Hydroxyapatite/MCM-41 and SBA-15 Nano-Composites: Preparation, Characterization and Applications

Science.gov (United States)

Anunziata, Oscar A.; Martínez, Maria L.; Beltramone, Andrea R.

2009-01-01

Composites of hydroxyapatite (HaP) and highly ordered large pore mesoporous silica molecular sieves such as, Al-SBA-15 and Al-MCM-41 (denoted as SBA-15 and MCM-41, respectively) were developed, characterized by XRD, BET, FTIR, HRTEM and NMR-MAS, and applied to fluoride retention from contaminated water. The proposed procedure by a new route to prepare the HaP/SBA-15 and HaP/MCM-41, composites generates materials with aluminum only in tetrahedral coordination, according to the 27Al NMR-MAS results. Free OH- groups of HaP nanocrystals, within the hosts, allowed high capacity fluoride retention. The activity of fluoride retention using HaP/MCM-41 or HaP/SBA-15 was 1-2 orders of magnitude greater, respectively, than with pure HaP.

Mesoporous Fe{sub 3}O{sub 4}/hydroxyapatite composite for targeted drug delivery

Energy Technology Data Exchange (ETDEWEB)

Gu, Lina; He, Xiaomei; Wu, Zhenyu, E-mail: zhenyuwuhn@sina.com

2014-11-15

Highlights: • Mesoporous Fe{sub 3}O{sub 4}/hydroxyapatite composite was synthesized by a simple, efficient and environmental friendly method. • The prepared material had a large surface area, high pore volume, and good magnetic separability. • DOX-loaded Fe{sub 3}O{sub 4}/hydroxyapatite composite exhibited surprising slow drug release behavior and pH-dependent behavior. - Abstract: In this contribution, we introduced a simple, efficient, and green method of preparing a mesoporous Fe{sub 3}O{sub 4}/hydroxyapatite (HA) composite. The as-prepared material had a large surface area, high pore volume, and good magnetic separability, which made it suitable for targeted drug delivery systems. The chemotherapeutic agent doxorubicin (DOX) was used to investigate the drug release behavior of Fe{sub 3}O{sub 4}/HA composite. The drug release profiles displayed a little burst effect and pH-dependent behavior. The release rate of DOX at pH 5.8 was larger than that at pH 7.4, which could be attributed to DOX protonation in acid medium. In addition, the released DOX concentrations remained at 0.83 and 1.39 μg/ml at pH 7.4 and 5.8, respectively, which indicated slow, steady, and safe release rates. Therefore, the as-prepared Fe{sub 3}O{sub 4}/hydroxyapatite composite could be an efficient platform for targeted anticancer drug delivery.

Preparation and characterization of composites based on the blends of collagen, chitosan and hyaluronic acid with nano-hydroxyapatite.

Science.gov (United States)

Sionkowska, Alina; Kaczmarek, Beata

2017-09-01

3D porous composites based on the blend of chitosan, collagen and hyaluronic acid with the addition of nano-hydroxyapatite were prepared. SEM images for the composites were made and the structure was assessed. Mechanical properties were studied using a Zwick&Roell Testing Mashine. In addition, the porosity and density of composites were measured. The concentration of calcium ions released from the material was detected by the complexometric titration method. The results showed that in 3D porous sponge based on the blend of chitosan, collagen and hyaluronic acid, inorganic particles of nanohydroxyapatite can be incorporated, as well as that the properties of 3D composites depend on the material composition. Mechanical parameters and thermal stability of ternary biopolymeric blends were improved by the addition of hydroxyapatite. Moreover, the porosity of ternary materials was higher than in materials based on pure chitosan or collagen. All composites were characterized by a porous structure with interconnected pores. Calcium ions can be released from the composite during its degradation in water. Copyright © 2017 Elsevier B.V. All rights reserved.

Improvement of mechanical and thermal properties of high energy electron beam irradiated HDPE/hydroxyapatite nano-composite

Science.gov (United States)

Mohammadi, M.; Ziaie, F.; Majdabadi, A.; Akhavan, A.; Shafaei, M.

2017-01-01

In this research work, the nano-composites of high density polyethylene/hydroxyapatite samples were manufactured via two methods: In the first method, the granules of high density polyethylene and nano-structure hydroxyapatite were processed in an internal mixer to prepare the nano-composite samples with a different weight percentage of the reinforcement phase. As for the second one, high density polyethylene was prepared in nano-powder form in boiling xylene. During this procedure, the hydroxyapatite nano-powder was added with different weight percentages to the solvent to obtain the nano-composite. In both of the procedures, the used hydroxyapatite nano-powder was synthesized via hydrolysis methods. The samples were irradiated under 10 MeV electron beam in 70-200 kGy of doses. Mechanical, thermal and morphological properties of the samples were investigated and compared. The results demonstrate that the nano-composites which we have prepared using nano-polyethylene, show better mechanical and thermal properties than the composites prepared from normal polyethylene granules, due to the better dispersion of nano-particles in the polymer matrix.

Preparation and characterization of nano-hydroxyapatite within chitosan matrix

International Nuclear Information System (INIS)

Rogina, A.; Ivanković, M.; Ivanković, H.

2013-01-01

Nano-composites that show some features of natural bone both in composition and in microstructure have been prepared by in situ precipitation method. Apatite phase has been prepared from cost-effective precursors (calcite and urea phosphate) within chitosan (CS) matrix dissolved in aqueous acetic acid solution. The compositional and morphological properties of composites were studied by means of Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD) thermogravimetric analysis (TGA) and transmission electron microscopy (TEM). Depending on the reaction conditions (temperature, reaction time, glucose addition and pH control) in addition to hydroxyapatite (HA) as a major phase, octacalcium hydrogen phosphate pentahydrate (OCP) and dicalcium phosphate anhydrate (DCPD) were formed as shown by XRD and FTIR. Crystallite lengths of precipitated HA estimated by Scherrer's equation were between 20 and 30 nm. A fibrous morphology (∼ 400 nm) of HA observed by TEM indicates that HA nucleates on chitosan chains. - Highlights: • Nano-hydroxyapatite (HA) was prepared by in situ precipitation within chitosan hydrogels and colloidal chitosan solution. • pH control was regulated by ammonia and urea degradation. • In situ urea degradation provides homogenous HA formation. • TEM imaging indicates fibrous morphology of HA with crystalline size of 400 nm. • Glucose addition and temperature variation affect inorganic phase formation

Microstructural Improvement of Hydroxyapatite-ZrO2 Composite Ceramics via Thermal Precipitation Techniques.

Science.gov (United States)

Sangmala, A.; Limsuwan, P.; Kaewwiset, W.; Naemchanthara, K.

2017-09-01

Hydroxyapatite-ZrO2 composite ceramic were synthesized using a thermal precipitation techniques. The chemical precursors were prepared from di-ammonium hydrogen orthophosphate, calcium oxide (CaO) derived from chicken eggshell, zirconium dioxide (ZrO2) and distilled water. The mixture were heated at the various temperatures from 100 to 700 °C in the furnace with an incremental temperature of 100 °C. The ZrO2 contents in the composite ceramic were varied from 0 to 15 percent weight of CaO. The prepared composites were then annealed at 300, 600 and 700 °C for 4 h in air. The crystal structure, function group and morphology of all samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), field emission scanning electron microscopy (FESEM) and universal testing machine (UTM), respectively. The results indicated that the undoped-ZrO2 samples hydroxyapatite phase with a hexagonal structure. However, the hydroxyapatite was transformed to the tri-calcium phosphate after thermal treatment at 700 °C. For the doped-ZrO2 samples, the hydroxyapatite and ZrO2 phases were found. Moreover, the result showed that the compressive strength of hydroxyapatite-ZrO2 composite ceramic increased with increasing the ZrO2 content.

Preparation and evaluation of cerium oxide-bovine hydroxyapatite composites for biomedical engineering applications.

Science.gov (United States)

Gunduz, O; Gode, C; Ahmad, Z; Gökçe, H; Yetmez, M; Kalkandelen, C; Sahin, Y M; Oktar, F N

2014-07-01

The fabrication and characterization of bovine hydroxyapatite (BHA) and cerium oxide (CeO2) composites are presented. CeO2 (at varying concentrations 1, 5 and 10wt%) were added to calcinated BHA powder. The resulting mixtures were shaped into green cylindrical samples by powder pressing (350MPa) followed by sintering in air (1000-1300°C for 4h). Density, Vickers microhardness (HV), compression strength, scanning electron microscopy (SEM) and X-ray diffraction (XRD) studies were performed on the products. The sintering behavior, microstructural characteristics and mechanical properties were evaluated. Differences in the sintering temperature (for 1wt% CeO2 composites) between 1200 and 1300°C, show a 3.3% increase in the microhardness (564 and 582.75HV, respectively). Composites prepared at 1300°C demonstrate the greatest compression strength with comparable results for 5 and 10wt% CeO2 content (106 and 107MPa) which are significantly better than those for 1wt% and those that do not include any CeO2 (90 and below 60MPa, respectively). The results obtained suggest optimal parameters to be used in preparation of BHA and CeO2 composites, while also highlighting the potential of such materials in several biomedical engineering applications. Copyright © 2014 Elsevier Ltd. All rights reserved.

Electrophoretic deposition of composite hydroxyapatite-chitosan coatings

International Nuclear Information System (INIS)

Pang Xin; Zhitomirsky, Igor

2007-01-01

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 μm. 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 substrates

Preparation and characterization of hydroxyapatite/chondroitin sulfate composites by biomimetic synthesis

International Nuclear Information System (INIS)

Xiao Xiufeng; He Dan; Liu Fang; Liu Rongfang

2008-01-01

Based on the principles of biomineralization, flakelike hydroxyapatite/chondroitin sulfate composites were synthesized through biomimetic method using Ca(NO 3 ) 2 .4H 2 O and (NH 4 ) 3 PO 4 .3H 2 O as reagents and chondroitin sulfate as template. The crystalline phase, microstructure, chemical composition, morphology and thermal behavior of the composites obtained in the experiment were characterized by means of X-ray diffraction (XRD), Fourier transform infrared spectroscope (FTIR), transmission electron microscope (TEM), Thermogravimetry-Differential thermal analyzer (TG-DTA) and Elemental analyzer, respectively. The interaction between the functional groups of ChS and HA was investigated by electrical conductivity and UV-vis spectrum. The results demonstrate that the as-prepared powders with small amount of carbonate have the component similar to human bone. It can be concluded that the nucleation and growth of HA crystals occurred through the chemical interactions between the HA crystals and preorganized functional groups of the ChS template. Furthermore, the concentration of ChS significantly affects the morphology of the composites. Short fiberlike crystals could be obtained at a low concentration of ChS, but flakelike crystals could be synthesized using a high concentration (≥0.5 wt%) of ChS as template

Preparation and characterization of hydroxyapatite/chondroitin sulfate composites by biomimetic synthesis

Energy Technology Data Exchange (ETDEWEB)

Xiao Xiufeng; He Dan; Liu Fang [College of Chemistry and Materials Science, Fujian Normal University, Fujian, Fuzhou 350007 (China); Liu Rongfang [College of Chemistry and Materials Science, Fujian Normal University, Fujian, Fuzhou 350007 (China)], E-mail: rfliu@vip.sina.com

2008-12-20

Based on the principles of biomineralization, flakelike hydroxyapatite/chondroitin sulfate composites were synthesized through biomimetic method using Ca(NO{sub 3}){sub 2}.4H{sub 2}O and (NH{sub 4}){sub 3}PO{sub 4}.3H{sub 2}O as reagents and chondroitin sulfate as template. The crystalline phase, microstructure, chemical composition, morphology and thermal behavior of the composites obtained in the experiment were characterized by means of X-ray diffraction (XRD), Fourier transform infrared spectroscope (FTIR), transmission electron microscope (TEM), Thermogravimetry-Differential thermal analyzer (TG-DTA) and Elemental analyzer, respectively. The interaction between the functional groups of ChS and HA was investigated by electrical conductivity and UV-vis spectrum. The results demonstrate that the as-prepared powders with small amount of carbonate have the component similar to human bone. It can be concluded that the nucleation and growth of HA crystals occurred through the chemical interactions between the HA crystals and preorganized functional groups of the ChS template. Furthermore, the concentration of ChS significantly affects the morphology of the composites. Short fiberlike crystals could be obtained at a low concentration of ChS, but flakelike crystals could be synthesized using a high concentration ({>=}0.5 wt%) of ChS as template.

