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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. 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

  3. 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.

  4. 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.

  5. 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.

  6. In vitro evaluation of human osteoblast-like cell proliferation and attachment on nanostructured fluoridated hydroxyapatite.

    PubMed

    Esnaashary, Mohammadhossein; Fathi, Mohammadhossein; Ahmadian, Mahdi

    2014-06-01

    The effect of the fluorine content and nano-structure of fluoridated hydroxyapatite (FHA) on human osteoblast-like (HO) cell behavior were investigated. FHA nanopowders and bulk nanostructured FHA, produced via mechanical alloying and two-step sintering, respectively, were used. The cytotoxicity of FHA nanopowders was assessed by MTT. Cell attachment to the surface of the bulk nanostructured FHA was evaluated by culturing of HO cells. Although HO cells proliferated 10 % more in contact with FHA nanopowders compared to culture medium without FHA nanopowders, an increase in the fluorine content of FHA caused a delay in the cell proliferation by about 2 days. Cell attachment on the bulk nanostructured FHA did not change the fluorine content. PMID:24563314

  7. Method for forming energetic nanopowders

    DOEpatents

    Lee, Kien-Yin; Asay, Blaine W.; Kennedy, James E.

    2013-10-15

    A method for the preparation of neat energetic powders, having nanometer dimensions, is described herein. For these neat powder, a solution of a chosen energetic material is prepared in an aprotic solvent and later combined with liquid hexane that is miscible with such solvent. The energetic material chosen is less soluble in the liquid hexane than in the aprotic solvent and the liquid hexane is cooled to a temperature that is below that of the solvent solution. In order to form a precipitate of said neat powders, the solvent solution is rapidly combined with the liquid hexane. When the resulting precipitate is collected, it may be dried and filtered to yield an energetic nanopowder material.

  8. 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

  9. 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.

  10. Synthesis of carbon nanostructures on iron nanopowders

    NASA Astrophysics Data System (ADS)

    Koshanova, A.; Partizan, G.; Mansurov, B.; Medyanova, B.; Mansurova, M.; Aliev, B.; Jiang, Xin

    2016-08-01

    This work presents the results of experiments on synthesis of carbon nanostructures (CNs) by the method of thermal chemical vapor deposition using iron nanopowders obtained by the method of electrical explosion of wires as catalysts. To study the process of nucleation and growth of individual carbon nanostructures, experiments were conducted not only on nanopowders, but also on the separated clusters. To determine the optimum conditions of the carbon nanostructures synthesis and lower temperature limit, experiments were performed at different temperatures (300-700°C) and pressures (100-400 mbar). The experiments have shown that the lower temperature limit for carbon nanostructures synthesis on the iron nanopowders is 350°C and in this process the growth of carbon nanostructures is not so massive. Stable growth of carbon nanostructures for nanopowders began from 400°C during the entire range of pressures. The analysis of Raman spectroscopy showed that the most optimum conditions for obtaining nanotubes of high quality are P = 100 mbar and T = 425°C.

  11. Nanoexplosion synthesis of multimetal oxide ceramic nanopowders.

    PubMed

    Vasylkiv, Oleg; Sakka, Yoshio

    2005-12-01

    Herein we demonstrate a unique processing technique for engineering multicomponent ceramic nanopowders with precise morphologies by "nanoblast" calcination/deagglomeration. Multiple "nanoexplosions" of C(3)H(6)N(6)O(6) nanoparticles embedded in preliminary engineered nanoreactors break apart the agglomerates because of the highly energetic impacts of the blast waves. Also, the solid-solubility of one component into the other is enhanced by the extremely high local temperature generated during the nanoexplosions. We applied this technique to produce nanosized agglomerate-free ceria-gadolinia solid solution powder with an average aggregate size of 42 nm. The described method opens the door to the synthesis of a wide range of multimetal oxide ceramic and metal-ceramic composite nanopowders, with precise stoichiometries and uniform morphologies. PMID:16351222

  12. 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.

  13. Calcium hydroxyapatite fillers.

    PubMed

    Tansavatdi, Kristina; Mangat, Devinder S

    2011-12-01

    Calcium hydroxyapatite fillers have unique advantages over other fillers in regards to duration of action and volume of product required for augmentation, especially in the midface and lower face. In this article, we describe our experience with calcium hydroxyapatite fillers and compare them with other available filler products.

  14. 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.

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

    NASA Astrophysics Data System (ADS)

    Shigeta, Masaya; Watanabe, Takayuki

    2010-08-01

    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.

  16. 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.

  17. 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.

  18. 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.

  19. 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.

  20. 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.

  1. 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

  2. Carbon dot based nanopowders and their application for fingerprint recovery.

    PubMed

    Fernandes, D; Krysmann, M J; Kelarakis, A

    2015-03-21

    The incorporation of a minor amount of carbogenic nanoparticles into powder compositions imparts remarkable colour-tuneability, without compromising the flowability. In a proof-of-concept demonstration we report the use of these hybrid nanopowders for the visual enhancement of latent fingerprints where they effectively resolve issues arising from poor contrast against multi-coloured or patterned backgrounds.

  3. 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.

  4. 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

  5. Shock-induced consolidation and spallation of Cu nanopowders

    SciTech Connect

    Huang, L.; Han, W. Z.; Luo, S. N.; An, Q.; Goddard, W. A. III

    2012-01-01

    A useful synthesis technique, shock synthesis of bulk nanomaterials from nanopowders, is explored here with molecular dynamics simulations. We choose nanoporous Cu ({approx}11 nm in grain size and 6% porosity) as a representative system, and perform consolidation and spallation simulations. The spallation simulations characterize the consolidated nanopowders in terms of spall strength and damage mechanisms. The impactor is full density Cu, and the impact velocity (u{sub i}) ranges from 0.2 to 2 km s{sup -1}. We present detailed analysis of consolidation and spallation processes, including atomic-level structure and wave propagation features. The critical values of u{sub i} are identified for the onset plasticity at the contact points (0.2 km s{sup -1}) and complete void collapse (0.5 km s{sup -1}). Void collapse involves dislocations, lattice rotation, shearing/friction, heating, and microkinetic energy. Plasticity initiated at the contact points and its propagation play a key role in void collapse at low u{sub i}, while the pronounced, grain-wise deformation may contribute as well at high u{sub i}. The grain structure gives rise to nonplanar shock response at nanometer scales. Bulk nanomaterials from ultrafine nanopowders ({approx}10 nm) can be synthesized with shock waves. For spallation, grain boundary (GB) or GB triple junction damage prevails, while we also observe intragranular voids as a result of GB plasticity.

  6. Functionalized diamond nanopowder for phosphopeptides enrichment from complex biological fluids.

    PubMed

    Hussain, Dilshad; Najam-ul-Haq, Muhammad; Jabeen, Fahmida; Ashiq, Muhammad N; Athar, Muhammad; Rainer, Matthias; Huck, Christian W; Bonn, Guenther K

    2013-05-01

    Diamond is known for its high affinity and biocompatibility towards biomolecules and is used exclusively in separation sciences and life science research. In present study, diamond nanopowder is derivatized as Immobilized Metal Ion Affinity Chromatographic (IMAC) material for the phosphopeptides enrichment and as Reversed Phase (C-18) media for the desalting of complex mixtures and human serum profiling through MALDI-TOF-MS. Functionalized diamond nanopowder is characterized by Fourier transform infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) spectroscopy. Diamond-IMAC is applied to the standard protein (β-casein), spiked human serum, egg yolk and non-fat milk for the phosphopeptides enrichment. Results show the selectivity of synthesized IMAC-diamond immobilized with Fe(3+) and La(3+) ions. To comprehend the elaborated use, diamond-IMAC is also applied to the serum samples from gall bladder carcinoma for the potential biomarkers. Database search is carried out by the Mascot program (www.matrixscience.com) for the assignment of phosphorylation sites. Diamond nanopowder is thus a separation media with multifunctional use and can be applied to cancer protein profiling for the diagnosis and biomarker identification.

  7. Functionalized diamond nanopowder for phosphopeptides enrichment from complex biological fluids.

    PubMed

    Hussain, Dilshad; Najam-ul-Haq, Muhammad; Jabeen, Fahmida; Ashiq, Muhammad N; Athar, Muhammad; Rainer, Matthias; Huck, Christian W; Bonn, Guenther K

    2013-05-01

    Diamond is known for its high affinity and biocompatibility towards biomolecules and is used exclusively in separation sciences and life science research. In present study, diamond nanopowder is derivatized as Immobilized Metal Ion Affinity Chromatographic (IMAC) material for the phosphopeptides enrichment and as Reversed Phase (C-18) media for the desalting of complex mixtures and human serum profiling through MALDI-TOF-MS. Functionalized diamond nanopowder is characterized by Fourier transform infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) spectroscopy. Diamond-IMAC is applied to the standard protein (β-casein), spiked human serum, egg yolk and non-fat milk for the phosphopeptides enrichment. Results show the selectivity of synthesized IMAC-diamond immobilized with Fe(3+) and La(3+) ions. To comprehend the elaborated use, diamond-IMAC is also applied to the serum samples from gall bladder carcinoma for the potential biomarkers. Database search is carried out by the Mascot program (www.matrixscience.com) for the assignment of phosphorylation sites. Diamond nanopowder is thus a separation media with multifunctional use and can be applied to cancer protein profiling for the diagnosis and biomarker identification. PMID:23601977

  8. Electrospinning biomedical nanocomposite fibers of hydroxyapatite/poly(lactic acid) for bone regeneration.

    PubMed

    Kim, Hae-Won; Lee, Hae-Hyoung; Knowles, J C

    2006-12-01

    Development of fibrous matrices of bioceramic-biopolymer nanocomposite offers great potential in the field of bone regeneration and tissue engineering. However, in order to produce electrospun fibers with homogeneous structure, it is essential for the ceramic powder to be fine and to remain stable in suspension. Herein, we developed a novel method whereby the bioceramic hydroxyapatite (HA) was kept in suspension in biopolymer poly(lactic acid) (PLA). The strategy was to introduce a surfactant hydroxysteric acid (HSA) between the hydrophilic HA powder and the hydrophobic chloroform-dissolved PLA. The HA nanopowder was dispersed effectively in HSA and mixed homogeneously with PLA. Continuous and uniform fibers were generated successfully with diameters of approximately 1-2 microm, and featured a well-developed nanocomposite structure of HA nanopowder-dispersed PLA. Initial cellular assays showed excellent cell attachment and proliferation and also enhanced expression of alkaline phosphatase at 7 days of culturing. The HA-PLA nanocomposite fibers may be potentially useful in tissue engineering applications, particularly as three-dimensional substrates for bone growth.

  9. Assignment of Appropriate Conditions for Synthesizing Tungsten Nanopowder by Electric Explosion of Conductors

    NASA Astrophysics Data System (ADS)

    Zhuravkov, S. P.; Pustovalov, A. V.; Kuznetsov, M. A.; Rosliy, I. S.; Zernin, E. A.

    2016-08-01

    The paper provides the results of experimental research into properties of tungsten nanopowders synthesized by electric explosion of a conductor in argon at various energies, put into the conductor when exploding. The authors have studied how the conditions of synthesizing the tungsten nanopowder influence on the average size of particles.

  10. Zirconia nanoceramic via redispersion of highly agglomerated nanopowder and spark plasma sintering.

    PubMed

    Suárez, Gustavo; Borodianska, Hanna; Sakka, Yoshio; Aglietti, Esteban F; Vasylkiv, Oleg

    2010-10-01

    A 2.7 mol% yttria stabilizing tetragonal zirconia (2.7Y-TZP) nanopowder was synthesized and stored for five years. Humidity and unsatisfactory storage conditions gradually caused heavy agglomeration. Within a few months, 2.7Y-TZP nanopowder became useless for any technological application. A bead-milling deagglomeration technique was applied to recover the heavily agglomerated yttria-stabilized zirconia nanopowder. Low-temperature sintering and spark plasma sintering (SPS) were performed, resulting in fully dense nanostructured ceramics. Compacts formed with heavily agglomerated powder present low sinterability and poor mechanical properties. Bead-milling suspension formed compacts exhibit mechanical properties in the range of the values reported for nanostructured zirconia. This observation confirms the effectiveness of bead-milling in the deagglomeration of highly agglomerated nanopowders. The high value of Vickers hardness of 13.6 GPa demonstrates the success of the processing technique for recovering long-time-stored oxide nanopowders. PMID:21137774

  11. 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.

  12. 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.

  13. Synthesis of AlNiCo core/shell nanopowders

    NASA Astrophysics Data System (ADS)

    Genc, A. M.; Akdeniz, M. V.; Ozturk, T.; Kalay, Y. E.

    2016-11-01

    Magnetic core/shell nanostructures have been recently received much interest owing to their utmost potential in permanent magnetic applications. In the present work, AlNiCo permanent magnet powders were synthesized by ball milling and a core/shell nanostructure was obtained using RF induced plasma. The effects of particle size and nanoshell structure on the magnetic properties were investigated in details. The coercivity of AlNiCo powders was found to increase with decreasing particle size, exclusively nanopowders encapsulated with Fe3O4 shell showed the highest coercivity values. The shell structure produced during plasma reaction was found to form a resistant layer against oxidation of metallic nanoparticles.

  14. 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.

  15. 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

  16. Nanofiber generation of hydroxyapatite and fluor-hydroxyapatite bioceramics.

    PubMed

    Kim, Hae-Won; Kim, Hyoun-Ee

    2006-05-01

    In this study, we produced hydroxyapatite (HA) and fluor-hydroxyapatite (FHA) bioceramics as a novel geometrical form, the nanoscale fiber, for the biomedical applications. Based on the sol-gel precursors of the apatites, an electrospinning technique was introduced to generate nanoscale fibers. The diameter of the fibers was exploited in the range of a few micrometers to hundreds of nanometers (1.55 microm-240 nm) by means of adjusting the concentration of the sols. Through the fluoridation of apatite, the solubility of the fiber was tailored and the fluorine ions were well released from the FHA. The HA and FHA nanofibers produced in this study are considered to find potential applications in the biomaterials and tissue engineering fields.

  17. Synthesis and Physical Properties of Nd:YVO4 Nanopowders prepared by a Chemical Method

    NASA Astrophysics Data System (ADS)

    Maleki, M. H.; Alhooie, S.; Dizaji, H. R.; Asgari, A.

    2014-01-01

    Single-phase Nd-doped YVO4 nanopowders were synthesized by a chemical method. The powders were heated at 1200°C for 1 h to obtain good crystallinity with better luminescence. Annealing temperature affects the crystal structure of the nanopowders. X-ray diffraction (XRD) revealed that a preferred crystallographic orientation is [200]. Measurements showed that the nanoparticles had an average size of 62.5 nm. A scanning electron microscope (SEM) image of the nanopowders indicated the formation of uniform and nearly spherical Nd:YVO4 particles. The transmittance spectrum of the nanopowders showed a broad absorption band around 808 nm. Photoluminescence studies on the annealed powders revealed their luminescence properties.

  18. 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.

  19. The effect of nanobioceramic reinforcement on mechanical and biological properties of Co-base alloy/hydroxyapatite nanocomposite.

    PubMed

    Bahrami, M; Fathi, M H; Ahmadian, M

    2015-03-01

    The goal of the present research was to fabricate, characterize, and evaluate mechanical and biological properties of Co-base alloy composites with different amounts of hydroxyapatite (HA) nanopowder reinforcement. The powder of Co-Cr-Mo alloy was mixed with different amounts of HA by ball milling and it was then cold pressed and sintered. X-ray diffraction (XRD) and scanning electron microscopy (SEM) techniques were used. Microhardness measurement and compressive tests were also carried out. Bioactivity behavior was evaluated in simulated body fluid (SBF). A significant decrease in modulus elasticity and an increase in microhardness of the sintered composites were observed. Apatite formation on the surface of the composites showed that it could successfully convert bioinert Co-Cr-Mo alloy to bioactive type by adding 10, 15, and 20wt.% HA which have lower modulus elasticity and higher microhardness.

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

    PubMed

    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.

  1. A comparative study of morphology and composition on oxide nanopowders elaborated by SPVD

    NASA Astrophysics Data System (ADS)

    Bârcă, E. S.; Rizea, V.; Abrudeanu, M.; Plaiasu, A. G.; Istrate, B.; Munteanu, C.

    2015-11-01

    The paper proposes a method of obtaining oxide nanopowders in a solar reactor using the solar energy (solar physical vapor deposition). The proposed method is a new method of obtaining nanopowders. Taking into consideration that the properties of the materials change once they get to nanodimensions it is desirable to obtain nanomaterials starting from base materials. Because of the properties that nanomaterials provide, the demand has grown in the last period of time. Also the last few years provided a various number of nanomaterials used in different fields of research. Among the materials that were obtained by SPVD there can be reminded the MoS2, the MoS2 doped with Zn, CeO2 doped with Zr. The CeO2 is used in applications such as catalysis, gas sensor, fuell cell as well as optical additives. All of the obtained nanopowders were analyzed and characterized by X-Ray diffraction (XRD) and by scanning electron microscopy (SEM) in order to acquire the information about the crystallography and morphology considering the reactions parameters that were used in obtaining the nanopowders. From the X-Ray diffraction can be concluded in the case of the CeO2 that doping occurred. By controlling the reactions parameters the end result is different in therms of obtained morphology of the nanopowders. All of the above elaborated nanopowders can be deposited in the form of thin films by laser ablation method in order to obtain better properties of the base material.

  2. 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

  3. 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

  4. Nanostructure of biocompatible titania/hydroxyapatite coatings

    NASA Astrophysics Data System (ADS)

    Fomin, Aleksandr A.; Rodionov, Igor V.; Steinhauer, Aleksey B.; Fomina, Marina A.; Petrova, Natalia V.; Zakharevich, Andrey M.; Skaptsov, Aleksandr A.; Gribov, Andrey N.; Atkin, Vsevolod S.

    2014-01-01

    The article describes prospective composite biocompatible titania coatings modified with hydroxyapatite nanoparticles and obtained on intraosseous implants fabricated from commercially pure titanium VT1-00. Consistency changes of morphological characteristics, crystalline structure, physical and mechanical properties and biocompatibility of experimental titanium implant coatings obtained by the combination of oxidation and surface modification with hydroxyapatite during induction heat treatment are defined.

  5. Application of hydroxyapatite-sol as drug carrier.

    PubMed

    Kano, S; Yamazaki, A; Otsuka, R; Ohgaki, M; Akao, M; Aoki, H

    1994-01-01

    The application of hydroxyapatite-sol as a drug carrier is being developed. Hydroxyapatite-sol which is a suspension consisting of hydroxyapatite nano-crystals, was synthesized using an ultrasonic homogenizer. The size of the crystals was 40 x 15 x 10 mm3 on average and their specific surface area was 100 m2/g. An amount of a glycoside antibiotics adsorbed onto hydroxyapatite nano-crystals was measured. The drug adsorbed 0.2 mg per 1 mg of hydroxyapatite. The affect of the drug adsorbed onto the hydroxyapatite was investigated using cancer cells. The drug, adsorbed onto the hydroxyapatite nano-crystals, inhibited cancer cell growth.

  6. Microstructured microspheres of hydroxyapatite bioceramic.

    PubMed

    Sunny, M C; Ramesh, P; Varma, H K

    2002-07-01

    Hydroxyapatite (HAP) particles having spherical geometry and 125-1000 microm in size range were prepared using a solid-in-water-in-oil (S/W/O) emulsion, cross-linking technique. An aqueous solution of chitosan containing different loading of HAP was dispersed as droplet in liquid paraffin using a stabilizing agent. Cross-linking of chitosan was induced by adding appropriate amount of glutaraldehyde saturated toluene. Chitosan microspheres containing HAP were sintered at 1150 degrees C to obtain pure HAP microspheres. The spheres thus produced were examined by scanning electron microscopy. The percentage yield and size distributions of the spheres were also determined.

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

    NASA Astrophysics Data System (ADS)

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

    2014-03-01

    Trivalent transition metal ions (Cr3+, Fe3+) 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 Cr3+ and Fe3+ ions in octahedral site symmetry. Crystal field (Dq) and inter-electronic repulsion (B and C) parameters are evaluated for Cr3+ doped CdO nanopowders as Dq = 1540, B = 619 and C = 3327 cm-1 and for Fe3+ doped CdO nanopowders Dq = 920, B = 690, C = 2750 cm-1. EPR spectra of the Cr3+ and Fe3+ 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 Cr3+ doped CdO, ultraviolet and blue emissions for Fe3+ 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.

  8. 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.

  9. 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

  10. 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

  11. 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.

  12. 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

  13. Stability of hydroxyapatite while processing short-fibre reinforced hydroxyapatite ceramics.

    PubMed

    Knepper, M; Moricca, S; Milthorpe, B K

    1997-12-01

    Reinforcement by short fibres has been adapted from modern ceramic processing technologies to achieve an improvement of structural properties of hydroxyapatite. However, the influence of the reinforcement fibres on the thermochemical behaviour of the hydroxyapatite has yet to be clarified comprehensively. Titanium, alumina and 316L-stainless steel, all materials with a proven record as implant materials, were chosen as reinforcement materials. Short fibres of these materials were incorporated in a matrix of hydroxyapatite to toughen the hydroxyapatite. Composites were processed by sintering in air, hot isostatic pressing and a method combining sintering in inert gas atmosphere and hot isostatic pressing. PMID:9430334

  14. Interaction of hydrogen with ZnO nanopowders--evidence of hydroxyl group formation.

    PubMed

    Wong, Kester W J; Field, Matthew R; Ou, Jian Zhen; Latham, Kay; Spencer, Michelle J S; Yarovsky, Irene; Kalantar-zadeh, Kourosh

    2012-01-13

    There have been many investigations to reveal the nature of the hydrogen gas and ZnO nanopowder interaction at elevated temperatures, while at present no conclusive description of such an interaction has been confidently reported. In this work, we demonstrate that a hydroxyl group is formed during this interaction, depending on size and relative crystallinity of nanopowders. Our in situ Raman spectroscopy investigations show that the interaction directly affects the intensity of the Raman signal at 483 cm(-1), relative to the peak at 519 cm(-1). Ex situ x-ray diffraction (XRD) and infrared spectroscopy also show extra peaks at 44° and 1618 cm(-1), respectively, after hydrogenation. These peaks were all identified as surface hydroxyl groups, which can be related to the formation of water on the ZnO nanopowder surfaces.

  15. 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.

  16. 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.

  17. 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

  18. 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

  19. 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.

  20. Enhanced osteoconductivity of sodium-substituted hydroxyapatite by system instability.

    PubMed

    Sang Cho, Jung; Um, Seung-Hoon; Su Yoo, Dong; Chung, Yong-Chae; Hye Chung, Shin; Lee, Jeong-Cheol; Rhee, Sang-Hoon

    2014-07-01

    The effect of substituting sodium for calcium on enhanced osteoconductivity of hydroxyapatite was newly investigated. Sodium-substituted hydroxyapatite was synthesized by reacting calcium hydroxide and phosphoric acid with sodium nitrate followed by sintering. As a control, pure hydroxyapatite was prepared under identical conditions, but without the addition of sodium nitrate. Substitution of calcium with sodium in hydroxyapatite produced the structural vacancies for carbonate ion from phosphate site and hydrogen ion from hydroxide site of hydroxyapatite after sintering. The total system energy of sodium-substituted hydroxyapatite with structural defects calculated by ab initio methods based on quantum mechanics was much higher than that of hydroxyapatite, suggesting that the sodium-substituted hydroxyapatite was energetically less stable compared with hydroxyapatite. Indeed, sodium-substituted hydroxyapatite exhibited higher dissolution behavior of constituent elements of hydroxyapatite in simulated body fluid (SBF) and Tris-buffered deionized water compared with hydroxyapatite, which directly affected low-crystalline hydroxyl-carbonate apatite forming capacity by increasing the degree of apatite supersaturation in SBF. Actually, sodium-substituted hydroxyapatite exhibited markedly improved low-crystalline hydroxyl-carbonate apatite forming capacity in SBF and noticeably higher osteoconductivity 4 weeks after implantation in calvarial defects of New Zealand white rabbits compared with hydroxyapatite. In addition, there were no statistically significant differences between hydroxyapatite and sodium-substituted hydroxyapatite on cytotoxicity as determined by BCA assay. Taken together, these results indicate that sodium-substituted hydroxyapatite with structural defects has promising potential for use as a bone grafting material due to its enhanced osteoconductivity compared with hydroxyapatite.

  1. 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.

  2. 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.

  3. Synthesis and Characterization of Rutile TiO2Nanopowders Doped with Iron Ions

    PubMed Central

    2009-01-01

    Titanium dioxide nanopowders doped with different amounts of Fe ions were prepared by coprecipitation method. Obtained materials were characterized by structural (XRD), morphological (TEM and SEM), optical (UV/vis reflection and photoluminescence, and Raman), and analytical techniques (XPS and ICP-OES). XRD analysis revealed rutile crystalline phase for doped and undoped titanium dioxide obtained in the same manner. Diameter of the particles was 5–7 nm. The presence of iron ions was confirmed by XPS and ICP-OES. Doping process moved absorption threshold of TiO2into visible spectrum range. Photocatalytic activity was also checked. Doped nanopowders showed normal and up-converted photoluminescence. PMID:20596442

  4. 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

  5. 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.

  6. 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

  7. 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

  8. 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

  9. 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.

  10. Synthesis and Characterization of Hydroxyapatite/Fullerenol Nanocomposites.

    PubMed

    Djordjevic, Aleksandar; Ignjatovic, Nenad; Seke, Mariana; Jovic, Danica; Uskokovic, Dragan; Rakocevic, Zlatko

    2015-02-01

    Fullerenols are polyhydroxylated, water soluble derivatives of fullerene C60, with potential application in medicine as diagnostic agents, antioxidants or nano drug carriers. This paper describes synthesis and physical characterization of a new nanocomposite hydroxyapatite/fullerenol. Surface of the nanocomposite hydroxyapatite/fullerenol is inhomogeneous with the diameter of the particles in the range from 100 nm to 350 nm. The ζ potential of this nanocomposite is ten times lower when compared to hydroxyapatite. Surface phosphate groups of hydroxyapatite are prone to forming hydrogen bonds, when in close contact with hydroxyl groups, which could lead to formation of hydrogen bonds between hydroxyapatite and hydroxyl groups of fullerenol. The surface of hydroxyapatite particles (-2.5 mV) was modified by fullerenol particles, as confirmed by the obtained ζ potential value of the nanocomposite biomaterial hydroxyapatite/fullerenol (-25.0 mV). Keywords: Hydroxyapatite, Fullerenol, Nanocomposite, Surface Analysis.

  11. The Study of Complex (Ti, Zr, Cs) Nanopowder Influencing the Effective Ionization Potential of Arc Discharge When Mma Welding

    NASA Astrophysics Data System (ADS)

    Sapozhkov, S. B.; Burakova, E. M.

    2016-08-01

    Strength is one of the most important characteristics of a weld joint. Mechanical properties of a weld metal can be improved in a variety of ways. One of the possibilities is to add a nanopowder to the weld metal. Authors of the paper suggest changing the production process of MMA welding electrodes via adding nanopowder Ti, Zr, Cs to electrode components through liquid glass. Theoretical research into the nanopowder influence on the effective ionization potential (Ueff) of welding arc discharge is also necessitated. These measures support arcing stability, improve strength of a weld joint, as the consequence, ensure quality enhancing of a weld joint and the structure on the whole.

  12. 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

  13. 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

  14. 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

  15. 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.

  16. 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.

  17. 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.

  18. 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.

  19. Recent advances in research applications of nanophase hydroxyapatite.

    PubMed

    Fox, Kate; Tran, Phong A; Tran, Nhiem

    2012-07-16

    Hydroxyapatite, the main inorganic material in natural bone, has been used widely for orthopaedic applications. Due to size effects and surface phenomena at the nanoscale, nanophase hydroxyapatite possesses unique properties compared to its bulk-phase counterpart. The high surface-to-volume ratio, reactivities, and biomimetic morphologies make nano-hydroxyapatite more favourable in applications such as orthopaedic implant coating or bone substitute filler. Recently, more efforts have been focused on the possibility of combining hydroxyapatite with other drugs and materials for multipurpose applications, such as antimicrobial treatments, osteoporosis treatments and magnetic manipulation. To build more effective nano-hydroxyapatite and composite systems, the particle synthesis processes, chemistry, and toxicity have to be thoroughly investigated. In this Minireview, we report the recent advances in research regarding nano-hydroxyapatite. Synthesis routes and a wide range of applications of hydroxyapatite nanoparticles will be discussed. The Minireview also addresses several challenges concerning the biosafety of the nanoparticles.

  20. 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.

  1. 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

  2. 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

  3. 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

  4. Capacity fade in Sn-C nanopowder anodes due to fracture.

    PubMed

    Aifantis, Katerina E; Huang, Tao; Hackney, Stephen A; Sarakonsri, Thapanee; Yu, Aishui

    2012-01-01

    Sn based anodes allow for high initial capacities, which however cannot be retained due to the severe mechanical damage that occurs during Li-insertion and de-insertion. To better understand the fracture process during electrochemical cycling three different nanopowders comprised of Sn particles attached on artificial graphite, natural graphite or micro-carbon microbeads were examined. Although an initial capacity of 700 mAh g(-1) was obtained for all Sn-C nanopowders, a significant capacity fade took place with continuous electrochemical cycling. The microstructural changes in the electrodes corresponding to the changes in electrochemical behavior were studied by transmission and scanning electron microscopy. The fragmentation of Sn observed by microscopy correlates with the capacity fade, but this fragmentation and capacity fade can be controlled by controlling the initial microstructure. It was found that there is a dependence of the capacity fade on the Sn particle volume and surface area fraction of Sn on carbon.

  5. 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.

  6. 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.

  7. 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

  8. 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.

