combination with various quantum mechanical (QM) and molecular mechanical (MM) methods from HypemChem 7.5/8.0. The data obtained were used for studies of HAp structures, the physical properties of HAp (density of electronic states—DOS, bulk modulus etc) and defects in HAp. Computed data confirmed that HAp can co-exist in different phases—hexagonal and monoclinic. Ordered monoclinic structures, which could reveal piezoelectric properties, are of special interest. The data obtained allow us to characterize the properties of the following defects in HAp: O, H and OH vacancies; H and OH interstitials; substitutions of Ca by Mg, Sr, Mn or Se, and P by Si. These properties reveal the appearance of additional energy levels inside the forbidden zone, shifts of the top of the valence band or the bottom of the conduction band, and subsequent changes in the width of the forbidden zone. The data computed are compared with other known data, both calculated and experimental, such as alteration of the electron work functions under different influences of various defects and treatments, obtained by photoelectron emission. The obtained data are very useful, and there is an urgent need for such analysis of modified HAp interactions with living cells and tissues, improvement of implant techniques and development of new nanomedical applications.

  3. Conversion of bulk seashells to biocompatible hydroxyapatite for bone implants.

    PubMed

    Vecchio, Kenneth S; Zhang, Xing; Massie, Jennifer B; Wang, Mark; Kim, Choll W

    2007-11-01

    Strombus gigas (conch) shells and Tridacna gigas (Giant clam) shells have dense, tailored structures that impart excellent mechanical properties to these shells. In this investigation, conch and clam seashells were converted to hydroxyapatite (HAP) by a hydrothermal method at different temperatures and for different conversion durations. Dense HAP structures were created from these shells throughout the majority of the samples at the relative low temperature of approximately 200 degrees C. The average fracture stress was found to be approximately 137-218MPa for partially converted conch shell samples and approximately 70-150MPa for original and converted clamshell samples, which is close to the mechanical strength of compact human bone. This indicates that the converted shell samples can be used as implants in load-bearing cases. In vivo tests of converted shell samples were performed in rat femoral defects for 6 weeks. The microtomography images at 6 weeks show that the implants did not move, and untreated control defects remain empty with no evidence of a spontaneous fusion. Histological study reveals that there is newly formed bone growing up to and around the implants. There is no evidence of a fibrosis tissue ring around the implants, also indicating that there is no loosening of the implants. In contrast, the untreated controls remain empty with some evidence of a fibrosis ring around the defect hole. These results indicate good biocompatibility and bioactivity of the converted shell implants. PMID:17684000

  4. Bacterial Cellulose-Hydroxyapatite Nanocomposites for Bone Regeneration

    PubMed Central

    Saska, S.; Barud, H. S.; Gaspar, A. M. M.; Marchetto, R.; Ribeiro, S. J. L.; Messaddeq, Y.

    2011-01-01

    The aim of this study was to develop and to evaluate the biological properties of bacterial cellulose-hydroxyapatite (BC-HA) nanocomposite membranes for bone regeneration. Nanocomposites were prepared from bacterial cellulose membranes sequentially incubated in solutions of CaCl2 followed by Na2HPO4. BC-HA membranes were evaluated in noncritical bone defects in rat tibiae at 1, 4, and 16 weeks. Thermogravimetric analyses showed that the amount of the mineral phase was 40%–50% of the total weight. Spectroscopy, electronic microscopy/energy dispersive X-ray analyses, and X-ray diffraction showed formation of HA crystals on BC nanofibres. Low crystallinity HA crystals presented Ca/P a molar ratio of 1.5 (calcium-deficient HA), similar to physiological bone. Fourier transformed infrared spectroscopy analysis showed bands assigned to phosphate and carbonate ions. In vivo tests showed no inflammatory reaction after 1 week. After 4 weeks, defects were observed to be completely filled in by new bone tissue. The BC-HA membranes were effective for bone regeneration. PMID:21961004

  5. Bioactive rosette nanotube-hydroxyapatite nanocomposites improve osteoblast functions.

    PubMed

    Sun, Linlin; Zhang, Lijie; Hemraz, Usha D; Fenniri, Hicham; Webster, Thomas J

    2012-09-01

    Inspired from biological systems, small synthetic organic molecules expressing the hydrogen bonding arrays of the DNA bases guanine and cytosine were prepared, and their self-assembly into rosette nanotubes (RNTs) was investigated. Due to their unique biological, physicochemical, and mechanical properties, RNTs could serve as the next generation of injectable orthopedic materials. In this study, a self-assembling module (termed twin base linkers or TBL) was synthesized, and the corresponding RNTs were used as bioactive components in composites of poly (2-hydroxyethyl methacrylate) (pHEMA) and hydroxyapatite (HA) nanoparticles (termed TBL/HA/pHEMA). The properties of these composites were characterized for solidification time, surface morphology, mechanical properties, and cytocompatibility. The experimental conditions were optimized to achieve solidification within 2-40 min, offering a range of properties for orthopedic applications. Composites with 20 wt% HA nanoparticles had a compressive strength (37.1 MPa) and an ultimate tensile stress (14.7 MPa) similar to that of a natural vertebral disc (5-30 MPa). Specifically, the TBL (0.01 mg/mL)/HA(20 wt%)/pHEMA composites improved long-term functions of osteoblasts (or bone-forming cells) in terms of collagen synthesis, alkaline phosphatase activity, and calcium deposition. Moreover, this composite inhibited fibroblast adhesion, thus decreasing the potential for undesirable fibrous tissue formation. In summary, this in vitro study provided evidence that TBL/HA/pHEMA composites are promising injectable orthopedic implant materials that warrant further mechanistic and in vivo studies. PMID:22530958

  6. Thin hydroxyapatite surface layers on titanium produced by ion implantation

    NASA Astrophysics Data System (ADS)

    Baumann, H.; Bethge, K.; Bilger, G.; Jones, D.; Symietz, I.

    2002-11-01

    In medicine metallic implants are widely used as hip replacement protheses or artificial teeth. The biocompatibility is in all cases the most important requirement. Hydroxyapatite (HAp) is frequently used as coating on metallic implants because of its high acceptance by the human body. In this paper a process is described by which a HAp surface layer is produced by ion implantation with a continuous transition to the bulk material. Calcium and phosphorus ions are successively implanted into titanium under different vacuum conditions by backfilling oxygen into the implantation chamber. Afterwards the implanted samples are thermally treated. The elemental composition inside the implanted region was determined by nuclear analysis methods as (α,α) backscattering and the resonant nuclear reaction 1H( 15N,αγ) 12C. The results of X-ray photoelectron spectroscopy indicate the formation of HAp. In addition a first biocompatibility test was performed to compare the growing of marrow bone cells on the implanted sample surface with that of titanium.