Formation mechanism and adhesive strength of a hydroxyapatite/TiO{sub 2} composite coating on a titanium surface prepared by micro-arc oxidation

Energy Technology Data Exchange (ETDEWEB)

Liu, Shimin, E-mail: lshm1216@163.com [Department of Gem and Material Technique, Tianjin University of Commerce, Tianjin 300134 (China); Li, Baoe; Liang, Chunyong; Wang, Hongshui [School of Materials Science and Engineering, Hebei University of Technology, Tianjin 300130 (China); Qiao, Zhixia [School of Mechanical Engineering, Tianjin University of Commerce, Tianjin 300134 (China)

2016-01-30

Graphical abstract: - Highlights: • Hydroxyapatite/TiO{sub 2} composite coating was prepared by one-step micro-arc oxidation. • The formation mechanism of composite coating was investigated. • Higher bonding strength between hydroxyapatite and TiO{sub 2} layer was obtained. - Abstract: A hydroxyapatite (HA)/TiO{sub 2} composite coating was prepared on a titanium surface by one-step micro-arc oxidation (MAO). The formation mechanism of the composite coating was investigated and the adhesion of the coating to the substrate was also measured. The results showed that flocculent structures could be obtained during the early stages of treatment. As the treatment period extended, increasing amounts of Ca–P precipitate appeared on the surface, and the flocculent morphology transformed into a plate-like morphology. Then the plate-like calcium and phosphate salt self-assembled to form flower-like apatite. The Ca/P atomic ratio gradually decreased, indicating that the amounts of Ca{sup 2+} ions which diffused into the coating decreased more rapidly than that of PO{sub 4}{sup 3−} or HPO{sub 4}{sup 2−}. The adhesive strength between the apatite and TiO{sub 2} coating was improved. This improvement is attributed to the interlocking effect between the apatite and TiO{sub 2} layer which formed simultaneously during the early stages of the one-step MAO. This study shows that it is a promising method to prepare bioactive coating on a titanium surface.

Preparing hydroxyapatite-silicon composite suspensions with homogeneous distribution of multi-walled carbon nano-tubes for electrophoretic coating of NiTi bone implant and their effect on the surface morphology

International Nuclear Information System (INIS)

Khalili, Vida; Khalil-Allafi, Jafar; Xia, Wei; Parsa, Alireza B.; Frenzel, Jan; Somsen, Christoph; Eggeler, Gunther

2016-01-01

Graphical abstract: - Highlights: • The stable composite suspensions of hydroxyapatite, silicon and multi-walled carbon nano-tubes was prepared using functionalization of and multi-walled carbon nano-tubes in HNO_3 vapor and triethanolamine as dispersing agent. • The zeta potential of composite suspensions is less than that of hydroxyapatite suspension. • The silicon particles presence in suspension causes to decrease the charge carrier in suspension and current density during electrophoretic deposition. • The orientation of multi-walled carbon nano-tubes to parallel direction of the applied electric field during electrophoretic deposition can facilitate their moving towards the cathode and increase current density. • The more zeta potential of suspension, the lower roughness of coatings during electrophoretic deposition. - Abstract: Preparing a stable suspension is a main step towards the electrophoretically depositing of homogeneous and dense composite coatings on NiTi for its biomedical application. In the present study, different composite suspensions of hydroxyapatite, silicon and multi-walled carbon nano-tubes were prepared using n-butanol and triethanolamine as media and dispersing agent, respectively. Multi-walled carbon nanotubes were first functionalized in the nitric acid vapor for 15 h at 175 °C, and then mixed into suspensions. Thermal desorption spectroscopy profiles indicate the formation of functional groups on multi-walled carbon nano-tubes. An excellent suspension stability can be achieved for different amounts of triethanolamine. The amount of triethanolamine can be increased by adding a second component to a stable hydroxyapatite suspension due to an electrostatic interaction between components in suspension. The stability of composite suspension is less than that of the hydroxyapatite suspension, due to density differences, which under the gravitational force promote the demixing. The scanning electron microscopy images of the

Nanocrystalline hydroxyapatite ceramics prepared by hydrolysis in polyol medium

Science.gov (United States)

Mechay, Abderrahmen; Feki, Hafed E. L.; Schoenstein, Fréderic; Jouini, Noureddine

2012-07-01

This Letter describes a new approach for the synthesis of hydroxyapatite nanoparticles, which involves precipitation and hydrolysis reactions conducted in polyol medium. In fact, ammonium-hydrogen phosphate and calcium nitrate were dissolved in polyol, and then heated at the boiling point of the polyol (ethane1, 2diol or propane1, 2diol). Besides, the phase and composition of the polycrystalline were studied by TGA/DTA, FT-IR, TEM and XRD techniques. The nanoparticles thus obtained present interesting morphological characters varying from needle to very thin platelet. Moreover, the hydroxyapatite prepared in ployol shows higher cristallinity in comparison with that obtained by other 'chimie douce' methods.

Preparation and characterization of dense nanohydroxyapatite/PLLA composites

International Nuclear Information System (INIS)

Gay, Sandrine; Arostegui, Saioa; Lemaitre, Jacques

2009-01-01

Synthetic bone graft substitutes based on PLLA have been largely studied during the past decade. PLLA/hydroxyapatite composites appear as promising materials for large bone defect healing. In this study dense PLLA/nano-hydroxyapatite composites were prepared by hot pressing. Dense samples were investigated rather than porous scaffolds, in order to shed light on possible correlations between intrinsic mechanical properties and nano-hydroxyapatite concentration. Hydroxyapatite deagglomerated by wet attrition milling, and further dispersed into chloroform was used (median diameter = 80 nm). Particle size distribution measurements and transmission electron microscopy show evidence that particle size and dispersion are maintained throughout the successive steps of composite processing. Mechanical properties were tested (uni-axial and diametral compression tests) as a function of nano-hydroxyapatite content. Increasing concentrations of nano-hydroxyapatite (0, 25 and 50 wt.%) increase the Young's modulus and the mechanical strength of the composite; at the same time, the failure mechanism of the material changes from plastic to brittle. Young's modulus over 6 GPa and uniaxial compressive strength over 100 MPa have been achieved. These values expressed in terms of intrinsic tensile and shear strengths indicate that 50 wt.% nano-hydroxyapatite containing samples develop properties comparable to those of cortical bone. PLLA/nano-hydroxyapatite composites are thus promising candidates to develop bioresorbable porous bone substitutes showing superior mechanical performance

Hydrothermal Preparation of Apatite Composite with Magnetite or Anatase

International Nuclear Information System (INIS)

Murakami, Setsuaki; Ishida, Emile H.; Ioku, Koji

2006-01-01

Microstructure designed porous hydroxyapatite (Ca10(PO4)6(OH)2) composites with magnetite (Fe3O4) particles or anatase (TiO2) dispersion were prepared by hydrothermal treatment. These composites had micro-pores of about 0.1-0.5 μm in size. Magnetite / Hydroxyapatite composites should be suitable for medical treatment of cancer, especially in bones, because HA can bond to bones directly and magnetite can generate heat. They must be used for hyperthermia therapies of cancer in bones. Meanwhile, anatase / Hydroxyapatite composite should be suitable for environmental purification, because HA rod-shape particles expose the specific crystal face, which adsorbs organic contaminants and so on

Characterization,Mechanical, and In Vitro Bioactivity Properties of Hydroxyapatite/Bioactive Glass Composite

Directory of Open Access Journals (Sweden)

Israa Kahatan Sabree

2016-12-01

Full Text Available Bioactive ceramic materials can help bone reparation and regeneration by offering support to bone growth. Biological hydroxyapatite powder was prepared by burning animal bone followed by studying the mechanical properties of hydroxyapatite (HA/ (20wt.%, and 40wt.% of binary bioactive glass (70% SiO2- 30% CaO in order to evaluate the influence of composition on the compressive strength and hardness. HA-composite material exhibited increasing density, microhardness, and compressive strength with increasing amount of glass addition. X-ray diffraction after sintering at 1200°C showed no alter of HA to secondary phases while the hydroxyapatite/ bioactive glass composites contained a HA phase and different amounts of wollastonite phase, depending on the amount of bioglass added. In vitro tests, the samples were soaked in simulated body fluid (SBF for ten days in order to evaluate the change in compression strength, weight loss, and pH. The HA composite reinforced with 40 wt % bioglass showed highest compression strength, and lowest weight loss

Preparation and properties of in-situ growth of carbon nanotubes reinforced hydroxyapatite coating for carbon/carbon composites

Energy Technology Data Exchange (ETDEWEB)

Liu, Shoujie, E-mail: jlliushoujie@126.com; Li, Hejun, E-mail: lihejun@nwpu.edu.cn; Su, Yangyang, E-mail: suyangyang@mail.nwpu.edu.cn; Guo, Qian, E-mail: 1729299905@163.com; Zhang, Leilei, E-mail: zhangleilei@nwpu.edu.cn

2017-01-01

Carbon nanotubes (CNTs) possess excellent mechanical properties for their role playing in reinforcement as imparting strength to brittle hydroxyapatite (HA) bioceramic coating. However, there are few reports relating to the in-situ grown carbon nanotubes reinforced hydroxyapatite (CNTs-HA) coating. Here we demonstrate the potential application in reinforcing biomaterials by an attempt to use in-situ grown of CNTs strengthen HA coating, using a combined method composited of injection chemical vapor deposition (ICVD) and pulsed electrodeposition. The microstructure, phases and chemical compositions of CNTs-HA coatings were characterized by various advanced methods. The scanning electron microscopy (SEM) images indicated that CNTs-HA coatings avoided the inhomogeneous dispersion of CNTs inside HA coating. The result show that the interfacial shear strength between CNTs-HA coating and the C/C composite matrix reaches to 12.86 ± 1.43 MPa. Potenitodynamic polarization and electrochemical impedance spectroscopy (EIS) studies show that the content of CNTs affects the corrosion resistance of CNTs-HA coating. Cell culturing and simulated body fluid test elicit the biocompatibility with living cells and bioactivity of CNTs-HA coatings, respectively. - Highlights: • A novel bioceramic composite coating of hydroxyapatite reinforced with in-situ grown carbon nanotubes was fabricated. • The doping of carbon nanotubes had almost no impact on the biocompatibility of hydroxyapatite coatings. • The doping of carbon nanotubes improved corrosion resistance of hydroxyapatite coatings in simulated human body solution.

Polyacrylamide-hydroxyapatite composite: Preparation, characterization and adsorptive features for uranium and thorium

Science.gov (United States)

Baybaş, Demet; Ulusoy, Ulvi

2012-10-01

The composite of synthetically produced hydroxyapatite (HAP) and polyacrylamide was prepared (PAAm-HAP) and characterized by BET, FT-IR, TGA, XRD, SEM and PZC analysis. The adsorptive features of HAP and PAAm-HAP were compared for UO22+ and Th4+. The entrapment of HAP into PAAm-HAP did not change the structure of HAP. Both structures had high affinity to the studied ions. The adsorption capacity of PAAm-HAP was than that of HAP. The adsorption dependence on pH and ionic intensity provided supportive evidences for the effect of complex formation on adsorption process. The adsorption kinetics was well compatible to pseudo second order model. The values of enthalpy and entropy changes were positive. Th4+ adsorption from the leachate obtained from a regional fluorite rock confirmed the selectivity of PAAm-HAP for this ion. In consequence, PAAm-HAP should be considered amongst favorite adsorbents for especially deposition of nuclear waste containing U and Th, and radionuclide at secular equilibrium with these elements.

Preparation and characterization of an iron oxide-hydroxyapatite nanocomposite for potential bone cancer therapy.

Science.gov (United States)

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.

Preparation and characterization of bio-composite PEEK/nHA

Science.gov (United States)

Jin, Y. S.; Bian, C. C.; Zhang, Z. Q.; Zhao, Y.; Yang, L.

2017-01-01

PEEK/nHA composite material, with excellent mechanical property as polyetheretherketone (PEEK) and biological activity as hydroxyapatite (HA), has attracted wide attention of medical experts and materials science experts. The addition of hydroxyapatite was the decisive factor for biological activity in PEEK/nHA composite. In this paper, acicular nanohydroxyapatite was prepared by chemical precipitation method with Ca(NO3)2, (NH4)2HPO4 as raw material; PEEK/nHA composite was prepared by solution blending and vacuum sintering method. The composite was characterized with FT-IR, XRD, DSC, TG and mechanical property test. Results showed that the composite has good thermal stability and compressive property when the mass ratio of PEEK to nHA is 10:3; and high nHA content can improve the biological activity of the composite, which can meet the basic requirements for bone tissue engineering scaffold.