  9. Formation regularities of AlOOH hollow spheres during aluminum nanopowder water oxidation

    NASA Astrophysics Data System (ADS)

    Lozhkomoev, Aleksandr S.; Glazkova, Elena A.; Svarovskaya, Natalia V.; Bakina, Olga V.; Kazantsev, Sergey O.; Lerner, Marat I.

    2015-10-01

    There described a novel environmentally friendly synthesis route of micro/nanostructured hollow spheres of AlOOH by oxidation of Al nanopowder in pure water under mild processing conditions. The reaction kinetics of the aluminum nanopowder interaction with water was studied using the method of continuous recording of suspension pH and temperature. There observed the change in Al3+ concentration in the reaction medium and the rate of hydrogen release as well as TEM investigations of the intermediate reaction products at different stages of the process were performed. It is shown that AlOOH hollow spheres are formed through the aluminum core dissolution, Al3+ ion diffusion through the surface oxide film and AlOOH nanosheets formation on the surface of the precursor oxide film.

  10. 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

  11. Multiple nano-blast synthesis of PT/8Y-ZP composite nanopowders.

    PubMed

    Vasylkiv, Oleg; Sakka, Yoshio; Skorokhod, Valeriy V

    2006-06-01

    We demonstrate a processing technique based on the synthesis of ceramic nanopowders and simultaneous impregnation with metallic nanoparticles by multiple 'nano-blasts' of embeded cyclotrimethylene trinitramine in preliminary engineered multi-component nano-reactors. 'Nano-blasts' of impregnated cyclotrimethylene trinitramine deagglomerate the nanopowder due to the high energetic impacts of the blast waves, while the decomposition of compounds and their solid-solubility is enhanced by the extremely high local temperature generated during the nano-explosions. We applied this technique to produce nanosized agglomerate-free 8 mol% yttria-doped cubic zirconia aggregates with an average size of 53 nm impregnated with 10 mass% of platinum particles of 2-14 nm. PMID:17025061

  12. 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.

  13. Continuous microwave flow synthesis of mesoporous hydroxyapatite.

    PubMed

    Akram, Muhammad; Alshemary, Ammar Z; Goh, Yi-Fan; Wan Ibrahim, Wan Aini; Lintang, Hendrik O; Hussain, Rafaqat

    2015-11-01

    We have successfully used continuous microwave flow synthesis (CMFS) technique for the template free synthesis of mesoporous hydroxyapatite. The continuous microwave flow reactor consisted of a modified 2.45GHz household microwave, peristaltic pumps and a Teflon coil. This cost effective and efficient system was exploited to produce semi-crystalline phase pure nano-sized hydroxyapatite. Effect of microwave power, retention time and the concentration of reactants on the phase purity, degree of crystallinity and surface area of the final product was studied in detail. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) were used to study the phase purity and composition of the product, while transmission electron microscopy (TEM) was used to study the effect of process parameters on the morphology of hydroxyapatite. The TEM analysis confirmed the formation of spherical particles at low microwave power; however the morphology of the particles changed to mesoporous needle and rod-like structure upon exposing the reaction mixture to higher microwave power and longer retention time inside the microwave. The in-vitro ion dissolution behavior of the as synthesized hydroxyapatite was studied by determining the amount of Ca(2+) ion released in SBF solution.

  14. Continuous microwave flow synthesis of mesoporous hydroxyapatite.

    PubMed

    Akram, Muhammad; Alshemary, Ammar Z; Goh, Yi-Fan; Wan Ibrahim, Wan Aini; Lintang, Hendrik O; Hussain, Rafaqat

    2015-11-01

    We have successfully used continuous microwave flow synthesis (CMFS) technique for the template free synthesis of mesoporous hydroxyapatite. The continuous microwave flow reactor consisted of a modified 2.45GHz household microwave, peristaltic pumps and a Teflon coil. This cost effective and efficient system was exploited to produce semi-crystalline phase pure nano-sized hydroxyapatite. Effect of microwave power, retention time and the concentration of reactants on the phase purity, degree of crystallinity and surface area of the final product was studied in detail. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) were used to study the phase purity and composition of the product, while transmission electron microscopy (TEM) was used to study the effect of process parameters on the morphology of hydroxyapatite. The TEM analysis confirmed the formation of spherical particles at low microwave power; however the morphology of the particles changed to mesoporous needle and rod-like structure upon exposing the reaction mixture to higher microwave power and longer retention time inside the microwave. The in-vitro ion dissolution behavior of the as synthesized hydroxyapatite was studied by determining the amount of Ca(2+) ion released in SBF solution. PMID:26249601

  15. 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.

  16. 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.

  17. Synthesis of nanopowders with a help of powerful CO2 laser

    NASA Astrophysics Data System (ADS)

    Osipov, V. V.; Lisenkov, V. V.; Platonov, V. V.

    2011-02-01

    The paper reports about the results of researches of nanopowder production with a help powerful repetitively pulsed CO2 laser "LAERT" which generated radiation with pulse energy of ~1 J, peak power of ~8 kW and mean power of 500 W. Laser radiation affected and evaporated the target. The target material vapor condensed into nanoparticles as a result of intermixing vapor with a flow of cold gas. In basic the air of atmospheric pressure was used as the carrier gas. However in some experiments were used He and Ar and the gas pressure also was changed. In our experiments we produced nanopowders of such materials as: YSZ, YSZ:Al2O3, Al2O3, CeO2:Gd2O3, 0.5%Nd:Y2O3, 1%Nd:YAG, Fe3O4and carbon with a middle size 10÷30 nm. Received nanopowders were also weakly agglomerated. We carried out 3D numerical modeling of thermo-hydrodynamic processes occurred during the laser evaporation of a target. Results of calculations have cleared up many details of target evaporation. In particular, influence of liquid melt movement on stoichiometry of evaporation of a target from oxide mixes is found out. Results of calculations are in a good agreement with experimental data.

  18. Solar physical vapor deposition: A new approach for preparing magnesium titanate nanopowders

    NASA Astrophysics Data System (ADS)

    Apostol, Irina; Saravanan, K. Venkata; Monty, Claude J. A.; Vilarinho, Paula M.

    2013-11-01

    Solar energy is a major factor in the equation of energy, because of the unlimited potential of the sun that eclipses all other renewable sources of energy. Solar physical vapor deposition (SPVD) is a core innovative, original and environmentally friendly process to prepare nanocrystalline materials in a powder form. The principle of this process is to melt the material under concentrated solar radiation, which evaporates and condenses as nanopowders on a cold surface. We synthesized nanopowders of magnesium titanate by the SPVD process at PROMES Laboratory in Odeillo-Font Romeu, France. The SPVD system consists of a parabolic mirror concentrator, a mobile plane mirror ("heliostat") tracking the sun and a solar reactor "heliotron". The synthesized nanopowders were analyzed by X-ray diffraction (XRD) to know their crystalline structure and scanning electron microscopy (SEM) was used for determining the surface morphology. We have shown that the characteristics of obtained nanotitanates were determined by the targets' composition and SPVD process parameters such as the working pressure inside the solar reactor and evaporation duration (process time).

  19. 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.

  20. [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.

  1. [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

  2. 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.

  3. 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.

  4. 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

  5. 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.

  6. Poly(ε-caprolactone)/nano fluoridated hydroxyapatite scaffolds for bone tissue engineering: in vitro degradation and biocompatibility study.

    PubMed

    Johari, N; Fathi, M H; Golozar, M A; Erfani, E; Samadikuchaksaraei, A

    2012-03-01

    In this study, biodegradation and biocompatibility of novel poly(ε-caparolactone)/nano fluoridated hydroxyapatite (PCL-FHA) scaffolds were investigated. The FHA nanopowders were prepared via mechanical alloying method and had a chemical composition of Ca(10)(PO(4))(6)OH(2-x )F(x) (where x values were selected equal to 0.5 and 2.0). In order to fabricate PCL-FHA scaffolds, 10, 20, 30 and 40 wt% of the FHA were added to the PCL. The PCL-FHA scaffolds were produced by the solvent casting/particulate leaching using sodium chloride particles (with diameters of 300-500 μm) as the porogen. The phase structure, microstructure and morphology of the scaffolds were evaluated using X-ray diffraction, Fourier transform infrared spectroscopy and scanning electron microscopy techniques. Porosity of the scaffolds was measured using the Archimedes' Principle. In vitro degradation of PCL-FHA scaffolds was studied by incubating the samples in phosphate buffered saline at 37°C and pH 7.4 for 30 days. Moreover, biocompatibility was evaluated by MTT assay after seeding and culture of osteoblast-like cells on the scaffolds. Results showed that the osteoblast-like cells attached to and proliferated on PCL-FHA and increasing the porosity of the scaffolds increased the cell viability. Also, degradation rate of scaffolds were increased with increasing the fluorine content in scaffolds composition. PMID:22190197

  7. Microstrain in hydroxyapatite carbon nanotube composites.

    PubMed

    Kealley, Catherine; Elcombe, Margaret; van Riessen, Arie

    2008-01-01

    Synchrotron radiation diffraction data were collected from hydroxyapatite-carbon nanotube bioceramic composites to determine the crystallite size and to measure changes in non-uniform strain. Estimates of crystallite size and strain were determined by line-profile fitting of discrete peaks and these were compared with a Rietveld whole-pattern analysis. Overall the two analysis methods produced very similar numbers. In the commercial hydroxyapatite material, one reflection in particular, (0 2 3), has higher crystallite size and lower strain values in comparison with laboratory-synthesized material. This could indicate preferential crystal growth in the [0 2 3] direction in the commercial material. From the measured strains in the pure material and the composite, there was a degree of bonding between the matrix and strengthening fibres. However, increasing the amount of carbon nanotubes in the composite has increased the strain in the material, which is undesirable for biomedical implant applications.

  8. 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.

  9. 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

  10. 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.

  11. Space-cutting model of hydroxyapatite.

    PubMed

    Okazaki, M; Sato, M; Takahashi, J

    1995-01-01

    The possibility of substitution of trace elements such as Mg2+, Sr2+ and Ba2+ into the columnar Ca2+ positions of hydroxyapatite was examined by computer graphics with a personal computer and a space-cutting method. Data on the structural coordinates of the hydroxyapatite were put into a protein graphics program in Angstrom units. The connection of each element, with front and rear, was displayed by the shade-line erasing method, and the solidity of the image was expressed by the degree of lightness from the light source. The space-cutting model was obtained by selecting the cutting plane with three atoms in the crystal. Rotating the graphics freely around the X, Y and Z axes gives a view from any direction. The computer graphics suggested visually how the lattice dimensions expand with Sr2+ and Ba2+ substitution and contract with Mg2+ substitution.

  12. 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.

  13. 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

  14. The hydroxyapatite orbital implant: a prospective study.

    PubMed

    Ashworth, J L; Rhatigan, M; Sampath, R; Brammar, R; Sunderland, S; Leatherbarrow, B

    1996-01-01

    The hydroxyapatite orbital implant was first released for use as an orbital implant in humans in August 1989. It has been shown to be well tolerated, providing good motility of the artificial eye with a low complication rate when used as a primary implant. This prospective study evaluated the hydroxyapatite orbital implant used as both a primary and a secondary implant. Sixty patients were implanted between October 1992 and November 1994, 28 being implanted as a primary procedure at the time of enucleation or evisceration, and 32 as a secondary procedure. Seven patients underwent second-stage drilling and pegging of the implant. The mean follow-up time was 13 months (range 2-26 months). A standardised operative and post-operative protocol was followed. The patients were evaluated post-operatively for the amount of enophthalmos, degree of upper lid sulcus deformity, motility of the prosthesis, location of the implant in the socket, socket status and the presence or absence of discharge, position of the drill hole and coverage of the implant. Complications and their management were documented. Both patient and surgeon made a subjective assessment of cosmesis and the patient's satisfaction with the overall result was noted. The results of this study show the hydroxyapatite orbital implant to provide excellent motility of the artificial eye and good cosmesis with a low rate of complications when used both as a primary and as a secondary implant.

  15. Synthesis, properties and host effects of rare-earth doped silica nanopowders for photonic applications

    NASA Astrophysics Data System (ADS)

    Halpern, Susan B.

    In this study, SiO2/Al2O3/Er2O 3 (SAE) nanopowders were fabricated by the CF-CVC technique with average primary particle sizes ranging from 10--30 nm. Fluorescence and lifetime measurements were made both on as-prepared powders, as well as heat treated powders, with the latter exhibiting significantly higher emission intensities. At ˜1000°C, the SAE became partially devitrified with extremely broad (FWHM ≈ 78 nm) and flat emission spectra, which is highly desirable for Wavelength Division Multiplexing (WDM) in optical amplifiers. The unique optical properties of the powders are attributed to the formation of a metastable phase consisting of an uniform nano-scale dispersion of a metastable intermediate SiO2 (Al,Er)2O3 phase in an amorphous SiO 2 matrix. At higher heat treatments (1400°C), a dual-phase equilibrium structure was formed, consisting of a pyrochlore phase in a crystobalite matrix. The SAE nanopowders were incorporated into various optical hybrid glass hosts for active planar waveguide applications. Host selection was dependent on transparency in the wavelength region of interest (900 nm--1600 nm), index matching (n ˜ 1.5), chemical/thermal stability, and ease of processing. Furthermore, the inorganic-organic glasses were hydrophobic, resulting in a minimal level of residual OH- which can quench fluorescence emission. Four separate groups of host materials were studied: Perfluoro-alkyl Hybrid Glass (n ≈ 1.42), Alumina-Silica Hybrid Glass (n ≈ 1.49), Polyurethane-Silica Hybrid Glass (n ≈ 1.44), and Methyl/Epoxy Group Hybrid Glass (n ≈ 1.48). All hosts showed high spectral transparency, uniform dispersion of the nanopowder in the host, and minimal surface quenching of emission, and therefore represent excellent candidates for fabrication of next generation nanophotonic planar devices.

  16. Preparation and properties of Ba1-xCaxTiO3 nanopowders obtained by mechanochemical synthesis

    NASA Astrophysics Data System (ADS)

    Szafraniak-Wiza, Izabela; Kozielski, Lucjan; Sebastian, Tutu

    2016-08-01

    The calcium-substituted barium titanate nanopowders Ba1-xCaxTiO3 (0.2 ≤ x ≤ 0.3) have been obtained at room temperature by mechanochemical synthesis. The formation of the perovskite phase was controlled by X-ray diffraction studies at various milling duration. The powders possess the perovskite crystallographic structure directly after milling longer than 10 h. The dielectric properties of the ceramics obtained by sintering of the nanopowders were investigated in the temperature range between 300 and 500 K. The temperature dependence of permittivity exhibited a single anomaly, which corresponds to the ferroelectric-paraelectric phase transition.

  17. The effect of annealing on properties of europium doped ZnO nanopowders obtained by a microwave hydrothermal method

    NASA Astrophysics Data System (ADS)

    Wolska-Kornio, E.; Kaszewski, J.; Witkowski, B. S.; Wachnicki, Ł.; Godlewski, M.

    2016-09-01

    Europium doped ZnO nanopowders made by microwave hydrothermal method are investigated. As zinc oxide precursor zinc nitrate(V) hexahydrate (Zn(NO3)2·6H2O) was used. Two types of nanopowder samples are examined: as grown and annealed at 750 °C in air atmosphere. We investigate the structural, morphological and optical prosperities of europium doped ZnO. Results of scanning electron microscopy, X-ray diffraction, photo- and cathodoluminescence investigations and also CIE1961 chromaticity diagram are presented.

  18. A new technique for introducing chromium dopant into a phosphor synthesized from alumina nanopowder

    NASA Astrophysics Data System (ADS)

    Zvonarev, S. V.; Kortov, V. S.; Chikin, A. V.; Sannikov, P. P.

    2016-09-01

    A technique of doping a phosphor synthesized from an alumina nanopowder with chromium was developed and tested. Doping was performed through dipping Al2O3 host-matrix into the chromium nitrate solution with varying time and number of impregnation cycles. The following annealing in vacuum at 1500 °C for 3 hours resulted in the formation of Cr3+ luminescent centers which replaced Al atoms in the lattice sites. The results were verified by measuring photo- and cathode luminescence spectra. Concentration dependences were found at various impregnation parameters.

  19. Combustion synthesis and optical properties of ceria doped gadolinium-oxide nanopowder

    NASA Astrophysics Data System (ADS)

    Tamrakar, Raunak Kumar; Bisen, D. P.

    2013-06-01

    The Ceria doped Gadolinium (Gd2O3) nanopowder was synthesized by combustion synthesis by using urea as a fuel. The combustion synthesis method which is reported here is advantageous from the perspectives of small size of the nanoparticle. The structural and photoluminescence (PL) property of sample was studies. Gd2O3:Ce3+ nanoparticles exhibit green emission around 543 nm. The result of XRD show that synthesized sample has cubic structure. The average size of particle is found to be 45 nm. The surface morphology of the films is also presented.

  20. 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.

  1. 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

  2. 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.

  3. Bone remodeling and hydroxyapatite resorption in coated primary hip prostheses.

    PubMed

    Tonino, Alphons J; van der Wal, Bart C H; Heyligers, Ide C; Grimm, Bernd

    2009-02-01

    Hydroxyapatite coatings for THA promote bone ongrowth, but bone and coating are exposed to stress shielding-driven osteoclastic resorption. We asked: (1) if the resorption of hydroxyapatite coating and bone ongrowth correlated with demographics; (2) if the resorption related to the stem level; and (3) what happens to the implant-bone interface when all hydroxyapatite coating is resorbed? We recovered 13 femoral components from cadaveric specimens 3.3 to 11.2 years after uneventful primary THA. Three cross sections (proximal, medial, distal) of the hydroxyapatite-coated proximal implant sleeve were analyzed by measuring the percentage of residual hydroxyapatite and bone ongrowth on the implant perimeter. Hydroxyapatite resorption was independent of patient age but increased with time in vivo and mostly was gone after 8 years. Bone ongrowth was independent of time in vivo but decreased with aging patients. Only in the most proximal section did less residual hydroxyapatite correlate with less bone ongrowth. Hydroxyapatite resorption, which was more proximal than distal, showed no adverse effects on the implant-bone interface.

  4. 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.

  5. 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.

  6. 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.

  7. 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

  8. 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.

  9. 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.

  10. 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.

  11. 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

  12. 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.

  13. Bulk synthesis of monodisperse magnetic FeNi3 nanopowders by flow levitation method.

    PubMed

    Chen, Shanjun; Chen, Yan; Kang, Xiaoli; Li, Song; Tian, Yonghong; Wu, Weidong; Tang, Yongjian

    2013-10-01

    In this work, a novel bulk synthesis method for monodisperse FeNi3 nanoparticles was developed by flow levitation method (FL). The Fe and Ni vapours ascending from the high temperature levitated droplet was condensed by cryogenic Ar gas under atmospheric pressure. X-ray diffraction was used to identify and characterize the crystal phase of prepared powders exhibiting a FeNi3 phase. The morphology and size of nanopowders were observed by transmission electron microscopy (TEM). The chemical composition of the nanoparticles was determined with energy dispersive spectrometer (EDS). The results indicated that the FeNi3 permalloy powders are nearly spherical-shaped with diameter about 50-200 nm. Measurement of the magnetic property of nanopowders by a superconducting quantum interference device (SQUID, Quantum Design MPMS-7) showed a symmetric hysteresis loop of ferromagnetic behavior with coercivity of 220 Oe and saturation magnetization of 107.17 emu/g, at 293 K. At 5 K, the obtained saturation magnetization of the sample was 102.16 emu/g. The production rate of FeNi3 nanoparticles was estimated to be about 6 g/h. This method has great potential in mass production of FeNi3 nannoparticles. PMID:24245162

  14. 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

  15. Ablation of oxide materials and production of nanopowders by ytterbium fiber laser

    NASA Astrophysics Data System (ADS)

    Osipov, Vladimir V.; Lisenkov, Vasily V.; Platonov, Vladislav V.

    2015-03-01

    In this paper, laser radiation action on Nd3+:Y2O3 targets having the absorption 13-1.7 × 103 cm-1 is studied. During the experiment, we used the ytterbium fiber laser, which can operate both in continuous and pulse mode with the pulse duration time 0.1-1.9 ms. Laser radiation power was 200-700 W, and power density was (0.2-1.2) × 106 W/cm2. We found out the spike behavior of laser plume luminescence, large statistical variability of delay time of laser plume appearance, and spallation of front surface of the target. Aiming to explain these facts, we developed the numeric model of radiation impact on substance with non-uniform absorption coefficient. We found out the optimal laser oblation mode for nanopowder production. At laser power of 700 W, we received Nd3+:Y2O3 nanopowder with productivity up to 27 g/h. Average size of nanoparticles is 13.6 nm, and their phase is monoclinic.

  16. Low temperature synthesis of pure cubic ZrO2 nanopowder: structural and luminescence studies.

    PubMed

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

    2014-03-25

    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.

  17. 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.

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

    NASA Astrophysics Data System (ADS)

    Żyła, Gaweł; Cholewa, Marian; Witek, Adam

    2012-07-01

    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.

  19. 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.

  20. Low temperature synthesis of pure cubic ZrO2 nanopowder: structural and luminescence studies.

    PubMed

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

    2014-03-25

    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. PMID:24317256

  1. Microstructure and composition of biosynthetically synthesised hydroxyapatite.

    PubMed

    Medina Ledo, Hilda; Thackray, Ania C; Jones, Ian P; Marquis, Peter M; Macaskie, Lynne E; Sammons, Rachel L

    2008-11-01

    Biosynthetic hydroxyapatite (HA) manufactured utilising the bacterium Serratia sp. NCIMB40259 was characterised using X-ray diffraction (XRD), Fourier transform infra-red spectroscopy (FTIR), energy dispersive X-ray analysis (EDX) scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electron diffraction (ED). SEM/EDX showed that the non-sintered material consisted mainly of calcium-deficient HA (CDHA) with a Ca/P ratio of 1.61 +/- 0.06 and crystal size (from TEM) of 50 +/- 10 nm. ED analysis of non-sintered powder showed resolvable ring patterns ascribed to (0002), (1122) and (0006) planes of crystalline HA. The crystallinity of the samples improved with heat treatment from approximately 9.4% (non-sintered) to 53% (1,200 degrees C). Samples heated at 600 degrees C and sintered at 1,200 degrees C were identified by XRD and FTIR as mainly CDHA with some sodium calcium phosphate in the sintered samples. Ca/P ratios (SEM/EDX) were 1.62 and 1.52, respectively. Single crystal spot patterns characteristic of HA were seen with commercial HA and Serratia HA heated at 600 degrees C. After sintering at 1,200 degrees C the material consisted of needle-like crystals with a length between 86 and 323 nm (from TEM) or 54-111 nm (from XRD) and lattice parameters of a = 9.441 A and c = 6.875 A. This study indicated that the material produced by Serratia bacteria was initially mainly nanophase calcium deficient hydroxyapatite, which sintered to a more highly crystalline form. With further refinements the method could be used as an inexpensive route for hydroxyapatite production for biomaterials applications.

  2. Thermal effect on thermoluminescence response of hydroxyapatite.

    PubMed

    Zarate-Medina, J; Sandoval-Cedeño, K J; Barrera-Villatoro, A; Lemus-Ruiz, J; Rivera Montalvo, T

    2015-06-01

    This paper presents the experimental results of the thermoluminescence (TL) induced by gamma radiation in synthetic hydroxyapatite (HAp) obtained by the precipitation method, using Ca(NO3)2·4H2O and (NH4)2HPO4 and calcined at different temperatures. The structural and morphological characterization was carried out by X-ray diffraction (XRD) and scanning electron microscopy (SEM) techniques. TL response as a function of gamma radiation dose was in a wide range, where intensity was enhanced in the sample annealed at 900°C, which tricalcium diphosphate (TCP) phase appear. Fading of the TL was also studied.

  3. 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.

  4. Surface properties of calcium and magnesium oxide nanopowders grafted with unsaturated carboxylic acids studied with inverse gas chromatography.

    PubMed

    Maciejewska, Magdalena; Krzywania-Kaliszewska, Alicja; Zaborski, Marian

    2012-09-28

    Inverse gas chromatography (IGC) was applied at infinite dilution to evaluate the surface properties of calcium and magnesium oxide nanoparticles and the effect of surface grafted unsaturated carboxylic acid on the nanopowder donor-acceptor characteristics. The dispersive components (γ(s)(D)) of the free energy of the nanopowders were determined by Gray's method, whereas their tendency to undergo specific interactions was estimated based on the electron donor-acceptor approach presented by Papirer. The calcium and magnesium oxide nanoparticles exhibited high surface energies (79 mJ/m² and 74 mJ/m², respectively). Modification of nanopowders with unsaturated carboxylic acids decreased their specific adsorption energy. The lowest value of γ(s)(D) was determined for nanopowders grafted with undecylenic acid, approximately 55 mJ/m². The specific interactions were characterised by the molar free energy (ΔG(A)(SP)) and molar enthalpy (ΔH(A)(SP)) of adsorption as well as the donor and acceptor interaction parameters (K(A), K(D)). PMID:22907042

  5. 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.

  6. Effect of Nb doping on structural, optical and photocatalytic properties of flame-made TiO2 nanopowder.

    PubMed

    Michalow, Katarzyna A; Flak, Dorota; Heel, Andre; Parlinska-Wojtan, Magdalena; Rekas, Mieczyslaw; Graule, Thomas

    2012-11-01

    TiO(2):Nb nanopowders within a dopant concentration in the range of 0.1-15 at.% were prepared by one-step flame spray synthesis. Effect of niobium doping on structural, optical and photocatalytic properties of titanium dioxide nanopowders was studied. Morphology and structure were investigated by means of Brunauer-Emmett-Teller isotherm, X-ray diffraction and transmission electron microscopy. Diffuse reflectance and the resulting band gap energy were determined by diffuse reflectance spectroscopy. Photocatalytic activity of the investigated nanopowders was revised for the photodecomposition of methylene blue (MB), methyl orange (MO) and 4-chlorophenol under UVA and VIS light irradiation. Commercial TiO(2)-P25 nanopowder was used as a reference. The specific surface area of the powders was ranging from 42.9 m(2)/g for TiO(2):0.1 at.% Nb to 90.0 m(2)/g for TiO(2):15 at.% Nb. TiO(2):Nb particles were nanosized, spherically shaped and polycrystalline. Anatase was the predominant phase in all samples. The anatase-related transition was at 3.31 eV and rutile-related one at 3.14 eV. TiO(2):Nb nanopowders exhibited additional absorption in the visible range. In comparison to TiO(2)-P25, improved photocatalytic activity of TiO(2):Nb was observed for the degradation of MB and MO under both UVA and VIS irradiation, where low doping level (Nb < 1 at.%) was the most effective. Niobium doping affected structural, optical and photocatalytic properties of TiO(2). Low dopant level enhanced photocatalytic performance under UVA and VIS irradiation. Therefore, TiO(2):Nb (Nb < 1 at.%) can be proposed as an efficient selective solar light photocatalyst. PMID:23054731

  7. Hydroxyapatite surface-induced peptide folding.

    PubMed

    Capriotti, Lisa A; Beebe, Thomas P; Schneider, Joel P

    2007-04-25

    Herein, we describe the design and surface-binding characterization of a de novo designed peptide, JAK1, which undergoes surface-induced folding at the hydroxyapatite (HA)-solution interface. JAK1 is designed to be unstructured in buffered saline solution, yet undergo HA-induced folding that is largely governed by the periodic positioning of gamma-carboxyglutamic acid (Gla) residues within the primary sequence of the peptide. Circular dichroism (CD) spectroscopy and analytical ultracentrifugation indicate that the peptide remains unfolded and monomeric in solution under normal physiological conditions; however, CD spectroscopy indicates that in the presence of hydroxyapatite, the peptide avidly binds to the mineral surface adopting a helical structure. Adsorption isotherms indicate nearly quantitative surface coverage and Kd = 310 nM for the peptide-surface binding event. X-ray photoelectron spectroscopy (XPS) coupled with the adsorption isotherm data suggests that JAK1 binds to HA, forming a self-limiting monolayer. This study demonstrates the feasibility of using HA surfaces to trigger the intramolecular folding of designed peptides and represents the initial stages of defining the design rules that allow HA-induced peptide folding.

  8. Inflammatory response to nano- and microstructured hydroxyapatite.

    PubMed

    Mestres, Gemma; Espanol, Montserrat; Xia, Wei; Persson, Cecilia; Ginebra, Maria-Pau; Ott, Marjam Karlsson

    2015-01-01

    The proliferation and activation of leukocytes upon contact with a biomaterial play a crucial role in the degree of inflammatory response, which may then determine the clinical failure or success of an implanted biomaterial. The aim of this study was to evaluate whether nano- and microstructured biomimetic hydroxyapatite substrates can influence the growth and activation of macrophage-like cells. Hydroxyapatite substrates with different crystal morphologies consisting of an entangled network of plate-like and needle-like crystals were evaluated. Macrophage proliferation was evaluated on the material surface (direct contact) and also in extracts i.e. media modified by the material (indirect contact). Additionally, the effect of supplementing the extracts with calcium ions and/or proteins was investigated. Macrophage activation on the substrates was evaluated by quantifying the release of reactive oxygen species and by morphological observations. The results showed that differences in the substrate's microstructure play a major role in the activation of macrophages as there was a higher release of reactive oxygen species after culturing the macrophages on plate-like crystals substrates compared to the almost non-existent release on needle-like substrates. However, the difference in macrophage proliferation was ascribed to different ionic exchanges and protein adsorption/retention from the substrates rather than to the texture of materials.