  7. Synthesis and characterization of hydroxyapatite from fish bone waste

    NASA Astrophysics Data System (ADS)

    Marliana, Ana; Fitriani, Eka; Ramadhan, Fauzan; Suhandono, Steven; Yuliani, Keti; Windarti, Tri

    2015-12-01

    Waste fish bones is a problem stemming from activities in the field of fisheries and it has not been used optimally. Fish bones contain calcium as natural source that used to synthesize hydroxyapatite (HA). In this research, HA synthesized from waste fish bones as local wisdom in Semarang. The goal are to produce HA with cheaper production costs and to reduce the environmental problems caused by waste bones. The novelty of this study was using of local fish bone as a source of calcium and simple method of synthesis. Synthesis process of HA can be done through a maceration process with firing temperatures of 1000°C or followed by a sol-gel method with firing at 550°C. The results are analyzed using FTIR (Fourier Transform Infrared), XRD (X-Ray Diffraction) and SEM-EDX (Scanning Electron Microscopy-Energy Dispersive X-Ray). FTIR spectra showed absorption of phosphate and OH group belonging to HA as evidenced by the results of XRD. The average grain size by maceration and synthesized results are not significant different, which is about 69 nm. The ratio of Ca/P of HA by maceration result is 0.89, then increase after continued in the sol-gel process to 1.41. Morphology of HA by maceration results are regular and uniform particle growth, while the morphology of HA after the sol-gel process are irregular and agglomerated.

  8. Continuous delivery of azidothymidine by hydroxyapatite or tricalcium phosphate ceramics.

    PubMed

    Cannon, M R; Bajpai, P K

    1995-01-01

    A ceramic drug delivery system was developed for continuous release of azidothymidine (AZT). Tricalcium phosphate (TCP) and hydroxyapatite (HA) ceramics were used to fabricate ceramic devices. Each group of devices consisted of three replicates. Ceramic and AZT mixtures were compressed at a load of 3000 lbs in a 10 mm diameter die using a hydraulic press. For in vitro studies, vitamin E oil was incorporated in six different ratios in devices containing HA (500 mg) and AZT (250 mg). Each device was suspended in phosphate buffered saline (pH 7.4). Devices containing oil released AZT in significantly lower amounts than devices containing no oil. In vivo studies were conducted with devices composed of homogeneous mixtures of 250 mg AZT and 500 mg TCP with and without vitamin E oil in the following combinations: AZT and TCP (Group I), Oil saturated TCP and AZT (Group II), and AZT pellet inserted in an oil saturated TCP shell (Group III). These devices were implanted subcutaneously in Sprague Dawley rats for two weeks. Group II and III devices delivered AZT at a significantly lower rate than Group I devices. Results of both studies suggest that treatment of ceramic devices with oil decreases the release rate and prolongs the delivery of AZT. PMID:7654955

  9. Plasma Sprayed Hydroxyapatite Coatings: Influence of Spraying Power on Microstructure

    SciTech Connect

    Mohd, S. M.; Abd, M. Z.; Abd, A. N.

    2010-03-11

    The plasma sprayed hydroxyapatite (HA) coatings are used on metallic implants to enhance the bonding between the implant and bone in human body. The coating process was implemented at different spraying power for each spraying condition. The coatings formed from a rapid solidification of molten and partly molten particles that impact on the surface of substrate at high velocity and high temperature. The study was concentrated on different spraying power that is between 23 to 31 kW. The effect of different power on the coatings microstructure was investigated using scanning electron microscope (SEM) and phase composition was evaluated using X-ray diffraction (XRD) analysis. The coatings surface morphology showed distribution of molten, partially melted particles and some micro-cracks. The produced coatings were found to be porous as observed from the cross-sectional morphology. The coatings XRD results indicated the presence of crystalline phase of HA and each of the patterns was similar to the initial powder. Regardless of different spraying power, all the coatings were having similar XRD patterns.

  10. Osteogenic responses to zirconia with hydroxyapatite coating by aerosol deposition.

    PubMed

    Cho, Y; Hong, J; Ryoo, H; Kim, D; Park, J; Han, J

    2015-03-01

    Previously, we found that osteogenic responses to zirconia co-doped with niobium oxide (Nb2O5) or tantalum oxide (Ta2O5) are comparable with responses to titanium, which is widely used as a dental implant material. The present study aimed to evaluate the in vitro osteogenic potential of hydroxyapatite (HA)-coated zirconia by an aerosol deposition method for improved osseointegration. Surface analysis by scanning electron microscopy and x-ray diffraction proved that a thin as-deposited HA film on zirconia showed a shallow, regular, crater-like surface. Deposition of dense and uniform HA films was measured by SEM, and the contact angle test demonstrated improved wettability of the HA-coated surface. Confocal laser scanning microscopy indicated that MC3T3-E1 pre-osteoblast attachment did not differ notably between the titanium and zirconia surfaces; however, cells on the HA-coated zirconia exhibited a lower proliferation than those on the uncoated zirconia late in the culture. Nevertheless, ALP, alizarin red S staining, and bone marker gene expression analysis indicated good osteogenic responses on HA-coated zirconia. Our results suggest that HA-coating by aerosol deposition improves the quality of surface modification and is favorable to osteogenesis. PMID:25586588

  11. Dissolving Hydroxyolite: A DNA Molecule into Its Hydroxyapatite Mold.

    PubMed

    Bertran, Oscar; Revilla-López, Guillermo; Casanovas, Jordi; Del Valle, Luis J; Turon, Pau; Puiggalí, Jordi; Alemán, Carlos

    2016-05-01

    In spite of the clinical importance of hydroxyapatite (HAp), the mechanism that controls its dissolution in acidic environments remains unclear. Knowledge of such a process is highly desirable to provide better understanding of different pathologies, as for example osteoporosis, and of the HAp potential as vehicle for gene delivery to replace damaged DNA. In this work, the mechanism of dissolution in acid conditions of HAp nanoparticles encapsulating double-stranded DNA has been investigated at the atomistic level using computer simulations. For this purpose, four consecutive (multi-step) molecular dynamics simulations, involving different temperatures and proton transfer processes, have been carried out. Results are consistent with a polynuclear decalcification mechanism in which proton transfer processes, from the surface to the internal regions of the particle, play a crucial role. In addition, the DNA remains protected by the mineral mold and transferred proton from both temperature and chemicals. These results, which indicate that biomineralization imparts very effective protection to DNA, also have important implications in other biomedical fields, as for example in the design of artificial bones or in the fight against osteoporosis by promoting the fixation of Ca(2+) ions. PMID:27038364