Preparation and characterization of hydroxyapatite/gelatin composite membranes for immunoisolation

International Nuclear Information System (INIS)

Chen, Jyh-Ping; Chang, Feng-Nian

2012-01-01

Highlights: ► Cross-linking gelatin in the presence of hydroxyapatite forms composite membranes. ► The membrane was used for immunoisolation and encapsulation of cells. ► Encapsulated islet cells secrete insulin in response to glucose concentrations. ► The membrane is a good candidate for bioartificial pancreas development. - Abstract: Composite membranes are fabricated from hydroxyapatite (HAP) and gelatin for immunoisolation of cells. The films were fabricated by crosslinking 5 wt%, 10 wt%, and 20 wt% gelatin with 1 wt% glutaraldehyde (GA) in the presence of HAP. Fourier transform infrared spectroscopy analysis confirms imide bond formation between GA and gelatin, while the crystal structure of HAP powder remains unchanged from X-ray diffraction analysis. The degree of crosslinking depends on crosslinking time and gelatin concentration. For 5% and 10% gelatin, the degree of crosslinking levels off at 90% within 48 h. From scanning electron microscopy micrographs, the microstructure of the composite membrane depends on the amount of gelatin used in the crosslinking reaction. The mechanical strength of the composite membrane could be enhanced by increasing the gelatin concentration. BET analysis indicates that pore size of the micropores on the surface HAP/gelatin agglomerates decreases with increasing gelatin concentration. However, the macropore, through which diffusion of molecules occurs, is larger at higher gelatin concentrations. The permeability coefficients of different molecules through a HAP/gelatin composite membrane increase with increasing gelatin concentration and is inversely correlated with the molecular weight of the molecule. For immunoisolation of cells, the diffusion of large molecules stimulated by the immune system can be rejected by a chamber constructed from the HAP/gelatin membrane. Insulinoma cells were encapsulated in alginate-poly-L-lysine-alginate microcapsules and enclosed in a HAP/gelatin chamber. The chamber did not impair

Preparation and characterization of hydroxyapatite/gelatin composite membranes for immunoisolation

Energy Technology Data Exchange (ETDEWEB)

Chen, Jyh-Ping, E-mail: jpchen@mail.cgu.edu.tw [Department of Chemical and Materials Engineering, Chang Gung University, 259 Wen Hwa 1st Rd., Kwei-San, Taoyuan 333, Taiwan (China); Chang, Feng-Nian [Department of Chemical and Materials Engineering, Chang Gung University, 259 Wen Hwa 1st Rd., Kwei-San, Taoyuan 333, Taiwan (China)

2012-12-01

Highlights: Black-Right-Pointing-Pointer Cross-linking gelatin in the presence of hydroxyapatite forms composite membranes. Black-Right-Pointing-Pointer The membrane was used for immunoisolation and encapsulation of cells. Black-Right-Pointing-Pointer Encapsulated islet cells secrete insulin in response to glucose concentrations. Black-Right-Pointing-Pointer The membrane is a good candidate for bioartificial pancreas development. - Abstract: Composite membranes are fabricated from hydroxyapatite (HAP) and gelatin for immunoisolation of cells. The films were fabricated by crosslinking 5 wt%, 10 wt%, and 20 wt% gelatin with 1 wt% glutaraldehyde (GA) in the presence of HAP. Fourier transform infrared spectroscopy analysis confirms imide bond formation between GA and gelatin, while the crystal structure of HAP powder remains unchanged from X-ray diffraction analysis. The degree of crosslinking depends on crosslinking time and gelatin concentration. For 5% and 10% gelatin, the degree of crosslinking levels off at 90% within 48 h. From scanning electron microscopy micrographs, the microstructure of the composite membrane depends on the amount of gelatin used in the crosslinking reaction. The mechanical strength of the composite membrane could be enhanced by increasing the gelatin concentration. BET analysis indicates that pore size of the micropores on the surface HAP/gelatin agglomerates decreases with increasing gelatin concentration. However, the macropore, through which diffusion of molecules occurs, is larger at higher gelatin concentrations. The permeability coefficients of different molecules through a HAP/gelatin composite membrane increase with increasing gelatin concentration and is inversely correlated with the molecular weight of the molecule. For immunoisolation of cells, the diffusion of large molecules stimulated by the immune system can be rejected by a chamber constructed from the HAP/gelatin membrane. Insulinoma cells were encapsulated in alginate

Evaluation of porous gradient hydroxyapatite/zirconia composites for repair of lumbar vertebra defect in dogs.

Science.gov (United States)

Shao, Rong-Xue; Quan, Ren-Fu; Huang, Xiao-Long; Wang, Tuo; Xie, Shang-Ju; Gao, Huan-Huan; Wei, Xi-Cheng; Yang, Di-Sheng

2016-04-01

To evaluate the effects of porous gradient composites with hydroxyapatite/zirconia and autologous iliac in repair of lumbar vertebra body defects in dogs. (1) New porous gradient hydroxyapatite/zirconia composites were prepared using foam immersion, gradient compound and high temperature sintering; (2) A total of 18 adult beagle dogs, aged five to eight months and weighted 10-13 kg, were randomly assigned into two subgroups, which were implanted with new porous gradient hydroxyapatite/zirconia composites (subgroup A in 12) or autologous iliac bone (subgroup B in 6); (3) The post-operative data were analyzed and compared between the subgroups to repair the vertebral body defect by roentgenoscopy, morphology and biomechanics. The porosity of new porous gradient hydroxyapatite/zirconia composites is at 25 poles per inch, and the size of pores is at between 150 and 300 µm. The post-operative roentgenoscopy displayed that new-bone formation is increased gradually, and the interface between composites and host-bone becomes became blur, and the new-bone around the composites were integrated into host-bone at 24 weeks postoperatively in subgroup A. As to subgroup B, the resorption and restructure were found at six weeks after the surgery, and the graft-bone and host-bone have been integrated completely without obvious boundary at 24 weeks postoperatively. Histomorphologic study showed that the amount of bone within pores of the porous gradient hydroxyapatite/zirconia composites increased continuously with a prolonged implantation time, and that partial composites were degradated and replaced by new-bone trabeculae. There was no significant difference between subgroups (P > 0.05) in the ultimate compressive strengths. New porous gradient hydroxyapatite/zirconia composites can promote the repair of bony defect, and induce bone tissue to ingrow into the pores, which may be applied widely to the treatment of bony defect in the future. © The Author(s) 2016.

Carbonate hydroxyapatite and silicon-substituted carbonate hydroxyapatite

DEFF Research Database (Denmark)

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

2014-01-01

The present study investigates the chemical composition, solubility, and physical and mechanical properties of carbonate hydroxyapatite (CO3Ap) and silicon-substituted carbonate hydroxyapatite (Si-CO3Ap) which have been prepared by a simple precipitation method. X-ray diffraction (XRD), Fourier......(3-)) site and also entered simultaneously into the hydroxyapatite structure. The Si-substituted CO3Ap reduced the powder crystallinity and promoted ion release which resulted in a better solubility compared to that of Si-free CO3Ap. The mean particle size of Si-CO3Ap was much finer than that of CO3Ap...

Carbon foam/hydroxyapatite coating for carbon/carbon composites: Microstructure and biocompatibility

Energy Technology Data Exchange (ETDEWEB)

Zhang, Leilei, E-mail: zhangleilei1121@aliyun.com; Li, Hejun; Li, Kezhi; Zhang, Shouyang; Lu, Jinhua; Li, Wei; Cao, Sheng; Wang, Bin

2013-12-01

To improve the surface biocompatibility of carbon/carbon composites, a carbon foam/hydroxyapatite coating was applied using a combination method of slurry procedure and ultrasound-assisted electrochemical deposition procedure. The morphology, microstructure and chemical composition of the coating were investigated by scanning electron microscopy, energy dispersive X-ray spectroscopy, Fourier transform infrared spectroscopy, Raman spectroscopy and X-ray diffraction. The biocompatibility of the carbon foam/hydroxyapatite coating was investigated by osteoblast-like MG63 cell culture tests. The results showed that the carbon foam could provide a large number of pores on the surface of carbon/carbon composites. The hydroxyapatite crystals could infiltrate into the pores and form the carbon foam/hydroxyapatite coating. The coating covered the carbon/carbon composites fully and uniformly with slice morphology. The cell response tests showed that the MG63 cells on carbon foam/hydroxyapatite coating had a better cell adhesion and cell proliferation than those on uncoated carbon/carbon composites. The carbon foam/hydroxyapatite coatings were cytocompatible and were beneficial to improve the biocompatibility. The approach presented here may be exploited for fabrication of carbon/carbon composite implant surfaces.

Carbon foam/hydroxyapatite coating for carbon/carbon composites: Microstructure and biocompatibility

International Nuclear Information System (INIS)

Zhang, Leilei; Li, Hejun; Li, Kezhi; Zhang, Shouyang; Lu, Jinhua; Li, Wei; Cao, Sheng; Wang, Bin

2013-01-01

To improve the surface biocompatibility of carbon/carbon composites, a carbon foam/hydroxyapatite coating was applied using a combination method of slurry procedure and ultrasound-assisted electrochemical deposition procedure. The morphology, microstructure and chemical composition of the coating were investigated by scanning electron microscopy, energy dispersive X-ray spectroscopy, Fourier transform infrared spectroscopy, Raman spectroscopy and X-ray diffraction. The biocompatibility of the carbon foam/hydroxyapatite coating was investigated by osteoblast-like MG63 cell culture tests. The results showed that the carbon foam could provide a large number of pores on the surface of carbon/carbon composites. The hydroxyapatite crystals could infiltrate into the pores and form the carbon foam/hydroxyapatite coating. The coating covered the carbon/carbon composites fully and uniformly with slice morphology. The cell response tests showed that the MG63 cells on carbon foam/hydroxyapatite coating had a better cell adhesion and cell proliferation than those on uncoated carbon/carbon composites. The carbon foam/hydroxyapatite coatings were cytocompatible and were beneficial to improve the biocompatibility. The approach presented here may be exploited for fabrication of carbon/carbon composite implant surfaces.

Development of high strength hydroxyapatite for bone tissue regeneration using nanobioactive glass composites

Science.gov (United States)

Shrivastava, Pragya; Dalai, Sridhar; Sudera, Prerna; Sivam, Santosh Param; Vijayalakshmi, S.; Sharma, Pratibha

2013-02-01

With an increasing demand of biocompatible bone substitutes for the treatment of bone diseases and bone tissue regeneration, bioactive glass composites are being tested to improvise the osteoconductive as well as osteoinductive properties. Nanobioactive glass (nBG) composites, having composition of SiO2 70 mol%, CaO 26 mol % and P2O5 4 mol% were prepared by Freeze drying method using PEG-PPG-PEG co-polymer. Polymer addition improves the mechanical strength and porosity of the scaffold of nBG. Nano Bioactive glass composites upon implantation undergo specific reactions leading to the formation of crystalline hydroxyapatite (HA). This is tested in vitro using Simulated Body Fluid (SBF). This high strength hydroxyapatite (HA) layer acts as osteoconductive in cellular environment, by acting as mineral base of bones, onto which new bone cells proliferate leading to new bone formation. Strength of the nBG composites as well as HA is in the range of cortical and cancellous bone, thus proving significant for bone tissue regeneration substitutes.

Development of high strength hydroxyapatite for bone tissue regeneration using nanobioactive glass composites

International Nuclear Information System (INIS)

Shrivastava, Pragya; Dalai, Sridhar; Vijayalakshmi, S.; Sudera, Prerna; Sivam, Santosh Param; Sharma, Pratibha

2013-01-01

With an increasing demand of biocompatible bone substitutes for the treatment of bone diseases and bone tissue regeneration, bioactive glass composites are being tested to improvise the osteoconductive as well as osteoinductive properties. Nanobioactive glass (nBG) composites, having composition of SiO 2 70 mol%, CaO 26 mol % and P 2 O 5 4 mol% were prepared by Freeze drying method using PEG-PPG-PEG co-polymer. Polymer addition improves the mechanical strength and porosity of the scaffold of nBG. Nano Bioactive glass composites upon implantation undergo specific reactions leading to the formation of crystalline hydroxyapatite (HA). This is tested in vitro using Simulated Body Fluid (SBF). This high strength hydroxyapatite (HA) layer acts as osteoconductive in cellular environment, by acting as mineral base of bones, onto which new bone cells proliferate leading to new bone formation. Strength of the nBG composites as well as HA is in the range of cortical and cancellous bone, thus proving significant for bone tissue regeneration substitutes.