  9. Nano hydroxyapatite structures influence early bone formation.

    PubMed

    Meirelles, Luiz; Arvidsson, Anna; Andersson, Martin; Kjellin, Per; Albrektsson, Tomas; Wennerberg, Ann

    2008-11-01

    In a study model that aims to evaluate the effect of nanotopography on bone formation, micrometer structures known to alter bone formation, should be removed. Electropolished titanium implants were prepared to obtain a surface topography in the absence of micro structures, thereafter the implants were divided in two groups. The test group was modified with nanosize hydroxyapatite particles; the other group was left uncoated and served as control for the experiment. Topographical evaluation demonstrated increased nanoroughness parameters for the nano-HA implant and higher surface porosity compared to the control implant. The detected features had increased size and diameter equivalent to the nano-HA crystals present in the solution and the relative frequency of the feature size and diameter was very similar. Furthermore, feature density per microm(2) showed a decrease of 13.5% on the nano-HA implant. Chemical characterization revealed calcium and phosphorous ions on the modified implants, whereas the control implants consisted of pure titanium oxide. Histological evaluation demonstrated significantly increased bone formation to the coated (p < 0.05) compared to uncoated implants after 4 weeks of healing. These findings indicate for the first time that early bone formation is dependent on the nanosize hydroxyapatite features, but we are unaware if we see an isolated effect of the chemistry or of the nanotopography or a combination of both.

  10. Hydroxyapatite surface-induced peptide folding.

    PubMed

    Capriotti, Lisa A; Beebe, Thomas P; Schneider, Joel P

    2007-04-25

    Herein, we describe the design and surface-binding characterization of a de novo designed peptide, JAK1, which undergoes surface-induced folding at the hydroxyapatite (HA)-solution interface. JAK1 is designed to be unstructured in buffered saline solution, yet undergo HA-induced folding that is largely governed by the periodic positioning of gamma-carboxyglutamic acid (Gla) residues within the primary sequence of the peptide. Circular dichroism (CD) spectroscopy and analytical ultracentrifugation indicate that the peptide remains unfolded and monomeric in solution under normal physiological conditions; however, CD spectroscopy indicates that in the presence of hydroxyapatite, the peptide avidly binds to the mineral surface adopting a helical structure. Adsorption isotherms indicate nearly quantitative surface coverage and Kd = 310 nM for the peptide-surface binding event. X-ray photoelectron spectroscopy (XPS) coupled with the adsorption isotherm data suggests that JAK1 binds to HA, forming a self-limiting monolayer. This study demonstrates the feasibility of using HA surfaces to trigger the intramolecular folding of designed peptides and represents the initial stages of defining the design rules that allow HA-induced peptide folding. PMID:17397165

  11. 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

  12. 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.

  13. 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

  14. Direct formation of nanophase hydroxyapatite on cathodically polarized electrodes.

    PubMed

    Shirkhanzadeh, M

    1998-02-01

    Ultrafine-grained, nanophase coatings of hydroxyapatite were synthesized by electrocrystallization from dilute electrolytes ([Ca]=6.1 x 10-4 M, [phosphate]=3.6 x 10-4 M) at pH values comparable with the biological pH. At these comparatively low supersaturations, hydroxyapatite is shown to be precipitated without the formation of a precursor phase. A description of the sequence of events occurring at the electrode-electrolyte interface is given to explain the mechanism involved in the direct formation of nanophase hydroxyapatite on polarized electrodes.

  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. Structural studies of magnesium doped hydroxyapatite coatings after osteoblast culture

    NASA Astrophysics Data System (ADS)

    Mróz, W.; Bombalska, A.; Burdyńska, S.; Jedyński, M.; Prokopiuk, A.; Budner, B.; Ślósarczyk, A.; Zima, A.; Menaszek, E.; Ścisłowska-Czarnecka, A.; Niedzielski, K.

    2010-08-01

    Hydroxyapatite and magnesium modified hydroxyapatite were deposited on nitrited Ti6Al4V substrates by use of pulsed laser deposition technique. Three target materials consisting of non-modified and magnesium modified hydroxyapatite with Mg content of 0.6 wt.% and 1.8 wt.% were ablated using an ArF excimer laser. The obtained coatings were analyzed using X-ray diffraction, FTIR and AFM methods in order to determine the influence of magnesium on their phase and chemical composition, crystallinity, surface morphology and biological properties. Doping with low concentration of Mg does not significantly influence the HA morphology but improves osteoblast adhesion as compared to pure HA.

  17. Cytotoxicity of hydroxyapatite, fluorapatite and fluor-hydroxyapatite: a comparative in vitro study.

    PubMed

    Theiszova, M; Jantova, S; Letasiova, S; Palou, M; Cipak, L

    2008-01-01

    The purpose of this study was to evaluate the cytotoxicity of two formulations of hydroxyapatite (HA), namely fluorapatite (FA) and fluor-hydroxyapatite (FHA). HA is used as carrier material for antibiotics or anticancer drugs during treatment of bone metastasis. Negative control, represented by HA, was included for comparative purposes. Leukemia cells were used as a model cell line, and the effect of eluates of tested biomaterials on cell proliferation/viability and mechanism of antiproliferative activity were assessed. Study design attempted to reveal the toxicity of tested biomaterials with an emphasis to decide if tested biomaterials have promise for further studies in vivo. Results showed that eluates of FA and FHA inhibit the growth of leukemia cells and induce programmed cell death through mitochondrial/caspase-9/caspase-3-dependent pathway. Due to these differences compare to HA, it is concluded that FA and FHA have promise for evaluation of their behaviour in vivo.

  18. 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.

  19. 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

  20. 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

  1. 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.

  2. 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...

  3. 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.

  4. 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.

  5. 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.

  6. 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

  7. 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

  8. 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.

  9. 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

  10. 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.

  11. 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.

  12. 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.

  13. Nanophase hydroxyapatite as a biomaterial in advanced hard tissue engineering: a review.

    PubMed

    Zakaria, Siti Maisurah; Sharif Zein, Sharif Hussein; Othman, Mohd Roslee; Yang, Fang; Jansen, John A

    2013-10-01

    Hydroxyapatite is a biocompatible material that is extensively used in the replacement and regeneration of bone material. In nature, nanostructured hydroxyapatite is the main component present in hard body tissues. Hence, the state of the art in nanotechnology can be exploited to synthesize nanophase hydroxyapatite that has similar properties with natural hydroxyapatite. Sustainable methods to mass-produce synthetic hydroxyapatite nanoparticles are being developed to meet the increasing demand for these materials and to further develop the progress made in hard tissue regeneration, especially for orthopedic and dental applications. This article reviews the current developments in nanophase hydroxyapatite through various manufacturing techniques and modifications.

  14. 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.

  15. 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.

  16. Improvement of the stability of hydroxyapatite through glass ceramic reinforcement.

    PubMed

    Ha, Na Ra; Yang, Zheng Xun; Hwang, Kyu Hong; Kim, Tae Suk; Lee, Jong Kook

    2010-05-01

    Hydroxyapatite has achieved significant application in orthopedic and dental implants due to its excellent biocompatibility. Sintered hydroxyapatites showed significant dissolution, however, after their immersion in water or simulated body fluid (SBF). This grain boundary dissolution, even in pure hydroxyapatites, resulted in grain separation at the surfaces, and finally, in fracture. In this study, hydroxyapatite ceramics containing apatite-wollastonite (AW) or calcium silicate (SG) glass ceramics as additives were prepared to prevent the dissolution. AW and SG glass ceramics were added at 0-7 wt% and powder-compacted uniaxially followed by firing at moisture conditions. The glass phase was incorporated into the hydroxyapatite to act as a sintering aid, followed by crystallization, to improve the mechanical properties without reducing the biocompatibility. As seen in the results of the dissolution test, a significant amount of damage was reduced even after more than 14 days. TEM and SEM showed no decomposition of HA to the secondary phase, and the fracture toughness increased, becoming even higher than that of the commercial hydroxyapatite.

  17. 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.

  18. Novel hydroxyapatite biomaterial covalently linked to raloxifene.

    PubMed

    Meme, L; Santarelli, A; Marzo, G; Emanuelli, M; Nocini, P F; Bertossi, D; Putignano, A; Dioguardi, M; Lo Muzio, L; Bambini, F

    2014-01-01

    Since raloxifene, a drug used in osteoporosis therapy, inhibits osteoclast, but not osteoblast functions, it has been suggested to improve recovery during implant surgery. The present paper describes an effective method to link raloxifene, through a covalent bond, to a nano-Hydroxyapatite-based biomaterial by interfacing with (3-aminopropyl)-Triethoxysilane as assessed by Infra Red-Fourier Transformed (IR-FT) spectroscopy and Scanning Electron Microscope (SEM). To evaluate the safety of this modified new material, the vitality of osteoblast-like cells cultured with the new biomaterial was then investigated. Raloxifene-conjugated HAbiomaterial has been shown to be a safe material easy to obtain which could be an interesting starting point for the use of a new functional biomaterial suitable in bone regeneration procedures. PMID:25280036

  19. [Diffusion bonding of hydroxyapatite ceramics and biometals].

    PubMed

    Yamane, F

    1990-03-01

    To improve the mechanical characteristics of hydroxyapatite (HAP) ceramics, a metal-ceramic composite formed by a solid state direct diffusion bonding system was studied. The joining treatment was carried out of a high vacuum and high temperature, for the bioactive ceramics (HAP) and the following biometals; platinum, gold-platinum alloy, titanium and titanium alloys, zirconium, niobium and aluminium alloy. The effects of the variations of thermal expansion mismatch and the interactive reactions at the interface were investigated by fractographic observation (SEM), X-ray diffraction method and EPMA analysis. On some of these joining combinations, the bonding strength had the same bonding strength as the adhesive materials. The results of interface observations showed that the bonding strength is affected by the interface reactions and the diffusion phenomena. PMID:2135505

  20. 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

  1. Electrophoretic deposition of porous hydroxyapatite scaffold.

    PubMed

    Ma, J; Wang, C; Peng, K W

    2003-09-01

    Bioactive porous hydroxyapatite (HA) scaffold was fabricated using electrophoretic deposition (EPD) technique in the present work. Bulk HA scaffold was achieved by repeated deposition. The green scaffold was sintered at 1200 degrees C to 82% of the theoretical density. Scanning electron microscopy examination and mercury porosimetry measurement have shown that the porosity remains interconnected and a range of pore size from several microns to hundreds of microns was obtained. X-ray diffraction analysis was performed and confirmed that there is no HA decomposition during the sintering process. Mechanical characterization has also shown that the EPD scaffold possesses excellent properties. Cell culturing experiment was carried out and the result shows that the scaffold bioactivity is not only dependent on the interconnectivity of the pores, but also the pore size.

  2. Hydroxyapatite motility implants in ocular prosthetics.

    PubMed

    Cowper, T R

    1995-03-01

    For the past 5 years, an increasing number of ophthalmologists have been using hydroxyapatite (HA) motility implants after uncomplicated enucleation or evisceration of the eye. Unlike previous implant materials, HA promotes fibrovascular ingrowth and seemingly true integration of the motility implant to the residual ocular structures. As a result, a more stable defect and greater movement of the overlying prosthesis is produced. In addition, the problems of long-term orbital implant migration and the vexing postenucleation socket syndrome are thought to be minimized. This article briefly reviews the history and development of orbital implants and HA implant surgical and prosthetic procedures. It is concluded that HA implant rehabilitation is indicated after most uncomplicated enucleations or eviscerations where there is small likelihood of complication.

  3. Hydroxyapatite chromatography of phage-display virions.

    PubMed

    Smith, George P; Gingrich, Todd R

    2005-12-01

    Hydroxyapatite column chromatography can be used to purify filamentous bacteriophage--the phage most commonly used for phage display. Virions that have been partially purified from culture supernatant by two cycles of precipitation in 2% polyethylene glycol are adsorbed onto the matrix at a density of at least 7.6 x 10(13) virions (about 3 mg) per milliliter of packed bed volume in phosphate-buffered saline (PBS; 0.15 M NaCl, 5 mM NaH2PO4, pH-adjusted to 7.0 with NaOH). The matrix is washed successively with wash buffer I(150 mM NaCl, 125 mM phosphate, pH 7.0), wash buffer II (2.55 M NaCl, 125 mM phosphate, pH 7.0), and wash buffer I; after which virions are desorbed in desorption buffer (150 mM NaCl, 200 mM phosphate, pH 7.0), and the matrix is stripped with stripping buffer (150 mM NaCl, 1 Mphosphate, pH 7.0). About half of the applied virions are recovered in desorption buffer. Western blot analysis shows that they have undetectable levels of host-derived protein contaminants that are present in the input virions and in virions purified by CsCl equilibrium density gradient centrifugation--the method most commonly used to prepare virions in high purity. Hydroxyapatite chromatography is thus an attractive alternative method for purifying filamentous virions, particularly when the scale is too large for ultracentrifugation to be practical. PMID:16382907

  4. The analysis of biomedical hydroxyapatite powders and hydroxyapatite coatings on metallic medical implants by near-IR Fourier transform Raman spectroscopy

    NASA Astrophysics Data System (ADS)

    Tudor, A. M.; Melia, C. D.; Davies, M. C.; Anderson, D.; Hastings, G.; Morrey, S.; Domingos-Sandos, J.; Barbosa, M.

    1993-06-01

    In this paper we discuss the application of Fourier transform Raman (FTR) spectroscopy to the in situ analysis of the inorganic bioceramic hydroxyapatite in both powder form and as a thermally sprayed hydroxyapatite coating on metals currently employed in medical implants for orthopaedic surgery. The derivation of the FTR spectrum of hydroxyapatite is attempted by the analysis of the pure powders of its known constituents. The FTR spectra of hydroxyapatite powders sintered up to 1300°C suggest significant structural changes in the region of 1250°C. The FTR spectra of coated metal systems clearly distinguish between samples of differing crystallinity and provide some information on the effect of the coating process on the hydroxyapatite material. The preliminary examination of hydroxyapatite coated dental screws shows a change in the nature of the hydroxyapatite coating on recovery after clinical use.

  5. Preparation, structural and spectroscopic studies of (Y xLu 1-x) 2O 3:Eu 3+ nanopowders

    NASA Astrophysics Data System (ADS)

    Antić, Željka; Krsmanović, Radenka; Wojtowicz, Marcin; Zych, Eugeniusz; Bártová, Barbora; Dramićanin, Miroslav D.

    2010-10-01

    Lutetium and yttrium oxides are promising scintillating materials suitable for use in medical planar X-ray imaging and mammography. In this paper the procedure for preparation of europium doped mixed lutetium-yttrium oxide nanopowders using polymer complex solution synthesis method is presented. Detailed information on nanopowder phase, morphology and crystallinity are obtained using X-ray powder diffraction, SEM and TEM while optical properties are investigated by photoluminescence and radioluminescence measurements. Constituting nanoparticles are 20-40 nm in size, and have excellent structural ordering in cubic bixbyite-type. Unit cell parameter, ionic coordinates, crystal coherence size and microstrain are determined from Rietveld analysis. All powders show strong Eu 3+-characteristic red emission, with an average 5D 0 emission lifetime of 1.5 ms. Radioluminescence efficiency is about 15% of the commercial micron-sized Gd 2O 2S:Eu 3+ powder while negligible level of afterglow is found.

  6. 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.

  7. A study on the production of titanium carbide nano-powder in the nanostate and its properties

    NASA Astrophysics Data System (ADS)

    Shiryaeva, L. S.; Rudneva, S. V.; Galevsky, G. V.; Garbuzova, A. K.

    2016-09-01

    The plasma synthesis of titanium carbide nano-powder in the conditions close to industrial was studied. Titanium carbide TiC is a wear- and corrosion-resistant, hard, chemically inert material, demanded in various fields for the production of hard alloys, metal- ceramic tools, heat-resistant products, protective metal coatings. New perspectives for application titanium carbide in the nanostate can be found in the field of alloys modification with different composition and destination.

  8. 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.

  9. The Preventive Effects of Nanopowdered Peanut Sprout-added Caciocavallo Cheese on Collagen-induced Arthritic Mice

    PubMed Central

    Chang, Yoon Hyuk

    2014-01-01

    The present study was carried out to investigate the effects of nanopowdered peanut sprout-added Caciocavallo cheese (NPCC) on the prevention and treatment of rheumatoid arthritis in DBA/IJ mice immunized with type II collagen. After the induction of arthritis, the mice were being divided into five groups: (1) normal, no immunization; (2) CIA, collagen-induced arthritis; (3) MTX, collagen-induced arthritis treated with methotrexate (0.3 mg/kg body weight); (4) CC, collagen-induced arthritis treated with Caciocavallo cheese (0.6 g/d); (5) NPCC, collagen-induced arthritis treated with nanopowdered peanut sprout-added Caciocavallo cheese (0.6 g/d). Nanopowdered peanut sprout was ranged from 300 to 350 nm, while regular powdered peanut sprouts were ranged from 50 to 150 μm. The NPCC group had considerable reductions of clinical scores and paw thicknesses at the end of experiment as compared to the CIA group. In the serum analysis, the TNF-α, IL-1β, IL- 6 and IgG1 levels in the NPCC group have decreased by 69.4, 75.9, 66.6, and 61.9%, respectively, when compared to the CIA group. The histological score and spleen index of the NPCC group were significantly lower than the CIA group. In conclusion, the feeding NPCC method could delay and/or prevent the rheumatoid arthritis in the collagen-induced arthritis mouse model. Based on this study, nanopowdered peanut sprouts could be applied to various functional cheeses. PMID:26760745

  10. TiC nanocrystal formation from carburization of laser-grown Ti/O/C nanopowders for nanostructured ceramics.

    PubMed

    Leconte, Y; Maskrot, H; Herlin-Boime, N; Porterat, D; Reynaud, C; Gierlotka, S; Swiderska-Sroda, A; Vicens, J

    2006-01-12

    Refractory carbide ceramics (TiC and ZrC) raise interest as promising materials for high-temperature applications such as structural materials for the future generation of nuclear reactors. In this context, nanostructured ceramics are expected to exhibit improved thermomechanical properties as well as better behavior under irradiation when compared to conventional materials. It is therefore necessary to synthesize carbide nanocrystals of such materials to elaborate the ceramics. We report here the formation study of TiC nanocrystals through the direct carburization of Ti/O/C nanopowders grown by laser pyrolysis. A spray of titanium tetraisopropoxide was laser pyrolyzed with ethylene as the sensitizer, leading to Ti/O/C nanopowders with various C contents controlled by the synthesis conditions. Annealing treatments performed on these nanopowders under an inert atmosphere without any C addition enabled the formation of TiC grains through the carburization of the oxide phase by free C incorporated during the synthesis. The powders were characterized by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. The final TiC grain size was about 80 nm, and the grains were monocrystalline. The influence of the free C content on the grain growth during the annealing step, together with its effects on the densification of the ceramics after sintering by high-pressure flash sintering, was examined. A 93% densification was finally achieved.

  11. 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.

  12. Tuning the combined magnetic and antibacterial properties of ZnO nanopowders through Mn doping for biomedical applications

    NASA Astrophysics Data System (ADS)

    Ravichandran, K.; Karthika, K.; Sakthivel, B.; Jabena Begum, N.; Snega, S.; Swaminathan, K.; Senthamilselvi, V.

    2014-05-01

    Manganese (Mn) doped ZnO nanopowders (0, 2, 4, 6, 8 and 10 at%) were synthesized using a simple soft chemical route and their structural, optical, surface morphological, magnetic and antibacterial properties were investigated. Structural studies show that the nanopowders exhibit hexagonal wurtzite structure of ZnO. No other secondary phases like MnO2, MnO, Mn3O4 and Mn2O3 are observed. The blue shift observed in the photoluminescence spectra beyond the Mn doping level of 6 at% shows that there is an increase in the carrier concentration, caused by the interstitial incorporation of Zn and Mn in the ZnO matrix. From the antibacterial studies, it is found that ZnO:Mn nanopowders with higher Mn doping level (8 and 10 at%) exhibit good antibacterial efficiency against Escherichia coli (E. coli) bacteria. The magnetization curves obtained using vibrating sample magnetometer (VSM) show a sign of strong room temperature ferromagnetic behavior when the Mn doping level is 6 at% and a weak room temperature ferromagnetic behavior, when the Mn doping level is below 6 at%. Beyond 6 at% they are found to exhibit antiferromagnetic and paramagnetic properties, when the Mn doping levels are 8 and 10 at%, respectively. The SEM images indicate that there is a gradual decrease in the grain size with increase in the Mn doping level. The EDAX profile clearly confirms the presence of expected elements in the final product, in appropriate proportions.

  13. Initial bone matrix formation at the hydroxyapatite interface in vivo.

    PubMed

    de Bruijn, J D; van Blitterswijk, C A; Davies, J E

    1995-01-01

    Dense, sintered, slip-cast hydroxyapatite rods were implanted transfemorally in young adult rats. The femora were excised after 2 and 4 weeks and, following fixation, either embedded in methyl methacrylate for light microscopy, decalcified and prepared for transmission electron microscopy, or freeze fractured in liquid nitrogen for scanning electron microscopic analysis. The latter was performed on the two tissue fragments that remained after freeze fracturing, from which the first contained the implants and the second comprised tissue that had been immediately adjacent to the hydroxyapatite rods. Undecalcified light microscopic sections revealed extensive bone tissue formation around and in contact with the hydroxyapatite rods. The initial bone matrix apposed to the implant surface, as demonstrated with scanning electron microscopy, was either composed of globular deposits or an organized network of collagen fibers. The deposits, which ranged in size from 0.1-1.1 microns, fused to form a cement-like matrix to which collagen fibers were attached. Degradation of the hydroxyapatite surface resulted in the presence of unidirectionally aligned crystallites, with which the newly formed bone matrix was closely associated. Ultrastructural analysis of the bone-hydroxyapatite interface with transmission electron microscopy revealed a 50-600-nm-wide collagen-free granular zone, comprising one or more 40-100-nm-thick electron-dense layer(s). These structural arrangements most probably partially represent the globular deposits and proteinaceous material adsorbed onto and partially in the degrading hydroxyapatite surface. Although the latter change in surface topography may have enhanced bonding of the cement-like matrix to the hydroxyapatite, the cause for this change in topography and the type of bond formed are, at present, unknown. PMID:7713963

  14. 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

  15. 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.

  16. Effect of collagen on the mechanical properties of hydroxyapatite coatings.

    PubMed

    Ou, Keng-Liang; Chung, Ren-Jei; Tsai, Fu-Yi; Liang, Pei-Yu; Huang, Shih-Wei; Chang, Shou-Yi

    2011-05-01

    In this study, the mechanical properties of bioactive coatings on Ti6Al4V substrates were investigated using instrumented nanoindentation. The aim was to observe the differences in the mechanical properties before and after immersion in collagen solution. The hydroxyapatite coatings were prepared through two processes: self-assembly in simulated body fluid and a hydrothermal method. Sintered hydroxyapatite disks were used as controls. The test samples were then incubated in a dilute collagen solution for 24 hours to produce composite coatings. The materials were investigated using XRD, SEM and nanoindentation. The results showed that the grain sizes of the hydroxyapatite coatings formed using two processes were 1 μm and 10 μm, respectively. The Young's modulus of the pure hydroxyapatite, the disk and the coatings, was 3.6 GPa. After collagen incubation treatment, the composites had a Young's modulus of 7.5 GPa. The results also showed that the strengthening phenomena of collagen were more obvious for homogeneous and small-grain hydroxyapatite coatings. These results suggest that there are similarities between these HAp/collagen composited and natural composite materials, such as teeth and bones.

  17. 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.

  18. 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.

  19. 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

  20. 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.

  1. Hydroxyapatite and urate crystal induced cytokine release by macrophages.

    PubMed Central

    Alwan, W H; Dieppe, P A; Elson, C J; Bradfield, J W

    1989-01-01

    Destructive osteoarthritis is characterised by rapidly progressive joint destruction associated with intra-articular deposition of hydroxyapatite crystals. The possible role of such crystals in the pathogenesis of this condition was investigated by testing the ability of hydroxyapatite crystals to stimulate the production of bone resorbing activity from mouse peritoneal macrophages. Urate crystals were used for comparison. Culture supernatants were tested for bone resorbing activity using the mouse calvarial bone resorption assay, for interleukin 1 using a standard lymphocyte activation assay, and for prostaglandin E2 by radioimmunoassay. Culture supernatants from macrophages incubated with hydroxyapatite crystals contained dialysable bone resorbing activity, high concentrations of prostaglandin E2, but no interleukin 1 like activity. The production of the bone resorbing agent was prevented by culturing macrophages with hydroxyapatite crystals in the presence of indomethacin. By contrast, culture supernatants from macrophages incubated with urate crystals contained bone resorbing activity, which was only partly removed by dialysis, and interleukin 1 like activity. The latter was shown to be increased in culture supernatants from macrophages incubated with urate crystals in the presence of indomethacin, while production of bone resorbing activity was partially inhibited. It is considered that the bone resorbing activity liberated from macrophages stimulated by hydroxyapatite crystals can be explained by the presence of prostaglandin E2 alone, whereas the activity liberated by urate crystals is due to both prostaglandin E2 and interleukin 1. PMID:2545171

  2. Ultrastructural comparison of hydroxyapatite and silicon-substituted hydroxyapatite for biomedical applications.

    PubMed

    Porter, Alexandra E; Best, Serena M; Bonfield, William

    2004-01-01

    Silicon-substituted hydroxyapatite (Si-HA) has been shown to lead to significantly increased rates of bone apposition when compared with phase-pure hydroxyapatite (HA) bioceramic implants (Patel N, et al. J Mater Sci Mater Med 2002;13:1199-1206). However, uncertainty remains about the mechanism by which Si increases the in vivo bioactivity. In this study, defect structures in Si-HA were observed and characterized for the first time using high-resolution transmission electron microscopy. Using tilting experiments and the g. b = 0 criterion for invisibility, the Burgers vectors of dislocations in phase-pure HA and 0.8 wt % Si-HA were characterized to be screw and mixed in character. Dislocations were observed in both pure HA and 0.8 wt % Si-HA with no significant difference in dislocation density between HA and Si-HA. However, our findings suggest that an increased number of triple junctions in Si-HA may have a significant role in increasing the solubility of the material and the subsequent rate at which bone apposes Si-HA ceramics.

  3. Production of hydroxyapatite from waste mussel shells

    NASA Astrophysics Data System (ADS)

    Jones, Mark I.; Barakat, Haneen; Patterson, Darrell Alec

    2011-10-01

    This work describes the formation of Hydroxyaptite, Ca10(PO4)6(OH)2, from waste mussel shells from the New Zealand aquaculture industry. The raw shells are first calcined to produce lime (CaO) and then reacted in a purpose built reactor to form the Hydroxyapatite (HA) in a low temperature batch process. The calcination was studied in terms of the effects of temperature, heating rate, holding time, nitrogen flow rate and particle size. The crystals formed in the batch reactor were characterized by X-Ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Energy Dispersive Spectroscopy (EDS) and X-Ray Photoelectron Spectroscopy (XPS). Optimised conditions in the calcination stage resulted in powder with around 95% conversion to lime. The as-produced HA showed poor crystallinity and the presence of impurities, although both of these features were improved by a suitable post heat treatment process. The post treated material showed good crystallinity and was comparable to commercially produced material. Preliminary biocompatibility experiments showed that the HA stimulated cell growth and promoted mineralization. The production of HA from mussel shells in a room temperature, ambient pressure process is not only a sustainable use of waste material, but also from an industrial point of view the process has considerable potential for reducing costs associated with both starting materials and energy.

  4. [Synthesis and characteristics of porous hydroxyapatite bioceramics].

    PubMed

    Niu, Jinlong; Zhang, Zhenxi; Jiang, Dazong

    2002-06-01

    The macroporous structure of human bone allows the ingrowth of the soft tissues and organic cells into the bone matrix, profits the development and metabolism of bone tissue, and adapts the bone to the change of load. There is great requirement for artificial biomimic porous bioactive ceramics with the similar structure of bone tissue that can be used clinically for repairing lost bone. Fine hydroxyapatite (HAp) powder produced by wet chemical reaction was mixed with hydrogen peroxide (H2O2), polyvinyl alcohol, methyl cellulose or other pores-making materials to form green cake. After drying at low temperature (below 100 degrees C) and decarbonizing at about 300 degrees C-400 degrees C, the spongy ceramic block was sintered at high temperature, thus, macroporous HAp bioceramic with interconnected pores and reasonable porosity and pore-diameter was manufactured. This kind of porous HAp bioceramics were intrinsically osteoinductive to a certain degree, but its outstanding property was that they can absorb human bone morphogenetic proteins and other bone growth factors to form composites, so that the macroporous HAp bioactive ceramic has appropriate feasibility for clinical application. From the point of biomedical application, the recent developments in synthesis and characteristics investigation of macroporous HAp are reviewed in this paper.

  5. Hydroxyapatite growth on cotton fibers modified chemically

    NASA Astrophysics Data System (ADS)

    Varela Caselis, J. L.; Reyes Cervantes, E.; Landeta Cortés, G.; Agustín Serrano, R.; Rubio Rosas, E.

    2014-09-01

    We have prepared carboxymethyl cellulose fibers (CMC) by chemically modifying cotton cellulose with monochloroacetic acid and calcium chloride solution. This modification favored the growth of hydroxyapatite (HAP) on the surface of the CMC fibers in contact with simulated body fluid solutions (SBF). After soaking in SBF for periods of 7, 14 and 21 days, formation of HAP was observed. Analysis by scanning electron microscopy and X-ray diffraction showed that crystallinity, crystallite size, and growth of HAP increased with the soaking time. The amount of HAP deposited on CMC fibers increased greatly after 21 days of immersion in the SBF, while the substrate surface was totally covered with hemispherical aggregates with the size of the order of 2 microns. Elemental analysis showed the presence of calcium and phosphate, with calcium/phosphate atomic ratio of 1.54. Fourier transform infrared spectroscopy bands confirmed the presence of HAP. The results suggest that cotton modified by calcium treatment has a nucleating ability and can accelerate the nucleation of HAP crystals.