  12. Interfacial bond strength of electrophoretically deposited hydroxyapatite coatings on metals.

    PubMed

    Wei, M; Ruys, A J; Swain, M V; Kim, S H; Milthorpe, B K; Sorrell, C C

    1999-07-01

    Hydroxyapatite (HAp) coatings were deposited onto substrates of metal biomaterials (Ti, Ti6Al4V, and 316L stainless steel) by electrophoretic deposition (EPD). Only ultra-high surface area HAp powder, prepared by the metathesis method 10Ca(NO3)2 + 6(NH4)2HPO4 + 8NH4OH), could produce dense coatings when sintered at 875-1000degreesC. Single EPD coatings cracked during sintering owing to the 15-18% sintering shrinkage, but the HAp did not decompose. The use of dual coatings (coat, sinter, coat, sinter) resolved the cracking problem. Scanning electron microscopy/energy dispersive spectroscopy (SEM/EDS) inspection revealed that the second coating filled in the "valleys" in the cracks of the first coating. The interfacial shear strength of the dual coatings was found, by ASTM F1044-87, to be approximately 12 MPa on a titanium substrate and approximately 22 MPa on 316L stainless steel, comparing quite favorably with the 34 MPa benchmark (the shear strength of bovine cortical bone was found to be 34 MPa). Stainless steel gave the better result since -316L (20.5 microm mK(-1)) > alpha-HAp (approximately 14 microm mK(-1)), resulting in residual compressive stresses in the coating, whereas alpha-titanium (approximately 10.3 microm mK(-1)) < alpha-HAp, resulting in residual tensile stresses in the coating. PMID:15348125

  13. Increased risk of revision of acetabular cups coated with hydroxyapatite

    PubMed Central

    Lazarinis, Stergios; Kärrholm, Johan

    2010-01-01

    Background Hydroxyapatite (HA) is the main inorganic component of bone, and HA coating is widely used on acetabular cups in hip arthroplasty. It has been suggested that this surface finish improves cup survival. Methods All patients registered in the Swedish Hip Arthroplasty Register between 1992 and 2007 with an uncemented acetabular implant that was available either with or without HA coating were identified. 8,043 total hip arthroplasties (THAs) with the most common cup types (Harris-Galante, Romanus, and Trilogy) were investigated. A Cox regression model including type of coating, age, sex, primary diagnosis, cup type, and type of stem fixation was used to calculate adjusted risk ratios (RRs) for the risk of revision. Results HA coating was a risk factor for cup revision due to aseptic loosening (adjusted RR 1.7; 95% CI: 1.3–2). Age at primary arthroplasty of < 50 years, a diagnosis of pediatric hip disease, the use of a cemented stem, and the Romanus and Harris-Galante cup types were also associated with statistically significantly increased risk of cup revision due to aseptic loosening. Interpretation Our findings question the routine use of HA-coated cups in primary total hip arthroplasty. With some designs, this practice may even increase the risk of loosening—resulting in revision surgery. PMID:19968603

  14. Risedronate/zinc-hydroxyapatite based nanomedicine for osteoporosis.

    PubMed

    Khajuria, Deepak Kumar; Disha, Choudhary; Vasireddi, Ramakrishna; Razdan, Rema; Mahapatra, D Roy

    2016-06-01

    Targeting of superior osteogenic drugs to bone is an ideal approach for treatment of osteoporosis. Here, we investigated the potential of using risedronate/zinc-hydroxyapatite (ZnHA) nanoparticles based formulation in a rat model of experimental osteoporosis. Risedronate, a targeting moiety that has a strong affinity for bone, was loaded to ZnHA nanoparticles by adsorption method. Prepared risedronate/ZnHA drug formulation was characterized by field-emission scanning electron microscopy, X-ray diffraction analysis and fourier transform infrared spectroscopy. In vivo performance of the prepared risedronate/ZnHA nanoparticles was tested in an experimental model of postmenopausal osteoporosis. Therapy with risedronate/ZnHA drug formulation prevented increase in serum levels of bone-specific alkaline phosphatase and tartrate-resistant acid phosphatase 5b better than risedronate/HA or risedronate. With respect to improvement in the mechanical strength of the femoral mid-shaft and correction of increase in urine calcium and creatinine levels, the therapy with risedronate/ZnHA drug formulation was more effective than risedronate/HA or risedronate therapy. Moreover, risedronate/ZnHA drug therapy preserved the cortical and trabecular bone microarchitecture better than risedronate/HA or risedronate therapy. Furthermore, risedronate/ZnHA drug formulation showed higher values of calcium/phosphorous ratio and zinc content. The results strongly implicate that risedronate/ZnHA drug formulation has a therapeutic advantage over risedronate or risedronate/HA therapy for the treatment of osteoporosis. PMID:27040198

  15. Iron, Manganese and Copper Release from Synthetic Hydroxyapatite

    NASA Technical Reports Server (NTRS)

    Sutter, B.; Hossner, L. R.; Ming, Douglas W.

    1999-01-01

    Kinetic stir-flow dissolution experiments were performed on iron- (Fe-SHA), manganese- (Mn-SHA), and copper- (Cu-SHA) containing synthetic hydroxyapatites. Solution treatments consisted of de-ionized water, citric acid and DTPA. Initially, Mn concentrations were higher than Cu concentrations and Fe concentrations were the lowest in all treatments. At later times Mn and Cu concentrations dropped in the DTPA treatment while Fe rose to the concentration similar to Mn and Cu. At all times, metal release concentrations in the water and citric acid treatments followed the trend of Mn>Cu>Fe. Rietveld analysis of x-ray diffraction data and ^31P NMR indicated that the metals substituted for Ca in the SHA structure. However, EPR data suggested that a metal (hydr)oxide phase existed either on the SHA surface or between the SHA crystallites. The metal concentration trend of Mn>Cu>Fe suggested that the initial solution metal concentrations are dependent on the dissolution of (hydr)oxides from SHA surfaces or between SHA crystallites. Similar metal concentrations at later times in the DTPA experiments suggests that metal concentrations were controlled by the release of Mn, Cu, or Fe from the SHA structure.

  16. Nanocomposite bone scaffolds based on biodegradable polymers and hydroxyapatite.

    PubMed

    Becker, Johannes; Lu, Lichun; Runge, M Brett; Zeng, Heng; Yaszemski, Michael J; Dadsetan, Mahrokh

    2015-08-01

    In tissue engineering, development of an osteoconductive construct that integrates with host tissue remains a challenge. In this work, the effect of bone-like minerals on maturation of pre-osteoblast cells was investigated using polymer-mineral scaffolds composed of poly(propylene fumarate)-co-poly(caprolactone) (PPF-co-PCL) and nano-sized hydroxyapatite (HA). The HA of varying concentrations was added to an injectable formulation of PPF-co-PCL and the change in thermal and mechanical properties of the scaffolds was evaluated. No change in onset of degradation temperature was observed due to the addition of HA, however compressive and tensile moduli of copolymer changed significantly when HA amounts were increased in composite formulation. The change in mechanical properties of copolymer was found to correlate well to HA concentration in the constructs. Electron microscopy revealed mineral nucleation and a change in surface morphology and the presence of calcium and phosphate on surfaces was confirmed using energy dispersive X-ray analysis. To characterize the effect of mineral on attachment and maturation of pre-osteoblasts, W20-17 cells were seeded on HA/copolymer composites. We demonstrated that cells attached more to the surface of HA containing copolymers and their proliferation rate was significantly increased. Thus, these findings suggest that HA/PPF-co-PCL composite scaffolds are capable of inducing maturation of pre-osteoblasts and have the potential for use as scaffold in bone tissue engineering. PMID:25504776