Fabrication and mechanical evaluation of hydroxyapatite/oxide nano-composite materials

Energy Technology Data Exchange (ETDEWEB)

Mohamed, Khaled R., E-mail: Kh_rezk1966@yahoo.com [Biomaterials Dept., National Research Centre, El-Behoos St., Cairo (Egypt); Beherei, Hanan H. [Biomaterials Dept., National Research Centre, El-Behoos St., Cairo (Egypt); Physics Dept., Faculty of Science, El-Taif University (Saudi Arabia); El Bassyouni, Gehan T. [Biomaterials Dept., National Research Centre, El-Behoos St., Cairo (Egypt); Medical Physics Dept., Faculty of Medicine, El-Taif University (Saudi Arabia); El Mahallawy, Nahed [Design and Production Engineering Department, Faculty of Engineering, Ain Shams University on secondment to the German University in Cairo (Egypt)

2013-10-15

In the current study, the semiconducting metal oxides such as nano-ZnO and SiO{sub 2} powders were prepared via sol–gel technique and conducted on nano-hydroxyapatite (nHA) which was synthesized by chemical precipitation. The properties of fabricated nano-structured composites containing different ratios of HA, ZnO and SiO{sub 2} were examined using X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, scanning electron microscope (SEM) and transmission electron microscope (TEM) techniques. The effect of the variation of ratios between the three components on mechanical, microstructure and in-vitro properties was assessed to explore the possibility of enhancing these properties. The results proved that the mechanical properties exhibited an increment with increasing the ZnO content at the extent of HA. In-vitro study proved the formation and nucleation of apatite onto the surface of the fabricated composites after one week of immersion. It is concluded that HA composites containing SiO{sub 2} or SiO{sub 2}/ZnO content had a suitable mechanical properties and ability to form apatite particles onto the composite surface. Based on bioactivity behavior, Si-HA is more bioactive than pure hydroxyapatite and nano-arrangements will provide an interface for better bone formation. Therefore, these nano-composites will be promising as bone substitutes especially in load bearing sites. - Graphical abstract: Nano-structures of (a) HA, (b) ZnO and (c) SiO{sub 2} powders. Highlights: • The nano-structured composites containing different ratios of HA, ZnO and SiO{sub 2} were prepared. • ZnO helps improve the mechanical properties of HA composites. • SiO{sub 2} helps improve the bioactivity of HA composites.

Preparation and characterization of chitosan-silver/hydroxyapatite composite coatings onTiO{sub 2} nanotube for biomedical applications

Energy Technology Data Exchange (ETDEWEB)

Yan, Yajing [Institute of Life Science and Technology, University of Electronic Science and Technology of China, Chengdu 610054 (China); Zhang, Xuejiao [Medical Informatics, Hebei North University, Zhangjiakou 075000 (China); Li, Caixia [Institute of Life Science and Technology, University of Electronic Science and Technology of China, Chengdu 610054 (China); Huang, Yong [Institute of Life Science and Technology, University of Electronic Science and Technology of China, Chengdu 610054 (China); College of Lab Medicine, Hebei North University, Zhangjiakou 075000 (China); Ding, Qiongqiong [Institute of Life Science and Technology, University of Electronic Science and Technology of China, Chengdu 610054 (China); Pang, Xiaofeng, E-mail: xfpang@aliyun.com [Institute of Life Science and Technology, University of Electronic Science and Technology of China, Chengdu 610054 (China)

2015-03-30

Highlights: • Chitosan/silver-doped hydroxyapatite biocomposite coating was successfully deposited on anodized Ti by electrochemical deposition. • The chemical state of silver in the synthesized coatings was studied by XPS peak deconvolution. • The synthesized coatings have excellent antibacterial activity because of synergistic effect of the Ag and CS. • The CSAgHAp coatings showed good biocompatibility and no adverse effect in cell culture tests. - Abstract: A biocomposite coating containing chitosan, silver, and hydroxyapatite was developed on anodized titanium substrate by electrochemical deposition. Coatings were characterized by field-emission scanning electron microscopy, X-ray diffraction, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy and polarisation studies. Results showed that the prepared coatings had compact and dense morphology with a thickness of 6.2 ± 0.7 μm and that silver was evenly distributed. Testing the prepared coatings with Gram-positive and Gram-negative bacterial strains exhibited antibacterial activity because of the synergistic effect of silver and chitosan. The prepared coatings were also found to be nontoxic to MC3T3-E1 cells. These results suggested that chitosan/silver-hydroxyapatite biocomposite coatings can prevent the bacterial infection of implants.

Cytotoxic evaluation of hydroxyapatite-filled and silica/hydroxyapatite-filled acrylate-based restorative composite resins: An in vitro study.

Science.gov (United States)

Chadda, Harshita; Naveen, Sangeetha Vasudevaraj; Mohan, Saktiswaren; Satapathy, Bhabani K; Ray, Alok R; Kamarul, Tunku

2016-07-01

Although the physical and mechanical properties of hydroxyapatite-filled dental restorative composite resins have been examined, the biocompatibility of these materials has not been studied in detail. The purpose of this in vitro study was to analyze the toxicity of acrylate-based restorative composite resins filled with hydroxyapatite and a silica/hydroxyapatite combination. Five different restorative materials based on bisphenol A-glycidyl methacrylate (bis-GMA) and tri-ethylene glycol dimethacrylate (TEGDMA) were developed: unfilled (H0), hydroxyapatite-filled (H30, H50), and silica/hydroxyapatite-filled (SH30, SH50) composite resins. These were tested for in vitro cytotoxicity by using human bone marrow mesenchymal stromal cells. Surface morphology, elemental composition, and functional groups were determined by scanning electron microscopy (SEM), energy-dispersive x-ray spectroscopy (EDX), and Fourier-transformed infrared spectroscopy (FTIR). The spectra normalization, baseline corrections, and peak integration were carried out by OPUS v4.0 software. Both in vitro cytotoxicity results and SEM analysis indicated that the composite resins developed were nontoxic and supported cell adherence. Elemental analysis with EDX revealed the presence of carbon, oxygen, calcium, silicon, and gold, while the presence of methacrylate, hydroxyl, and methylene functional groups was confirmed through FTIR analysis. The characterization and compatibility studies showed that these hydroxyapatite-filled and silica/hydroxyapatite-filled bis-GMA/TEGDMA-based restorative composite resins are nontoxic to human bone marrow mesenchymal stromal cells and show a favorable biologic response, making them potential biomaterials. Copyright © 2016 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

Preparation and bioactivity evaluation of hydroxyapatite-titania/chitosan-gelatin polymeric biocomposites

International Nuclear Information System (INIS)

Mohamed, Khaled R.; Mostafa, Amani A.

2008-01-01

Biocomposites consisting of hydroxyapatite (HA) and natural polymers such as collagen, chitosan, chitin,and gelatin have been extensively investigated. However, studies on the combination of HA and titania with chitosan and gelatin have not been conducted yet. Novel biodegradable hydroxyapatite-titania/chitosan-gelatin polymeric composites were fabricated. In this work, our results are concerning with the preparation and characterization of HA powder and HA filler containing titania powder (10 and 30%) with a chitosan and gelatin copolymer matrix. The present research focuses on characterizing the structure of this novel class of biocomposites. Thermogravimetric analysis (TGA), X-ray diffraction (XRD), and Fourier Transformed Infrared Spectroscopy (FT-IR), Scanning electron microscopy (SEM-EDAX) were employed to assess the produced composites. The mechanical properties in terms of compressive strength and hardness test were also investigated. The in vitro study in simulated body fluid (SBF) was performed to assess the bioactivity of composites. The results proved that apatite resembling natural bone are formed faster and greater in the case the composite of HA containing 10% titania into chitosan-gelatin polymeric matrix when they are soaked in a simulated body fluid (SBF) than the composite containing 30% titania. The biocomposites containing HA with 10% titania are expected to be attractive for bioapplications as bone substitutes and scaffolds for tissue engineering in future

Hydroxyapatite/zirconia-microfibre composites with controlled microporosity and fracture properties prepared by electrophoretic deposition

Czech Academy of Sciences Publication Activity Database

Drdlík, D.; Sláma, M.; Hadraba, Hynek; Cihlář, J.

2015-01-01

Roč. 41, č. 9 (2015), s. 11202-11212 ISSN 0272-8842 R&D Projects: GA ČR(CZ) GAP108/11/1644; GA MŠk(CZ) ED1.1.00/02.0068 Institutional support: RVO:68081723 Keywords : hydroxyapatite * zirconia * composite * electrophoretic deposition * porosity Subject RIV: JH - Ceramics, Fire-Resistant Materials and Glass Impact factor: 2.758, year: 2015

Fabrication and mechanical evaluation of hydroxyapatite/oxide nano-composite materials.

Science.gov (United States)

Mohamed, Khaled R; Beherei, Hanan H; El Bassyouni, Gehan T; El Mahallawy, Nahed

2013-10-01

In the current study, the semiconducting metal oxides such as nano-ZnO and SiO2 powders were prepared via sol-gel technique and conducted on nano-hydroxyapatite (nHA) which was synthesized by chemical precipitation. The properties of fabricated nano-structured composites containing different ratios of HA, ZnO and SiO2 were examined using X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, scanning electron microscope (SEM) and transmission electron microscope (TEM) techniques. The effect of the variation of ratios between the three components on mechanical, microstructure and in-vitro properties was assessed to explore the possibility of enhancing these properties. The results proved that the mechanical properties exhibited an increment with increasing the ZnO content at the extent of HA. In-vitro study proved the formation and nucleation of apatite onto the surface of the fabricated composites after one week of immersion. It is concluded that HA composites containing SiO2 or SiO2/ZnO content had a suitable mechanical properties and ability to form apatite particles onto the composite surface. Based on bioactivity behavior, Si-HA is more bioactive than pure hydroxyapatite and nano-arrangements will provide an interface for better bone formation. Therefore, these nano-composites will be promising as bone substitutes especially in load bearing sites. Copyright © 2013 Elsevier B.V. All rights reserved.

Effect of the addition of collagen in the preparation of hydroxyapatite, aiming the application of pulp capping

International Nuclear Information System (INIS)

Ribeiro, Geysy L.; Mendes, Luis C.

2011-01-01

This work studied the action of collagen (COLL) in the hydroxyapatite (HA) synthesis, produced through sol-gel process, in order to mimetize the chemical composition of dental tissue. The resulting material was characterized by energy dispersive X-ray spectroscopy (EDX), Fourier transform infrared spectroscopy (FT-IR), wide-angle X-ray diffraction (WAXD) and scanning electron microscopy (SEM). The Ca/P ratio was determined through EDX - 1,89 e 2,38, with and without collagen, respectively. The FT-IR analysis showed no significant interaction between the constituents of the composite. The R-ray diffractograms indicated an increase of the resolution and intensity of the HA peak. The photomicrographies showed that the preparation method exhibited significantly influence onto the hydroxyapatite morphology, as well as resulted in a homogeneously dispersed composite. (author)

Protein Adsorption and Antibacterial Behavior for Hydroxyapatite Nanocrystals Prepared by Hydrothermal Method

OpenAIRE

笠原, 英充; 小形, 信男; 荻原, 隆

2005-01-01

Homogeneous hydroxyapatite nanocrystals which have aspect ratio with more than four were synthesized by hydrothermal method. X-ray fluorescence analysis revealed that the Ca/P ratio of hydroxyapatite nanocrystals was maintaining start composition. The protein adsorption properties and bacteria-resistant of hydroxyapatite nanocrystals were investigated. The protein adsorption properties of hydroxyapatite nanocrystals were improvement after the hydrothermal treatment. Bacteria-resistant behavio...

Preparation and Characterization of Starch-g-PVA/Nano-hydroxyapatite Complex Hydrogel

Institute of Scientific and Technical Information of China (English)

无

2005-01-01

Starch-g-PVA/hydroxyapatite complex hydrogel was prepared with two-repeated freezing/ thawing circles. SEM observation results exhibits that hydroxyapatite is dispersed in starch-g-PVA in nanoscale. Thermogravimetric analysis curves show that the remained fraction keeps the same at the temperatures higher than 490℃ . It was found the dried starch-g- PVA/ hydroxyapatite films could reswell within 12 minutes.

Preparation and characterization of a novel degradable nano-hydroxyapatite/poly(lactic-co-glycolic) composite reinforced with bamboo fiber.

Science.gov (United States)

Jiang, Liuyun; Li, Ye; Xiong, Chengdong; Su, Shengpei

2017-06-01

It is a promising and challenging to achieve an ideal poly (lactic-co-glycolic) (PLGA)-based composite. In this paper, bamboo fiber (BF) was firstly designed to incorporate into nano-hydroxyapatite/PLGA (n-HA/PLGA) composite, and a series of novel biodegradable BF/n-HA/PLGA ternary composites with different BF amounts (0wt%, 5wt%, 10wt% and 20wt%) were prepared by solution mixing method. The effect of BF content on the crystallization behavior, interface structure and mechanical property of BF/n-HA/PLGA ternary composite was investigated by X-ray diffraction pattern (XRD), differential scanning calorimeter (DSC) and scanning electron microscope (SEM), comparing with pure PLGA and n-HA/PLGA composite. The results showed that BF further promoted the crystallization of PLGA acting as a heterogeneous nucleation agent, and the addition of 10wt% BF was the best benefit to promote the crystallization. However, the higher addition content of BF caused more agglomeration in n-HA/PLGA matrix, which decreased gradually the mechanical properties of the BF/n-HA/PLGA composite. In conclusion, the addition content of 5wt% BF to n-HA/PLGA matrix was an appropriate proportion, which can achieved the best mechanical reinforce effectiveness, suggesting that BF/n-HA/PLGA composite had more potential in biomedical application than n-HA/PLGA composite. Copyright © 2017 Elsevier B.V. All rights reserved.

Properties of poly(lactic acid)/hydroxyapatite composite through the use of epoxy functional compatibilizers for biomedical application.