  6. Bone formation on synthetic precursors of hydroxyapatite.

    PubMed

    Suzuki, O; Nakamura, M; Miyasaka, Y; Kagayama, M; Sakurai, M

    1991-05-01

    The aim of this study was to investigate the reaction of skeletal tissue to various synthetic calcium phosphate (Ca-P) compounds in vivo. Five synthetic Ca-P compounds were implanted into the subperiosteal area of the calvaria of 7-week-old BALB/c mice for one to 15 weeks. Synthetic compounds were dicalcium phosphate (DCP), octacalcium phosphate (OCP), amorphous calcium phosphate (ACP), Ca-deficient hydroxyapatite and hydroxyapatile (HA). Implanted DCP, OCP and ACP were found to be converted to apatitic phase by x-ray microdiffraction analysis using undecalcified specimens. Structure of bone was found out on all of Ca-P compounds eventually at late stage under the light microscope, but the rate of bone formation calculated from a number of experiments varied on respective synthetic Ca-P compound. It was high as 80% for DCP, OCP and ACP, but was low as 5.6% for Ca-deficient HA, and no reaction was found for HA at the stage of 3 weeks. Fine filaments and granular materials in the newly formed bone matrix were detected at 7 days around the remnants of OCP particles which already converted to apatitic phase by ultrastructural study of decalcified specimens. These structures were very similar to the components of bone nodules seen in intramembranous osteogenesis. It is postulated that the precursors of HA have an important role in intramembranous osteogenesis.

  7. Excimer laser deposition of hydroxyapatite thin films.

    PubMed

    Singh, R K; Qian, F; Nagabushnam, V; Damodaran, R; Moudgil, B M

    1994-06-01

    We have demonstrated a new and simple in situ method to fabricate adherent and dense hydroxyapatite (HA) coatings at relatively low deposition temperatures (500-600 degrees C). Under optimum processing conditions, the HA coatings possess a nominal Ca:P ratio of 1.65 and exhibit a fully crystalline single-phase structure. This deposition technique is based on the application of a pulsed excimer laser (wavelength lambda = 248 nm, pulse duration tau = 25 x 10(-9) s) to ablate a dense stoichiometric HA target. The HA target was prepared by standard ceramic coprecipitation techniques followed by cold pressing and further sintering at 1200 degrees C in air. High substrate temperatures (> or = 600 degrees C) during film deposition led to phosphorus deficient coatings because of re-evaporation of phosphorus during the deposition process. The stabilization of various calcium and phosphorus phases in the film was controlled by a number of process parameters such as substrate temperature, chamber pressure and presence of water vapour in the chamber. This is particularly advantageous for production of HA coatings, since it is known that HA decomposes at high temperatures due to the uncertainty in the starting material stoichiometry. Rutherford backscattering spectrometry, energy dispersive X-ray analysis, transmission electron microscopy, scanning electron microscopy and X-ray diffraction techniques were employed to determine the structure-processing relationships. Qualitative scratch measurements were conducted to determine the adhesion strength of the films.

  8. Biodegradable magnesium-hydroxyapatite metal matrix composites.

    PubMed

    Witte, Frank; Feyerabend, Frank; Maier, Petra; Fischer, Jens; Störmer, Michael; Blawert, Carsten; Dietzel, Wolfgang; Hort, Norbert

    2007-04-01

    Recent studies indicate that there is a high demand to design magnesium alloys with adjustable corrosion rates and suitable mechanical properties. An approach to this challenge might be the application of metal matrix composite (MMC) based on magnesium alloys. In this study, a MMC made of magnesium alloy AZ91D as a matrix and hydroxyapatite (HA) particles as reinforcements have been investigated in vitro for mechanical, corrosive and cytocompatible properties. The mechanical properties of the MMC-HA were adjustable by the choice of HA particle size and distribution. Corrosion tests revealed that HA particles stabilised the corrosion rate and exhibited more uniform corrosion attack in artificial sea water and cell solutions. The phase identification showed that all samples contained hcp-Mg, Mg(17)Al(12), and HA before and after immersion. After immersion in artificial sea water CaCO3 was found on MMC-HA surfaces, while no formation of CaCO3 was found after immersion in cell solutions with and without proteins. Co-cultivation of MMC-HA with human bone derived cells (HBDC), cells of an osteoblasts lineage (MG-63) and cells of a macrophage lineage (RAW264.7) revealed that RAW264.7, MG-63 and HBDC adhere, proliferate and survive on the corroding surfaces of MMC-HA. In summary, biodegradable MMC-HA are cytocompatible biomaterials with adjustable mechanical and corrosive properties.

  9. Characterization of hydroxyapatite by electron microscopy.

    PubMed

    Rodríguez-Lugo, V; Hernández, J Sanchez; Arellano-Jimenez, Ma J; Hernández-Tejeda, P H; Recillas-Gispert, S

    2005-12-01

    The obtention of hydroxyapatite (HAp) is reported using brushite (CaHPO4.2H2O) and the skeleton of a starfish (Mellita eduardobarrosoi sp. nov.), primarily composed of magnesian calcite ((Ca,Mg)CO3) as precursors. Stoichiometric amounts of both were reacted under hydrothermal conditions: a pressure of 5.8 MPa and a temperature of 200 degrees C for 2, 4, 6, 8, 10, and 20 h of reaction times. The samples obtained were characterized by means of scanning electron microscopy, X-ray diffraction, infrared spectroscopy, and transmission electron microscopy. Two defined populations of HAp fibers were found: A bundle of fibers 75 mum in length and 1-13 mum in diameter, and a second bundle of fibers 5 mum in length and less than 0.5 mum in diameter. Furthermore, an increase in HAp formation and a Ca/P ratio as a function of reaction time were observed. The growth mechanism of HAp is also discussed. PMID:17481330

  10. Characterization of Hydroxyapatite by Electron Microscopy

    NASA Astrophysics Data System (ADS)

    Rodríguez-Lugo, V.; Sanchez Hernández, J.; Arellano-Jimenez, Ma. J.; Hernández-Tejeda, P. H.; Recillas-Gispert, S.

    2005-12-01

    The obtention of hydroxyapatite (HAp) is reported using brushite (CaHPO4·2H2O) and the skeleton of a starfish (Mellita eduardobarrosoi sp. nov.), primarily composed of magnesian calcite ((Ca,Mg)CO3) as precursors. Stoichiometric amounts of both were reacted under hydrothermal conditions: a pressure of 5.8 MPa and a temperature of 200°C for 2, 4, 6, 8, 10, and 20 h of reaction times. The samples obtained were characterized by means of scanning electron microscopy, X-ray diffraction, infrared spectroscopy, and transmission electron microscopy. Two defined populations of HAp fibers were found: A bundle of fibers 75 [mu]m in length and 1 13 [mu]m in diameter, and a second bundle of fibers 5 [mu]m in length and less than 0.5 [mu]m in diameter. Furthermore, an increase in HAp formation and a Ca/P ratio as a function of reaction time were observed. The growth mechanism of HAp is also discussed.

  11. Ion exchange in hydroxyapatite with lanthanides.

    PubMed

    Cawthray, Jacqueline F; Creagh, A Louise; Haynes, Charles A; Orvig, Chris

    2015-02-16

    Naturally occurring hydroxyapatite, Ca5(PO4)3(OH) (HAP), is the main inorganic component of bone matrix, with synthetic analogues finding applications in bioceramics and catalysis. An interesting and valuable property of both natural and synthetic HAP is the ability to undergo cationic and anionic substitution. The lanthanides are well-suited for substitution for the Ca(2+) sites within HAP, because of their similarities in ionic radii, donor atom requirements, and coordination geometries. We have used isothermal titration calorimetry (ITC) to investigate the thermodynamics of ion exchange in HAP with a representative series of lanthanide ions, La(3+), Sm(3+), Gd(3+), Ho(3+), Yb(3+) and Lu(3+), reporting the association constant (Ka), ion-exchange thermodynamic parameters (ΔH, ΔS, ΔG), and binding stoichiometry (n). We also probe the nature of the La(3+):HAP interaction by solid-state nuclear magnetic resonance ((31)P NMR), X-ray diffraction (XRD), and inductively coupled plasma-optical emission spectroscopy (ICP-OES), in support of the ITC results. PMID:25594577

  12. Comparison of periodontal ligament cells responses to dense and nanophase hydroxyapatite.

    PubMed

    Sun, Weibin; Chu, Chenlin; Wang, Juan; Zhao, Huating

    2007-05-01

    Hydroxyapatite, a synthetic calcium phosphate ceramic, is used as a biomaterial for the restoration of human hard tissue as well as in techniques which aim to regenerate periodontal tissues. Generally, hydroxyapatite is believed to have osteoconductive effects and to be non-bioresorbable but not to induce to periodontal tissue regeneration. No report has been found on responses of periodontal ligament cells (PDLC), the main contributor to periodontal tissue regeneration, to nanoparticles of hydroxyapatite. The objective of this study was to investigate the possible effects of nanophase powder of hydroxyapatite on proliferation of periodontal ligament cells. Using a sol-gel method, the nanophase hydroxyapatite powders were fabricated. These powders were proved to comprise nanoparticles by transmission electron microscope examination. The primary periodontal ligament cells were cultured on dense particle hydroxyapatite and nanometer particle hydroxyapatite. The effects on proliferation of periodontal ligament cells on dense and nanoparticle hydroxyapatite were examined in vitro using a methyl thiazolil tetracolium (MTT) test. The intercellular effects were studied with scanning electron microscopy (SEM), transmission electron microscopy (TEM) and energy dispersive X-ray (EDX). In addition, the influence of the two materials on osteogenic differentiation was determined through measurement of alkaline phosphatase activity and flow cytometry. About 2, 3, and 4 days after treatment with nanoparticles of hydroxyapatite, the proliferation activity of the PDLC increased significantly compared with those proliferating on dense hydroxyapatite and of control PDLC, but no significant difference was found between the PDLC proliferation on dense hydroxyapatite and the control PDLCs. After 3 and 5 days' incubation with nanoparticles of hydroxyapatite, alkaline phosphatase activity was significantly increased as compared to PDLCs incubated with dense hydroxyapatite and control

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

    PubMed

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

    2015-12-21

    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.

  14. 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.

  15. 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

  16. 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

  17. [IN VIVO EVALUATION OF POLYCAPROLACTONE-HYDROXYAPATITE SCAFFOLD BIOCOMPATIBILITY].

    PubMed

    Ivanov, A N; Kozadaev, M N; Bogomolova, N V; Matveeva, O V; Puchinyan, D M; Norkin, I A; Sal'kovskii, Yu E; Lyubun, G P

    2015-01-01

    Biocompatibility is one of the main and very important properties for scaffolds. The aim of the present study was to investigate cells population dynamics in vivo in the process of original polycaprolactone-hydroxyapatite scaffold colonization, as well as tissue reactions to the implantation to assess the biocompatibility of the matrix. It has been found that tissue reactive changes in white rats subside completely up to the 21st day after subcutaneous polycaprolactone-hydroxyapatite scaffold implantation. Matrix was actively colonized by connective tissue cells in the period from the 7th to the 21st day of the experiment. However, intensive scaffold vascularization started from the 14th day after implantation. These findings suggest a high degree of the polycaprolactone-hydroxyapatite scaffold biocompatiblilitye.

  18. Recent Advances in Hydroxyapatite Scaffolds Containing Mesenchymal Stem Cells.

    PubMed

    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.

  19. 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.

  20. Exchange Bias Effect in La1-xAgxMnO3 Nanopowders

    NASA Astrophysics Data System (ADS)

    Mihalik, M.; Antoňák, M.; Csach, K.; Fitta, M.; Mihalik, M.; Vavra, M.; Zentková, M.

    2013-01-01

    Exchange bias (EB) phenomena were first observed in the La1-xAgxMnO3 as prepared and heat treated (300 °C/2 hours) nanopowders (x = 0.10, 0.15 and 0.20) which were synthetized by self-combustion glycine-nitrate method. These nanoparticles have an average size of about 25 nm and adopt orthorhombic Pnma crystal structure. Cooling in magnetic field Hcf ≠ 0 through the Curie temperature TC shifts hysteresis loop in horizontal and vertical direction. The values of exchange bias field HE, coercive field Hc, remnant asymmetry μE and coercive magnetization μc increase with increasing value of cooling field Hcf. In addition the training effect was observed. Basic magnetic properties like the Curie temperature TC and the saturated magnetization µs increase and HE or µE decrease with heat treatment. Heat treatment at 600 °C/2 hours increases the average size of nanoparticles to about 55 nm, crystal structure changes to rhombohedral structure (space group R3c) and EB effect vanishes.

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

    NASA Astrophysics Data System (ADS)

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

    2015-07-01

    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 ˜1019 m-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.

  2. CO sensing properties under UV radiation of Ga-doped ZnO nanopowders

    NASA Astrophysics Data System (ADS)

    Dhahri, R.; Hjiri, M.; Mir, L. El.; Bonavita, A.; Iannazzo, D.; Leonardi, S. G.; Neri, G.

    2015-11-01

    In this study, the effect of Ga-doping and UV radiation on CO sensing of ZnO nano-powders has been investigated. GZO nanoparticles with different Ga loadings were prepared using a modified sol-gel route and charaterized by means of trasmission electron microscopy (TEM), X-ray diffraction (XRD) and photoluminescence (PL) analysis. Electrical and CO-sensing tests were performed on resistive planar devices consisting of thick films of GZO deposited on interdigitated alumina substrates in both dark and illumination condition by exposing the samples to UV radiation (λ = 400 nm). The baseline resistance in dark decreases strongly with the increase of Ga loading. This effect is reinforced by using UV radiation at low temperature in samples containing up to 3 at.% of Ga, which suggests also an effect of the microstructure of GZO on UV light promoting mechanism. The combined effect of Ga doping and UV irradiation allowed to monitor CO in air at low concentration with high sensitivity and lower operating temperature than on unpromoted ZnO sensor.

  3. 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.

  4. 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.

  5. Preparation and structural characterization of vulcanized natural rubber nanocomposites containing nickel-zinc ferrite nanopowders.

    PubMed

    Bellucci, F S; Salmazo, L O; Budemberg, E R; da Silva, M R; Rodríguez-Pérez, M A; Nobre, M A L; Job, A E

    2012-03-01

    Single-phase polycrystalline mixed nickel-zinc ferrites belonging to Ni0.5Zn0.5Fe2O4 were prepared on a nanometric scale (mean crystallite size equal to 14.7 nm) by chemical synthesis named the modified poliol method. Ferrite nanopowder was then incorporated into a natural rubber matrix producing nanocomposites. The samples were investigated by means of infrared spectroscopy, X-ray diffraction, scanning electron microscopy and magnetic measurements. The obtained results suggest that the base concentration of nickel-zinc ferrite nanoparticles inside the polymer matrix volume greatly influences the magnetic properties of nanocomposites. A small quantity of nanoparticles, less than 10 phr, in the nanocomposite is sufficient to produce a small alteration in the semi-crystallinity of nanocomposites observed by X-ray diffraction analysis and it produces a flexible magnetic composite material with a saturation magnetization, a coercivity field and an initial magnetic permeability equal to 3.08 emu/g, 99.22 Oe and 9.42 x 10(-5) respectively. PMID:22755110

  6. 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

  7. 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.

  8. ZnO and ZnTiO3 nanopowders for antimicrobial stone coating

    NASA Astrophysics Data System (ADS)

    Ruffolo, S. A.; La Russa, M. F.; Malagodi, M.; Oliviero Rossi, C.; Palermo, A. M.; Crisci, G. M.

    2010-09-01

    In the past a great variety of biocidal compounds and persistent organic pesticides were applied on a large scale for preventive measures aimed at the long-term preservation of our cultural heritage. Only recently, public and expert attention has started to focus increasingly on the risks resulting from these treatments on human health, works of art and environment in general. The work done in this field demonstrated that the most effective way for inactivation can be achieved by using highly efficient photocatalysts with the illumination of UV radiation. Following this direction our group focused its attention on well-known photocatalysts, ZnO and ZnTiO3, in the degradation and complete mineralisation of environmental pollutants. This explorative work deals with an experimental investigation on biocidal efficient of ZnO and ZnTiO3. In particular micro-quantities of the two nanopowdered photocatalysts were spread on plated dishes. They were filled by the MEA (Malt Extract Agar) medium containing given quantities of Aspergillus Niger (a chromogen filamentous fungus involved in biodeterioration). At the same time the two oxides were dispersed in different polymeric matrices, acrylic and fluorinated, in order to obtain a new coating technology, with hydrophobic, consolidant and biocidal properties for the restoration of building stone material. The mixtures obtained were applied on marble samples and capillary water absorption, simulated solar ageing, colourimetric measurements and contact angle measurements have been performed to evaluate its properties.

  9. 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.

  10. 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

  11. 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.

  12. 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.

  13. SANS study of microstructural inhomogeneities on Al nano-powder compacts

    NASA Astrophysics Data System (ADS)

    Han, Young Soo; Seong, Baek Seok; Lee, Chang Hee; Lee, Geun Hee; Rhee, Chang Kyu; Kim, Whung Whoe; Wiedenmann, A.

    2004-07-01

    The nano-crystalline materials have excellent mechanical and electrical properties compared to conventional materials. These advantages mainly come from their nano-sized grain structure. Usually the nano-crystalline materials are fabricated using nano powder. The optimum consolidation process is essential to obtain a fully densified structure. The quantitative characterization of remaining pores is important to study the consolidation process. SANS is the best technique to characterize the nano sized inhomogeneities in bulk samples. Al nano powder was synthesized by pulsed wire evaporation (PWE) method and the nano-powder compacts were fabricated by magnetic pulse compaction (MPC) method. The Aluminum oxide was observed by transmission electron microscopy (TEM) at the surface of Al nano powder. The small angle neutron scattering experiments were performed both at the instrument V4 in HMI and at the SANS facility in Korea Atomic Energy Research Institute (KAERI). The SANS data measured in KAERI were compared with the SANS data measured in HMI. The scattering intensity at high Q region increases with decreasing relative density, while the intensity at low Q region increases with increasing relative density in the Al nano powder compacts. The scattering intensity depends on the content of residual pores and Al oxide particles. The volume fraction of Al oxide particle increases with relative density due to the fragmentation of Al oxide layer. The extra scattering at low Q region results from the presence of Al oxide particles.

  14. Production of zinc substituted hydroxyapatite using various precipitation routes.

    PubMed

    Shepherd, David; Best, Serena M

    2013-04-01

    Substituted hydroxyapatites have been investigated for use as bone grafts and have been investigated for many years. Zinc is of interest due to its potential to reduce bone resorption and antibacterial properties. However, it has proven problematic to substitute biologically significant levels of zinc into the crystal structure through wet chemical routes, whilst retaining the high temperature phase stability required for processing. The aim of this study is to investigate two different precipitation routes used to synthesize zinc substituted hydroxyapatite and to explore the effects of ammonia used in the reactions on the levels of zinc substituted into the crystal lattice. It was found that considerable amounts of ammonia are required to maintain a pH sufficiently high for the production of stoichiometric hydroxyapatite using a reaction between calcium nitrate, zinc nitrate and ammonium phosphate. X-ray fluorescence analysis showed that a significant proportion of the zinc added did not substitute into the hydroxyapatite lattice. Fourier transform infrared spectroscopy revealed the existence of a zinc-ammonia complex that, it is proposed, inhibits zinc substitution for calcium. It was found that by reacting orthophosphoric acid with calcium nitrate and zinc nitrate, the volume of ammonia required in the reaction was reduced and higher levels of zinc substitution were achieved, with up to 0.58 wt% incorporated into the hydroxyapatite lattice. The resulting products were found to be stoichiometric hydroxyapatite and did not appear to contain any extraneous calcium phosphate phases after heat treatment up to 1100 °C. X-ray diffraction and Rietveld analysis revealed that the effect of substituting zinc into the HA lattice was to decrease the a-lattice parameter whilst increasing the c-lattice. Transmission electron microscopy also showed that the incorporation of zinc reduced both the length and width of the precipitated crystals.

  15. 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.

  16. 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

  17. Localized drugs delivery hydroxyapatite microspheres for osteoporosis therapy

    NASA Astrophysics Data System (ADS)

    Lee, J. H.; Ko, I. H.; Jeon, S.-H.; Chae, J. H.; Lee, E. J.; Chang, J. H.

    2011-10-01

    This study describes the preparation of hydroxyapatite microspheres for local drugs delivery. The formation of the hydroxyapatite microspheres was initiated by enzymatic decomposition of urea and accomplished by emulsification process (water-in-oil). The microspheres obtained were sintered at 500°C. Scanning electron microscope (SEM) indicated that the microspheres have various porous with random size, which maximizes the surface area. Cytotoxicity was not observed after sintering. Osteoporosis drugs, alendronate and BMP-2, were loaded into HAp microspheres and the releases of both molecules showed sustained releasing profiles.

  18. Effect of Mg doping level on the antibacterial activity of (Mg + F)-doped ZnO nanopowders synthesized using a soft chemical route

    NASA Astrophysics Data System (ADS)

    Ravichandran, K.; Snega, S.; Jabena Begum, N.; Christena, L. Rene; Dheivamalar, S.; Swaminathan, K.

    2014-08-01

    ZnO nanopowders simultaneously doped with fluorine (20 at.%) and magnesium (4, 8, 12 and 16 at.%) (ZnO:F:Mg) have been synthesized using an inexpensive simple soft chemical route for the first time. The effect of Mg doping level on certain physical properties and antibacterial activities of ZnO:F:Mg nanopowders has been investigated and reported. XRD studies showed that the products have the hexagonal wurtzite structure of ZnO. Fourier transform infrared spectra authenticate the presence of MgO stretching vibration, which is responsible for the increased antibacterial activity of the synthesized samples. The antibacterial activity of ZnO:F:Mg nanopowders was found to be enhanced with increase in Mg doping level as it causes a reduction in the grain size.

  19. Reaction of the dental pulp to hydroxyapatite.

    PubMed

    Jaber, L; Mascrès, C; Donohue, W B

    1992-01-01

    The purpose of this study was to evaluate the action of hydroxyapatite (HA) (Osteogen HA Resorb, GBD Marketing Group Inc., Valley Stream, N.Y.) on the dental pulp of rats. Four upper molar pulps in 45 rats were exposed and capped with synthetic HA (Osteogen) with a stereoscopic microscope. Pulps capped with calcium hydroxide (Dycal, L.D. Caulk Co., Milford, Del.) served as controls. The cavities were filled with amalgam, and the molars on each side of the maxilla were protected by the placement of a pedodontic steel crown. Pulp inflammation and dentin repair were compared by histologic observations and computer image analysis after 7, 14, and 28 days. After 7 days a partial acute pulpitis were observed in specimens treated with Osteogen or Dycal. Reparative dentin formation along the pulp walls was also seen. After 14 days the pulpitis was more extensive in the Osteogen-treated teeth than in the control teeth. Dentin formation as measured by morphometric analysis was more pronounced in Osteogen-treated teeth. Neo-odontoblasts were observed after the use of both materials. After 28 days an acute inflammatory reaction was still evident in the Osteogen-treated group. A complete dentinal bridge was observed more frequently with Dycal than with Osteogen. Despite the putative abilities of HA to be osteoconductive, osteogenic, and dentinogenic, the results of this study indicate that it should not be used as a pulp-capping agent because of its tendency to cause scattered dystrophic calcification in the dental pulp, which could interfere with future endodontic treatment. PMID:1318535

  20. Hydrolysis of dicalcium phosphate dihydrate to hydroxyapatite.

    PubMed

    Fulmer, M T; Brown, P W

    1998-04-01

    Dicalcium phosphate dihydrate (DCPD) was hydrolysed in water and in 1 M Na2HPO4 solution at temperatures from 25-60 degrees C. Hydrolysis was incomplete in water. At 25 degrees C, DCPD partially hydrolysed to hydroxyapatite (HAp). Formation of HAp is indicative of incongruent DCPD dissolution. At the higher temperatures, hydrolysis to HAp was more extensive and was accompanied by the formation of anhydrous dicalcium phosphate (DCP). Both of these processes are endothermic. When hydrolysis was carried out in 1 M Na2HPO4 solution, heat absorption was greater at any given temperature than for hydrolysis in water. Complete hydrolysis to HAp occurred in this solution. The hydrolysis of DCPD to HAp in sodium phosphate solution was also endothermic. The complete conversion of DCPD to HAp in sodium phosphate solution would not be expected if the only effect of this solution was to cause DCPD dissolution to become congruent. Because of the buffering capacity of a dibasic sodium phosphate solution, DCPD hydrolysed completely to HAp. Complete conversion to HAp was accompanied by the conversion of dibasic sodium phosphate to monobasic sodium phosphate. The formation of DCP was not observed indicating that the sodium phosphate solution precluded the DCPD-to-DCP dehydration reaction. In addition to affecting the extent of hydrolysis, reaction in the sodium phosphate solution also caused a morphological change in the HAp which formed. HAp formed by hydrolysis in water was needle-like to globular while that formed in the sodium phosphate solution exhibited a florette-like morphology.

  1. Hydroxyapatite-reinforced collagen tissue engineering scaffolds

    NASA Astrophysics Data System (ADS)

    Kane, Robert J.

    Scaffolds have been fabricated from a wide variety of materials and most have showed some success, either as bone graft substitutes or as tissue engineering scaffolds. However, all current scaffold compositions and architectures suffer from one or more flaws including poor mechanical properties, lack of biological response, nondegradability, or a scaffold architecture not conducive to osteointegration. Biomimetic approaches to scaffold design using the two main components of bone tissue, collagen and hydroxyapatite, resulted in scaffolds with superior biological properties but relatively poor mechanical properties and scaffold architecture. It was hypothesized that by optimizing scaffold composition and architecture, HA-collagen bone tissue engineering scaffolds could provide both an excellent biological response along with improved structural properties. The mechanical properties of freeze-dried HA-collagen scaffolds, the most common type of porous HA-collagen material, were first shown to be increased by the addition of HA reinforcements, but scaffold stiffness still fell far short of the desired range. Based on limitations inherent in the freeze-dried process, a new type of leached-porogen scaffold fabrication process was developed. Proof-of-concept scaffolds demonstrated the feasibility of producing leached-porogen HA-collagen materials, and the scaffold architecture was optimized though careful selection of porogen particle size and shape along with an improved crosslinking technique. The final scaffolds exhibited substantially increased compressive modulus compared to previous types HA-collagen scaffolds, while the porosity, pore size, and scaffold permeability were tailored to be suitable for bone tissue ingrowth. An in vitro study demonstrated the capacity of the leached-porogen scaffolds to serve as a substrate for the differentiation of osteoblasts and subsequent production of new bone tissue. The new leached-porogen scaffold HA-collagen scaffolds were

  2. Mechanism of Zn stabilization in hydroxyapatite and hydrated (0 0 1) surfaces of hydroxyapatite.

    PubMed

    Matos, M; Terra, J; Ellis, D E

    2010-04-14

    A basic understanding of Zn incorporation on bulk and hydrated (0 0 1) surfaces of hydroxyapatite (HA) is attained through electronic structure calculations which use a combined first principles density functional (DFT) and extended Hückel tight binding (EHTB) methodology. A Zn substituted hydroxyapatite relaxed structure is obtained through a periodic cell DFT geometry optimization method. Electronic structure properties are calculated by using both cluster DFT and periodic cell EHTB methods. Bond order calculations show that Zn preference for the Ca2 vacancy, near the OH channel and with greater structural flexibility, is associated with the formation of a four-fold (bulk) and nearly four-fold (surface) coordination, as in ZnO. When occupying the octahedral Ca1 vacancy, Zn remains six-fold in the bulk, but coordination decreases to five-fold in the surface. In the bulk and surface, Zn2 is found to be more covalent than Zn1, due to a decrease in bond lengths at the four-fold site, which approach the 1.99 Å ZnO value. Zn is however considerably less bound in the biomaterial than in the oxide, where calculated bond orders are twice as large as in HA. Surface phosphate groups (PO(4)) and hydroxide ions behave as compact individual units as in the bulk; no evidence is found for the presence of HPO(4). Ca-O bond orders decrease at the surface, with a consequent increase in ionicity. Comparison between DFT and EHTB results show that the latter method gives a good qualitative account of charge and bonding in these systems. PMID:21389531

  3. 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.

  4. 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...

  5. Complications of motility peg placement for porous hydroxyapatite orbital implants

    PubMed Central

    Lin, C-J; Liao, S-L; Jou, J-R; Kao, S C S; Hou, P-K; Chen, M-S

    2002-01-01

    Aim: To evaluate the complications associated with pegging of porous hydroxyapatite orbital implants. Methods: Complications associated with pegging were retrospectively reviewed from the charts of 100 of 133 patients with hydroxyapatite implantation from 1993 to 2000. Results: 48 (48%) of the 100 hydroxyapatite implanted patients who had undergone pegging were found to have problems with their pegs, including discharge (45.8%), peg falling out (20.8%), pyogenic granulomas (16.7%), popping peg (14.6%), hydroxyapatite visible around peg hole (8.3%), part of peg shaft visible (6.2%), peg drilled off centre (6.2%), peg drilled at an angle (4.2%), and excess movement of peg (4.2%). The standard peg fell out statistically more often than the peg and sleeve system (Yates's corrected χ2, p=0.038). There was a trend towards complications of the peg with use of a standard peg (versus sleeved peg) (p=0.226). Conclusions: There are several potential complications of pegging. Most complications are minor and can be managed successfully. PMID:11914206

  6. Bone-Like Hydroxyapatite Formation in Human Blood

    ERIC Educational Resources Information Center

    Titov, Anatoly T.; Larionov, Peter M.; Ivanova, Alexandra S.; Zaikovskii, Vladimir I.; Chernyavskiy, Mikhail A.

    2016-01-01

    The purpose of this study was to prove the mechanism of mineralization, when hydroxyapatite (HAP) is formed in blood plasma. These observations were substantiated by in vitro simulation of HAP crystallization in the plasma of healthy adults in a controllable quasi-physiological environment (T = 37°C, pH = 7.4) and at concentrations of dissolved Ca…

  7. 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

  8. 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.

  9. 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%.

  10. 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

  11. 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).