  17. Biomedical nanocomposites of hydroxyapatite/polycaprolactone obtained by surfactant mediation.

    PubMed

    Kim, Hae-Won

    2007-10-01

    The composite approach to combining bioactive ceramic and degradable polymer is a promising strategy in the development of bone regenerative matrices. Moreover, in the fabrication of composites, the nanoscale organization of each component should improve the level of structural integration as well as the resultant mechanical and biological properties. The aim of this study was to develop a novel nanocomposite system consisting of hydroxyapatite (HA) and poly(epsilon-caprolactone) (PCL), wherein the HA nanoparticles were uniformly dispersed within the PCL matrix. The strategy was based on applying an amphiphilic surfactant, oleic acid in this case, between the HA and PCL. Oleic acid, which belongs to the fatty acid family and is generally noncytotoxic at the levels used in this study, is believed to mediate the interaction between the hydrophilic HA and hydrophobic PCL. With the mediation of oleic acid, the HA nanoparticles were distributed uniformly within the PCL matrix on the nanoscale (distributed particle size of less than 1 microm), which is in marked contrast to the conventionally mixed HA-PCL composite, in which the HA particles were severely agglomerated. The developed nanocomposite had significantly higher mechanical strength than did the conventional composite and the pure PCL. Moreover, the osteoblastic cells showed a better proliferation behavior on the nanocomposite than on the conventional composite. This HA-PCL nanocomposite mediated by oleic acid is expected to be useful in the bone regeneration field. Moreover, this methodology is applicable to the nanocomposite processing of other biomedical materials. PMID:17390319

  18. Development of electrochemical folic acid sensor based on hydroxyapatite nanoparticles

    NASA Astrophysics Data System (ADS)

    Kanchana, P.; Sekar, C.

    2015-02-01

    We report the synthesis of hydroxyapatite (HA) nanoparticles (NPs) by a simple microwave irradiation method and its application as sensing element for the precise determination of folic acid (FA) by electrochemical method. The structure and composition of the HA NPs characterized using XRD, FTIR, Raman and XPS. SEM and EDX studies confirmed the formation of elongated spherical shaped HA NPs with an average particle size of about 34 nm. The HA NPs thin film on glassy carbon electrode (GCE) were deposited by drop casting method. Electrocatalytic behavior of FA in the physiological pH 7.0 was investigated by cyclic voltammetry (CV), linear sweep voltammetry (LSV) and chronoamperometry. The fabricated HA/GCE exhibited a linear calibration plot over a wide FA concentration ranging from 1.0 × 10-7 to 3.5 × 10-4 M with the detection limit of 75 nM. In addition, the HA NPs modified GCE showed good selectivity toward the determination of FA even in the presence of a 100-fold excess of ascorbic acid (AA) and 1000-fold excess of other common interferents. The fabricated biosensor exhibits good sensitivity and stability, and was successfully applied for the determination of FA in pharmaceutical samples.

  19. Synthesis and characterisation of copper doped Ca-Li hydroxyapatite

    NASA Astrophysics Data System (ADS)

    Pogosova, M. A.; Kazin, P. E.; Tretyakov, Y. D.

    2012-08-01

    Hydroxyapapites M10(PO4)6(OH)2 (MHAP), where M is an alkaline earth metal, colored by incorporation of copper ions substituting protons, were discovered recently [1]. Now this kind of apatite-type materials can be used as inorganic pigments. Until now blue (BaHAP), violet (SrHAP) and wine-red (CaHAP) colors were achieved by the copper ions introduction [2]. The task of the present work was to study possibility of further M-ion substitution to affect the color and shift it toward the red-orange tint. Polycrystalline hydroxyapatites Ca10-xLix+yCuz(PO4)6O2H2-y-z-σ (Ca-LiHAP) were synthesized by solid state reaction at 1150 °C (ceramic method) and studied by X-ray powder diffraction (XRD), infrared absorption and diffuse-reflectance spectroscopy. Refinement of the X-ray diffraction patterns by the Rietveld method shows that CaHAP unit cell parameters are a little bigger, than Ca-LiHAP ones. Small difference between unit cell parameters could be caused by two ways of the Li+ ions introduction: (1) at the Ca2+ sites (Ca-Li substitution); (2) into hexagonal channels (H-Li substitution). The Li ions doping changes the color of the copper doped CaHAP from wine-red to pink and red.

  20. Fracture mechanics of hydroxyapatite single crystals under geometric confinement.

    PubMed

    Libonati, Flavia; Nair, Arun K; Vergani, Laura; Buehler, Markus J

    2013-04-01

    Geometric confinement to the nanoscale, a concept that refers to the characteristic dimensions of structural features of materials at this length scale, has been shown to control the mechanical behavior of many biological materials or their building blocks, and such effects have also been suggested to play a crucial role in enhancing the strength and toughness of bone. Here we study the effect of geometric confinement on the fracture mechanism of hydroxyapatite (HAP) crystals that form the mineralized phase in bone. We report a series of molecular simulations of HAP crystals with an edge crack on the (001) plane under tensile loading, and we systematically vary the sample height whilst keeping the sample and the crack length constant. We find that by decreasing the sample height the stress concentration at the tip of the crack disappears for samples with a height smaller than 4.15nm, below which the material shows a different failure mode characterized by a more ductile mechanism with much larger failure strains, and the strength approaching that of a flaw-less crystal. This study directly confirms an earlier suggestion of a flaw-tolerant state that appears under geometric confinement and may explain the mechanical stability of the reinforcing HAP platelets in bone. PMID:23500480

  1. Synthesis and characterization of hydroxyapatite from fish bone waste

    SciTech Connect

    Marliana, Ana Fitriani, Eka; Ramadhan, Fauzan; Suhandono, Steven; Yuliani, Keti; Windarti, Tri

    2015-12-29

    Waste fish bones is a problem stemming from activities in the field of fisheries and it has not been used optimally. Fish bones contain calcium as natural source that used to synthesize hydroxyapatite (HA). In this research, HA synthesized from waste fish bones as local wisdom in Semarang. The goal are to produce HA with cheaper production costs and to reduce the environmental problems caused by waste bones. The novelty of this study was using of local fish bone as a source of calcium and simple method of synthesis. Synthesis process of HA can be done through a maceration process with firing temperatures of 1000°C or followed by a sol-gel method with firing at 550°C. The results are analyzed using FTIR (Fourier Transform Infrared), XRD (X-Ray Diffraction) and SEM-EDX (Scanning Electron Microscopy-Energy Dispersive X-Ray). FTIR spectra showed absorption of phosphate and OH group belonging to HA as evidenced by the results of XRD. The average grain size by maceration and synthesized results are not significant different, which is about 69 nm. The ratio of Ca/P of HA by maceration result is 0.89, then increase after continued in the sol-gel process to 1.41. Morphology of HA by maceration results are regular and uniform particle growth, while the morphology of HA after the sol-gel process are irregular and agglomerated.