Science.gov (United States)

Monmaturapoj, Naruporn; Srion, Autcharaporn; Chalermkarnon, Prasert; Buchatip, Suthawan; Petchsuk, Atitsa; Noppakunmongkolchai, Warobon; Mai-Ngam, Katanchalee

2017-08-01

A composite of 70/30 poly(lactic acid)/hydroxyapatite was systematically prepared using various amounts of glycidyl methacrylate as reactive compatibilizer or Joncryl ADR®-4368 containing nine glycidyl methacrylate functions as a chain extension/branching agent to improve the mechanical and biological properties for suitable usage as internal bone fixation devices. The effect of glycidyl methacrylate/Joncryl on mechanical properties of poly(lactic acid)/hydroxyapatite was investigated through flexural strength. Cell proliferation and differentiation of osteoblast-like MC3T3-E1 cells cultured on the composite samples were determined by Alamar Blue assay and alkaline phosphatase expression, respectively. Result shows that flexural strength tends to decrease, as glycidyl methacrylate content increases except for 1 wt.% glycidyl methacrylate. With an addition of dicumyl peroxide, the flexural strength shows an improvement than that of without dicumyl peroxide probably due to the chemical bonding of the hydroxyapatite and poly(lactic acid) as revealed by FTIR and NMR, whereas the composite with 5 wt.% Joncryl shows the best result, as the flexural strength increases getting close to pure poly(lactic acid). The significant morphology change could be seen in composite with Joncryl where the uniform agglomeration of hydroxyapatite particles oriented in poly(lactic acid) matrix. Addition of the epoxy functional compatibilizers at suitable percentages could also have benefits to cellular attachment, proliferation, differentiation and mineralization. So that, this poly(lactic acid)/hydroxyapatite composite could be a promising material to be used as internal bone fixation devices such as screws, pins and plates.

Microstructure and property evolutions of titanium/nano-hydroxyapatite composites in-situ prepared by selective laser melting.

Science.gov (United States)

Han, Changjun; Wang, Qian; Song, Bo; Li, Wei; Wei, Qingsong; Wen, Shifeng; Liu, Jie; Shi, Yusheng

2017-07-01

Titanium (Ti)-hydroxyapatite (HA) composites have the potential for orthopedic applications due to their favorable mechanical properties, excellent biocompatibility and bioactivity. In this work, the pure Ti and nano-scale HA (Ti-nHA) composites were in-situ prepared by selective laser melting (SLM) for the first time. The phase, microstructure, surface characteristic and mechanical properties of the SLM-processed Ti-nHA composites were studied by X-ray diffraction, transmission electron microscope, atomic force microscope and tensile tests, respectively. Results show that SLM is a suitable method for fabricating the Ti-nHA composites with refined microstructure, low modulus and high strength. A novel microstructure evolution can be illustrated as: Relatively long lath-shaped grains of pure Ti evolved into short acicular-shaped and quasi-continuous circle-shaped grains with the varying contents of nHA. The elastic modulus of the Ti-nHA composites is 3.7% higher than that of pure Ti due to the effect of grain refinement. With the addition of 2% nHA, the ultimate tensile strength significantly reduces to 289MPa but still meets the application requirement of bone implants. The Ti-nHA composites exhibit a remarkable improvement of microhardness from 336.2 to 600.8 HV and nanohardness from 5.6 to 8.3GPa, compared to those of pure Ti. Moreover, the microstructure and property evolution mechanisms of the composites with the addition of HA were discussed and analyzed. It provides some new knowledge to the design and fabrication of biomedical material composites for bone implant applications. Copyright © 2017 Elsevier Ltd. All rights reserved.

Preparation of nano-hydroxyapatite/poly(l-lactide) biocomposite microspheres

International Nuclear Information System (INIS)

Qiu Xueyu; Han Yadong; Zhuang Xiuli; Chen Xuesi; Li Yuesheng; Jing Xiabin

2007-01-01

Nano-hydroxyapatite (HA)/poly(l-lactide) (PLLA) composite microspheres with relatively uniform size distribution were prepared by a solid-in-oil-in-water (s/o/w) emusion solvent evaporation method. The encapsulation of the HA nanopaticles in microshperes was significantly improved by grafting PLLA on the surface of the HA nanoparticles (p-HA) during emulsion process. This procedure gave a possibility to obtain p-HA/PLLA composite microspheres with uniform morphology and the encapsulated p-HA nanoparticle loading reached up to 40 wt% (33 wt% of pure HA) in the p-HA/PLLA composite microspheres. The microstructure of composite microspheres from core-shell to single phase changed with the variation of p-HA to PLLA ratios. p-HA/PLLA composite microspheres with the diameter range of 2-3 μm were obtained. The entrapment efficiency of p-HA in microspheres could high up to 90 wt% and that of HA was only 13 wt%. Surface and bulk characterizations of the composite microspheres were performed by measurements such as wide angle X-ray diffraction (WAXD), thermal gravimetric analysis (TGA), environmental scanning electron microscope (ESEM) and transmission electron microscopy (TEM)

Fabrication of naturel pumice/hydroxyapatite composite for biomedical engineering.

Science.gov (United States)

Komur, Baran; Lohse, Tim; Can, Hatice Merve; Khalilova, Gulnar; Geçimli, Zeynep Nur; Aydoğdu, Mehmet Onur; Kalkandelen, Cevriye; Stan, George E; Sahin, Yesim Muge; Sengil, Ahmed Zeki; Suleymanoglu, Mediha; Kuruca, Serap Erdem; Oktar, Faik Nuzhet; Salman, Serdar; Ekren, Nazmi; Ficai, Anton; Gunduz, Oguzhan

2016-07-07

We evaluated the Bovine hydroxyapatite (BHA) structure. BHA powder was admixed with 5 and 10 wt% natural pumice (NP). Compression strength, Vickers micro hardness, Fourier transform infrared spectroscopy, scanning electron microscopy (SEM) and X-ray diffraction studies were performed on the final NP-BHA composite products. The cells proliferation was investigated by MTT assay and SEM. Furthermore, the antimicrobial activity of NP-BHA samples was interrogated. Variances in the sintering temperature (for 5 wt% NP composites) between 1000 and 1300 °C, reveal about 700 % increase in the microhardness (~100 and 775 HV, respectively). Composites prepared at 1300 °C demonstrate the greatest compression strength with comparable result for 5 wt% NP content (87 MPa), which are significantly better than those for 10 wt% and those that do not include any NP (below 60 MPa, respectively). The results suggested the optimal parameters for the preparation of NP-BHA composites with increased mechanical properties and biocompatibility. Changes in micro-hardness and compression strength can be tailored by the tuning the NP concentration and sintering temperature. NP-BHA composites have demonstrated a remarkable potential for biomedical engineering applications such as bone graft and implant.

Titanium-hydroxyapatite composites sintered at low temperature for tissue engineering: in vitro cell support and biocompatibility.

Science.gov (United States)

Comín, Romina; Cid, Mariana P; Grinschpun, Luciano; Oldani, Carlos; Salvatierra, Nancy A

2017-04-26

In clinical orthopedics, a critical problem is the bone tissue loss produced by a disease or injury. The use of composites from titanium and hydroxyapatite for biomedical applications has increased due to the resulting advantageous combination of hydroxyapatite bioactivity and favorable mechanical properties of titanium. Powder metallurgy is a simple and lower-cost method that uses powder from titanium and hydroxyapatite to obtain composites having hydroxyapatite phases in a metallic matrix. However, this method has certain limitations arising from thermal decomposition of hydroxyapatite in the titanium-hydroxyapatite system above 800°C. We obtained a composite from titanium and bovine hydroxyapatite powders sintered at 800°C and evaluated its bioactivity and cytocompatibility according to the ISO 10993 standard. Surface analysis and bioactivity of the composite was evaluated by X-ray diffraction and SEM. MTT assay was carried out to assess cytotoxicity on Vero and NIH3T3 cells. Cell morphology and cell adhesion on the composite surface were analyzed using fluorescence and SEM. We obtained a porous composite with hydroxyapatite particles well integrated in titanium matrix which presented excellent bioactivity. Our data did not reveal any toxicity of titanium-hydroxyapatite composite on Vero or NIH3T3 cells. Moreover, extracts from composite did not affect cell morphology or density. Finally, NIH3T3 cells were capable of adhering to and proliferating on the composite surface. The composite obtained displayed promising biomedical applications through the simple method of powder metallurgy. Additionally, these findings provide an in vitro proof for adequate biocompatibility of titanium-hydroxyapatite composite sintered at 800°C.

Hydroxyapatite-alginate nanocomposite as drug delivery matrix for sustained release of ciprofloxacin.

Science.gov (United States)

Venkatasubbu, G Devanand; Ramasamy, S; Ramakrishnan, V; Kumar, J

2011-12-01

Hydroxyapatite is a bioceramic which has a wide range of medical application for bone diseases. To enhance its usage, we have prepared ciprofloxacin loaded nano hydroxyapatite (HA) composite with a natural polymer, alginate, using wet chemical method at low temperature. The prepared composites were analyzed by various physicochemical methods. The results show that the nano HA crystallites are well intact with the alginate macromolecules. For the composite system FT-IR and micro Raman results are reported in this paper. Studies on the drug loading and drug release have been done. The drug is pre-adsorbed onto the ceramic particle before the formation of composite. The thermal behavior of composite has been studied using thermo gravimetric analysis (TGA). This work, reports that the nanocomposite prepared under optimum condition could prolong the release of ciprofloxacin compared with the ciprofloxacin loaded hydroxyapatite.

Photo-oxidation of gaseous ethanol on photocatalyst prepared by acid leaching of titanium oxide/hydroxyapatite composite

International Nuclear Information System (INIS)

Ono, Y.; Rachi, T.; Yokouchi, M.; Kamimoto, Y.; Nakajima, A.; Okada, K.

2013-01-01

Highlights: ► Photocatalyst powder was prepared by acid leaching of TiO 2 /apatite composite. ► The photocatalytic activity was evaluated from in situ FT-IR study using ethanol. ► Apatite in the composite had positive effect for the photo-oxidation of ethanol. ► The enhanced oxidation rate was explained by the difference in deactivation rate. - Abstract: Highly active photocatalysts were synthesized by leaching of heat-treated titanium dioxide (TiO 2 )/hydroxyapatite (HAp) powder with hydrochloric acid at 0.25, 0.50, 0.75 mol/l, and their photocatalytic activities were evaluated from in situ Fourier transform infrared (FT-IR) study of photo-oxidation of gaseous ethanol. By changing the acid concentration, the TiO 2 /HAp composite had different atomic ratios of Ca/Ti (0.0–2.8) and P/Ti (0.3–2.1). It was found that phosphate group remained on the surface of TiO 2 particle even in the sample treated with concentrated acid (0.75 mol/l). These acid-treated samples showed higher rates for ethanol photo-oxidation than the commercial TiO 2 powder, Degussa P25. The highest rate was obtained in the TiO 2 /HAp composite treated with the dilute (0.25 mol/l) acid in spite of its low content of TiO 2 photocatalyst. This enhanced photocatalytic activity was attributed to the result that the deactivation with repeated injections of ethanol gas was suppressed in the TiO 2 /HAp composites compared with the TiO 2 powders

Mechanical Properties of Chitosan-Starch Composite Filled Hydroxyapatite Micro- and Nanopowders

Directory of Open Access Journals (Sweden)

Jafar Ai

2011-01-01

Full Text Available Hydroxyapatite is a biocompatible ceramic and reinforcing material for bone implantations. In this study, Starch-chitosan hydrogel was produced using the oxidation of starch solution and subsequently cross-linked with chitosan via reductive alkylation method (weight ratio (starch/chitosan: 0.38. The hydroxyapatite micropowders and nanopowders synthesized by sol-gel method (10, 20, 30, 40 %W were composited to hydrogels and were investigated by mechanical analysis. The results of SEM images and Zetasizer experiments for synthesized nanopowders showed an average size of 100 nm. The nanoparticles distributed as uniform in the chitosan-starch film. The tensile modulus increased for composites containing hydroxyapatite nano-(size particle: 100 nanometer powders than composites containing micro-(size particle: 100 micrometer powders. The swelling percentage decreased for samples containing hydroxyapatite nanopowder than the micropowders. These nanocomposites could be applied for hard-tissue engineering.

Microwave sintering of hydroxyapatite-based composites

International Nuclear Information System (INIS)

Fang, Y.; Roy, D.M.; Cheng, J.; Roy, R.; Agrawal, D.K.