  12. Reverse micelle synthesis of oxide nanopowders: mechanisms of precipitate formation and agglomeration effects.

    PubMed

    Graeve, Olivia A; Fathi, Hoorshad; Kelly, James P; Saterlie, Michael S; Sinha, Kaustav; Rojas-George, Gabriel; Kanakala, Raghunath; Brown, David R; Lopez, Enrique A

    2013-10-01

    We present an analysis of reverse micelle stability in four model systems. The first two systems, composed of unstable microemulsions of isooctane, water, and Na-AOT with additions of either iron sulfate or yttrium nitrate, were used for the synthesis of iron oxide or yttrium oxide powders. These oxide powders were of nanocrystalline character, but with some level of agglomeration that was dependent on calcination temperature and cleaning procedures. Results show that even though the reverse micellar solutions were unstable, nanocrystalline powders with very low levels of agglomeration could be obtained. This effect can be attributed to the protective action of the surfactant on the surfaces of the powders that prevents neck formation until after all the surfactant has volatilized. A striking feature of the IR spectra collected on the iron oxide powders is the absence of peaks in the ~1715 cm(-1) to 1750 cm(-1) region, where absorption due to the symmetric C=O (carbonyl) stretching occurs. The lack of such peaks strongly suggests the carbonyl group is no longer free, but is actively participating in the surfactant-precipitate interaction. The final two microemulsion systems, containing CTAB as the surfactant, showed that loss of control of the reverse micelle synthesis process can easily occur when the amount of salt in the water domains exceeds a critical concentration. Both model systems eventually resulted in agglomerated powders of broad size distributions or particles that were large compared to the sizes of the reverse micelles, consistent with the notion that the microemulsions were not stable and the powders were precipitated in an uncontrolled fashion. This has implications for the synthesis of nanopowders by reverse micelle synthesis and provides a benchmark for process control if powders of the highest quality are desired. PMID:23906861

  13. Evaluation of leakage from fume hoods using tracer gas, tracer nanoparticles and nanopowder handling test methodologies.

    PubMed

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

    2014-01-01

    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 ft/min) 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 airflows. 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

  14. Spectral investigations on undoped and Cu2+ doped ZnO-CdS composite nanopowders

    NASA Astrophysics Data System (ADS)

    Thirumala Rao, G.; Babu, B.; Joyce Stella, R.; Pushpa Manjari, V.; Ravikumar, R. V. S. S. N.

    2015-03-01

    Undoped and Cu2+ doped ZnO-CdS composite nanopowders were synthesized by simple chemical precipitation method. Structural and spectroscopic properties of the prepared samples have been characterized by XRD, SEM with EDS, TEM, FT-IR, UV-Vis, EPR and Photoluminescence studies. X-ray diffraction pattern contains a series of peaks corresponds to hexagonal phase of ZnO and CdS. The average crystallite sizes of undoped and Cu2+ doped samples are determined and are in the range of 25-30 nm. SEM and TEM micrographs reveal that the samples show spherical like structures with little agglomeration. FT-IR spectra show the fundamental mode of vibrations of Znsbnd O at 515 cm-1, Cdsbnd S at 621 cm-1 and other functional groups. Optical absorption spectrum of Cu2+ doped sample consists of three bands at 665, 823 and 1192 nm attributed to the transitions 2B1g → 2Eg, 2B2g and 2A1g respectively. Crystal field and tetragonal field parameters are evaluated as Dq = 1214, Ds = 1610 and Dt = 389 cm-1. From EPR, spin-Hamiltonian and hyperfine splitting parameters are evaluated for Cu2+ doped sample as g‖ = 2.3391, g⊥ = 2.0550 and A‖ = 130 × 10-4 cm-1, A⊥ = 36 × 10-4 cm-1. The optical and EPR data suggests that Cu2+ entered into host lattice as tetragonally distorted octahedral site symmetry. PL spectra consists two emission bands at 367, 380 nm in UV region. A sharp blue emission peak at 425 nm and a broad green emission peak in the range of 450-570 nm are observed. The enhanced visible emission is observed after doping.

  15. Evaluation of leakage from fume hoods using tracer gas, tracer nanoparticles and nanopowder handling test methodologies.

    PubMed

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

    2014-01-01

    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 ft/min) 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 airflows. 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

  16. 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

  17. Physicochemical, microbial, and sensory properties of yogurt supplemented with nanopowdered chitosan during storage.

    PubMed

    Seo, M H; Lee, S Y; Chang, Y H; Kwak, H S

    2009-12-01

    This study was carried out to determine the possibility of adding nanopowdered chitosan (NPC) into cholesterol-reduced yogurt to improve the functionality of yogurt and the effects of adding NPC on the physicochemical, microbial, and sensory properties of the products during storage. The pH values and mean lactic acid bacteria counts of NPC-added (0.3 to approximately 0.7%, wt/vol) and cholesterol-reduced yogurt ranged from 4.19 to 4.41 and from 4.75 x 10(8) to 9.70 x 10(8) cfu/mL, respectively, when stored at 4 degrees C for 20 d, thereby indicating a possibility of prolonging the shelf life of yogurt. In color, the a* and b* values for cholesterol-reduced yogurt were not significantly influenced by the addition of NPC (0.1 to approximately 0.7%, wt/vol); however, the L* values significantly decreased with the addition of the greatest concentration (0.7%, wt/vol) of NPC at 0-d storage. The sensory test revealed that the astringency scores significantly increased at 0-d storage when the greatest concentration (0.7%, wt/vol) of NPC was added into cholesterol-reduced yogurt. Based on the data obtained from the current study, it is concluded that concentrations (0.3 to ~0.5%, vol/vol) of NPC could be used to produce an NPC-added and cholesterol-reduced yogurt without significantly adverse effects on the physicochemical, microbial, and sensory properties.

  18. 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.

  19. 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

  20. Ultrafast synthesis of yolk-shell and cubic NiO Nanopowders and application in lithium ion batteries.

    PubMed

    Choi, Seung Ho; Kang, Yun Chan

    2014-02-26

    A continuous one-pot method was employed to synthesize yolk-shell and single-crystalline cubic NiO powders in a few seconds. Submicrometer-sized NiO yolk-shell particles were prepared by spray pyrolysis at 900 °C. Single-crystalline cubic NiO nanopowders were prepared by one-pot flame spray pyrolysis from NiO vapors. Particle surface areas of the yolk-shell and single-crystalline cubic NiO powders as obtained using the Brunauer-Emmett-Teller method were 8 and 5 m(2) g(-1), respectively. The mean crystallite sizes of the yolk-shell-structured and cubic NiO powders were 50 and 80 nm, respectively. The yolk-shell and single-crystalline cubic NiO powders delivered discharge capacities of 951 and 416 mA h g(-1), respectively, after 150 cycles, and the corresponding capacity retentions measured after the first cycle were 106 and 66%, respectively. The yolk-shell-structured NiO powders showed rate performance better than that of the single-crystalline cubic NiO nanopowders. Even at a high current density of 1 A g(-1), the discharge capacity of the yolk-shell-structured NiO powders was as high as 824 mA h g(-1) after 50 cycles, in which the current densities were increased stepwise. PMID:24490667

  1. 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

  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. Sub-10 nm Ytterbium Oxide Nanopowder-doped Silicone Rubber Acoustic Lens Material for Medical Echo Array Probe

    NASA Astrophysics Data System (ADS)

    Yamashita, Yohachi (John); Hosono, Yasuharu; Itsumi, Kazuhiro

    2007-09-01

    The effects of 8-nm-Yb2O3-nanopowders dopant, on the physical and acoustical properties of high-temperature-vulcanization (HTV) silicone (Q) rubber have been investigated, to develop a low acoustic attenuation (α) lens material for medical array probes. A 35 wt % (6 vol %) Yb2O3-doped HTV Q rubber showed a sound velocity (c) = 867 m/s, an acoustic impedance (Z) = 1.36× 106 kg\\cdotm-2\\cdots-1, an acoustic attenuation α = 0.66 dB\\cdotmm-1\\cdotMHz-1, and an α-figure of merits (FOM) (α× c) = 574 at 37 °C. The α-FOM value with Z = 1.36× 106 kg\\cdotm-2\\cdots-1 for a Q rubber lens material is the lowest attenuation ever reported. Microstructure observation revealed that the low-α rubber showed a uniform Yb2O3 nanopowder distribution in the rubber matrix.

  4. 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.

  5. The effect of partially stabilized zirconia on the mechanical properties of the hydroxyapatite-polyethylene composites.

    PubMed

    Sadi, A Yari; Homaeigohar, S Sh; Khavandi, A R; Javadpour, J

    2004-08-01

    The effect of partially stabilized zirconia (PSZ) on the mechanical properties of the hydroxyapatite-high density polyethylene composites was studied by investigating the effect of hydroxyapatite and the simultaneous effect of hydroxyapatite and PSZ volume fractions on fracture strength, modulus of elasticity, and absorbed energy in the composite samples. The results showed a decrease in fracture strength, and absorbed energy with an increase in the volume fraction of hydroxyapatite content in the hydroxyapatite-polyethylene samples. Partial replacement of hydroxyapatite with PSZ particles was beneficial in the improvement of both the fracture strength and failure energy values in the composite samples. A transition from ductile to brittle behavior was observed as the volume fraction of ceramic filler particles increased in the samples.

  6. Hydroxyapatite nanorods: soft-template synthesis, characterization and preliminary in vitro tests.

    PubMed

    Nguyen, Nga Kim; Leoni, Matteo; Maniglio, Devid; Migliaresi, Claudio

    2013-07-01

    Synthetic hydroxyapatite nanorods are excellent candidates for bone tissue engineering applications. In this study, hydroxyapatite nanorods resembling bone minerals were produced by using soft-template method with cetyltrimethylammonium bromide. Composite hydroxyapatite/poly(D, L)lactic acid films were prepared to evaluate the prepared hydroxyapatite nanorods in terms of cell affinity. Preliminary in vitro experiments showed that aspect ratio and film surface roughness play a vital role in controlling adhesion and proliferation of human osteoblast cell line MG 63. The hydroxyapatite nanorods with aspect ratios in the range of 5.94-7 were found to possess distinctive properties, with the corresponding hydroxyapatite/poly(D, L)lactic acid films promoting cellular confluence and a fast formation of collagen fibers as early as after 7 days of culture.

  7. 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.

  8. Synthesis of BaTi2O5 Nanopowders by Sol-Gel Method and the Dielectric Properties of the Ceramics

    NASA Astrophysics Data System (ADS)

    Akishige, Yukikuni; Xu, Jun; Shigematsu, Hirotake; Morito, Shigekazu; Ohba, Takuya

    2009-05-01

    A sol-gel process using barium diethoxide and titanium tetraisopropoxide as the sources for Ba and Ti, respectively, was employed to synthesize BaTi2O5 nanopowders and ceramics. BaTi2O5 nanopowders in the range of 20-50 nm in size were obtained by calcination of the gel precursors at 650 °C. By a further firing at 1000 °C, some BaTi2O5 nanopowders were grown to 200 nm in size. Conventional sintering at 1150 °C using these BaTi2O5 nanopowders yields BaTi2O5 ceramics of 80-85% relative density. A dense BaTi2O5 ceramic with a relative density of above 95% was fabricated by spark plasma sintering (SPS) at 1000 °C. Furthermore, by SPS combined with the hot-forging technique, we obtained a certain degree of grain orientation along the b-axis in the dense BaTi2O5 ceramic and observed an increase in the dielectric constant reaching 580.

  9. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2010-10-01

    Thick film ceramics of 8% mol Y2O3 doped-ZrO2 (8YSZ)-La0.8Sr0.2Ga0.2Mg0.8O3 (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 ZrOCl2ṡ8H2O derived from local zircon as byproduct of Tin processing at Bangka Island using caustic fussion method, and Y(NO3)3. The thick films were produced by screen printing technique on alumina substrates. The films were sintered at 1500° 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.

  11. 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.

  12. 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

  13. [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.

  14. Investigation on the effect of collagen and vitamins on biomimetic hydroxyapatite coating formation on titanium surfaces.

    PubMed

    Ciobanu, Gabriela; Ciobanu, Octavian

    2013-04-01

    This study uses an in vitro experimental approach to investigate the roles of collagen and vitamins in regulating the deposition of hydroxyapatite layer on the pure titanium surface. Titanium implants were coated with a hydroxyapatite layer under biomimetic conditions by using a supersaturated calcification solution (SCS), modified by adding vitamins A and D3, and collagen. The hydroxyapatite deposits on titanium were investigated by means of scanning electron microscopy (SEM) coupled with X-ray analysis (EDX), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and Fourier transformed infrared (FTIR) spectroscopy. The results obtained have shown that hydroxyapatite coatings were produced in vitro under vitamins and collagen influence.

  15. 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.

  16. 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.

  17. 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

  18. 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

  19. 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.

  20. 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.

  1. 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.

  2. 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)

  3. Comparison of in vivo dissolution processes in hydroxyapatite and silicon-substituted hydroxyapatite bioceramics.

    PubMed

    Porter, A E; Patel, N; Skepper, J N; Best, S M; Bonfield, W

    2003-11-01

    The incorporation of silicate into hydroxyapatite (HA) has been shown to significantly increase the rate of bone apposition to HA bioceramic implants. However, uncertainty remains about the mechanism by which silicate increases the in vivo bioactivity of HA. In this study, high-resolution transmission electron microscopy was used to observe dissolution from HA, 0.8 wt% Si-HA and 1.5 wt% Si-HA implants after 6 and 12 weeks in vivo. Our observations confirmed that defects, in particular those involving grain boundaries, were the starting point of dissolution in vivo. Dissolution was observed to follow the order 1.5 wt% Si-HA>0.8 wt% Si-HA>pure HA and it was found to be particularly prevalent at grain boundaries and triple-junctions. These observations may help to explain the mechanism by which silicate ions increase the in vivo bioactivity of pure HA, and highlight the enhanced potential of these ceramics for biomedical applications.

  4. Surface Corrosion of Nanoscaled Hydroxyapatite During an In Vivo Experiment.

    PubMed

    Seo, Dong Seok; Lee, Jong Kook; Hwang, Kyu Hong

    2015-10-01

    Hydroxyapatite (HA) is widely used as a bioactive ceramics as it forms a chemical bond with bone. However, the drawback to using this material is its inferior mechanical properties. In this research, surface corrosion and disintegration of nanoscaled HA in a dog were studied, and the mechanism by which phase-pure HA dissolved in vivo was investigated. Biological properties of HA in vivo are affected by the grain-boundary dissolution followed by a surface corrosion and microstructural disintegration. This kind of dissolution process, apparently evidenced at the grain boundary, causes particle generation, which indicates that both long-term bone in-growth and mechanical properties can dramatically deteriorate. Implant dissolution by osteoclasts in vivo is also observed on the surface of hydroxyapatite. Implant surface showed an aggressive corrosion by an osteoclast resorption. Severe and deeper dissolution underwent close to osteoclast resulting in formation of smaller and more round particle shape.

  5. Biological activity of lactoferrin-functionalized biomimetic hydroxyapatite nanocrystals

    PubMed Central

    Nocerino, Nunzia; Fulgione, Andrea; Iannaccone, Marco; Tomasetta, Laura; Ianniello, Flora; Martora, Francesca; Lelli, Marco; Roveri, Norberto; Capuano, Federico; Capparelli, Rosanna

    2014-01-01

    The emergence of bacterial strains resistant to antibiotics is a general public health problem. Progress in developing new molecules with antimicrobial properties has been made. In this study, we evaluated the biological activity of a hybrid nanocomposite composed of synthetic biomimetic hydroxyapatite surface-functionalized by lactoferrin (LF-HA). We evaluated the antimicrobial, anti-inflammatory, and antioxidant properties of LF-HA and found that the composite was active against both Gram-positive and Gram-negative bacteria, and that it modulated proinflammatory and anti-inflammatory responses and enhanced antioxidant properties as compared with LF alone. These results indicate the possibility of using LF-HA as an antimicrobial system and biomimetic hydroxyapatite as a candidate for innovative biomedical applications. PMID:24623976

  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. 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.

  8. 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.

  9. Phosphonate-hydroxyapatite hybrid compounds prepared by hydrothermal method

    NASA Astrophysics Data System (ADS)

    Agougui, H.; Aissa, A.; Maggi, S.; Debbabi, M.

    2010-12-01

    Calcium hydroxyapatite (CaHAp) was prepared in the presence of two alkylphosphonates, the tert-butyl phosphonic acid TBPOH and the 2-carboxyletylphosphonic acid 2-CEPA, by hydrothermal method at 120 °C for 15 h. The modification of hydroxyapatite by grafting organic moieties is confirmed by IR and NMR MAS ( 1H and 31P) spectroscopy and chemical analysis. X-ray powder diffraction patterns show that the incorporation of organic moieties induces a significant loss of the material crystallinity and a clear increase of the unit cell lattice parameter a as function of 2-CEPA grafting rate. The specific surface area (SSA) increases with increasing phosphonate amount especially for 2-CEPA. All techniques show the lower reactivity of TBPOH due to the steric effects of tert-butyl, whereas the 2-CEPA with a linear chain and double acidic functions is more reactive and can replace the OH - groups of the apatitic structure.

  10. Comparison of Electrical Properties between Fluoroapatite and Hydroxyapatite Materials

    NASA Astrophysics Data System (ADS)

    Laghzizil, A.; El Herch, N.; Bouhaouss, A.; Lorente, G.; Macquete, J.

    2001-01-01

    By appropriate modifications of existing precipitation methods, apatite samples of formula M10(PO4)6X2 (M=Ca, Pb, Ba and X=F, OH) were prepared at 80°C. Samples were characterized using X-ray diffraction, infrared, 31P NMR, SEM, and chemical analysis. By comparing the effect of fluoride and hydroxide ions on ionic conductivity measurements, it was concluded that the fluorinated materials (MFAp) were better conductors than other hydroxyapatites (MHAp). The F- and H+ ions are the main charge carriers, respectively, in fluoroapatite and in hydroxyapatite compounds. The most pronounced effect on the conduction properties was observed in the lead apatite material. These results should provide important physico-chemical information for ionic diffusion of the roles played by fluoride in inhibiting dental caries.

  11. Sorption behavior of fluoride ions from aqueous solutions by hydroxyapatite.

    PubMed

    Jiménez-Reyes, M; Solache-Ríos, M

    2010-08-15

    The effects of pH, contact time, fluoride-ion concentration, and the dose of sorbent on the sorption of fluoride ions by hydroxyapatite were studied. Equilibrium was reached in 16 h of contact time and the maximum sorption of fluoride ions was in the pH(eq) range between 5 and 7.3. The highest efficiency in the sorption system was determined by using 0.01 g of hydroxyapatite and 25 mL of solution. The pseudo-second order model described the kinetic sorption processes, and the Freundlich model, the sorption isotherm process. These results indicated that the mechanism was chemisorption on a heterogeneous material. Fluoride ions were partially desorbed using an alkaline solution.

  12. Structural properties of silver doped hydroxyapatite and their biocompatibility.

    PubMed

    Ciobanu, C S; Iconaru, S L; Pasuk, I; Vasile, B S; Lupu, A R; Hermenean, A; Dinischiotu, A; Predoi, D

    2013-04-01

    The aim of this study was to obtain a novel hydroxyapatite-based material with high biocompatibility. The structural properties of the samples were well characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and X-ray Photoelectron Spectroscopy (XPS). The X-ray diffraction studies revealed the characteristic peaks of hydroxyapatite in each sample. Other phases or impurities were not observed. The scanning electron microscopy observations suggest that the doping components have no influence on the surface morphology of the samples, 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) and X-ray Photoelectron Spectroscopy analyses. Nanocrystalline silver doped HAp stimulated viability and potentiated the activation of murine macrophages.

  13. Modification of the supramolecular structure of collagen with nanodisperse hydroxyapatite

    NASA Astrophysics Data System (ADS)

    Voloskova, E. V.; Berdnikova, L. K.; Poluboyarov, V. A.; Gur'yanova, T. I.

    2015-02-01

    The influence of nanodisperse particles of hydroxyapatite on the structure of films based on collagen with a molecular mass of 360 kDa was studied. When coatings formed, the collagen macromolecules aggregated into spherulites; modification led to structural changes related to the decomposition of the spherulite structure and the formation of a grain structure. The variation of the physicomechanical properties of film materials directly depends on the size of the structural units.

  14. Repairing the hole in hydroxyapatite orbital implants following peg removal.

    PubMed

    Jordan, D R

    2000-01-01

    Pegging hydroxyapatite implants may lead to improved prosthetic eye movement but may also be associated with complications that may occasionally require peg removal. Removing the peg and leaving the peg hole to spontaneously granulate in, is one technique to deal with the remaining implant hole. The author describes a simple technique to fill the peg hole that provides a smooth implant-conjunctival-prosthesis interface and may potentially allow repegging.

  15. Laser microfabrication of hydroxyapatite-osteoblast-like cell composites.

    PubMed

    Doraiswamy, A; Narayan, R J; Harris, M L; Qadri, S B; Modi, R; Chrisey, D B

    2007-03-01

    We have developed a novel approach for layer-by-layer growth of tissue-engineered materials using a direct writing process known as matrix assisted pulsed laser evaporation direct write (MAPLE DW). Unlike conventional cell-seeding methods, this technique provides the possibility for cell-material integration prior to artificial tissue fabrication. This process also provides greater flexibility in selection and processing of scaffold materials. In addition, MAPLE DW offers rapid computer-controlled deposition of mesoscopic voxels at high spatial resolutions. We have examined MAPLE DW processing of zirconia and hydroxyapatite scaffold materials that can provide a medical device with nearly inert and bioactive implant-tissue interfaces, respectively. We have also demonstrated codeposition of hydroxyapatite, MG 63 osteoblast-like cells, and extracellular matrix using MAPLE DW. We have shown that osteoblast-like cells remain viable and retain the capacity for proliferation when codeposited with bioceramic scaffold materials. Our results on MG 63-hydroxyapatite composites can be extended to develop other integrated cell-scaffold structures for medical and dental applications.

  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. 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

  18. 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.

  19. 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.

  20. 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.

  1. Selecting metal oxide nanomaterials for arsenic removal in fixed bed columns: from nanopowders to aggregated nanoparticle media.

    PubMed

    Hristovski, Kiril; Baumgardner, Andrew; Westerhoff, Paul

    2007-08-17

    This paper investigates the feasibility of arsenate removal by aggregated metal oxide nanoparticle media in packed bed columns. Batch experiments conducted with 16 commercial nanopowders in four water matrices were used to select a metal oxide nanoparticle that both amply removes arsenate and can be aggregated using an inert binder. TiO2, Fe(2)O(3), ZrO2 and NiO nanopowders, which exhibited the highest arsenate removal in all water matrices, were characterized with fitted Freundlich adsorption isotherm (q=KC(e)(1/n)) parameters. In 10 mM NaHCO3 buffered nanopure water and at both pH approximately 6.7 and 8.4, K ranged from 1.3 to 12.09(mg As/g(media))(L/mg As)(1/n), and 1/n ranged from 0.21 to 0.52. Under these conditions, the fitted Freundlich isotherm parameters for TiO2 nanoparticles aggregated with inorganic and organic binders (K of 4.75-28.45(mg As/g(media))(L/mg As)(1/n) and 1/n of 0.37-0.97) suggested favorable arsenate adsorption. To demonstrate that aggregated nanoparticle media would allow rapid mass transport of arsenate in a fixed bed adsorber setting, short bed adsorber (SBA) tests were conducted on TiO2 nanoparticle aggregates at empty bed contact times (EBCT) of 0.1-0.5 min and Re x Sc=1000 and 2000. These SBA tests suggested that the binder has a negligible role in adsorbing arsenic and that mass transport is controlled by rapid intraparticle diffusion rather than external film diffusion. PMID:17254707

  2. 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.

  3. One-pot rapid synthesis of core-shell structured NiO@TiO2 nanopowders and their excellent electrochemical properties as anode materials for lithium ion batteries.

    PubMed

    Choi, Seung Ho; Lee, Jong-Heun; Kang, Yun Chan

    2013-12-21

    Core-shell structured NiO@TiO2 nanopowders for application as anode materials for lithium ion batteries are prepared by one-pot flame spray pyrolysis from aqueous spray solution containing Ni and Ti components. A new formation mechanism of the core-shell structured nanopowders in the flame spray pyrolysis is proposed. Composite nanopowders are first formed by surface growth and coagulation from NiO and TiO2 vapors. A small amount of TiO2 in composite powders disturbs the crystallization of TiO2. Therefore, the TiO2 component moves out to the surface of the powders forming an amorphous shell during the formation of single crystalline NiO. The initial discharge and charge capacities of the NiO@TiO2 nanopowders at a current density of 300 mA g(-1) are 1302 and 937 mA h g(-1), respectively. The discharge capacities of the pure NiO and NiO@TiO2 nanopowders after 80 cycles are 542 and 970 mA h g(-1), respectively. The capacity retentions of the pure NiO and NiO@TiO2 nanopowders after 80 cycles measured after the first cycles are 75 and 108%, respectively. PMID:24177597

  4. 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.

  5. 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...

  6. 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.

  7. 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.

  8. 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.

  9. 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.

  10. 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

  11. [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

  12. 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.

  13. [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.

  14. 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.

  15. 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.

  16. 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.

  17. Aging of ceramic carbonized hydroxyapatite at room temperature

    NASA Astrophysics Data System (ADS)

    Tkachenko, M. V.; Kamzin, A. S.

    2016-08-01

    The process of aging of ceramic carbonized hydroxyapatite (CHA) produced in a dry carbon dioxide atmosphere at temperatures of 800-1200°C has been studied by chemical and X-ray structural analysis, infrared spectroscopy, and scanning electron microscopy methods. The phase composition and structure of initial prepared ceramics samples and those aged for a year have been compared. It has been shown that relaxation of internal stresses occurring during pressed sample sintering causes plastic deformation of crystallites at room temperature, accompanied by redistribution of carbonate ions between A1, A2, B1, and B2 sites and CHA decomposition with the formation of CaO separations.

  18. Development of biomimetic nano-hydroxyapatite/poly(hexamethylene adipamide) composites.

    PubMed

    Wang, Xuejiang; Li, Yubao; Wei, Jie; de Groot, Klass

    2002-12-01

    In this study, acicular nano-hydroxyapatite (n-HA) was used to make a new biomimetic composite with polyamide (poly hexamethylene adipamide) by a unique technique. The physical and chemical characteristics of the composites were tested. It was found that these synthesized n-HA crystals were similar to bone apatite in size, phase composition and crystal structure. The biomimetic n-HA crystals were uniformly distributed in the polymer matrix and its content can reach 65%, close to that in natural bone. Chemical binding between inorganic n-HA and polyamide was investigated and discussed. The mechanical properties of the composites were found to match well with those of natural bone.

  19. Synthesis and application of hydroxyapatite and fluoroapatite to scorodite encapsulation

    NASA Astrophysics Data System (ADS)

    Katsarou, Lydia

    Recent research has investigated the precipitation of crystalline scorodite (FeAsO4˙2H2O) as a method to stabilise arsenic for disposal due to its good stability performance according to EPA's TCLP test. It has been determined, however, that scorodite releases arsenic in significant concentrations under alkaline pH or under anoxic conditions. With the objective of enhancing the stability of scorodite, its encapsulation with minerals inert to pH and redox potential variations is considered in this work. Such encapsulation materials are hydroxyapatite (HAP-Ca5(PO4)3OH) and fluoroapatite (FAP-Ca5(PO4)3F), the two most stable of the calcium phosphates. The work described in this thesis includes: 1) the preparation of hydroxyapatite and fluoroapatite powders and their characterisation, 2) the synthesis of crystalline scorodite under atmospheric conditions and its characterisation, 3) the encapsulation of scorodite with hydroxyapatite and fluoroapatite, and 4) the long term stability testing of the encapsulated solids. Hydroxyapatite and fluoroapatite were prepared first by homogeneous precipitation from a metastable solution, to which "Ca" and "PO4" source reagents of different concentrations were added at variable rates. The crystallinity of the produced materials was found to increase with temperature. Crystalline scorodite was produced by seeded crystallisation in ambient pressure. For the encapsulation of the scorodite particles various methods of direct precipitation by controlled supersaturation were attempted, by adjusting the pH and adding/mixing feed solutions of individual calcium and phosphate source reagents. Heterogeneous deposition of HAP on scorodite proved rather difficult. Optimum results were obtained via prior conditioning of the scorodite substrate in a calcium solution and employment of low agitation regime and high (37 °C rather than 22°C) temperature. The stability tests were done in oxic and anoxic environments and their results demonstrated

  20. X-ray diffraction study of cadmium hydroxyapatite

    NASA Astrophysics Data System (ADS)

    Nounah, A.; Maroufi, N.; Ichou, Y. Ait; Lacout, J. L.; Savariault, J. M.

    2005-03-01

    Solid solutions of cadmium and calcium hydroxyapatite [ Ca{10-x}Cdx(PO{4})6(OH){2} (0 ≤ x ≤ 10)] were synthesized by a wet process in a basic medium. The lattice dimensions of these compounds vary linearly with the atom percent cadmium. The distribution of the calcium and cadmium ions between two non-equivalent crystallographic sites, (1) and (2), were determined by the Rietveld method. The site-occupancy factors of atoms indicate a slight preference of cadmium for site (2) in the apatite structure.

  1. 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

  2. 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.

  3. Preparation and Characterization of Fluorescence Probe from Assembly Hydroxyapatite Nanocomposite

    PubMed Central

    2010-01-01

    A new nanocomposite fluorescence probe with thioglycolic acid (TA) functional layers embedded inside the hydroxyapatite nanoribbon spherulites has been synthesized. The fluorescence intensity of the novel probe is about 1.5–3.3-fold increase compared with the probe containing no TA. When used to detect cadmium ion, the most of original assembly nanoribbon spherulites structure in the novel probe is found to have been damaged to new flake structures. The mechanism of determining cadmium ion in alcohol solution has been studied. The present systematic study provides significant information on the effect of assembly nanostructure on the metal-enhanced fluorescence phenomenon. PMID:20672031

  4. Preparation and characterization of hydroxyapatite/liposome core shell nanocomposites

    NASA Astrophysics Data System (ADS)

    Chu, Maoquan; Liu, Guojie

    2005-08-01

    Hydroxyapatite (HAP)/liposome core-shell nanocomposites have been prepared at room temperature. The liposome shells and the precipitate cores ranged in diameter mainly from 80 to 140 nm and from 40 to 120 nm, respectively. Rod-like whiskers ranging in length mainly from 10 to 30 nm were obtained after separating the precipitates from the liposomes. In contrast, the whiskers synthesized without liposomes ranged in length mainly from 70 to 140 nm. The precipitates synthesized both with and without liposomes were poorly crystalline, and had a similar chemical composition to the natural HAP.