  2. Synthesis and characterization of cadmium-calcium hydroxyapatite solid solutions

    NASA Astrophysics Data System (ADS)

    Zhao, Xin; Zhu, Yi-nian; Dai, Liu-qin

    2014-06-01

    A series of cadmium-calcium hydroxyapatite solid solutions was prepared by an aqueous precipitation method. By various means, the characterizations confirmed the formation of continuous solid solutions over all ranges of Cd/(Cd+Ca) atomic ratio. In the results, both lattice parameters a and c display slight deviations from Vegard's rule when the Cd/(Cd+Ca) atomic ratio is greater than 0.6. The particles change from smaller acicular to larger hexagonal columnar crystals as the Cd/(Cd+Ca) atomic ratio increases from 0-0.60 to 0.60-1.00. The area of the phosphate peak for symmetric P-O stretching decreases with the increase in Cd/(Cd+Ca) atomic ratio, and the peak disappears when the Cd/(Cd+Ca) atomic ratio is greater than 0.6; the two phosphate peaks of P-O stretching gradually merge together for the Cd/(Cd+Ca) atomic ratio near 0.60. These variations can be explained by a slight tendency of larger Cd ions to occupy M(2) sites and smaller Ca ions to prefer M(1) sites in the structure.

  3. Biomechanical evaluation of different hydroxyapatite coatings on titanium for keratoprosthesis

    NASA Astrophysics Data System (ADS)

    Dong, Ying; Qiu, Zhiye; Liu, Xiaoyu; Wang, Liqiang; Yang, Jingxin; Huang, Yifei; Cui, Fuzhai

    2015-09-01

    Stable tissue integration is important to keratoprosthesis (KPro). The aim of this study was to evaluate the tissue bonding ability of hydroxyapatite (HAp)-coated titanium KPro. The samples were divided into three groups: test groups (IBAD group and AD group) and Ti control. The coated samples had a HAp layer created by ion beam assisted deposition (IBAD) or aerosol deposition (AD). The surface characteristics were analyzed with SEM, AFM, and XRD. The samples were surgically inserted into the muscles of rabbits. Eight weeks after healing, the attachment to the tissue was tested with a universal test device. The three samples exhibited distinctive surface morphology. The force to remove the HAp implants from the muscles was significantly greater than that of Ti group ( P < 0.01), with the AD samples requiring the greatest force ( P < 0.01). After removal, SEM showed that the tissue was firmly attached to the surface of AD samples. Photomicrographs of the peri-implant muscles showed a layer of aligned fibrous tissue without severe inflammation. The AD samples had more fibroblasts. Results indicate that because of enhanced mechanical adhesion of soft tissue to the implants, HAp-coated Ti by AD is a suitable KPro skirt material.

  4. Microcracks induce osteoblast alignment and maturation on hydroxyapatite scaffolds

    NASA Astrophysics Data System (ADS)

    Shu, Yutian

    Physiological bone tissue is a mineral/collagen composite with a hierarchical structure. The features in bone, such as mineral crystals, fibers, and pores can range from the nanometer to the centimeter in size. Currently available bone tissue scaffolds primarily address the chemical composition, pore size, and pore size distribution. While these design parameters are extensively investigated for mimicking bone function and inducing bone regeneration, little is known about microcracks, which is a prevalent feature found in fractured bone in vivo and associated with fracture healing and repair. Since the purpose of bone tissue engineering scaffold is to enhance bone regeneration, the coincidence of microcracks and bone densification should not be neglected but rather be considered as a potential parameter in bone tissue engineering scaffold design. The purpose of this study is to test the hypothesis that microcracks enhance bone healing. In vitro studies were designed to investigate the osteoblast (bone forming cells) response to microcracks in dense (94%) hydroxyapatite substrates. Microcracks were introduced using a well-established Vickers indentation technique. The results of our study showed that microcracks induced osteoblast alignment, enhanced osteoblast attachment and more rapid maturation. These findings may provide insight into fracture healing mechanism(s) as well as improve the design of bone tissue engineering orthopedic scaffolds for more rapid bone regeneration.

  5. Effect of hydroxyapatite surface morphology on cell adhesion.

    PubMed

    Iwamoto, Takashi; Hieda, Yohki; Kogai, Yasumichi

    2016-12-01

    We obtained hydroxyapatite (HAp) materials as a block by mixing HAp nanoparticles and polymer, and then calcining the mixtures. The surface morphology of the HAp materials was tuned by varying heat treatment conditions. After calcining the mixtures at 1200 or 800°C for 4h, the surface morphology of the HAp materials was flat or convexo-concave, respectively. The flat surface morphology, which showed micrometer-ordered grain boundaries, was formed by the aggregation of HAp nanoparticles. On the other hand, the convexo-concave surface morphology resulted from the agglomeration of HAp nanoparticles after heat treatment at 800°C for 4h with nanometer-ordered particle size. We tested cell adhesion to HAp materials with flat or convexo-concave surface morphology and found that cells adhered well to the flat HAp materials but not to the convexo-concave HAp materials. This technique for selectively preparing HAp materials with flat or convexo-concave surface morphology was very easy because we merely mixed commercial HAp nanoparticles with polymer and then calcined the mixtures. As a result, the heat treatment temperature affected the surface morphology of our HAp materials, and their surface morphologies contributed to cell adhesion independently of other material properties. PMID:27612825

  6. Development and Characterization of Biphasic Hydroxyapatite/β-TCP Cements

    PubMed Central

    Gallinetti, Sara; Canal, Cristina; Ginebra, Maria-Pau; Ferreira, J

    2014-01-01

    Biphasic calcium phosphate bioceramics composed of hydroxyapatite (HA) and β-tricalcium phosphate (β-TCP) have relevant properties as synthetic bone grafts, such as tunable resorption, bioactivity, and intrinsic osteoinduction. However, they have some limitations associated to their condition of high-temperature ceramics. In this work self-setting Biphasic Calcium Phosphate Cements (BCPCs) with different HA/β-TCP ratios were obtained from self-setting α-TCP/β-TCP pastes. The strategy used allowed synthesizing BCPCs with modulated composition, compressive strength, and specific surface area. Due to its higher solubility, α-TCP was fully hydrolyzed to a calcium-deficient HA (CDHA), whereas β-TCP remained unreacted and completely embedded in the CDHA matrix. Increasing amounts of the non-reacting β-TCP phase resulted in a linear decrease of the compressive strength, in association to the decreasing amount of precipitated HA crystals, which are responsible for the mechanical consolidation of apatitic cements. Ca2+ release and degradation in acidic medium was similar in all the BCPCs within the timeframe studied, although differences might be expected in longer term studies once β-TCP, the more soluble phase was exposed to the surrounding media. PMID:25866411