1993-01-01

Composites of hydroxyapatite/partially stabilized zirconia (HAp/PSZ) and hydroxyapatite/silicon carbide whiskers (HAp/SiC) were sintered at 1100-1200 degrees C by microwave at 2.45 GHz. Characterization of the sintered composites was carried out by density, microstructure, phase composition, and fracture toughness measurements. The results show that although not yet fully densified, a much higher sintered density in the HAp/PSZ composite was achieved by microwave sintering than by conventional sintering at the same temperature. A relative density of 93% was achieved by 20 min. microwave processing at 1200 degrees C. Comparatively, 2 h conventional sintering of the same material at 1200 degrees C led to only 75.5% relative density. K IC of this microwave sintered HAp/PSZ of 93% density was found to be 3.88 MPa√m, which is 250% of the value for pure HAp of the same density. A further increase in K IC could be expected if full or nearly full densification was achieved. Sintering of PSZ particles in the HAp/PSZ composite was also observed in the microwave processed sample. Microwave sintering of HAp/SiC was not successful in the current study due to the oxidation of SiC in air at high temperature. 8 refs., 4 figs., 1 tab

Bio-based polyurethane for tissue engineering applications: How hydroxyapatite nanoparticles influence the structure, thermal and biological behavior of polyurethane composites.

Science.gov (United States)

Gabriel, Laís P; Santos, Maria Elizabeth M Dos; Jardini, André L; Bastos, Gilmara N T; Dias, Carmen G B T; Webster, Thomas J; Maciel Filho, Rubens

2017-01-01

In this work, thermoset polyurethane composites were prepared by the addition of hydroxyapatite nanoparticles using the reactants polyol polyether and an aliphatic diisocyanate. The polyol employed in this study was extracted from the Euterpe oleracea Mart. seeds from the Amazon Region of Brazil. The influence of hydroxyapatite nanoparticles on the structure and morphology of the composites was studied using scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS), the structure was evaluated by Fourier transform infrared spectroscopy (FT-IR), thermal properties were analyzed by thermogravimetry analysis (TGA), and biological properties were studied by in vitro and in vivo studies. It was found that the addition of HA nanoparticles promoted fibroblast adhesion while in vivo investigations with histology confirmed that the composites promoted connective tissue adherence and did not induce inflammation. In this manner, this study supports the further investigation of bio-based, polyurethane/hydroxyapatite composites as biocompatible scaffolds for numerous tissue engineering applications. Copyright © 2016 Elsevier Inc. All rights reserved.

[Study on the antibacterial activity of four kinds of nano-hydroxyapatite composites against Enterococcus faecalis].

Science.gov (United States)

Liu, Yi; Zhou, Rongjing; Wu, Hongkun

2015-06-01

This study aims to compare and determine a kind of nano-hydroxyapatite composite material with good antibacterial efficacy on Enterococcusfaecalis (E. faecalis) in vitro. We investigated the antimicrobial activity of four kinds of nano-hydroxyapatite composites, namely, silver/hydroxyapatite composite nanoparticles (Ag/nHA), yttrium/hydroxyapatite composite nanoparticles (Yi/nHA), cerium/hydroxyapatite composite nanoparticles (Ce/nHA), and hydroxyapatite nanoparticles (nHA), against E. faecalis in vitro using the agar diffusion and broth dilution method by measuring the growth inhibition zone and the minimum inhibitory concentration (MIC), respectively. The agar diffusion test results showed that Ag/nHA displayed an obvious growth inhibition zone, whereas Yi/nHA, Ce/nHA, and nHA showed no influence on E. faecalis. The MIC value of Ag/nHA was 1.0 g.L-1, and the three other materials had no effect on E.faecalis even at the high concentration of 32.0 g.L-1. Ag/nHA display a potential antimicrobial efficacy to planktonic E.faecalis. Whereas, the three other kinds of nano-hydroxyapatite composites (Yi/nHA, Ce/nHA, nHA) show no influence.

Synthesis and in-depth analysis of highly ordered yttrium doped hydroxyapatite nanorods prepared by hydrothermal method and its mechanical analysis

International Nuclear Information System (INIS)

Nathanael, A. Joseph; Mangalaraj, D.; Hong, S.I.; Masuda, Y.

2011-01-01

In this study, undoped and yttrium (Y) doped nanocrystalline hydroxyapatite crystals were synthesized by the hydrothermal method at 180 °C for 24 h. Highly ordered and oriented hydroxyapatite (HAp) nanorods were prepared by yttrium doping and their nanostructure and physical properties were compared with those of undoped HAp rods. FESEM images showed that the doping with Y ions reduced the diameter (from 25 nm to 15 nm) and increased the length (from 95 nm to 115 nm) of the synthesized rods. The aspect ratio of the undoped and Y-doped nanorods were calculated to be 4.303 (SD = 0.0959) and 7.61 (SD = 0.0355), respectively. Specific surface area (SSA) analysis showed that SSA also increased from 66.74 m 2 /g to 68.57 m 2 /g with the addition of yttrium. Y-doped HAp nanorod reinforced HMWPE composites displayed the better mechanical performance than those reinforced with pure HAp nanorods. The possible strengthening of nanorods and the increase of SSA due to the reduction in the size of nanorods in the presence of yttrium may have contributed to the strengthening of Y-doped HAp/HMWPE composites. - Graphical Abstract: Highly ordered and oriented yttrium doped hydroxyapatite (HAp) nanorods were prepared by hydrothermal method. For undoped HAp the average length of the nanorod is 95 nm with mean diameter of 24 nm and for a Y doped nanorod the average length is ∼ 115 nm and the mean diameter is 15 nm. Mechanical analysis was carried out by polymer/nanoparticle composite method. Highlights: ► Yttrium doped hydroxyapatite nanorods were prepared by hydrothermal method. ► The nanorods have highly uniform size distribution. ► Yttrium substitution and nanostructure formation was confirmed by careful analysis. ► Mechanical strength was analyzed by polymer nanoparticle reinforcement method.

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

International Nuclear Information System (INIS)

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

2014-01-01

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 ± 20.4 nm 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 5.0 wt.% 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. - Highlights: • SF fibers were firstly successfully dissolved in FA/HAp solution. • The rheological behavior of SF solution was significantly influenced by HAp contents. • SF nanofibrils were observed in FA/HAp solution with 103.6 ± 20.4 nm in diameter. • SF films prepared by FA/HAp dissolution method had higher mechanical properties

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

Energy Technology Data Exchange (ETDEWEB)

Ming, Jinfa, E-mail: jinfa.ming@gmail.com [National Engineering Laboratory for Modern Silk, Soochow University, Suzhou 215123 (China); College of Textile and Clothing Engineering, Soochow University, Suzhou 215021 (China); Liu, Zhi; Bie, Shiyu [National Engineering Laboratory for Modern Silk, Soochow University, Suzhou 215123 (China); College of Textile and Clothing Engineering, Soochow University, Suzhou 215021 (China); Zhang, Feng [Jiangsu Province Key Laboratory of Stem Cell Research, Medical College, Soochow University, Suzhou 215006 (China); Zuo, Baoqi, E-mail: bqzuo@suda.edu.cn [National Engineering Laboratory for Modern Silk, Soochow University, Suzhou 215123 (China); College of Textile and Clothing Engineering, Soochow University, Suzhou 215021 (China)

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 ± 20.4 nm 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 5.0 wt.% 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. - Highlights: • SF fibers were firstly successfully dissolved in FA/HAp solution. • The rheological behavior of SF solution was significantly influenced by HAp contents. • SF nanofibrils were observed in FA/HAp solution with 103.6 ± 20.4 nm in diameter. • SF films prepared by FA/HAp dissolution method had higher mechanical properties.

Mechanical and microstructure of reinforced hydroxyapatite/calcium silicate nano-composites materials

International Nuclear Information System (INIS)

Beheri, Hanan H.; Mohamed, Khaled R.; El-Bassyouni, Gehan T.

2013-01-01

Highlights: ► Nano sized of HA and CS powders were prepared. ► Mechanical of HACS composites enhanced with content of CS. ► The apatite formation onto the composites is proved. -- Abstract: In this study, the nano sized hydroxyapatite (HA) and calcium silicate (CS) powders prepared by both chemical precipitation and sol–gel methods respectively. Biphasic nano-composites materials containing different ratios of HA and CS were fabricated and assessed using X-ray diffraction (XRD), Fourier transmission infrared reflectance (FT-IR), transmission electron microscopy (TEM) and scanning electron microscopy (SEM) techniques. The effect of variation of ratios between HA and CS on mechanical properties, microstructure and in vitro study was studied. The results proved that the mechanical properties were enhanced with increasing the CS ratio in the composite. In vitro study proved the formation and nucleation of apatite onto composites surfaces which contain low content of CS after one week of immersion. Finally, it is concluded that the HACS composites containing high HA content at the expense of CS content will be promising for bone substitute’s applications, especially in load bearing sites.

Processing and characterization of glass reinforced biogenic hydroxyapatite composites with ferromagnetic additives

Directory of Open Access Journals (Sweden)

Nataliya Pinchuk

2008-06-01

Full Text Available Biogenic hydroxyapatite-glass composites, with addition of up to 2 wt.% of Fe or Fe3O4, were fabricated from biogenic hydroxyapatite powder and four types of reinforcing glasses by sintering under different conditions. It has been established that the relative density, mechanical and magnetic properties of the prepared composites depend on the composition and sintering conditions. The composites with 1 wt.% Fe or Fe3O4 sintered at 500°С in vacuum have a magnetic susceptibility of 2–3·10-3 cm3/g. This parameter decreases to 0.858·10-3 cm3/g for the specimens with 1 wt.% additives sintered at 800°С in vacuum and to 0.27–1.3·10-3cm3/g for the specimens with 2 wt.% additives sintered at 500°С under the usual atmospheric conditions. The magnetic susceptibility for the specimens with 2 wt.% additives sintered at 780°С under the same atmospheric conditions decreases to 0.24–1.25·10-6 cm3/g. These ferromagnetic additives influence the degradation rate in vitro within the first 40 min of the composite soaking. Short-term treatment of specimens by the magnetic field leads to an increase in the initial degradation rate, but insignificantly influences it within more prolonged soaking.

Photo-oxidation of gaseous ethanol on photocatalyst prepared by acid leaching of titanium oxide/hydroxyapatite composite

Energy Technology Data Exchange (ETDEWEB)

Ono, Y., E-mail: ono-y@kanagawa-iri.go.jp [Mechanical and Material Engineering Division, Kanagawa Industrial Technology Center, Ebina, Kanagawa 243-0435 (Japan); Rachi, T.; Yokouchi, M.; Kamimoto, Y. [Mechanical and Material Engineering Division, Kanagawa Industrial Technology Center, Ebina, Kanagawa 243-0435 (Japan); Nakajima, A. [Department of Metallurgy and Ceramics Science, Tokyo Institute of Technology, Meguro, Tokyo 152-8552 (Japan); Okada, K. [Materials and Structures Laboratory, Tokyo Institute of Technology, Midori, Yokohama, Kanagawa 226-8503 (Japan)

2013-06-01

Highlights: ► Photocatalyst powder was prepared by acid leaching of TiO{sub 2}/apatite composite. ► The photocatalytic activity was evaluated from in situ FT-IR study using ethanol. ► Apatite in the composite had positive effect for the photo-oxidation of ethanol. ► The enhanced oxidation rate was explained by the difference in deactivation rate. - Abstract: Highly active photocatalysts were synthesized by leaching of heat-treated titanium dioxide (TiO{sub 2})/hydroxyapatite (HAp) powder with hydrochloric acid at 0.25, 0.50, 0.75 mol/l, and their photocatalytic activities were evaluated from in situ Fourier transform infrared (FT-IR) study of photo-oxidation of gaseous ethanol. By changing the acid concentration, the TiO{sub 2}/HAp composite had different atomic ratios of Ca/Ti (0.0–2.8) and P/Ti (0.3–2.1). It was found that phosphate group remained on the surface of TiO{sub 2} particle even in the sample treated with concentrated acid (0.75 mol/l). These acid-treated samples showed higher rates for ethanol photo-oxidation than the commercial TiO{sub 2} powder, Degussa P25. The highest rate was obtained in the TiO{sub 2}/HAp composite treated with the dilute (0.25 mol/l) acid in spite of its low content of TiO{sub 2} photocatalyst. This enhanced photocatalytic activity was attributed to the result that the deactivation with repeated injections of ethanol gas was suppressed in the TiO{sub 2}/HAp composites compared with the TiO{sub 2} powders.