  5. 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.

  6. [Hemispheric hydroxyapatite coated cups in total hip arthroplasty].

    PubMed

    Blacha, J; Bednarek, A; Gagała, J

    1998-01-01

    The paper presents principles of implantation as well as clinical and radiological results of hemispheric hydroxyapatite coated cups use in total hip replacement. Eighty-seven patients (60 females, 27 males) aged from 16 to 72 years (mean 49 years) underwent 96 total hip replacements with the use of 51 ABG and 45 OCTOFIT hemispheric cups. Clinical results were satisfactory with an average Harris Hip Score of 89 to 91 at final follow-up. We have found total ingrowth and osteointegration of nearly all cups. In one case of acetabular reconstruction with bone grafts cup migration has been observed and revision was necessary.

  7. [Laboratory evaluation of tooth whitening agents in hydroxyapatite samples].

    PubMed

    Poiurovskaia, I Ia; D'iakonenko, E E; Pozharkova, M E

    2013-01-01

    The paper presents laboratory model for evaluation of the effectiveness of tooth whitening agents on pure and technical hydroxyapatite (HAP) samples. HAP samples were exposed in distilled water, and colour measurements were taken after coloration in tea extract and using of "Blend-a-med delicate bleaching" ("Procter & Gamble", Germany) toothpaste. The proposed laboratory model allows imitating discoloration by food dye (tea) and measure the whitening toothpaste effect by significant change in colour characteristics in the CIE L*a*b* system. PMID:23994846

  8. 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

  9. 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.

  10. 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.

  11. Effects of Cd concentration on structure and optical properties of the ternary Zn1-xCdxO nanopowder prepared by sol-gel method

    NASA Astrophysics Data System (ADS)

    Sui, Y. R.; Cao, Y.; Li, X. F.; Yue, Y. G.; Yao, B.; Lang, J. H.; Li, X. Y.; Yang, J. H.

    2015-06-01

    Zn1-xCdxO nanocrystalline powder with different Cd contents (0≤x≤1) has been prepared by new facile sol-gel route. The crystal structure and optical properties were investigated by X-ray diffraction patterns, Transmission electron microscope, X-ray photoelectron spectroscopy, Photoluminescence. As x varied from x=0 to 0.25, the Zn1-xCdxO nanopowder exhibits a hexagonal wurtzite structure of pure ZnO without any significant formation of a separated CdO phase. For the samples with 0.5≤x≤0.85, the Zn1-xCdxO nanopowder exhibits the coexistence of hexagonal ZnO and cubic CdO phase, meanwhile, the content of ZnO phase decreases while that of CdO increases with increasing the Cd content x. The ultra-violet near-band-edge emission of the Zn1-xCdxO nanopowder was monotonously red-shifted from 389 nm (x=0) to 406 nm (x=0.25) due to the direct modulation of band gap caused by Cd substitution.

  12. Comparison of murine fibroblast cell response to fluor-hydroxyapatite composite, fluorapatite and hydroxyapatite by eluate assay.

    PubMed

    Jantová, Sona; Letasiová, Silvia; Theiszová, Marica; Palou, M

    2009-03-01

    Fluorapatite (FA) is one of the inorganic constituents of bone or teeth used for hard tissue repairs and replacements. Fluor-hydroxyapatite (FHA) is a new synthetic composite that contains the same molecular concentration of OH(-) groups and F(-) ions. The aim of this experiment was to evaluate the cellular responses of murine fibroblast NIH-3T3 cells in vitro to solid solutions of FHA and FA and to compare them with the effect of hydroxyapatite (HA). We studied 24, 48 and 72 h effects of biomaterials on cell morphology, proliferation and cell cycle of NIH-3T3 cells by eluate assay. Furthermore, we examined the ability of FHA, FA and HA to induce cell death and DNA damage. Our cytotoxic/antiproliferative studies indicated that any of tested biomaterials did not cause the total inhibition of cell division. Biomaterials induced different antiproliferative effects increasing in the order HA < FHA < FA which were time- and concentration-dependent. None of the tested biomaterials induced necrotic/apoptotic death of NIH-3T3 cells. On the other hand, after 72 h we found that FHA and FA induced G0/G1 arrest of NIH-3T3 cells, while HA did not affect any cell cycle phases. Comet assay showed that while HA demonstrated weaker genotoxicity, DNA damage induced by FHA and FA caused G0/G1 arrest of NIH-3T3 cells. Fluoridation of hydroxyapatite and different FHA and FA structure caused different cell response of NIH-3T3 cells to biomaterials.

  13. In vitro and in vivo evaluation of silicated hydroxyapatite and impact of insulin adsorption.

    PubMed

    Lasgorceix, M; Costa, A M; Mavropoulos, E; Sader, M; Calasans, M; Tanaka, M N; Rossi, A; Damia, C; Chotard-Ghodsnia, R; Champion, E

    2014-10-01

    This study evaluates the biological behaviour, in vitro and in vivo, of silicated hydroxyapatite with and without insulin adsorbed on the material surface. Insulin was successfully adsorbed on hydroxyapatite and silicated hydroxyapatite bioceramics. The modification of the protein secondary structure after the adsorption was investigated by means of infrared and circular dichroism spectroscopic methods. Both results were in agreement and indicated that the adsorption process was likely to change the secondary structure of the insulin from a majority of α-helix to a β-sheet form. The biocompatibility of both materials, with and without adsorbed insulin on their surface, was demonstrated in vitro by indirect and direct assays. A good viability of the cells was found and no proliferation effect was observed regardless of the material composition and of the presence or absence of insulin. Dense granules of each material were implanted subcutaneously in mice for 1, 3 and 9 weeks. At 9 weeks of implantation, a higher inflammatory response was observed for silicated hydroxyapatite than for pure hydroxyapatite but no significant effect of adsorbed insulin was detected. Though the presence of silicon in hydroxyapatite did not improve the biological behaviour, the silicon substituted hydroxyapatite remained highly viable.

  14. 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.

  15. Cadmium uptake by hydroxyapatite synthesized in different conditions and submitted to thermal treatment.

    PubMed

    da Rocha, Nilce C C; de Campos, Reinaldo C; Rossi, Alexandre M; Moreira, Elizabeth L; Barbosa, Ademarlaudo do F; Moure, Gustavo T

    2002-04-01

    This paper intends to evaluate the uptake of cadmium ions from aqueous solution by 21 hydroxyapatite samples which have been synthesized in different conditions. It has been determined thatthe variation on the hydroxyapatite sorption capacity is neither related to sample solubility nor to hydroxyapatite Ca/P molar ratio. Cd2+ sorption is controlled by sample BET surface area, which shows a direct dependence on the hydroxyapatite crystallite dimensions. The hydroxyapatite pore distribution presented modes at 1000 and 60,000 A, corresponding to intracrystallite voids and voids between the agglomerate of these crystallites, respectively. Pores belonging to the former mode immobilize the major part of Cd2+. The influence of sample thermal treatment on Cd2+ sorption efficiency has been studied using hydroxyapatite samples calcined at temperatures ranging from 500 to 1140 degrees C. Similarly to nonthermally treat samples, the Cd2+ sorption on calcined hydroxyapatite could be described by Langmuir isotherms. The results showed that the maximum sorption capacity decreased from 0.631 mmol g(-1) for the noncalcined sample to 0.150 mmol g(-1) for the one calcined at 900 degrees C. This drop in the sorption capacity could also be explained by a reduction in its specific surface area, which is induced bythe increase of the crystal size.

  16. 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

  17. A highly reproducible continuous process for hydroxyapatite nanoparticles synthesis.

    PubMed

    Gomes, Paulo J; Silva, Viviana M T M; Quadros, Paulo A; Dias, Madalena M; Lopes, José C B

    2009-06-01

    This work presents a continuous process for producing hydroxyapatite nanoparticles (NanoXIM) in a network reactor, NETmix, fed by a calcium solution, a phosphorus solution and an alkaline solution. Hydroxyapatite is considered a biomaterial, used as: food additives and nutritional supplements; bone graft for bone replacement, growth and repair; biocements and coating of metallic implant. Some of the most recent applications include their use in cosmetics, toothpaste and in esthetical treatments for diminishing wrinkles by stimulating conjunctive tissue formation. The proposed process enables the micromixing control, which is essential to form nanometric structures, but it is also a determining factor in the crystals purity, crystallinity and morphology. The reactants distribution scheme at the inlet of the reactor and along the reactor, performed continuously or varying in time, is also a crucial factor to programme the properties of reactant media along the reactor, such as the pH, the supersaturation degree, the Ca/P molar ratio, and the temperature. The calcium phosphate nanoparticles suspension that exits the reactor is submitted to further aging, separation, drying, sintering and milling processes. PMID:19504858

  18. 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.

  19. Functionally Graded Hydroxyapatite Coatings Doped with Antibacterial Components

    SciTech Connect

    Bai, Xiao; More, Karren Leslie; Rouleau, Christopher M; Rabiei, Afsaneh

    2010-01-01

    A series of functionally graded hydroxyapatite (FGHA) coatings incorporated with various percentages of silver were deposited on titanium substrates using ion beam assisted deposition (IBAD). The analysis of the coating s cross-section using transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM), equipped with energy dispersive X-ray spectroscopy (EDS), has shown a decreased crystallinity as well as a distribution of nano scale (10 ~ 50nm) silver particles from the coating/substrate interface to top surface. Both X-ray diffraction (XRD) and fourier transform infrared spectroscopy (FTIR) results revealed the presence of hydroxyapatite within the coatings. The amount of Ag (wt. %) on the outer surface of the FGHA, as determined from X-ray photoelectron spectroscopy (XPS), ranged from 1.09 ~ 6.59, which was about half of the average Ag wt. % incorporated in the entire coating. Average adhesion strengths evaluated by pull-off tests were in the range of 83 6 - 88 3 MPa, which is comparable to 85 MPa for FGHA without silver. Further optical observations of failed areas illustrated that the dominant failure mechanism was epoxy failure and FGHA coating delamination was not observed.

  20. 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.

  1. 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.

  2. Coating of titanium with hydroxyapatite leads to decreased bone formation

    PubMed Central

    Bøe, B. G.; Støen, R. Ø.; Solberg, L. B.; Reinholt, F. P.; Ellingsen, J. E.; Nordsletten, L.

    2012-01-01

    Objectives An experimental rabbit model was used to test the null hypothesis, that there is no difference in new bone formation around uncoated titanium discs compared with coated titanium discs when implanted into the muscles of rabbits. Methods A total of three titanium discs with different surface and coating (1, porous coating; 2, porous coating + Bonemaster (Biomet); and 3, porous coating + plasma-sprayed hydroxyapatite) were implanted in 12 female rabbits. Six animals were killed after six weeks and the remaining six were killed after 12 weeks. The implants with surrounding tissues were embedded in methyl methacrylate and grinded sections were stained with Masson-Goldners trichrome and examined by light microscopy of coded sections. Results Small amounts of bone were observed scattered along the surface of five of the 12 implants coated with porous titanium, and around one out of 12 porous coated surfaces with Bonemaster. No bone formation could be detected around porous coated implants with plasma-sprayed hydroxyapatite. Conclusion Porous titanium coating is to some degree osteoinductive in muscles. PMID:23610682

  3. Phase purity of sol-gel-derived hydroxyapatite ceramic.

    PubMed

    Hsieh, M F; Perng, L H; Chin, T S; Perng, H G

    2001-10-01

    Calcium oxide was reported in the sol-gel-derived hydroxyapatite (HA) as an unavoidable major impurity. In this study phase purity of HA synthesized by sol-gel route was explored using precursors of calcium nitrate tetrahydrate and triethyl phosphate. Two different drying methods, the fast drying of as-prepared precursors and the slow drying of aged precursors were adopted as major processing variables. The dried gels were subsequently calcined up to 600 degrees C. In the calcined powder from fast-dried gel, X-ray diffraction (XRD) patterns revealed an intense CaO peak. For the slow-dried gel, thermogravimetric analysis revealed a 2-step weight-loss behavior during heating. XRD analysis of the calcined powder, corresponding to the second weight-loss step, showed major peaks of hydroxyapatite and a very weak CaO peak. P-31 NMR analysis indicated formation of calcium phosphate complex during aging. Complete incorporation of Ca(NO3)2 into the complex due to proper aging therefore diminishes CaO formation. It was also found that the minor CaO derived in the slow drying method can be easily and completely washed out just by distilled water.

  4. Hydroxyapatite synthesis on solid surfaces using a biological approach

    NASA Astrophysics Data System (ADS)

    Wang, A.; Mei, J.; Tse, Y. Y.; Jones, I. P.; Sammons, R. L.

    2012-12-01

    Many naturally occurring mineralisation processes yield hydroxyapatite (HA) or related salts, but biological routes to calcification have not generally been exploited for production of hydroxyapatite for clinical and industrial applications. Serratia sp. NCIMB 40259 is a non-pathogenic Gram-negative bacterium which is capable of growing as a biofilm on many surfaces and can be used to form HA coatings on a variety of polymeric and metallic materials, including titanium. Here we review previous work and report the results of more recent studies on the influence of titanium compositional and surface properties on Serratia adherence and proliferation and biomineralisation on commercially pure titanium (cp Ti) discs and a Ti mesh. Bacterial adherence was equivalent on cpTi and Ti6Al4V, and biofilms formed on both rough and mirror-polished cpTi surfaces. Embedded alumina particles and alkali treatment did not noticeably alter the precipitation of Serratia HA, nor the structure of the coating in comparison with non-treated substrates. Coatings were retained after sintering at 800°C in argon, although the original curved plate-like crystals changed to nano-scale β-tricalcium phosphate particles. A phosphorous-rich diffusion zone formed at the coating-titanium interface. Bacterial mineralisation may have applications as a method for producing coatings on implants in non load-bearing sites, and non-clinical applications where a high surface area is the major concern.

  5. 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.

  6. 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.

  7. 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.

  8. 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.

  9. Thermal and structural characterization of synthetic and natural nanocrystalline hydroxyapatite.

    PubMed

    Sofronia, Ancuta M; Baies, Radu; Anghel, Elena M; Marinescu, Cornelia A; Tanasescu, Speranta

    2014-10-01

    The aim of this work was to study the thermal stability on heating and to obtain the processing parameters of synthetic and bone-derived hydroxyapatite over temperatures between room temperature and 1400°C by thermal analysis (thermogravimetry (TG)/differential scanning calorimetry (DSC) and thermo-mechanical analysis-TMA). Structural and surface modifications related to samples origin and calcination temperature were investigated by Fourier transformed infrared (FTIR) and Raman spectroscopy, X-ray diffraction (XRD) and BET method. FTIR spectra indicated that the organic constituents and carbonate are no longer present in the natural sample calcined at 800°C. Raman spectra highlighted the decomposition products of the hydroxyapatite. The calcination treatment modifies the processes kinetics of the synthetic samples, being able to isolate lattice water desorption processes of decarbonization and the dehydroxylation processes. Shrinkage of calcined synthetic sample increases by 10% compared to uncalcined synthetic powder. From the TMA correlated with TG analysis and heat capacity data it can be concluded that sintering temperature of the synthetic samples should be chosen in the temperature range of the onset of dehydroxylation and the temperature at which oxyapatite decomposition begins.

  10. 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.

  11. 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.

  12. Tailoring the Microstructure of Sol–Gel Derived Hydroxyapatite/Zirconia Nanocrystalline Composites

    PubMed Central

    2011-01-01

    In this study, we tailor the microstructure of hydroxyapatite/zirconia nanocrystalline composites by optimizing processing parameters, namely, introducing an atmosphere of water vapor during sintering in order to control the thermal stability of hydroxyapatite, and a modified sol–gel process that yields to an excellent intergranular distribution of zirconia phase dispersed intergranularly within the hydroxyapatite matrix. In terms of mechanical behavior, SEM images of fissure deflection and the presence of monoclinic ZrO2 content on cracked surface indicate that both toughening mechanisms, stress-induced tetragonal to monoclinic phase transformation and deflection, are active for toughness enhancement. PMID:24764458

  13. [Effects of hydroxyapatite on growth and quality of potato (Solanum tuberosum L.) in Cd polluted soil].

    PubMed

    Song, Yong; He, Tan; Liu, Ming-Yue; Zeng, Min; Liao, Bo-Han

    2010-09-01

    A pot experiment was conducted in a glasshouse to study effects of hydroxyapatite amending Cd polluted soil on growth and quality of potato (Solanum tuberosum L.). In the experiment, 3 levels of Cd pollution (0, 5, and 10 mg x kg(-1)) and 6 levels of hydroxyapatite application (0, 4, 8, 10, 16, and 30 g x kg(-1)) in soil were prepared to plant 2 potato varieties (Zhongshusanhao and Daxiyang in Chinese system). The results showed that Cd pollution in soil resulted in decrease in yield per plant of potato; for example, in the soils with 5 and 10 mg x kg(-1) of Cd, the yield per plant decreased 24%-31% and 41%-45%, respectively. Applying hydroxyapatite to Cd pollution could greatly increase yield per plant of potato. Compared to the soil without hydroxyapatite, 10 or 30 g x kg(-1) hydroxyapatite added to the soil with 5 or 10 mg x kg(-1) of Cd increased 17%-9% or 45%-58% in yield per plant. Due to hydroxyapatite amending Cd polluted soil, chlorophyll contents in leaves and superoxide dismutase (SOD) activities in tubers enhanced and malondialdehyde (MDA) contents in tubers declined apparently. Meanwhile, quality of potato tubers was obviously improved, such as increase in vitamin C contents, starch contents, and protein contents in potato tubers. With hydroxyapatite applying from 0 to 30 g x kg(-1), Cd contents in potato tubers deceased from 0.87-0.95 mg x kg(-1) to 0.13-0.21 mg x kg(-1) by 78%-85% in the soils with 5 mg x kg(-1) of Cd, and from 1.86-1.93 mg x kg(-1) to 0.52-0.65 mg x kg(-1) by 66%-72% in the soils with 10 mg x kg(-1) of Cd. The experiment indicated that the mechanism of hydroxyapatite alleviating soil Cd toxicity main included rising soil pH values, reducing effective Cd contents in soil, and Ca from hydroxyapatite blocking soil Cd moving to potato. However, ability of hydroxyapatite alleviating soil Cd toxicity was limited, and excessive hydroxyapatite to soil exhibited stress effects on growth and quality of potato. In the Cd polluted soils with

  14. 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

  15. 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

  16. Hydroxyapatite, fluor-hydroxyapatite and fluorapatite produced via the sol-gel method: dissolution behaviour and biological properties after crystallisation.

    PubMed

    Tredwin, Christopher J; Young, Anne M; Abou Neel, Ensanya A; Georgiou, George; Knowles, Jonathan C

    2014-01-01

    Hydroxyapatite (HA), fluor-hydroxyapatite (FHA) with varying levels of fluoride ion substitution and fluorapatite (FA) were synthesised by the sol-gel method as possible implant coating or bone-grafting materials. Calcium nitrate and triethyl phosphite were used as precursors under an ethanol-water based solution. Different amounts of ammonium fluoride were incorporated for the preparation of the FHA and FA sol-gels. After heating and powdering the sol-gels, dissolution behaviour was assessed using ion chromatography to measure Ca(2+) and PO4 (3-) ion release. Biological behaviour was assessed using cellular proliferation with human osteosarcoma cells and alamarBlue™ assay. Statistical analysis was performed with a two way analysis of variance and post hoc testing with a Bonferroni correction. Increasing fluoride substitution into an apatite structure decreased the dissolution rate. Increasing the firing temperature of the HA, FHA and FA sol-gels up to 1,000 °C decreased the dissolution rate. There was significantly higher cellular proliferation on highly substituted FHA and FA than on HA or Titanium. The properties of an implant coating or bone grafting material can be tailored to meet specific requirements by altering the amount of fluoride that is incorporated into the original apatite structure. The dissolution behaviour can further be altered by the temperature at which the sol-gel is fired.

  17. 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

  18. 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.

  19. Towards the synthesis of hydroxyapatite/protein scaffolds with controlled porosities: bulk and interfacial shear rheology of a hydroxyapatite suspension with protein additives.

    PubMed

    Maas, Michael; Bodnar, Pedro Marcus; Hess, Ulrike; Treccani, Laura; Rezwan, Kurosch

    2013-10-01

    The synthesis of porous hydroxyapatite scaffolds is essential for biomedical applications such as bone tissue engineering and replacement. One way to induce macroporosity, which is needed to support bone in-growth, is to use protein additives as foaming agents. Another reason to use protein additives is the potential to introduce a specific biofunctionality to the synthesized scaffolds. In this work, we study the rheological properties of a hydroxyapatite suspension system with additions of the proteins bovine serum albumin (BSA), lysozyme (LSZ) and fibrinogen (FIB). Both the rheology of the bulk phase as well as the interfacial shear rheology are studied. The bulk rheological data provides important information on the setting behavior of the thixotropic suspension, which we find to be faster with the addition of FIB and LSZ and much slower with BSA. Foam bubble stabilization mechanisms can be rationalized via interfacial shear rheology and we show that it depends on the growth of interfacial films at the suspension/air interface. These interfacial films support the stabilization of bubbles within the ceramic matrix and thereby introduce macropores. Due to the weak interaction of the protein molecules with the hydroxyapatite particles of the suspension, we find that BSA forms the most stable interfacial films, followed by FIB. LSZ strongly interacts with the hydroxyapatite particles and thus only forms thin films with very low elastic moduli. In summary, our study provides fundamental rheological insights which are essential for tailoring hydroxyapatite/protein suspensions in order to synthesize scaffolds with controlled porosities.

  20. 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.

  1. Dielectric response and specific heat studies of Cd2Nb2O7 ceramics obtained from mechano-synthesized nanopowders.

    PubMed

    Połomska, Maria; Hilczer, Bożena; Markiewicz, Ewa; Trybuła, Zbigniew; Andrzejewski, Bartłomiej; Szafraniak-Wiza, Izabela; Pietraszko, Adam

    2013-08-01

    Cd(2)Nb(2)O(7) is still an interesting ferroelectric material because of its high permittivity value at helium temperatures and a variety of dielectric relaxation processes, the origin of which is still puzzling. We prepared hot-pressed ceramics, with grain sizes from 100 to 150 nm, obtained from Cd(2)Nb(2)O(7) nanopowders synthesized by high-energy milling of CdO and Nb(2)O(5) and studied their dielectric response and thermal properties. The nanoceramics were characterized by X-ray diffraction and their dielectric properties were measured at temperatures from 4K to 575K. Dielectric response of the nanoceramics was found to consist of a huge anomaly at ~150K with complex dielectric absorption and three relaxation processes apparent in frequency and temperature dependences of the imaginary part of permittivity in the temperature range from 18K to 145K. The anomaly at ~150K is related to overlapping contributions from the Curie point (shifted downward because of the size effect) and a dielectric relaxation process. The behavior of three relaxation modes observed at temperatures below 145K is discussed, based on the model proposed by Malcherek of polar nanoregions in the orthorhombic phase of Cd(2)Nb(2)O(7) and the theory of dielectric response of ferroelectric relaxors by Bokov and Ye.

  2. CONDENSED MATTER: STRUCTURE, MECHANICAL AND THERMAL PROPERTIES: Comparative Study of Activity of Different Agings of Aluminum Nanopowders

    NASA Astrophysics Data System (ADS)

    Yan, Zheng-Xin; Deng, Jun; Wanf, Ya-Min; Liu, Wei

    2009-08-01

    The structure and activity of aluminum nanopowders with a 3 nm oxide layer on their surface (3-nm-OLA) and 30 nm oxide layers on their surface (30-nm-OLA) are investigated comparably under the same normal incident shock wave intensity. Their corresponding reaction products are characterized by x-ray diffraction, high-resolution transmission electron microscopy and x-ray photoelectron spectroscopy. The spectrum of x-ray diffraction shows that there are different phases of alumina in their products, which evidences directly the different reacting temperature in the shock tube. The x-ray photoelectron spectroscopy reveals that the oxide layer thickness is 30 nm on the product surface of 30-nm-OLA, while it is only 3 nm on 3-nm-OLA. Images of transmission electron microscopy present additional evidence that the agglomeration mechanism is over sintering one in the containing-30-nm-OLA system, the reversed mechanism is observed in the containing-3-nm-OLA reaction system.

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. Application of the soluble salt-assisted route to scalable synthesis of ZnO nanopowder with repeated photocatalytic activity

    NASA Astrophysics Data System (ADS)

    Lv, Yingying; Yu, Leshu; Huang, Heyong; Feng, Yuying; Chen, Dongzhen; Xie, Xin

    2012-02-01

    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.

  8. 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.

  9. 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.

  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. Optical Imaging of Hydroxyapatite in the Calcified Vasculature of Transgenic Animals

    PubMed Central

    Zaheer, Atif; Murshed, Monzur; De Grand, Alec M.; Morgan, Timothy G.; Karsenty, Gerard; Frangioni, John V.

    2009-01-01

    Objective To detect the hydroxyapatite component of vascular calcification in vivo so that the process of calcium deposition can be studied in transgenic model systems. Methods and Results We have previously developed a near-infrared fluorescent bisphosphonate derivative that binds with high affinity and specificity to hydroxyapatite, and an intraoperative near-infrared fluorescence imaging system for small animals. Using these tools, and a transgenic mouse strain with homozygous deletion of the matrix GLA protein (mgp−/−), we demonstrate that the hydroxyapatite component of vascular calcification can be detected in vivo with high sensitivity, specificity and resolution. Conclusions The hydroxyapatite component of vascular calcification can be detected optically, in real-time, without sacrifice of the animal. It is now possible to study the earliest events associated with vascular mineralization, at the cell and organ level, and to monitor the process in living animals. PMID:16484598

  13. 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.

  14. Synthesis and cellular biocompatibility of two nanophase hydroxyapatite with different Ca/P ratio.

    PubMed

    Zhao, Yantao; Zhang, Yumei; Zhao, Yimin; Hou, Shuxun; Chu, Paul K

    2011-12-01

    The cellular biocompatibility of two types of nanophase hydroxyapatites including nanophase standard hydroxyapatite (n-HA) and nanophase calcium deficient hydroxyapatite (n-CDHA) synthesized by a wet chemical method were assessed using primary cultured osteoblasts. Cytotoxicity of both materials was investigated with L929 cell line. The MTT method was used to evaluate the proliferation of osteoblasts on the third day and ALP activity assay was carried out on the fifth day. SEM was used to observe the morphology of the osteoblasts on the third day. Two types of nanophase hydroxyapatite both showed no cytotoxicity. Higher cell proliferation was observed on n-CDHA than n-HA. At the same time, cells spread more actively on the n-CDHA group. The ALP level of n-CDHA was also significantly higher on the former. Our results show that the n-CDHA is more suitable for osteoblasts growth and is also helpful for ALP synthesis.

  15. 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

  16. 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

  17. Novel silk fibroin films prepared by formic acid/hydroxyapatite dissolution method.

    PubMed

    Ming, Jinfa; Liu, Zhi; Bie, Shiyu; Zhang, Feng; Zuo, Baoqi

    2014-04-01

    Bombyx mori silk fibroin from the silkworm was firstly found to be soluble in formic acid/hydroxyapatite system. The rheological behavior of silk fibroin solution was significantly influenced by HAp contents in dissolved solution. At the same time, silk fibroin nanofibers were observed in dissolved solution with 103.6±20.4nm in diameter. Moreover, the structure behavior of SF films prepared by formic acid/hydroxyapatite dissolution method was examined. The secondary structure of silk fibroin films was attributed to silk II structure (β-sheet), indicating that the hydroxyapatite contents in dissolved solution were not significantly affected by the structure of silk fibroin. The X-ray diffraction results exhibited obviously hydroxyapatite crystalline nature existing in silk fibroin films; however, when the hydroxyapatite content was 5.0wt.% in dissolved solution, some hydroxyapatite crystals were converted to calcium hydrogen phosphate dehydrate in silk fibroin dissolution process. This result was also confirmed by Fourier transform infrared analysis and DSC measurement. In addition, silk fibroin films prepared by this dissolution method had higher breaking strength and extension at break. Based on these analyses, an understanding of novel SF dissolution method may provide an additional tool for designing and synthesizing advanced materials with more complex structures, which should be helpful in different fields, including biomaterial applications.

  18. In Vitro Evaluation of Nanoscale Hydroxyapatite-Based Bone Reconstructive Materials with Antimicrobial Properties.

    PubMed

    Ajduković, Zorica R; Mihajilov-Krstev, Tatjana M; Ignjatović, Nenad L; Stojanović, Zoran; Mladenović-Antić, Snezana B; Kocić, Branislava D; Najman, Stevo; Petrović, Nenad D; Uskoković, Dragan P

    2016-02-01

    In the field of oral implantology the loss of bone tissue prevents adequate patient care, and calls for the use of synthetic biomaterials with properties that resemble natural bone. Special attention is paid to the risk of infection after the implantation of these materials. Studies have suggested that some nanocontructs containing metal ions have antimicrobial properties. The aim of this study was to examine the antimicrobial and hemolytic activity of cobalt-substituted hydroxyapatite nanoparticles, compared to hydroxyapatite and hydroxyapatite/poly-lactide-co-glycolide. The antibacterial effects of these powders were tested against two pathogenic bacterial strains: Escherichia coi (ATCC 25922) and Staphylococcus aureus (ATCC 25923), using the disc diffusion method and the quantitative antimicrobial test in a liquid medium. The quantitative antimicrobial test showed that all of the tested biomaterials have some antibacterial properties. The effects of both tests were more prominent in case of S. aureus than in E coli. A higher percentage of cobalt in the crystal structure of cobalt-substituted hydroxyapatite nanoparticles led to an increased antimicrobial activity. All of the presented biomaterial samples were found to be non-hemolytic. Having in mind that the tested of cobalt-substituted hydroxyapatite (Ca/Co-HAp) material in given concentrations shows good hemocompatibility and antimicrobial effects, along with its previously studied biological properties, the conclusion can be reached that it is a potential candidate that could substitute calcium hydroxyapatite as the material of choice for use in bone tissue engineering and clinical practices in orthopedic, oral and maxillofacial surgery.