  7. Controlled degradation pattern of hydroxyapatite/calcium carbonate composite microspheres.

    PubMed

    Yang, Ning; Zhong, Qiwei; Zhou, Ying; Kundu, Subhas C; Yao, Juming; Cai, Yurong

    2016-06-01

    Hydroxyapatite (HAP) is widely used in clinic due to its good biocompatibility and osteoconductivity except for its slow degradation speed. In the present study, spherical calcium carbonate (CaCO3 ) is fabricated in the presence of silk protein sericin, which is transmuted into HAP microsphere in phosphate solution with the assistance of microwave irradiation. The effect of reaction conditions on the conversion of CaCO3 is investigated including reaction time, chemical composition of phosphate solution, and microwave power to get a series of HAP/CaCO3 composites. The degradation property of the composites is evaluated in vitro. Results show the degradation speed of the composite with higher HAP content is slower. The degradation rate of the composite could be changed effectively by modulating the proportion of HAP and CaCO3 . This work provides a feasible method for the preparation of spherical HAP/CaCO3 composite with controllable degradability. The composite thus obtained may be an ideal material for bone tissue engineering application. Microsc. Res. Tech. 79:518-524, 2016. © 2016 Wiley Periodicals, Inc. PMID:27037606

  8. Substitution mechanism of alkali metals for strontium in strontium hydroxyapatite

    SciTech Connect

    Naddari, Thouraya; Hamdi, Besma; Savariault, Jean Michel; El Feki, Hafed; Ben Salah, Abdelhamid

    2003-01-25

    Strontium hydroxyapatites substituted by alkali metals are synthesized by double decomposition method in basic medium. Structures of Sr{sub 9.50}Na{sub 0.30}(PO{sub 4}){sub 6}(OH){sub 1.30} (SrNaHAp) and Sr{sub 9.81}K{sub 0.12}(PO{sub 4}){sub 6}(OH){sub 1.74} (SrKHAp) are determined by X-ray powder diffraction. Both compounds are isotypic and crystallize in hexagonal system (space group P63/m) with the following cells: a=9.751(3) A and c=7.279(3) A for SrNaHAp and a=9.755(4) A and c=7.284(3) A for SrKHAp. Results are compared to those of Sr{sub 10}(PO{sub 4}){sub 6}(OH){sub 2}. According to the site occupancy factors, in SrNaHAp sodium is localized in site (I) and in SrKHAp potassium in site (II). Both structures contain vacancies in hydroxyl and metal sites. The mechanism of alkali metals substitution for strontium proposed explains the vacancies formation.

  9. Optimization of physiological properties of hydroxyapatite as a vaccine adjuvant.

    PubMed

    Hayashi, Masayuki; Aoshi, Taiki; Kogai, Yasumichi; Nomi, Daisuke; Haseda, Yasunari; Kuroda, Etsushi; Kobiyama, Kouji; Ishii, Ken J

    2016-01-12

    Various particles such as Alum or silica are known to act as an adjuvant if co-administered with vaccine antigens. Several reports have demonstrated that the adjuvanticity is strongly affected by the physicochemical properties of particles such as the size, shape and surface charge, although the required properties and its relationship to the adjuvanticity are still controversial. Hydroxyapatite particle (HAp) composed of calcium phosphate has been shown to work as adjuvant in mice. However, the properties of HAp required for the adjuvanticity have not been fully characterized yet. In this study, we examined the role of size or shape of HAps in the antibody responses after immunization with antigen. HAps whose diameter ranging between 100 and 400 nm provided significantly higher antibody responses than smaller or larger ones. By comparison between sphere and rod shaped HAps, rod shaped HAps induced stronger inflammasome-dependent IL-1β production than the sphere shaped ones in vitro. However, sphere- and rod-shaped HAp elicited comparable antibody response in WT mice. Vice versa, Nlrp3(-/-), Asc(-/-) or Caspase1(-/-) mice provided comparable level of antibody responses to HAp adjuvanted vaccination. Collectively, our results demonstrated that the size rather than shape is a more critical property, and IL-1β production via NLRP3 inflammasome is dispensable for the adjuvanticity of HAps in mice. PMID:26667613

  10. Enhanced Osteogenesis by Reduced Graphene Oxide/Hydroxyapatite Nanocomposites

    PubMed Central

    Lee, Jong Ho; Shin, Yong Cheol; Lee, Sang-Min; Jin, Oh Seong; Kang, Seok Hee; Hong, Suck Won; Jeong, Chang-Mo; Huh, Jung Bo; Han, Dong-Wook

    2015-01-01

    Recently, graphene-based nanomaterials, in the form of two dimensional substrates or three dimensional foams, have attracted considerable attention as bioactive scaffolds to promote the differentiation of various stem cells towards specific lineages. On the other hand, the potential advantages of using graphene-based hybrid composites directly as factors inducing cellular differentiation as well as tissue regeneration are unclear. This study examined whether nanocomposites of reduced graphene oxide (rGO) and hydroxyapatite (HAp) (rGO/HAp NCs) could enhance the osteogenesis of MC3T3-E1 preosteoblasts and promote new bone formation. When combined with HAp, rGO synergistically promoted the spontaneous osteodifferentiation of MC3T3-E1 cells without hindering their proliferation. This enhanced osteogenesis was corroborated from determination of alkaline phosphatase activity as early stage markers of osteodifferentiation and mineralization of calcium and phosphate as late stage markers. Immunoblot analysis showed that rGO/HAp NCs increase the expression levels of osteopontin and osteocalcin significantly. Furthermore, rGO/HAp grafts were found to significantly enhance new bone formation in full-thickness calvarial defects without inflammatory responses. These results suggest that rGO/HAp NCs can be exploited to craft a range of strategies for the development of novel dental and orthopedic bone grafts to accelerate bone regeneration because these graphene-based composite materials have potentials to stimulate osteogenesis. PMID:26685901