Preparation and characterization of hydroxyapatite/gelatin composite membranes for immunoisolation

Science.gov (United States)

Chen, Jyh-Ping; Chang, Feng-Nian

2012-12-01

Composite membranes are fabricated from hydroxyapatite (HAP) and gelatin for immunoisolation of cells. The films were fabricated by crosslinking 5 wt%, 10 wt%, and 20 wt% gelatin with 1 wt% glutaraldehyde (GA) in the presence of HAP. Fourier transform infrared spectroscopy analysis confirms imide bond formation between GA and gelatin, while the crystal structure of HAP powder remains unchanged from X-ray diffraction analysis. The degree of crosslinking depends on crosslinking time and gelatin concentration. For 5% and 10% gelatin, the degree of crosslinking levels off at 90% within 48 h. From scanning electron microscopy micrographs, the microstructure of the composite membrane depends on the amount of gelatin used in the crosslinking reaction. The mechanical strength of the composite membrane could be enhanced by increasing the gelatin concentration. BET analysis indicates that pore size of the micropores on the surface HAP/gelatin agglomerates decreases with increasing gelatin concentration. However, the macropore, through which diffusion of molecules occurs, is larger at higher gelatin concentrations. The permeability coefficients of different molecules through a HAP/gelatin composite membrane increase with increasing gelatin concentration and is inversely correlated with the molecular weight of the molecule. For immunoisolation of cells, the diffusion of large molecules stimulated by the immune system can be rejected by a chamber constructed from the HAP/gelatin membrane. Insulinoma cells were encapsulated in alginate-poly-L-lysine-alginate microcapsules and enclosed in a HAP/gelatin chamber. The chamber did not impair the viability and function of insulinoma cells and cells can secrete insulin in response to glucose concentration change. The chamber is therefore useful for the physiologically controlled secretion of insulin in response to the blood glucose level. Intraperitoneal transplantation of the chamber into streptozotocin-induced diabetic SD rats could

Porous hydroxyapatite composite with alumina for bone repair

International Nuclear Information System (INIS)

Rusnah Mustaffa; Mohd Reusmaazran Mohd Yusof; Idris Besar

2010-01-01

Porous fabrications, a number of techniques were investigated using polyurethane foam as the scaffold. These techniques involve dipping of the foam into a slurry prepared by mixing of HA+Al 2 O 3 powder with PVA and Sago as binder and subjecting to burn off procedure to get the porous products. Sintering parameter was studied at 1100, 1200 and 1300 degree Celsius. Initially HA powder was prepared by the sol-gel precipitation method using calcium hydroxide and ortho-phosphoric acid meanwhile Al 2 O 3 powder from supplier (MERK). The fine HA powder, measuring 2 O 3 . These techniques also produce the uniformity pore shape. Characterization of the physical analysis, porosity, surface morphology by Scanning Electron Microscopy analysis (SEM) and compression strength were studied. Mechanical properties showing that the composite of porous HA+Al 2 O 3 gives higher maximum compression strength compared to the porous hydroxyapatite itself. Observation from this studied the increasing of temperature will increase the strength. (author)

Preparation and Characterization of Biomimetic Hydroxyapatite-Resorbable Polymer Composites for Hard Tissue Repair

Science.gov (United States)

Hiebner, Kristopher Robert

Autografts are the orthopedic "gold standard" for repairing bone voids. Autografts are osteoconductive and do not elicit an immune response, but they are in short supply and require a second surgery to harvest the bone graft. Allografts are currently the most common materials used for the repair of segmental defects in hard tissue. Unlike autografts, allografts can cause an undesirable immune response and the possibility of disease transmission is a major concern. As an alternative to the above approaches, recent research efforts have focused on the use of composite materials made from hydroxyapatite (HA) and bioresorbable polymers, such as poly-L-lactide (PLLA). Recent results have shown that the surface hydroxides on HA can initiate the ring opening polymerization (ROP) of L-lactide and other lactones creating a composite with superior interfacial strength. This thesis demonstrates that the surface of porous biologically derived HA substrates, such as coralline HA and trabecular bone, can be used to initiate the ROP of L-lactide and other lactones from the vapor phase. This process increases the strength of the porous scaffold through the deposition of a thin, uniform polymer coating, while maintaining the porous structure. The kinetics of the chemical vapor deposition polymerization (CVDP) are described using a quartz crystal microbalance (QCM). The reaction temperature and monomer vapor pressure are found to affect the rate of the polymerization. Also described in this thesis is the preparation of a porous polymer scaffold that mimics the structure of demineralized bone matrix (DBM). This demineralized bone matrix simulant (DBMS) is created using anorganic bovine bone as a template to initiate the polymerization of various lactones, followed by the removal of the HA scaffold. This material retained its shape and exhibits mechanical properties superior to DBM. Finally it is shown that HA can be used to initiate the ROP of a-caprolactam and the biocompatibility

Preparation and characterization of a novel degradable nano-hydroxyapatite/poly(lactic-co-glycolic) composite reinforced with bamboo fiber

Energy Technology Data Exchange (ETDEWEB)

Jiang, Liuyun, E-mail: jlytxg@163.com [Key Laboratory of Sustainable Resources Processing and Advanced Materials, College of Chemistry and Chemical Engineering, Hunan Normal University, Changsha 410081 (China); Li, Ye; Xiong, Chengdong [Chengdu Institute of Organic Chemistry, Chinese Academy of Sciences, Chengdu 610041 (China); Su, Shengpei [Key Laboratory of Sustainable Resources Processing and Advanced Materials, College of Chemistry and Chemical Engineering, Hunan Normal University, Changsha 410081 (China)

2017-06-01

It is a promising and challenging to achieve an ideal poly (lactic-co-glycolic) (PLGA)-based composite. In this paper, bamboo fiber (BF) was firstly designed to incorporate into nano-hydroxyapatite/PLGA (n-HA/PLGA) composite, and a series of novel biodegradable BF/n-HA/PLGA ternary composites with different BF amounts (0 wt%, 5 wt%, 10 wt% and 20 wt%) were prepared by solution mixing method. The effect of BF content on the crystallization behavior, interface structure and mechanical property of BF/n-HA/PLGA ternary composite was investigated by X-ray diffraction pattern (XRD), differential scanning calorimeter (DSC) and scanning electron microscope (SEM), comparing with pure PLGA and n-HA/PLGA composite. The results showed that BF further promoted the crystallization of PLGA acting as a heterogeneous nucleation agent, and the addition of 10 wt% BF was the best benefit to promote the crystallization. However, the higher addition content of BF caused more agglomeration in n-HA/PLGA matrix, which decreased gradually the mechanical properties of the BF/n-HA/PLGA composite. In conclusion, the addition content of 5 wt% BF to n-HA/PLGA matrix was an appropriate proportion, which can achieved the best mechanical reinforce effectiveness, suggesting that BF/n-HA/PLGA composite had more potential in biomedical application than n-HA/PLGA composite. - Highlights: • Bamboo fiber was firstly design to incorporate into n-HA/PLGA composite. • The effect of bamboo fiber content on the n-HA/PLGA composite was studied in detail. • Isothermal crystallization, microstructure and mechanical property were studied. • The relation between bamboo fiber content and properties of n-HA/PLGA composite was found. • An appropriate proportion of bamboo fiber in n-HA/PLGA composite was obtained.

Preparation and characterization of a novel degradable nano-hydroxyapatite/poly(lactic-co-glycolic) composite reinforced with bamboo fiber

International Nuclear Information System (INIS)

Jiang, Liuyun; Li, Ye; Xiong, Chengdong; Su, Shengpei

2017-01-01

It is a promising and challenging to achieve an ideal poly (lactic-co-glycolic) (PLGA)-based composite. In this paper, bamboo fiber (BF) was firstly designed to incorporate into nano-hydroxyapatite/PLGA (n-HA/PLGA) composite, and a series of novel biodegradable BF/n-HA/PLGA ternary composites with different BF amounts (0 wt%, 5 wt%, 10 wt% and 20 wt%) were prepared by solution mixing method. The effect of BF content on the crystallization behavior, interface structure and mechanical property of BF/n-HA/PLGA ternary composite was investigated by X-ray diffraction pattern (XRD), differential scanning calorimeter (DSC) and scanning electron microscope (SEM), comparing with pure PLGA and n-HA/PLGA composite. The results showed that BF further promoted the crystallization of PLGA acting as a heterogeneous nucleation agent, and the addition of 10 wt% BF was the best benefit to promote the crystallization. However, the higher addition content of BF caused more agglomeration in n-HA/PLGA matrix, which decreased gradually the mechanical properties of the BF/n-HA/PLGA composite. In conclusion, the addition content of 5 wt% BF to n-HA/PLGA matrix was an appropriate proportion, which can achieved the best mechanical reinforce effectiveness, suggesting that BF/n-HA/PLGA composite had more potential in biomedical application than n-HA/PLGA composite. - Highlights: • Bamboo fiber was firstly design to incorporate into n-HA/PLGA composite. • The effect of bamboo fiber content on the n-HA/PLGA composite was studied in detail. • Isothermal crystallization, microstructure and mechanical property were studied. • The relation between bamboo fiber content and properties of n-HA/PLGA composite was found. • An appropriate proportion of bamboo fiber in n-HA/PLGA composite was obtained.

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

Science.gov (United States)

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.

Hydroxyapatite nanocrystals: Simple preparation, characterization and formation mechanism

International Nuclear Information System (INIS)

Mohandes, Fatemeh; Salavati-Niasari, Masoud; Fathi, Mohammadhossein; Fereshteh, Zeinab

2014-01-01

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. - Highlights: • HAP nanobundles and nanoparticles have been prepared by a precipitation method. • Morphologies of HAP nanocrystals were controlled by different coordination ligands. • The formation mechanism of hydroxyapatite nanocrystals was also considered

Hydroxyapatite nanocrystals: Simple preparation, characterization and formation mechanism

Energy Technology Data Exchange (ETDEWEB)

Mohandes, Fatemeh [Department of Inorganic Chemistry, Faculty of Chemistry, University of Kashan, Kashan, P. O. Box. 87317-51167, Islamic Republic of Iran (Iran, Islamic Republic of); Salavati-Niasari, Masoud, E-mail: salavati@kashanu.ac.ir [Department of Inorganic Chemistry, Faculty of Chemistry, University of Kashan, Kashan, P. O. Box. 87317-51167, Islamic Republic of Iran (Iran, Islamic Republic of); Institute of Nano Science and Nano Technology, University of Kashan, Kashan, P. O. Box 87317-51167, Islamic Republic of Iran (Iran, Islamic Republic of); Fathi, Mohammadhossein [Biomaterials Research Group, Department of Materials Engineering, Isfahan University of Technology, Isfahan 8415683111, Islamic Republic of Iran (Iran, Islamic Republic of); Dental Materials Research Center, Isfahan University of Medical Sciences, Isfahan, Islamic Republic of Iran (Iran, Islamic Republic of); Fereshteh, Zeinab [Biomaterials Research Group, Department of Materials Engineering, Isfahan University of Technology, Isfahan 8415683111, Islamic Republic of Iran (Iran, Islamic Republic of)

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 ({sup 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. - Highlights: • HAP nanobundles and nanoparticles have been prepared by a precipitation method. • Morphologies of HAP nanocrystals were controlled by different coordination ligands. • The formation mechanism of hydroxyapatite nanocrystals was also considered.

Mechanically-reinforced electrospun composite silk fibroin nanofibers containing hydroxyapatite nanoparticles

International Nuclear Information System (INIS)

Kim, Hyunryung; Che, Lihua; Ha, Yoon; Ryu, WonHyoung

2014-01-01

Electrospun silk fibroin (SF) scaffolds provide large surface area, high porosity, and interconnection for cell adhesion and proliferation and they may replace collagen for many tissue engineering applications. Despite such advantages, electrospun SF scaffolds are still limited as bone tissue replacement due to their low mechanical strengths. While enhancement of mechanical strengths by incorporating inorganic ceramics into polymers has been demonstrated, electrospinning of a mixture of SF and inorganic ceramics such as hydroxyapatite is challenging and less studied due to the aggregation of ceramic particles within SF. In this study, we aimed to enhance the mechanical properties of electrospun SF scaffolds by uniformly dispersing hydroxyapatite (HAp) nanoparticles within SF nanofibers. HAp nanoaprticles were modified by γ-glycidoxypropyltrimethoxysilane (GPTMS) for uniform dispersion and enhanced interfacial bonding between HAp and SF fibers. Optimal conditions for electrospinning of SF and GPTMS-modified HAp nanoparticles were identified to achieve beadless nanofibers without any aggregation of HAp nanoparticles. The MTT and SEM analysis of the osteoblasts-cultured scaffolds confirmed the biocompatibility of the composite scaffolds. The mechanical properties of the composite scaffolds were analyzed by tensile tests for the scaffolds with varying contents of HAp within SF fibers. The mechanical testing showed the peak strengths at the HAp content of 20 wt.%. The increase of HAp content up to 20 wt.% increased the mechanical properties of the composite scaffolds, while further increase above 20 wt.% disrupted the polymer chain networks within SF nanofibers and weakened the mechanical strengths. - Highlights: • Electrospun composite silk fibroin scaffolds were mechanically-reinforced. • GPTMS enhanced hydroxyapatite distribution in silk fibroin nanofibers. • Mechanical property of composite scaffolds increased up to 20% of hydroxyapatite. • Composite

Preparation and characterization of nano hydroxyapatite/polymeric composites materials. Part I

Energy Technology Data Exchange (ETDEWEB)

Mohamed, Khaled R., E-mail: kh_rezk1966@yahoo.com [Biomaterials Dept., National Research Centre, Dokki, Cairo (Egypt); El-Rashidy, Zenab M. [Biomaterials Dept., National Research Centre, Dokki, Cairo (Egypt); Salama, Aida A. [Biophysics Dept., Faulty of Science, El-Azhar Univ., Cairo (Egypt)

2011-10-17

Highlights: {yields} The formation and coating of CHA increased by increasing polymer content. {yields} The size of the prepared CHA was within nano-range scale. {yields} The composites had homogeneity and CHA formed within the polymeric matrix. - Abstract: The present study is focused on preparation of nano composite materials and the effect of citric acid on their different properties. The formation of nano HA and its interaction with chitosan (C), gelatin (G) polymers and citric acid (CA) materials were studied. The Fourier Transformed Infrared Spectroscopy (FT-IR), X-ray diffraction (XRD), thermo-gravimetric analysis (TGA), transmission electron microscope (TEM), and scanning electron microscope (SEM) were used to characterize these composite materials. The compressive strength (CS) was also measured to know the reinforcement of the prepared composites. The results show that carboxylic and amino groups play crucial role for HA formation on chitosan-gelatin polymeric matrix in the presence of citric acid (CA). The formation of nano HA particles and its average size of crystallite is increased with increase of CG content and decreased with addition of CA. Also, the HA formation and binding strength between its particles are improved into the composites especially with CA. The nano-composites containing the best ratio of nHA (70%) with CA (0.2 M) are promising for medical applications in the future.