  19. Interactions between dodecyl phosphates and hydroxyapatite or tooth enamel: relevance to inhibition of dental erosion.

    PubMed

    Jones, Siân B; Barbour, Michele E; Shellis, R Peter; Rees, Gareth D

    2014-05-01

    Tooth surface modification is a potential method of preventing dental erosion, a form of excessive tooth wear facilitated by softening of tooth surfaces through the direct action of acids, mainly of dietary origin. We have previously shown that dodecyl phosphates (DPs) effectively inhibit dissolution of native surfaces of hydroxyapatite (the type mineral for dental enamel) and show good substantivity. However, adsorbed saliva also inhibits dissolution and DPs did not augment this effect, which suggests that DPs and saliva interact at the hydroxyapatite surface. In the present study the adsorption and desorption of potassium and sodium dodecyl phosphates or sodium dodecyl sulphate (SDS) to hydroxyapatite and human tooth enamel powder, both native and pre-treated with saliva, were studied by high performance liquid chromatography-mass Spectrometry. Thermo gravimetric analysis was used to analyse residual saliva and surfactant on the substrates. Both DPs showed a higher affinity than SDS for both hydroxyapatite and enamel, and little DP was desorbed by washing with water. SDS was readily desorbed from hydroxyapatite, suggesting that the phosphate head group is essential for strong binding to this substrate. However, SDS was not desorbed from enamel, so that this substrate has surface properties different from those of hydroxyapatite. The presence of a salivary coating had little or no effect on adsorption of the DPs, but treatment with DPs partly desorbed saliva; this could account for the failure of DPs to increase the dissolution inhibition due to adsorbed saliva.

  20. Biocompatibility of hydroxyapatite scaffolds processed by lithography-based additive manufacturing.

    PubMed

    Tesavibul, Passakorn; Chantaweroad, Surapol; Laohaprapanon, Apinya; Channasanon, Somruethai; Uppanan, Paweena; Tanodekaew, Siriporn; Chalermkarnnon, Prasert; Sitthiseripratip, Kriskrai

    2015-01-01

    The fabrication of hydroxyapatite scaffolds for bone tissue engineering applications by using lithography-based additive manufacturing techniques has been introduced due to the abilities to control porous structures with suitable resolutions. In this research, the use of hydroxyapatite cellular structures, which are processed by lithography-based additive manufacturing machine, as a bone tissue engineering scaffold was investigated. The utilization of digital light processing system for additive manufacturing machine in laboratory scale was performed in order to fabricate the hydroxyapatite scaffold, of which biocompatibilities were eventually evaluated by direct contact and cell-culturing tests. In addition, the density and compressive strength of the scaffolds were also characterized. The results show that the hydroxyapatite scaffold at 77% of porosity with 91% of theoretical density and 0.36 MPa of the compressive strength are able to be processed. In comparison with a conventionally sintered hydroxyapatite, the scaffold did not present any cytotoxic signs while the viability of cells at 95.1% was reported. After 14 days of cell-culturing tests, the scaffold was able to be attached by pre-osteoblasts (MC3T3-E1) leading to cell proliferation and differentiation. The hydroxyapatite scaffold for bone tissue engineering was able to be processed by the lithography-based additive manufacturing machine while the biocompatibilities were also confirmed. PMID:26484553

  1. Biocompatibility of hydroxyapatite scaffolds processed by lithography-based additive manufacturing.

    PubMed

    Tesavibul, Passakorn; Chantaweroad, Surapol; Laohaprapanon, Apinya; Channasanon, Somruethai; Uppanan, Paweena; Tanodekaew, Siriporn; Chalermkarnnon, Prasert; Sitthiseripratip, Kriskrai

    2015-01-01

    The fabrication of hydroxyapatite scaffolds for bone tissue engineering applications by using lithography-based additive manufacturing techniques has been introduced due to the abilities to control porous structures with suitable resolutions. In this research, the use of hydroxyapatite cellular structures, which are processed by lithography-based additive manufacturing machine, as a bone tissue engineering scaffold was investigated. The utilization of digital light processing system for additive manufacturing machine in laboratory scale was performed in order to fabricate the hydroxyapatite scaffold, of which biocompatibilities were eventually evaluated by direct contact and cell-culturing tests. In addition, the density and compressive strength of the scaffolds were also characterized. The results show that the hydroxyapatite scaffold at 77% of porosity with 91% of theoretical density and 0.36 MPa of the compressive strength are able to be processed. In comparison with a conventionally sintered hydroxyapatite, the scaffold did not present any cytotoxic signs while the viability of cells at 95.1% was reported. After 14 days of cell-culturing tests, the scaffold was able to be attached by pre-osteoblasts (MC3T3-E1) leading to cell proliferation and differentiation. The hydroxyapatite scaffold for bone tissue engineering was able to be processed by the lithography-based additive manufacturing machine while the biocompatibilities were also confirmed.

  2. 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

  3. 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.

  4. 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.

  5. Review of ferroelectric hydroxyapatite and its application to biomedicine

    NASA Astrophysics Data System (ADS)

    Lang, Sidney B.

    2016-08-01

    Hydroxyapatite (HA) is a major component of bone in humans and animals. Until about 10 years ago, it was considered to have a centrosymmetric crystal structure and could not contribute to the well-known piezoelectric effect in bone. This review describes the theoretical and experimental studies that showed that HA does have a non-centrosymmetric structure. Recent experiments have shown that HA exhibits piezoelectricity, pyroelectricity, and ferroelectricity. It has been made in the form of thick films and as space-charge electrets. It has an important biomedical application as an implant for bone cell attachment and growth. This paper is contributed in honor of the 80th birthday of my long-time friend and colleague, Bozena Hilczer.

  6. Development of carbon nanotube-reinforced hydroxyapatite bioceramics

    NASA Astrophysics Data System (ADS)

    Kealley, Catherine; Elcombe, Margaret; van Riessen, Arie; Ben-Nissan, Besim

    2006-11-01

    This paper reports development of a production method to create a composite material that is biocompatible, which will have high mechanical strength and resilience, and be able to withstand exposure to the physiological environment. The chemical precipitation conditions necessary for the production of single-phase synthetic hydroxyapatite (HAp) and a HAp and carbon nanotube (CNT) composite material have been optimised. Neutron diffraction patterns collected before and after sintering show that the nanotubes have remained intact within the structure, while most of the remaining soot has burnt off. Small-angle neutron scattering, in conjunction with scanning electron microscopy (SEM), also shows preservation of the CNTs. Hot isostatically pressed samples showed excellent densification. Neutron diffraction data has enabled the positions of the hydroxide bonds to be determined, and shown that the addition of the CNTs has had no effect on the structural parameters of the HAp phase, with the exception of a slight reduction in the unit cell parameter a.

  7. 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

  8. Sulfobetaine as a zwitterionic mediator for 3D hydroxyapatite mineralization.

    PubMed

    Liu, Pingsheng; Song, Jie

    2013-03-01

    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

  9. 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.

  10. 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.

  11. 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.

  12. Structural and dielectric properties of yttrium-substituted hydroxyapatites.

    PubMed

    Kaygili, Omer; Dorozhkin, Sergey V; Ates, Tankut; Gursoy, N Canan; Keser, Serhat; Yakuphanoglu, Fahrettin; Selçuk, A Birkan

    2015-02-01

    Hydroxyapatite (HAp) samples doped with 0, 2 and 4 at.% of yttrium (Y) were characterized using X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy attached with energy dispersive X-ray (EDX) spectroscopy, antimicrobial activity tests and dielectric studies. The hydroxyl groups observed in FTIR spectra confirmed the formation of HAp phase in the studied samples. The crystallite size, crystallinity degree and lattice parameters of the samples were changed with Y content. The volume of the unit cell was gradually decreased with the addition of Y. Undoped and Y-containing HAp samples were screened to determine their in vitro antimicrobial activities against the standard strains. It was found that no samples have any antimicrobial effect. The relative dielectric permittivity and dielectric loss are affected by Y content. While the alternating current conductivity increases with increasing frequency, it decreases with increasing Y content.

  13. Textured hydroxyapatite interface onto biomedical titanium-based coatings.

    PubMed

    Manso, Miguel; Herrero, P; Fernández, M; Langlet, M; Martínez-Duart, J M

    2003-03-15

    Hydroxyapatite (HAP) bioceramic coatings grown onto titanium-nitride (TiN) buffer layers by the aerosol-gel procedure present interfaces with a preferred growth orientation. These coatings were crystallized at 800 degrees C and subsequently etched to ease the study of the interface by Auger electron spectroscopy depth profiling. Ion beam milling was applied to cross-section samples to analyze the interface structures using transmission electron microscopy. At the interface, the HAP crystals showed a <002> orientation. It was shown by Auger electron spectroscopy depth profiling that O atoms diffuse into the nitride interlayer, indicating that the formation of O channels in the HAP structure is the driving force inducing the textured film. The outstanding biocompatible properties of both the materials and properties of their interface suggest that HAP/TiN structures are particularly well suited for endoprosthetic applications.

  14. 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.

  15. 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

  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. 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.

  18. Recombinant human-like collagen directed growth of hydroxyapatite nanocrystals

    NASA Astrophysics Data System (ADS)

    Zhai, Y.; Cui, F. Z.

    2006-05-01

    Bones are biocomposites with hierarchical structure that require controlled mineral deposition during their self-assembly to form tissues with unique mechanical properties. Type I collagen proteins, acidic extracellular matrix proteins, play a critical role in mineral formation and many researches on artificial bones have been made inspired by nature using type I collagen derived from animal tissues. Here we report that recombinant human-like type I collagen, an acidic protein, can direct growth of hydroxyapatite (HA) nanocrystals in vitro in the form of self-assembly of nano-fibrils of mineralized collagen resembling extracellular matrix. The mineralized collagen fibrils aligned parallel to each other to form mineralized collagen fibers. HA nanocrystals grew on the surface of these collagen fibrils with the c-axis of nanocrystals of HA orienting along the longitudinal axis of the fibrils. These artificial analogs of bone have a potential clinical application in bone repair.

  19. Crystallinity and solubility behavior of iron-containing fluoridated hydroxyapatites.

    PubMed

    Okazaki, M; Takahashi, J; Kimura, H

    1986-09-01

    Iron-containing fluoridated hydroxyapatites with various fluoride contents were synthesized at 80 degrees C and pH 7.4 using FeCl2 X nH2O as a source of iron. The Fe2+ uptake of fluoridated apatites was independent of fluoride concentration in the solution. a-Axis dimensions of Fe-containing apatites decreased with the degree of fluoridation in addition to the decrease related to the substitution of Fe2+ ions. All Fe-containing fluoridated apatites were less well crystallized than Fe-free fluoridated apatites previously reported, although with increasing degree of fluoridation, the crystallinity behavior of the former apatites appeared analogous to that of the latter apatites. In contrast to this inhibited crystallinity behavior, the apparent solubility of Fe-containing fluoridated apatites decreased more than that of Fe-free fluoridated apatites at low fluoride content.

  20. 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

  1. Clinical and radiological results of hydroxyapatite-coated acetabular cups.

    PubMed

    Blacha, J; Gagała, J

    2004-12-01

    We prospectively studied a consecutive series of 60 primary total hip arthroplasties in 52 patients. All patients had a hydroxyapatite-coated hemispherical acetabular cup (OCTOFIT). Mean patient age was 52.5 (34-73) years. In 38 hips, a 28-mm and in 22 hips a 32-mm diameter cobalt-chrome femoral head was used. We could follow 53 hips for a mean of 81 (28-125) months. Four cups were revised because of osteolysis, and in another six cups, slight osteolysis without migration was seen. The average annual linear wear rate was 0.05 mm (+/-0.05) for 28-mm heads and 0.16 mm (+/-0.09) for 32-mm heads (p<0.0001). Survivorship analysis predicted a survival rate of 86+/-6.7% at 10 years.

  2. 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.

  3. 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

  4. 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

  5. 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.

  6. Mechanisms of uranium interactions with hydroxyapatite: implications for groundwater remediation.

    PubMed

    Fuller, C C; Bargar, J R; Davis, J A; Piana, M J

    2002-01-15

    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 apatite-based 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 microM 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 < or = 4,700 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 > or = 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.

  7. 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.

  8. 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.

  9. In vitro effects of fluor-hydroxyapatite, fluorapatite and hydroxyapatite on colony formation, DNA damage and mutagenicity.

    PubMed

    Jantová, S; Theiszová, M; Letasiová, S; Birosová, L; Palou, T M

    2008-04-30

    The number of biomaterials used in biomedical applications has rapidly increased in the past two decades. Fluorapatite (FA) is one of the inorganic constituents of bone or teeth used for hard-tissue repairs and replacements. Fluor-hydroxyapatite (FHA) is a new synthetically prepared composite that in its structure contains the same molecular concentration of OH(-) groups and F(-) ions. The aim of this experimental investigation was to evaluate cytotoxic, genotoxic and mutagenic effects of FHA and FA eluates on Chinese hamster V79 cells and to compare them with the effects of hydroxyapatite (HA) eluate. Cytotoxicity of the biomaterials tested was evaluated by use of the cell colony-formation assay and by direct counting of the cells in each colony. Genotoxicity was assessed by single-cell gel electrophoresis (comet assay) and mutagenicity was evaluated by the Hprt gene-mutation assay and in bacterial mutagenicity tests using Salmonella typhimurium TA100. The results show that the highest test concentrations of the biomaterials (100% and 75% eluates) induced very weak inhibition of colony growth (about 10%). On the other hand, the reduction of cell number per colony induced by these concentrations was in the range from 43% to 31%. The comet assay showed that biomaterials induced DNA breaks, which increased with increasing test concentrations in the order HA

  10. Thermally stimulated transformations in brookite-containing TiO2 nanopowders produced by the hydrolysis of TiCl4

    NASA Astrophysics Data System (ADS)

    Shul'ga, Yu. M.; Kabachkov, E. N.; Matyushenko, D. V.; Kurkin, E. N.; Domashnev, I. A.

    2011-01-01

    TiO2 nanopowder is produced by the low-temperature hydrolysis of TiCl4. The phase composition of the sample is found to form at a hydrolysis temperature of 30-38°C. Low-temperature annealing (up to 440°C) increases the degree of crystallinity of the phases present in the sample (anatase, brookite) and only weakly affects their ratio. At 500°C, the sample consists of three phases: rutile is detected apart from anatase and brookite. Brookite begins to fail at 600°C; at 700°C, crystalline brookite fails completely.

  11. 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.

  12. 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

  13. 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.

  14. Spectral investigations on undoped and Cu²⁺ doped ZnO-CdS composite nanopowders.

    PubMed

    Rao, G Thirumala; Babu, B; Stella, R Joyce; Manjari, V Pushpa; Ravikumar, R V S S N

    2015-03-15

    Undoped and Cu(2+) doped ZnO-CdS composite nanopowders were synthesized by simple chemical precipitation method. Structural and spectroscopic properties of the prepared samples have been characterized by XRD, SEM with EDS, TEM, FT-IR, UV-Vis, EPR and Photoluminescence studies. X-ray diffraction pattern contains a series of peaks corresponds to hexagonal phase of ZnO and CdS. The average crystallite sizes of undoped and Cu(2+) doped samples are determined and are in the range of 25-30 nm. SEM and TEM micrographs reveal that the samples show spherical like structures with little agglomeration. FT-IR spectra show the fundamental mode of vibrations of ZnO at 515 cm(-1), CdS at 621 cm(-1) and other functional groups. Optical absorption spectrum of Cu(2+) doped sample consists of three bands at 665, 823 and 1192 nm attributed to the transitions (2)B1g→(2)Eg, (2)B2g and (2)A1g respectively. Crystal field and tetragonal field parameters are evaluated as Dq=1214, Ds=1610 and Dt=389 cm(-1). From EPR, spin-Hamiltonian and hyperfine splitting parameters are evaluated for Cu(2+) doped sample as g‖=2.3391, g⊥=2.0550 and A‖=130×10(-4) cm(-1), A⊥=36×10(-4) cm(-1). The optical and EPR data suggests that Cu(2+) entered into host lattice as tetragonally distorted octahedral site symmetry. PL spectra consists two emission bands at 367, 380 nm in UV region. A sharp blue emission peak at 425 nm and a broad green emission peak in the range of 450-570 nm are observed. The enhanced visible emission is observed after doping.

  15. Ferromagnetism and optical properties of La1 − x Al x FeO3 nanopowders

    PubMed Central

    2014-01-01

    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. PMID:25246876

  16. Effects of Ytterbium Oxide Nanopowder Particle Size on the Acoustic Properties of Silicone Rubber Lens for Medical Echo Array Probe

    NASA Astrophysics Data System (ADS)

    Yohachi; Yamashita; Hosono, Yasuharu; Yamamoto, Noriko; Itsumi, Kazuhiro

    2008-05-01

    The effects of Yb2O3 powder particle size, namely, 2000, 16, and 8 nm, on the physical and acoustic properties of a high-temperature-vulcanization (HTV) silicone (Q) rubber have been investigated in order to develop an acoustic lens material with a low sound velocity (c) and acoustic attenuation coefficient (α). The Yb2O3-doped HTV Q rubber with the large particle size of 2000 nm showed a density (ρ) of 1.6×103 kg/m3, with c = 828 m/s, characteristic acoustic impedance (Z) = 1.32×106 kg·m-2·s-1, α= 1.32 dB·mm-1·MHz-1, and an α-figure of merit (FOM) (α×c) of 1090 at 5 MHz at 37 °C. For the Yb2O3-doped Q rubber with the small particle size of 8 nm, ρ= 1.57×103 kg/m3, c = 864 m/s, Z = 1.36×106 kg·m-2·s-1, α= 0.68 dB·mm-1·MHz-1, and α-FOM = 590. The 16 nm Yb2O3-doped Q rubber had intermediate values of α= 0.88 dB·mm-1·MHz-1 and α-FOM = 760. These results show that there is a clear dopant particle size dependence on the acoustic properties of Yb2O3-doped HTV Q rubbers. The 8-nm-doped HTV Q rubber also showed an excellent mechanical properties for practical application. Microstructure observation revealed that the low-α rubber shows a uniform Yb2O3 nanopowder distribution in the HTV Q rubber matrix.

  17. Effects of Ceramic Nanopowder Dopants on Acoustic Attenuation Properties of Silicone Rubber Lens for Medical Echo Probe

    NASA Astrophysics Data System (ADS)

    Yamashita, Yohachi (John); Hosono, Yasuharu; Itsumi, Kazuhiro

    2007-07-01

    The effects of fine ceramic powder dopants, namely, TiO2, Al2O3, BaSO4, Fe2O3, ZrO2, and Yb2O3 with primary particle sizes of 16-100 nm, on the acoustic properties of silicone rubber have been investigated, in order to develop an acoustic lens material for medical echo probes with a low acoustic attenuation (α). Silicone rubber doped with Yb2O3 powder having a high density (ρ) of 9.2× 103 kg/m3 and an average particle size of 16 nm showed a lower acoustic attenuation than silicone rubber doped with other powders. The materials showed ρ=1.54× 103 kg/m3, a sound velocity (c)=882 m/s, an acoustic impedance ρ\\cdot c (Z)=1.36× 106 kg m-2 s-1, and an acoustic attenuation α=0.93 dB mm-1 MHz-1 at 37 °C. Silicone rubber doped with Fe2O3 powder having ρ=5.2× 103 kg/m3 and an average particle size of 30 nm showed the highest α=2.36 dB mm-1 MHz-1 and Z=1.47× 106 kg m-2 s-1. Microstructure observation of the rubber by scanning microscopy revealed that the α of the powder-doped rubber is not only determined by the primary particle size of the powders but also by the dispersion and agglomeration of the secondary particles in the rubber matrix. The discovery of the process parameter required to reduce the α of the nanopowder-doped silicone rubber has an important practical consequence.

  18. 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.

  19. 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.

  20. 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.

  1. 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

  2. Healing of segmental bone defects with granular porous hydroxyapatite augmented with recombinant human osteogenic protein-1 or autologous bone marrow.

    PubMed

    den Boer, Frank C; Wippermann, Burkhard W; Blokhuis, Taco J; Patka, Peter; Bakker, Fred C; Haarman, Henk J Th M

    2003-05-01

    Hydroxyapatite is a synthetic bone graft, which is used for the treatment of bone defects and nonunions. However, it is a rather inert material with no or little intrinsic osteoinductive activity. Recombinant human osteogenic protein-1 (rhOP-1) is a very potent biological agent, that enhances osteogenesis during bone repair. Bone marrow contains mesenchymal stem cells, which are capable of new bone formation. Biosynthetic bone grafts were created by the addition of rhOP-1 or bone marrow to granular porous hydroxyapatite. The performance of these grafts was tested in a sheep model and compared to the results of autograft, which is clinically the standard treatment of bone defects and nonunions. A 3 cm segmental bone defect was made in the tibia and fixed with an interlocking intramedullary nail. There were five treatment groups: no implant (n=6), autograft (n=8), hydroxyapatite alone (n=8), hydroxyapatite loaded with rhOP-1 (n=8), and hydroxyapatite loaded with autologous bone marrow (n=8). At 12 weeks, healing of the defect was evaluated with radiographs, a torsional test to failure, and histological examination of longitudinal sections through the defect. Torsional strength and stiffness of the healing tibiae were about two to three times higher for autograft and hydroxyapatite plus rhOP-1 or bone marrow compared to hydroxyapatite alone and empty defects. The mean values of both combination groups were comparable to those of autograft. There were more unions in defects with hydroxyapatite plus rhOP-1 than in defects with hydroxyapatite alone. Although the differences were not significant, histological examination revealed that there was more often bony bridging of the defect in both combination groups and the autograft group than in the group with hydroxyapatite alone. Healing of bone defects, treated with porous hydroxyapatite, can be enhanced by the addition of rhOP-1 or autologous bone marrow. The results of these composite biosynthetic grafts are equivalent to

  3. 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

  4. 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%.

  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. 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.

  7. BMP2-loaded hollow hydroxyapatite microspheres exhibit enhanced osteoinduction and osteogenicity in large bone defects.

    PubMed

    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 m(2)/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.

  8. 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.

  9. 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.

  10. 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.

  11. 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

  12. 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

  13. 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.

  14. Ceramic and non-ceramic hydroxyapatite as a bone graft material: a brief review.

    PubMed

    Dutta, S R; Passi, D; Singh, P; Bhuibhar, A

    2015-03-01

    Treatment of dental, craniofacial and orthopedic defects with bone graft substitutes has shown promising result achieving almost complete bone regeneration depending on product resorption similar to human bone's physicochemical and crystallographic characteristics. Among these, non-ceramic and ceramic hydroxyapatite being the main inorganic salt of bone is the most studied calcium phosphate material in clinical practices ever since 1970s and non-ceramic since 1985. Its "chemical similarity" with the mineralized phase of biologic bone makes it unique. Hydroxyapatite as an excellent carrier of osteoinductive growth factors and osteogenic cell populations is also useful as drug delivery vehicle regardless of its density. Porous ceramic and non-ceramic hydroxyapatite is osteoconductive, biocompatible and very inert. The need for bone graft material keeps on increasing with increased age of the population and the increased conditions of trauma. Recent advances in genetic engineering and doping techniques have made it possible to use non-ceramic hydroxyapatite in larger non-ceramic crystals and cluster forms as a successful bone graft substitute to treat various types of bone defects. In this paper we have mentioned some recently studied properties of hydroxyapatite and its various uses through a brief review of the literatures available to date. PMID:25428698

  15. BMP2-loaded hollow hydroxyapatite microspheres exhibit enhanced osteoinduction and osteogenicity in large bone defects.

    PubMed

    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 m(2)/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

  16. 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

  17. 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

  18. Hydroxyapatite supported Ag3PO4 nanoparticles with higher visible light photocatalytic activity

    NASA Astrophysics Data System (ADS)

    Hong, Xiaoting; Wu, Xiaohui; Zhang, Qiuyun; Xiao, Mingfeng; Yang, Gelin; Qiu, Meirong; Han, Guocheng

    2012-03-01

    Hydroxyapatite supported Ag3PO4 nanocomposites have been synthesized by a wet impregnation process. UV-vis absorption spectra show a red shift of the absorption edges for the composite systems compared to pure hydroxyapatite support. The surface structure and morphology of the nanocomposites were characterized by Brunauer-Emmett-Teller (BET) apparatus, X-ray diffraction (XRD), transmission electron microscopy (TEM). The results suggest that Ag3PO4 nanoparticles (6-17 nm in diameter) are well dispersed on the hydroxyapatite support and Ag3PO4 nanoparticles density is larger for the higher Ag+ loading sample. The as-prepared nanocomposite photocatalysts showed a pronounced photocatalytic activity upon decomposition of methylene blue dye in aqueous solution under both visible light (wavelength > 400 nm) and UV-vis light irradiation. A synergic mechanism of inherent photocatalytic capability of Ag3PO4 and the accelerated electron/hole separation resulting from the photoinduced electrons captured by the slow-released Ag+ at the interface of Ag3PO4 and hydroxyapatite is proposed for the nanocomposites on the enhancement of photocatalytic performance in comparison to that of pure Ag3PO4 nanoparticles. The support of hydroxyapatite may also act as an absorbent which favors the mass transfer in heterogeneous photocatalysis reaction.

  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. Open-Porous Hydroxyapatite Scaffolds for Three-Dimensional Culture of Human Adult Liver Cells.

    PubMed

    Finoli, Anthony; 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.

  1. Nano-hydroxyapatite and its applications in preventive, restorative and regenerative dentistry: a review of literature.

    PubMed

    Pepla, Erlind; Besharat, Lait Kostantinos; Palaia, Gaspare; Tenore, Gianluca; Migliau, Guido

    2014-07-01

    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.

  2. Novel synthesis strategy for composite hydrogel of collagen/hydroxyapatite-microsphere originating from conversion of CaCO3 templates.

    PubMed

    Wei, Qingrong; Lu, Jian; Wang, Qiaoying; Fan, Hongsong; Zhang, Xingdong

    2015-03-20

    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.

  3. 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...

  4. Deformation band-like defects as possible precursors to microfracture planes, resulting in the generation of nanopowders on simulated fault planes

    NASA Astrophysics Data System (ADS)

    Toy, V. G.; Wirth, R.; Mitchell, T. M.

    2013-12-01

    The development of at least partially ';amorphous' and/or ';nanocrystalline' materials within fault principal slip zones has been shown to reduce frictional shear resistance during fault slip. Thus it is proposed generation of these materials facilitates shear localization and possibly even seismic slip. The generation of such materials has been demonstrated experimentally, both in high velocity friction experiments at ambient conditions (e.g. silica gels reported by Goldsby & Tullis, 2002: GRL 29, 1844; Di Toro et al., 2004: Nature 427, 436), and very low velocity shear experiments at higher temperatures and confining pressures (e.g. apparent pseudotachylytes reported by Pec et al, 2012: EPSL 355-356, 299). They have also been reported in natural fault zones (e.g. natural silica gel from the Corona Fault described by Kirkpatrick et al., in press: Geology). These materials commonly comprise some proportion of randomly-oriented nanocrystals embedded in a non-crystalline matrix that displays no TEM diffraction contrast or lattice fringes. Proposed generation mechanisms include: irradiation damage, deformation, application of pressure, and chemical reactions. In particular, Pec et al., (2012) proposed that micro-comminution processes precede the generation of lattice defects. In this study we show that partially-amorphous silica material can be generated experimentally on a saw-cut surface in novaculite during shear at ~8 x 10-4m/s, in a Griggs apparatus under Pconf ~0.5 GPa, T = 450 and 600°C. The material comprises angular nanocrystals ranging from 2-10 nm diameter in a entirely non-crystalline matrix,has variable density that increases with decreasing proportion of nanocrystal remnants, suggesting it is a partially compacted nanopowder. This material is restricted to a zone <50 μm wide between the sawcut sliders. We infer an origin by micro-comminution, wherein repeated microfracturing results in formation of a very high proportion of non-crystalline surfaces

  5. 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.

  6. 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.

  7. 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.

  8. Monitoring of hydroxyapatite crystal formation using field-effect transistor

    NASA Astrophysics Data System (ADS)

    Kajisa, Taira; Sakata, Toshiya

    2016-04-01

    The biomineralization process of hydroxyapatite (HAp) in simulated body fluid (SBF) was monitored in realtime using extended-gate FETs whose gate electrode was modified with a variety of alkanethiol self-assembled monolayers (SAMs). It was found that the gate surface potential of the carboxyl- and amino-group-terminated SAM-coated gate FET was increased in SBF as HAp crystals grew on the gate surface. Moreover, in the carboxyl-group-terminated SAM-coated gate FET, the rate of increase and the shift of gate surface potential of the FET were found to depend on the concentration of calcium ions in the SBF. It was concluded that the process of HAp crystallization at a SAM-modified surface can be detected using FETs. Thus, a FET device that enables the easy detection of ionic charges in a real-time and label-free manner, will be useful for evaluating biomaterials based on biomineralization such as those in the bone regeneration process.

  9. Impedance and modulus spectroscopic study of nano hydroxyapatite

    NASA Astrophysics Data System (ADS)

    Jogiya, B. V.; Jethava, H. O.; Tank, K. P.; Raviya, V. R.; Joshi, M. J.