  11. Bioactivity in in situ hydroxyapatite-polycaprolactone composites.

    PubMed

    Verma, Devendra; Katti, Kalpana; Katti, Dinesh

    2006-09-15

    In our previous work, hydroxyapatite (HAP) was synthesized under two conditions: one in the presence of polyacrylic acid (in situ HAP) and the other in the absence of polyacrylic acid (ex situ HAP). Composites of both HAPs with polycaprolactone (PCL) were investigated for their applicability as scaffolds for bone tissue engineering. In the current work, bioactivity of these composites has been investigated by soaking them in simulated body fluid for different intervals of time. Nucleation and growth mechanism of apatite on these composites has also been investigated. Fourier transform infrared spectroscopy study suggests that although apatite growth starts with an intermediate phase, it completely transforms to HAP after 4 days of soaking. Nanoindentation results suggest that the apatite growing on in situ HAP/PCL composites has much higher hardness and elastic modulus as compared to the apatite growing on ex situ HAP/PCL composites. The apatite grown on the ex situ composites has a net-like interconnected structure. The observed differences in mechanical properties and morphology of apatite have been described on the basis of nucleation mechanisms. The nucleation of apatite on the in situ HAP/PCL composites proceeds through the formation of a complex between Ca2+ and COO- groups; on the other hand, nucleation occurs because of dissolution reaction of apatite in ex situ HAP/PCL composites. PMID:16739180

  12. Osteoconductive hydroxyapatite coated PEEK for spinal fusion surgery

    NASA Astrophysics Data System (ADS)

    Hahn, Byung-Dong; Park, Dong-Soo; Choi, Jong-Jin; Ryu, Jungho; Yoon, Woon-Ha; Choi, Joon-Hwan; Kim, Jong-Woo; Ahn, Cheol-Woo; Kim, Hyoun-Ee; Yoon, Byung-Ho; Jung, In-Kwon

    2013-10-01

    Polyetheretherketone (PEEK) has attracted much interest as biomaterial for interbody fusion cages due to its similar stiffness to bone and good radio-transparency for post-op visualization. Hydroxyapatite (HA) coating stimulates bone growth to the medical implant. The objective of this work is to make an implant consisting of biocompatible PEEK with an osteoconductive HA surface for spinal or orthopedic applications. Highly dense and well-adhered HA coating was developed on medical-grade PEEK using aerosol deposition (AD) without thermal degradation of the PEEK. The HA coating had a dense microstructure with no cracks or pores, and showed good adhesion to PEEK at adhesion strengths above 14.3 MPa. The crystallinity of the HA coating was remarkably enhanced by hydrothermal annealing as post-deposition heat-treatment. In addition, in vitro and in vivo biocompatibility of PEEK, in terms of cell adhesion morphology, cell proliferation, differentiation, and bone-to-implant contact ratio, were remarkably enhanced by the HA coating through AD.

  13. Osteogenic Responses to Zirconia with Hydroxyapatite Coating by Aerosol Deposition

    PubMed Central

    Cho, Y.; Hong, J.; Ryoo, H.; Kim, D.; Park, J.

    2015-01-01

    Previously, we found that osteogenic responses to zirconia co-doped with niobium oxide (Nb2O5) or tantalum oxide (Ta2O5) are comparable with responses to titanium, which is widely used as a dental implant material. The present study aimed to evaluate the in vitro osteogenic potential of hydroxyapatite (HA)-coated zirconia by an aerosol deposition method for improved osseointegration. Surface analysis by scanning electron microscopy and x-ray diffraction proved that a thin as-deposited HA film on zirconia showed a shallow, regular, crater-like surface. Deposition of dense and uniform HA films was measured by SEM, and the contact angle test demonstrated improved wettability of the HA-coated surface. Confocal laser scanning microscopy indicated that MC3T3-E1 pre-osteoblast attachment did not differ notably between the titanium and zirconia surfaces; however, cells on the HA-coated zirconia exhibited a lower proliferation than those on the uncoated zirconia late in the culture. Nevertheless, ALP, alizarin red S staining, and bone marker gene expression analysis indicated good osteogenic responses on HA-coated zirconia. Our results suggest that HA-coating by aerosol deposition improves the quality of surface modification and is favorable to osteogenesis. PMID:25586588

  14. Citric acid-based hydroxyapatite composite scaffolds enhance calvarial regeneration.

    PubMed

    Sun, Dawei; Chen, Yuhui; Tran, Richard T; Xu, Song; Xie, Denghui; Jia, Chunhong; Wang, Yuchen; Guo, Ying; Zhang, Zhongmin; Guo, Jinshan; Yang, Jian; Jin, Dadi; Bai, Xiaochun

    2014-01-01

    Citric acid-based polymer/hydroxyapatite composites (CABP-HAs) are a novel class of biomimetic composites that have recently attracted significant attention in tissue engineering. The objective of this study was to compare the efficacy of using two different CABP-HAs, poly (1,8-octanediol citrate)-click-HA (POC-Click-HA) and crosslinked urethane-doped polyester-HA (CUPE-HA) as an alternative to autologous tissue grafts in the repair of skeletal defects. CABP-HA disc-shaped scaffolds (65 wt.-% HA with 70% porosity) were used as bare implants without the addition of growth factors or cells to renovate 4 mm diameter rat calvarial defects (n = 72, n = 18 per group). Defects were either left empty (negative control group), or treated with CUPE-HA scaffolds, POC-Click-HA scaffolds, or autologous bone grafts (AB group). Radiological and histological data showed a significant enhancement of osteogenesis in defects treated with CUPE-HA scaffolds when compared to POC-Click-HA scaffolds. Both, POC-Click-HA and CUPE-HA scaffolds, resulted in enhanced bone mineral density, trabecular thickness, and angiogenesis when compared to the control groups at 1, 3, and 6 months post-trauma. These results show the potential of CABP-HA bare implants as biocompatible, osteogenic, and off-shelf-available options in the repair of orthopedic defects. PMID:25372769

  15. Magnetic responsive hydroxyapatite composite scaffolds construction for bone defect reparation

    PubMed Central

    Zeng, Xiao Bo; Hu, Hao; Xie, Li Qin; Lan, Fang; Jiang, Wen; Wu, Yao; Gu, Zhong Wei

    2012-01-01

    Introduction In recent years, interest in magnetic biomimetic scaffolds for tissue engineering has increased considerably. A type of magnetic scaffold composed of magnetic nanoparticles (MNPs) and hydroxyapatite (HA) for bone repair has been developed by our research group. Aim and methods In this study, to investigate the influence of the MNP content (in the scaffolds) on the cell behaviors and the interactions between the magnetic scaffold and the exterior magnetic field, a series of MNP-HA magnetic scaffolds with different MNP contents (from 0.2% to 2%) were fabricated by immersing HA scaffold into MNP colloid. ROS 17/2.8 and MC3T3-E1 cells were cultured on the scaffolds in vitro, with and without an exterior magnetic field, respectively. The cell adhesion, proliferation and differentiation were evaluated via scanning electron microscopy; confocal laser scanning microscopy; and 3-(4,5-Dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT), alkaline phosphatase, and bone gla protein activity tests. Results The results demonstrated the positive influence of the magnetic scaffolds on cell adhesion, proliferation, and differentiation. Further, a higher amount of MNPs on the magnetic scaffolds led to more significant stimulation. Conclusion The magnetic scaffold can respond to the exterior magnetic field and engender some synergistic effect to intensify the stimulating effect of a magnetic field to the proliferation and differentiation of cells. PMID:22848165

  16. Enhancement of hydroxyapatite formation by laser-liquid-solid interaction

    NASA Astrophysics Data System (ADS)

    Pramatarova, Liliana; Pecheva, Emilia; Petrov, Todor S.; Minkovski, Nikolai I.; Kondyurin, Alexey; Pramatarova, Radina

    2004-06-01

    In this paper the use of stainless steel, silicon and silica glass substrates for the growth of hydroxyapatite (HA, widely used as artificial bone material), induced by a laser-liquid-solid-interaction is reported. The method allows growing of HA layer by using the interaction between a laser beam and a liquid precursor solution, as well as laser irradiation of the substrate during the laser-liquid interaction. The scanned laser beam (pulsed CuBr laser) is directed at the solid substrate, which is immersed in the solution, which resembles the ion composition and concentrations of the human blood plasma (simulated body fluid, SBF). The set-up includes an open deposition system, which allows the introduction of the laser beam led by a scanning system. It is shown that the proposed method enhances the HA formation, in comparison with the traditional methods of prolonged soaking in SBF. The HA layers grown in this manner are investigated by Light Microscopy (LM), Scanning Electron Microscopy (SEM), Energy Dispersive X-ray (EDX) Spectroscopy, X-ray Diffraction (XRD), Fourier Transform Infrared (FTIR) and Raman Spectroscopy.

  17. Biomimetic configurational arrays of hydroxyapatite nanocrystals on bio-organics.

    PubMed

    Rhee, S H; Suetsugu, Y; Tanaka, J

    2001-11-01

    Biomimetic configurational arrays of hydroxyapatite (HAp) nanocrystals on several bio-organics, collagen (Col), chondroitin sulfate (ChS), and their mixture, were comparatively studied. The nanocomposites of HAp/Col, HAp/ChS, and HAp/Col/ChS were synthesized through a precipitation method with calcium hydroxide suspension and phosphoric acid solution containing Col, ChS, and their mixture, respectively. The (0 0 2) diffraction of the synthesized HAp crystals on a Col fiber showed an around 60 arching angle, while that on a ChS fiber showed just around 10 degrees. The same configurational arrays of HAp crystals could also be obtained on the mixture of Col and ChS fibers. The different electron diffraction patterns of the HAp crystals on the Col and ChS fibers were explained by the different macromolecular configurations of the Col and ChS fibrils which compose their fibers. The results may be applicable to develop a bone substitute which mimics the peculiar configurational arrays of HAp crystals found in bone and their detailed organic composition. PMID:11561889

  18. Seeded growth of hydroxyapatite in the presence of dissolved albumin.

    PubMed

    Gilman, H; Hukins, D W

    1994-07-01

    Hydroxyapatite (HAP) crystals were grown from a supersaturated solution by the addition of a suspension of seed crystals at a controlled pH value of 7.4 and a temperature of 37 degrees C. The degree of supersaturation was comparable to that in biological fluids and was such that all HAP precipitated would be expected to deposit on the seeds. Albumin was added to some of the solutions to give a concentration in the range 75-250 micrograms cm-3. Samples of solution were removed at known times after the addition of seed crystals and their calcium ion concentrations were determined by atomic absorption spectroscopy. The decrease in the dissolved calcium concentration was taken to be a measure of crystal growth. In the absence of seeds, no decrease in calcium concentration occurred. The initial rate of HAP growth decreased linearly with albumin concentration, i.e., albumin was found to inhibit crystal growth. Inhibition kinetics were consistent with a Langmuir model in which a single albumin molecule was capable of binding to more than one growth site on the crystal surface. Comparison with published results indicated that albumin was a less potent inhibitor of HAP growth than phosphoproteins but was a more potent inhibitor than magnesium or citrate ions. PMID:8046435

  19. Hydroxyapatite composite resin cement augmentation of pedicle screw fixation.

    PubMed

    Turner, Alexander W L; Gillies, R Mark; Svehla, Martin J; Saito, Masanobu; Walsh, William R

    2003-01-01

    Pedicle screw stability is poor in osteopenic vertebrae attributable, in part, to low screw-bone interface strength. The current authors examined cement augmentation using a low curing temperature hydroxyapatite and bis-phenol-A glycidol methacrylate-based composite resin. This cement may stiffen the screw-bone interface and reduce the harmful effects associated with polymethylmethacrylate regarding temperature and toxic monomer. Thirty-five lumbar vertebrae from human cadavers were instrumented with pedicle screws, with one pedicle previously injected with cement and the other as the control. Caudocephalad toggling of +/- 1 mm for 1600 cycles was applied to the pedicle screws, and the resulting forces supported by the implant-bone interface were captured by a load cell. A curve was constructed from the peak caudal load for each cycle and three mechanical measures parameterized this curve: (1) initial load; (2) rate of load decay during the first 400 cycles; and (3) final load. The initial load increased by 16% as a result of cement augmentation, the final load increased by 65%, and the rate of load decay decreased by 59%. Cement augmentation of pedicle screws increased the stiffness and stability of the screw-bone interface. PMID:12579026

  20. Lysozyme loading and release from Se doped hydroxyapatite nanoparticles.

    PubMed

    Wang, Yanhua; Hao, Hang; Zhang, Shengmin

    2016-04-01

    Element-substituted hydroxyapatite (HA) based nanocomposites have become a promising therapeutic material for improving bone defect repair. Selenium substituted HA nanoparticles can both induce apoptosis of bone tumor cells and enhance osteointegration. However, the effect of selenite ions on the proteins in combination with the HA nanoparticles remains to be elucidated. Here, we investigated the influence of selenium doping concentration on the loading and release of lysozyme (LSM) as a model protein drug. The selenium substituted HA-LSM composites with different doping concentrations were synthesized and characterized. The subsequent delivery of lysozyme was studied in a phosphate buffer solution (PBS). We found that selenium substituted HA-LSM composites with Se:P=10% showed the highest amount of lysozyme loading (41.7%), whereas the amount of lysozyme loaded in undoped HA nanoparticles was the lowest (34.1%). The doped selenium interacts with lysozyme molecules, which leads to the increase of β-sheet and unordered, and the decrease of self-association, α-helix and β-turns in protein structures. Moreover, selenium addition significantly slows the protein release from HA-LSM composites. The composites with Se:P=10% release lysozyme at the slightly slower rate among the samples with different Se doping concentrations. It also shows that the released lysozyme retains most of its enzymatic activity. PMID:26838882