    2016-05-01

    Hydroxyapatite (Ca10 (PO4)6 (OH)2, HAP) is the main inorganic component of the hard tissues in bones and also important material for orthopedic and dental implant applications. Nano HAP is of great interest due to its various bio-medical applications. In the present work the nano HAP was synthesized by using surfactant mediated approach. Structure and morphology of the synthesized nano HAP was examined by the Powder XRD and TEM. Impedance study was carried out on pelletized sample in a frequency range of 100Hz to 20MHz at room temperature. The variation of dielectric constant, dielectric loss, and a.c. conductivity with frequency of applied field was studied. The Nyquist plot as well as modulus plot was drawn. The Nyquist plot showed two semicircle arcs, which indicated the presence of grain and grain boundary effect in the sample. The typical behavior of the Nyquist plot was represented by equivalent circuit having two parallel RC combinations in series.

  10. 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.

  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. 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

  13. Biofilm formation on nanostructured hydroxyapatite-coated titanium.

    PubMed

    Westas, Emma; Gillstedt, Martin; Lönn-Stensrud, Jessica; Bruzell, Ellen; Andersson, Martin

    2014-04-01

    Biofilm formation on medical devices is a common cause of implant failure, especially regarding implants that breach the epithelial tissue, so-called transcutaneous implants. Nanotechnology and the development of new nanomaterials have given the opportunity to design nanotextured implant surfaces. Such surfaces have been studied using various in vitro methods showing that nanosized features strongly benefit bone cell growth. However, little is known on how nanostructured features affect biofilm formation. The aim of this study was therefore to examine the shape- and chemical-dependent effect of a nanostructured hydroxyapatite (HA) coating on the degree of Staphylococcus epidermidis biofilm formation. Three different types of nanosized HA particles having different shapes and calcium to phosphate ratios were compared to uncoated turned titanium using safranin stain in a biofilm assay and confocal laser scanning microscopy (CLSM) for assessment of biofilm biomass and bacterial volume, respectively. No difference in biofilm biomass was detected for the various surfaces after 6 h incubation with S. epidermidis. Additionally, image analysis of CLSM Z-stacks confirmed the biofilm assay and showed similar results. In conclusion, the difference in nanomorphology and chemical composition of the surface coatings did not influence the adhesion and biofilm formation of S. epidermidis.

  14. 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

  15. [A novel nano-hydroxyapatite/aliphatic polyesteramide composite].

    PubMed

    Deng, Xia; Chen, Zhiqing; Qian, Zhiyong; Liu, Caibing; Li, Hong

    2008-04-01

    Hydrothermally synthesized nano-hydroxyapatite (n-HA) varying in weight from 10% to 30% was used as filler to make nanocomposites with novel aliphatic polyesteramide (PEA) in our laboratory. The structure and properties of PEA and its n-HA composites were investigated through transmission electron microscopy, infrared spectrometry, X-ray diffractioin, scanning electron microscopy and energy spectrometry. The shape and size of the n-HA crystals are similar to those of the apatite crystals in natural bone. Molecule interactions are present between the n-HA and PEA in the composite, which allows the uniform dispersion of n-HA in PEA matrix. This contributes enhanced mechanical property and bioactivity to the composite. The cytocompatibility of the composites has been investigated by culturing osteoblasts on the membranes. Good cell attachment and proliferation manner were observed on the membranes after 1 week. These results suggest that the PEA/n-HA composites prepared in this study may serve as potential candidate scaffold for tissue engineering.

  16. Interfacial stress transfer in a graphene nanosheet toughened hydroxyapatite composite

    NASA Astrophysics Data System (ADS)

    Zhang, L.; Zhang, X. G.; Chen, Y.; Su, J. N.; Liu, W. W.; Zhang, T. H.; Qi, F.; Wang, Y. G.

    2014-10-01

    In recent years, graphene has emerged as potential reinforcing nanofiller in the composites for structural engineering due to its extraordinary high elastic modulus and mechanical strength. As recognized, the transfer of stress from a low modulus matrix to a high-modulus reinforcing graphene and the interfacial behavior at a graphene-matrix interface is the fundamental issue in these composites. In the case of graphene nanosheet (GNS) reinforced hydroxyapatite (HA) composite, this research presented analytical models and simulated that the number of graphene layers of GNSs has little effect on the maximum axial stress (˜0.35 GPa) and the maximum shear stress (˜0.14 GPa) at a GNS-HA interface, and the energy dissipation by GNS pull-out decreases with increasing the number of graphene layers due to weak bonding between them. Also, GNS-HA interfacial delamination and/or GNS rupture were also indentified to be the two key failure mechanisms. The computed results are expected to facilitate a better understanding of the interfacial behavior at a GNS-ceramic interface and to achieve tough ceramics reinforced with GNSs.

  17. Hydroxyapatite moldable formulation using natural rubber latex as binder.

    PubMed

    Sailaja, G S; Ramesh, P; Varma, H K

    2007-07-01

    A simple but efficient processing method for shaping intricate bioceramic green bodies has been developed by using natural rubber latex as binder. Different shapes of hydroxyapatite Ca10(PO4)6(OH)2 (HAP) were molded from a composite formulation containing wet precipitated HAP, natural rubber latex (NRL), and a stabilizer. On controlled heat treatment followed by sintering, dense shapes of HAP contours were obtained. The thermal degradation profile of HAP-NRL composites shows that NRL degrades slowly without any abrupt exotherm. The results of energy dispersive X-ray analysis together with inductively coupled plasma (ICP) analysis indicate that the inorganic residue of NRL does not contain any heavy element. The sintered density of the samples increased with increased HAP content in the formulation and percentage shrinkage reduced accordingly. On varying the HAP content in the formulation from 35 to 95 wt %, the compositions with 85, 90, 92, and 95 wt % HAP showed better flexural strength in the range 40-54 MPa and a flexural modulus value in the range 36-50 GPa. The fracture morphology, as observed by the scanning electron microscope confirms that with increased HAP content in the formulation the sample microstructure attains higher uniformity. The Vickers microhardness for the samples sintered at two different temperatures (1150 and 1250 degrees C) showed that hardness increases with increase in the sintering temperature with a maximum for the highest HAP loaded formulation.

  18. Adsorption and spectroscopic characterization of lactoferrin on hydroxyapatite nanocrystals.

    PubMed

    Iafisco, Michele; Di Foggia, Michele; Bonora, Sergio; Prat, Maria; Roveri, Norberto

    2011-01-28

    Lactoferrin (LF), a well-characterized protein of blood plasma and milk with antioxidant, cariostatic, anticarcinogenic and anti-inflammatory properties, has been adsorbed onto biomimetic hydroxyapatite (HA) nanocrystals at two different pH values (7.4 and 9.0). The interaction was herein investigated by spectroscopic, thermal and microscopic techniques. The positive electrostatic surface potential of LF at pH 7.4 allows a strong surface interaction with the slightly negative HA nanocrystals and avoids the protein-protein interaction, leading to the formation of a coating protein monolayer. In contrast, at pH 9.0 the surface potential of LF is a mix of negative and positive zones favouring the protein-protein interaction and reducing the interaction with HA nanocrystals; as a result a double layer of coating protein was formed. These experimental findings are supported by the good fittings of the adsorption isotherms by different theoretical models according to Langmuir, Freundlich and Langmuir-Freundlich models. The nanosized HA does not appreciably affect the conformation of the adsorbed protein. In fact, using FT-Raman and FT-IR, we found that after adsorption the protein was only slightly unfolded with a small fraction of the α-helix structure being converted into turn, while the β-sheet content remained almost unchanged. The bioactive surface of HA functionalized with LF could be utilized to improve the material performance towards the biological environment for biomedical applications.

  19. 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

  20. A new hydroxyapatite-based biocomposite for bone replacement.

    PubMed

    Bellucci, Devis; Sola, Antonella; Gazzarri, Matteo; Chiellini, Federica; Cannillo, Valeria

    2013-04-01

    Since the 1970s, various types of ceramic, glass and glass-ceramic materials have been proposed and used to replace damaged bone in many clinical applications. Among them, hydroxyapatite (HA) has been successfully employed thanks to its excellent biocompatibility. On the other hand, the bioactivity of HA and its reactivity with bone can be improved through the addition of proper amounts of bioactive glasses, thus obtaining HA-based composites. Unfortunately, high temperature treatments (1200°C÷1300°C) are usually required in order to sinter these systems, causing the bioactive glass to crystallize into a glass-ceramic and hence inhibiting the bioactivity of the resulting composite. In the present study novel HA-based composites are realized and discussed. The samples can be sintered at a relatively low temperature (800 °C), thanks to the employment of a new glass (BG_Ca) with a reduced tendency to crystallize compared to the widely used 45S5 Bioglass®. The rich glassy phase, which can be preserved during the thermal treatment, has excellent effects in terms of in vitro bioactivity; moreover, compared to composites based on 45S5 Bioglass® having the same HA/glass proportions, the samples based on BG_Ca displayed an earlier response in terms of cell proliferation. PMID:23827547

  1. Surface characterization of hydroxyapatite: potentiometric titrations coupled with solubility measurements.

    PubMed

    Skartsila, Kyriaki; Spanos, Nikos

    2007-04-15

    The acid-base properties of synthetically prepared and well-characterized hydroxyapatite (HAP) in contact with KNO3 solutions were investigated at 25 degrees C, through potentiometric titrations, zeta-potential measurements, and surface complex modeling. Aliquots of suspension were withdrawn every 0.5 pH unit during the titration procedure and analyzed for calcium and phosphate. It was found that, even for rapid titration experiments, a remarkable amount of H+ ions (H+dissol.) is consumed in the bulk solution in reacting with species coming from the dissolution of HAP. These H+ ions must be taken into account in the H+ mass balance, in order for true value for the point of zero charge (pzc=6.5+/-0.2) and consequently true value for the surface charge (sigma0) to be obtained. Besides the conventional potentiometric titration technique, it was found that pzc may be determined much more easily as the intersection point of the suspension titration curve and the blank one modified to include the amount of H+dissol. obtained at one ionic strength. Finally, a surface complexation model was proposed for the development of surface charge. Experimental data were satisfactorily fitted by using the value of 4.2 F m-2 for the capacitance.

  2. 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.

  3. 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.

  4. 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

  5. Dental Hetero-Graft Materials with Nano Hydroxyapatite Surface Treatment.

    PubMed

    Kim, Dai-Hwan; Kim, Kyung-Il; Yoon, Seokyoung; Kim, Hyung-Jo; Ahn, Jin-Soo; Jun, Sang Ho; Kang, Ho Chang; Pang, Changhyun; Kim, Jaeyun; Cha, Hyung Joon; Han, Kwon-Hoon; Kim, Dong-Myong; Lee, Jung Heon

    2015-10-01

    We report the development of hydroxyapatite nanoparticle (HAp NP)-functionalized hetero-graft materials (HGMs) for dental applications. These HGMs were prepared by attaching platelet-, needle-, and sphere-shaped HAp NPs to the surface of xenograft materials through chemical conjugation. Although all three HAp NPs contributed to increase the surface area of bone graft material (BGM), the shape of the HAp NPs was a determining factor. Platelet HAp NPs were most effective, because they caused a 48.9% increase in BGM surface area whereas the influence of the spherical NP was only a 6.7% increase. This suggests that geometric factors regarding both the attached HAp NPs and graft material surface are essential in controlling the surface roughness of graft materials. Among the three HAp NPs, it was the platelet HAp NPs that helped to increase the efficacy of the BGM most significantly. Compared with BGM with no HAp NP attachment, HGM with platelet HAp NP ('platelet-HGM) treatment had ~46.1% higher cell attachment and proliferation rate. The MTT assay also showed that the HAp NP-treated hetero-graft materials had negligible cytotoxicity. PMID:26726444

  6. 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.

  7. 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

  8. Surface modification of hydroxyapatite. Part I. Dodecyl alcohol.

    PubMed

    Borum-Nicholas, L; Wilson, O C

    2003-09-01

    The influence of esterification reactions on the surface chemistry and colloid stability of hydroxyapatite (HAP) was studied by aging nanophase HAP in dodecyl alcohol at elevated temperatures (115 degrees C and 190 degrees C). The esterified HAP particles were characterized by X-ray diffraction, transmission electron microscopy, diffuse reflectance infra-red Fourier transform spectroscopy (DRIFTS), thermal gravimetric analysis, sedimentation time studies, and electrophoretic mobility (mu) measurements in water and ethyl alcohol. DRIFTS analysis revealed that the HAP surface was modified by dodecyl groups based on the appearance of C-H stretch vibrational modes at 2962, 2930, and 2860cm(-1). Dodecyl alcohol modified HAP exhibited a larger TGA mass loss upon heating (up to 4.8%) compared to untreated HAP (2.5-3.2wt%). Sedimentation studies revealed the following stability trends: HAP dispersed in water was approximately the same as esterified HAP in water (a few hours)

  9. Solution ripening of hydroxyapatite nanoparticles: effects on electrophoretic deposition.

    PubMed

    Wei, M; Ruys, A J; Milthorpe, B K; Sorrell, C C

    1999-04-01

    Electrophoretic deposition is a low-cost, simple, and flexible coating method for producing hydroxyapatite (Hap) coatings on metal implants. However, densification requires heating the coated metal to high temperatures, which, for commercial HAp powders, generally means at least 1200 degrees C. At such temperatures, the metal tends to react with the HAp coating, inducing decomposition, and the strength of titanium and stainless steel implants is severely degraded. With the use of raw uncalcined nanoparticulate Hap, densification can occur at 900 degrees -1050 degrees C; however, such coatings are prone to cracking due to the high drying shrinkage. This problem was solved by precipitating nanoparticulate HAp by the metathesis process [10Ca(NO3)2 + 6NH4H2PO4 + 8NH4OH] and optimizing the approximately 30 nm of nanoprecipitates by an Ostwald ripening approach, that is, by boiling and/or ambient aging in the mother liquor. While the as-precipitated nanoparticles produced severely cracked coatings, 2 h of boiling or 10 days of ambient aging ripened the "gel-like" mass into unagglomerated nanoparticles, which produced crack-free coatings. Since boiling enhanced particle size but ambient aging did not, crack elimination probably was due to the transition from the highly agglomerated gel-like state to the dispersed nanoparticulate state rather than to particle growth. Furthermore, boiling only reduced the amount of cracking whereas aging completely eliminated cracking.

  10. Porous hydroxyapatite tablets as carriers for low-dosed drugs.

    PubMed

    Cosijns, A; Vervaet, C; Luyten, J; Mullens, S; Siepmann, F; Van Hoorebeke, L; Masschaele, B; Cnudde, V; Remon, J P

    2007-09-01

    The present study evaluated an innovative technique for the manufacturing of low-dosed tablets. Tablets containing hydroxyapatite and a pore forming agent (50% (w/w) Avicel PH 200/20, 37.5% and 50% corn starch/37.5% sorbitol) were manufactured by direct compression followed by sintering. The influence of pore forming agent (type and concentration), sinter temperature and sinter time on tablet properties was investigated. Sintering (1250 degrees C) revealed tablets with an acceptable friability (<1%). Using 50% (w/w) Avicel PH 200 as pore forming agent resulted in tablets combining the highest porosity (50%) and the highest median pore diameter (5 microm). Aqueous drug solutions (metoprolol tartrate, riboflavin sodium phosphate) were spiked on the tablet surface. The maximum volume of drug solution absorbed was limited (2x100 microl), revealing that these porous carriers were ideal for low dosed formulations. Drug release from the tablets was slow, independent of the drug. To accelerate drug release, tablets were manufactured using a modified gelcasting technique yielding tablets with a median pore size of 60 and 80 microm. Release from these tablets was drastically increased indicating that the permeability of the tablets was influenced by the pore size, shape and connectivity of the porous network. Changing and controlling these parameters made it possible to obtain drug delivery systems providing different drug delivery behaviour.

  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.

  12. 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.

  13. 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

  14. Enhanced bone morphogenetic protein-2 performance on hydroxyapatite ceramic surfaces.

    PubMed

    Schuessele, A; Mayr, H; Tessmar, J; Goepferich, A

    2009-09-15

    The immobilization of biomolecules on biomaterial surfaces allows for the control of their localization and retention. In numerous studies, proteins have been simply adsorbed to enhance the biological performance of various materials in vivo. We investigated the potential of surface modification techniques on hydroxyapatite (HA) ceramic discs in an in vitro approach. A novel method for protein immobilization was evaluated using the aminobisphosphonates pamidronate and alendronate, which are strong Ca chelating agents, and was compared with the established silanization technique. Lysozyme and bone morphogenetic protein-2 (BMP-2) were used to assess the suitability of the two surface modification methods with regard to the enzymatic activity of lysozyme and to the capacity of BMP-2 to stimulate the osteoblastic differentiation of C2C12 mouse myoblasts. After immobilization, a 2.5-fold increase in enzymatic activity of lysozyme was observed compared with the control. The alkaline phosphatase activity per cell stimulated by immobilized BMP-2 was 2.5-fold higher [9 x 10(-6) I.U.] than the growth factor on unmodified surfaces [2-4 x 10(-6) I.U.]. With regard to the increase in protein activity, both procedures lead to equivalent results. Thus, the bisphosphonate-based surface modification represents a safe and easy alternative for the attachment of proteins to HA surfaces. PMID:18655137

  15. 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.

  16. 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.

  17. 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

  18. 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.

  19. [Adsorption of fluoride ions on a Ca-deficient hydroxyapatite].

    PubMed

    Li, Ling; Zhu, Zhi-Liang; Qiu, Yan-Ling; Zhang, Hua; Zhao, Jian-Fu

    2010-06-01

    A Ca-deficient hydroxyapatite (d-HAp) from the by-product of phosphate wastewater treatment has been used to remove fluoride ions. The effects of pH, coexistent calcium and magnesium ions, and chloride ions on the adsorption efficiency were investigated for the system. The results showed that d-HAp adsorbed F- efficiently within a wide pH range (4-7), and the defluoridation capacity of d-HAp remained 85%. There was no significant effect on removal of fluoride ions with addition of up to 200 times as high a concentration of Ca2+, Mg2+ and Cl-, so it suggested that d-HAp was applicable to high fluoride area. The adsorption kinetics can be described by Pseudo-second-order reaction model and the correlation coefficient R2 was 0.999 0. It was also found that the adsorption of F- on d-HAp followed the Langmuir model. The maximal static adsorption capacity was calculated as 26.11 mg x g(-1). It also suggested that ion exchange was the main mechanism during this adsorptive process. PMID:20698272

  20. 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.

  1. 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

  2. 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.

  3. Electrophoretic deposition of composite hydroxyapatite-silica-chitosan coatings

    SciTech Connect

    Grandfield, K.; Zhitomirsky, I.

    2008-01-15

    Electrophoretic deposition (EPD) method has been developed for the fabrication of nanocomposite silica-chitosan coatings. Cathodic deposits were obtained on various conductive substrates using suspensions of silica nanoparticles in a mixed ethanol-water solvent, containing dissolved chitosan. Co-deposition of silica and hydroxyapatite (HA) nanoparticles resulted in the fabrication of HA-silica-chitosan coatings. The deposition yield has been studied at a constant voltage mode at various deposition durations. The method enabled the formation of coatings of different thickness in the range of up to 100 {mu}m. Deposit composition, microstructure and porosity can be varied by variation of HA and silica concentration in the suspensions. It was demonstrated that EPD can be used for the fabrication of HA-silica-chitosan coatings of graded composition and laminates. The method enabled the deposition of coatings containing layers of silica-chitosan and HA-chitosan nanocomposites using suspensions with different HA and silica content. Obtained coatings were studied by X-ray diffraction, thermogravimetric and differential thermal analysis, scanning electron microscopy and energy dispersive spectroscopy. The mechanism of deposition is discussed.

  4. Biomechanical assessment of bone ingrowth in porous hydroxyapatite.

    PubMed

    Hing, K A; Best, S M; Tanner, K E; Bonfield, W; Revell, P A

    1997-12-01

    Porous hydroxyapatite (Endobon) specimens were implanted into the femoral condyle of New Zealand White rabbits for up to 6 months. After sacrifice, specimens were sectioned for histology and mechanical testing, where the extent of reinforcement by bony ingrowth was assessed by compression testing and fixation was assessed by push-out testing. From histological observations, it was established that the majority of bone ingrowth occurred between 10 day and 5 weeks after implantation and proceeded predominantly from the deep end of the trephined defect, with some integration from the circumferential sides. At 3 months, the implants were fully integrated, exhibiting bony ingrowth, vascularization and bone marrow stroma within the internal macropores. After 5 weeks, the mean ultimate compressive strength of retrieved implants (6.9 MPa) was found to be greater than that of the original implant (2.2 MPa), and by 3 months the fully integrated implants attained a compressive strength of approximately 20 MPa. Push-out testing demonstrated that after 5 weeks in vivo, the interfacial shear strength reached 3.2 MPa, increasing to 7.3 MPa at 3 and 6 months. PMID:15348781

  5. 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.

  6. Rapid biomimetic mineralization of hydroxyapatite-g-PDLLA hybrid microspheres.

    PubMed

    Du, Ke; Shi, Xudong; Gan, Zhihua

    2013-12-10

    Hydroxyapatite-graft-poly(D,L-lactide) (HA-g-PDLLA) nanoparticles were synthesized here to fabricate hybrid microspheres with diameter in the range of 150-200 μm by emulsion solvent evaporation techniques. The as-obtained microspheres were treated with alkaline solution in order to selectively degrade the PDLLA layer which covered on the surface of hybrid microspheres and instead to generate a dense coating of HA nanoparticles. The hybrid microspheres with enriched HA nanoparticles on the surface were further immersed in simulated body fluid (SBF) solution to evaluate the bone-forming ability of the bioactive hybrid microspheres via the in vitro biomimetic mineralization process. The resultant microspheres were analyzed by using X-ray photoelectron spectroscopy (XPS), X-ray powder diffraction (XRD), scanning electron microscopy (SEM), and thermogravimetric analysis (TGA) to understand the nucleation and growth of bioactive calcium phosphate (Ca-P) crystals as a function of surface treatment. Results in this work clearly demonstrated that the existing HA nanoparticles on the surface of hybrid microspheres after alkaline treatment greatly affect the growth of the bone-like Ca-P crystals in SBF solutions. The biomimetic hybrid microspheres were found to be excellent candidates for use as injectable scaffolds for bone tissue engineering.

  7. 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.

  8. Sphingoid bases inhibit acid-induced demineralization of hydroxyapatite.

    PubMed

    Valentijn-Benz, Marianne; van 't Hof, Wim; Bikker, Floris J; Nazmi, Kamran; Brand, Henk S; Sotres, Javier; Lindh, Liselott; Arnebrant, Thomas; Veerman, Enno C I

    2015-01-01

    Calcium hydroxyapatite (HAp), the main constituent of dental enamel, is inherently susceptible to the etching and dissolving action of acids, resulting in tooth decay such as dental caries and dental erosion. Since the prevalence of erosive wear is gradually increasing, there is urgent need for agents that protect the enamel against erosive attacks. In the present study we studied in vitro the anti-erosive effects of a number of sphingolipids and sphingoid bases, which form the backbone of sphingolipids. Pretreatment of HAp discs with sphingosine, phytosphingosine (PHS), PHS phosphate and sphinganine significantly protected these against acid-induced demineralization by 80 ± 17%, 78 ± 17%, 78 ± 7% and 81 ± 8%, respectively (p < 0.001). On the other hand, sphingomyelin, acetyl PHS, octanoyl PHS and stearoyl PHS had no anti-erosive effects. Atomic force measurement revealed that HAp discs treated with PHS were almost completely and homogeneously covered by patches of PHS. This suggests that PHS and other sphingoid bases form layers on the surface of HAp, which act as diffusion barriers against H(+) ions. In principle, these anti-erosive properties make PHS and related sphingosines promising and attractive candidates as ingredients in oral care products.

  9. 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

  10. Pulsed laser treatment of plasma-sprayed hydroxyapatite coatings.

    PubMed

    Cheang, P; Khor, K A; Teoh, L L; Tam, S C

    1996-10-01

    Plasma-sprayed hydroxyapatite (HA) coatings have complex microstructures. There are often variations in phase, structure and chemical composition among the starting material and coating. Some of these changes may not be acceptable for biomedical applications. Attaining all the requirements for a functional coating in a single spraying process is not easily achieved. Additional post-treatment may be necessary. This study examines the use of a pulsed laser to enhance the coating characteristics of plasma-sprayed HA coatings. Preliminary results show the laser-treated coatings having a modified microstructure with crack networks and pores in the size range 5-30 microns. The pores and cracks were quantified by an image analyser. The crack network is less significant in coatings that are treated at lower energy intensity and this could be interesting in that the laser can be used to alter the surface phase composition as well as the morphology. However, repetitive passes with the pulsed laser did not help to seal the cracks that formed.

  11. 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

  12. 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

  13. 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.

  14. 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.

  15. 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

  16. Effect of Hydrothermal Treatment on Sinterability of Hydroxyapatite

    SciTech Connect

    Kawagoe, D.; Fujimori, H.; Goto, S.; Yamasaki, N.; Ioku, K.

    2006-05-15

    Calcium hydroxyapatite, Ca10(PO4)6(OH)2:HA, is the inorganic principle component of natural bones and teeth. It has been already suggested that the amount of OH ion in the crystal structure of HA is closely related to the biocompatibility. The amount of OH ion in current HA, however, has not been controlled. In order to prepare more functional HA ceramics, the amount of OH ion must be controlled. In this study, HA ceramics with different OH amount were prepared from fine HA crystals by spark plasma sintering (SPS). Fine powder of HA was treated hydrothermally at 200 deg. C for 24 h with pH 10 NH3 aqueous solution. The samples were pressed uniaxialy under 60 MPa, and then they were SPS at 800 deg. C, 900 deg. C and 1000 deg. C for 10 min with the heating rate of 25 deg. C{center_dot}min-1. No phases other than HA were revealed by XRD for the starting samples after hydrothermal treatment and samples after sintering by SPS at 800 deg. C, 900 deg. C and 1000 deg. C for 10 min. The quantity of OH ion in HA ceramics sintered by SPS was decreased with increasing temperature of sintering. Transparent HA ceramics were prepared by SPS at 900 deg. C and 1000 deg. C.

  17. Copper doping improves hydroxyapatite sorption for arsenate in simulated groundwaters.

    PubMed

    Liu, Guojing; Talley, Jeffrey W; Na, Chongzheng; Larson, Steve L; Wolfe, Lawrence G

    2010-02-15

    Hydroxyapatite (HAP) has been widely used to immobilize many cationic heavy metals in water and soils. Compared with its strong sorption for metal cations, the abilities of HAP to sorb metal anions, such as arsenic, are less significant. Improving HAP sorption for anionic arsenic species is important for expanding its application potential because the presence of arsenic in the environment has raised serious health concerns and there is need for cost-effective remediation methods. In this work, we report an innovative method of copper doping to improve a synthetic HAP sorption for arsenate, which is a primary aqueous arsenic species, in simulated groundwaters. The undoped HAP and copper doped HAP (CuHAP) were characterized with XRD, FTIR, N(2) adsorption, and SEM, and then evaluated as sorbents for arsenate removal tests. The experimental results suggest that copper doping changed the morphology and increased the surface area of HAP. The CuHAP sorbed 1.6-9.1x more arsenate than the undoped HAP did in a simulated groundwater at pH of 7.7-8.0. The improved arsenate sorption is presumably due to the increase in surface area of HAP as a result of copper doping. In addition to the copper doping level, the arsenate sorption to HAP and CuHAP can also be increased with increasing water pH and calcium concentration. The experimental data indicate that sorbent dissolution is an important factor governing arsenate sorption to HAP and CuHAP.

  18. Effect of hydroxyapatite sintering temperature on intracellular ionic concentrations of monocytes: a TEM-cryo-X-ray microanalysis study.

    PubMed

    Laquerriere, P; Kilian, L; Bouchot, A; Jallot, E; Grandjean, A; Guenounou, M; Balossier, G; Frayssinet, P; Bonhomme, P

    2001-05-01

    Hydroxyapatite used as bone replacement can lead to particle release in the implantation site. These particles interact with monocytes, which are the first immune cells to colonize the implant and an inflammatory site. Thanks to cryo-X-ray microanalysis, we can observe cells in a state close to the physiological one and we have access to diffusible ions. We paid particular attention to the potassium-to-sodium ratio, which is one of the best viability criteria. We used this method to study the interaction between three hydroxyapatite particles treated at three different temperatures (not treated, treated at 600 degrees C and 1180 degrees C), and monocytes. In the culture condition, the hydroxyapatite treated at 1180 degrees C underwent the least dissolution. We demonstrate that monocytes were altered by the three hydroxyapatite particles. The hydroxyapatite particules treated at 600 degrees C were found to be more toxic.

  19. 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.

  20. Hydroxyapatite/regenerated silk fibroin scaffold-enhanced osteoinductivity and osteoconductivity of bone marrow-derived mesenchymal stromal cells.

    PubMed

    Jiang, Jia; Hao, Wei; Li, Yuzhuo; Yao, Jinrong; Shao, Zhengzhong; Li, Hong; Yang, Jianjun; Chen, Shiyi

    2013-04-01

    A novel hydroxyapatite/regenerated silk fibroin scaffold was prepared and investigated for its potential to enhance both osteoinductivity and osteoconductivity of bone marrow-derived mesenchymal stromal cells in vitro. Approx. 12.4 ± 0.06 % (w/w) hydroxyapatite was deposited onto the scaffold, and cell viability and DNA content were significantly increased (18.5 ± 0.6 and 33 ± 1.2 %, respectively) compared with the hydroxyapatite scaffold after 14 days. Furthermore, alkaline phosphatase activity in the novel scaffold increased 41 ± 2.5 % after 14 days compared with the hydroxyapatite scaffold. The data indicate that this novel hydroxyapatite/regenerated silk fibroin scaffold has a positive effect on osteoinductivity and osteoconductivity, and may be useful for bone tissue engineering.