Comparison between PCL/hydroxyapatite (HA) and PCL/halloysite nanotube (HNT) composite scaffolds prepared by co-extrusion and gas foaming.

Science.gov (United States)

Jing, Xin; Mi, Hao-Yang; Turng, Lih-Sheng

2017-03-01

In this work, three-dimensional poly(caprolactone) (PCL) tissue engineering scaffolds were prepared by co-extrusion and gas foaming. Biocompatible hydroxyapatite (HA) and halloysite nanotubes (HNT) were added to the polymer matrix to enhance the mechanical properties and bioactivity of the composite scaffolds. The effects of HA and HNT on the rheological behavior, microstructure, and mechanical properties of the composite scaffolds were systematically compared. It was found that the HNT improved viscosity more significantly than HA, and reduced the pore size of scaffolds, while the mechanical performance of PCL/HNT scaffolds was higher than PCL/HA scaffolds with the same filler content. Human mesenchymal stem cells (hMSCs) were used as the cell model to compare the biological properties of two composite scaffolds. The results demonstrated that cells could survive on all scaffolds, and showed a more flourishing living state on the composite scaffolds. The cell differentiation for 5% HA and 1% HNT scaffolds were significantly higher than other scaffolds, while the differentiation of 5% HNT scaffolds was lower than that of 1% HNT scaffolds mainly because of the reduced pore size and pore interconnectivity. Therefore, this study suggested that, with proper filler content and control of microstructure through processing, HNT could be a suitable substitute for HA for bone tissue engineering to reduce the cost and improve mechanical performance. Copyright © 2016. Published by Elsevier B.V.

Development and Characterization of Sr-Containing Glass-Ceramic Composites Based on Biogenic Hydroxyapatite

Science.gov (United States)

Kuda, Oleksii; Pinchuk, Nataliia; Bykov, Oleksandr; Tomila, Tamara; Olifan, Olena; Golovkova, Maryna

2018-05-01

Composite materials based on hydroxyapatite are widely used for bone tissue engineering. There is evidence of a positive effect of the presence of strontium in osteoplastic materials in the case of a Ca/Sr certain ratio. To examine the effect of the addition of Sr2+, a study was made by introducing it into the material composition based on biogenic hydroxyapatite and sodium borosilicate glass (50/50% wt.). The strontium was introduced into the composition in an amount of 1% wt. Composite materials were obtained at final sintering temperatures of 780 °C and a sintering time of 1 h. The effect of additions of glass phase and strontium affect changes in the crystal lattice of biogenic hydroxyapatite was investigated with the help of X-ray phase analysis, IR spectroscopy. Also the behavior of composites in vitro in physiological solution was studied.

Synthesis and characterization of hydroxyapatite-gelatine composite materials for orthopaedic application

International Nuclear Information System (INIS)

Yanovska, A.; Kuznetsov, V.; Stanislavov, A.; Husak, E.; Pogorielov, M.; Starikov, V.; Bolshanina, S.; Danilchenko, S.

2016-01-01

The composite materials based on hydroxyapatite (HA) and gelatine (Gel) with addition of silver and zirconium oxide were obtained. The study investigates a combination of low powered ultrasonic irradiation and low concentration of gelatine in the co-precipitation synthesis. These composites have different weight ratios of organic/inorganic components and may be synthesized in two ways: simple mixing and co-precipitation. Both of which were compared. The estimation of porosity, in vivo testing, surface morphology and phase composition as well as the IR-analysis were provided. Hydroxyapatite was the main crystalline phase in obtained composites. While around powdered HA-Gel composite the connective tissue capsule is formed without bone tissue formation, HA-Gel-Ag porous composite implantation leads to formation of new bone tissue and activation of cell proliferation. Addition of silver ions into composite material allows decreasing inflammation on the first stage of implantation and has positive effect on bone tissue formation. Some of the obtained composite materials containing silver or ZrO_2 are biocompatible. bio-resorbable and osteoconductive with high level of porosity (75–85%). - Highlights: • Hydroxyapatite-gelatine composites with addition of Ag"+ and ZrO_2 were obtained. • Composites were synthesized in two ways: simple mixing and co-precipitation. • Co-precipitation synthesis combined ultrasonic treatment and low concentration of gelatine. • Obtained composites have different weight ratios of organic/inorganic components. • Some composites are osteoconductive and all of them have high level of porosity (75–85%).

Hydroxyapatite coatings on titanium dioxide thin films prepared by pulsed laser deposition method

International Nuclear Information System (INIS)

Suda, Yoshiaki; Kawasaki, Hiroharu; Ohshima, Tamiko; Nakashima, Shouta; Kawazoe, Syuichi; Toma, Tetsuya

2006-01-01

Hydroxyapatite (HAp) coated on titanium dioxide (TiO 2 ) thin films has been developed to supplement the defects of both TiO 2 and HAp. Thin films have been prepared by pulsed laser deposition (PLD) method using HAp and HAp(10%) + TiO 2 targets. X-ray diffraction (XRD) shows that there are many small peaks of Ca 1 0(PO 4 ) 6 (OH) 2 crystal, and no impurity other than HAp is detected in HAp films prepared using pure HAp target. The composition ratio of the film was analyzed by X-ray photoelectron spectroscopy (XPS). HAp coatings on TiO 2 thin films have been prepared using HAp(10%) + TiO 2 targets. XRD and XPS measurements suggest that crystalline HAp + TiO 2 thin films are obtained by the PLD method using HAp(10%) + TiO 2 target

Hydroxyapatite-phosphonoformic acid hybrid compounds prepared by hydrothermal method

Science.gov (United States)

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.

Preparation and biological behaviour of samarium-153-hydroxyapatite particles for radiation synovectomy

International Nuclear Information System (INIS)

Agrueelles, M.G.; Luppi Berlanga, I.S.; Torres, E.A.; Rutty Sola, G.A.; Rimoldi, G.

1998-01-01

The preparation and labelling procedures of 153 Sm-hydroxyapatite ( 153 Sm-HA) are described in this paper. Hydroxyapatite (HA) was prepared and studied as a radiosynovectomy agent. HA particles were prepared from the reaction of calcium nitrate and ammonia phosphate at high pH Samarium-153 labelling was done in two steps with citric acid. A serie of experimental conditions, such as specific activity, citric acid mass, radioactive solution volume, in-vitro stability, have been carried out. Radiolabelling efficiency was greater than 95%. In vitro studies showed high stability (≥99%). Animal studies showed a good retention in the synovium, with a very low extra-articular leakage over 6 days after administration. (author)

Hydroxyapatite and zirconia composites: Effect of MgO and MgF2 on the stability of phases and sinterability

International Nuclear Information System (INIS)

Evis, Zafer; Usta, Metin; Kutbay, Isil

2008-01-01

Composites of hydroxyapatite with cubic zirconia with MgO or MgF 2 were pressureless sintered at temperatures from 1000 to 1300 deg. C. The reactions and transformations of phases were monitored with X-ray diffraction. For the hydroxyapatite and zirconia composites with MgO, calcium diffused from hydroxyapatite into the zirconia, and hydroxyapatite decomposed to tri-calcium phosphate at sintering temperatures higher than 1000 deg. C. Above about 1200 deg. C, CaZrO 3 was formed. Composites containing the MgF 2 decomposed slower than the composites with MgO which was verified by the changes in the lattice volume of the hydroxyapatite left in the composites. Fluorine ions in MgF 2 diffused into hydroxyapatite which resulted in thermal stability at high sintering temperatures. Composites with MgF 2 had higher hardness than those with MgO. The lowest porosity was found in a composite initially containing 10 wt% cubic zirconia and 5 wt% MgF 2

Synthesis and characterization of hydroxyapatite-gelatine composite materials for orthopaedic application

Energy Technology Data Exchange (ETDEWEB)

Yanovska, A., E-mail: biophy@yandex.ru [Institute of Applied Physics, National Academy of Sciences of Ukraine, 58 Petropavlovskaya Str., 40000, Sumy (Ukraine); Sumy State University, Ministry of Education and Science of Ukraine, 2 R. Korsakova Str., 40007, Sumy (Ukraine); Kuznetsov, V. [Institute of Applied Physics, National Academy of Sciences of Ukraine, 58 Petropavlovskaya Str., 40000, Sumy (Ukraine); Sumy State University, Ministry of Education and Science of Ukraine, 2 R. Korsakova Str., 40007, Sumy (Ukraine); Stanislavov, A. [Institute of Applied Physics, National Academy of Sciences of Ukraine, 58 Petropavlovskaya Str., 40000, Sumy (Ukraine); Husak, E. [Institute of Applied Physics, National Academy of Sciences of Ukraine, 58 Petropavlovskaya Str., 40000, Sumy (Ukraine); Sumy State University, Ministry of Education and Science of Ukraine, 2 R. Korsakova Str., 40007, Sumy (Ukraine); Pogorielov, M. [Sumy State University, Ministry of Education and Science of Ukraine, 2 R. Korsakova Str., 40007, Sumy (Ukraine); Starikov, V. [National Technical University ”Kharkov Polytechnic Institute”, 21 Frunze Str., 61002, Kharkov (Ukraine); Bolshanina, S. [Sumy State University, Ministry of Education and Science of Ukraine, 2 R. Korsakova Str., 40007, Sumy (Ukraine); Danilchenko, S. [Institute of Applied Physics, National Academy of Sciences of Ukraine, 58 Petropavlovskaya Str., 40000, Sumy (Ukraine)

2016-11-01

The composite materials based on hydroxyapatite (HA) and gelatine (Gel) with addition of silver and zirconium oxide were obtained. The study investigates a combination of low powered ultrasonic irradiation and low concentration of gelatine in the co-precipitation synthesis. These composites have different weight ratios of organic/inorganic components and may be synthesized in two ways: simple mixing and co-precipitation. Both of which were compared. The estimation of porosity, in vivo testing, surface morphology and phase composition as well as the IR-analysis were provided. Hydroxyapatite was the main crystalline phase in obtained composites. While around powdered HA-Gel composite the connective tissue capsule is formed without bone tissue formation, HA-Gel-Ag porous composite implantation leads to formation of new bone tissue and activation of cell proliferation. Addition of silver ions into composite material allows decreasing inflammation on the first stage of implantation and has positive effect on bone tissue formation. Some of the obtained composite materials containing silver or ZrO{sub 2} are biocompatible. bio-resorbable and osteoconductive with high level of porosity (75–85%). - Highlights: • Hydroxyapatite-gelatine composites with addition of Ag{sup +} and ZrO{sub 2} were obtained. • Composites were synthesized in two ways: simple mixing and co-precipitation. • Co-precipitation synthesis combined ultrasonic treatment and low concentration of gelatine. • Obtained composites have different weight ratios of organic/inorganic components. • Some composites are osteoconductive and all of them have high level of porosity (75–85%).

Investigation on Mechanical Properties and Microstructure of Hydroxyapatite-SiCw Composite Bioceramics

Institute of Scientific and Technical Information of China (English)

无

2005-01-01

Hydroxyapatite-SiCw composite micropowder was synthesized using in-situ composite method,and hydroxyapatite-SiCw composite bioceramics with different content of SiCw were produced by hot pressing sintering method. The microstructures of the materials were analyzed by SEM, and the relative density, bending strength and fracture toughness of the materials were tested. The results show that the mechanical properties of composite material are best when the whisker content is 20-23.7% . The mechanical properties of the material are the best when the tensile stress acted on the composite material is parallel with the hot pressing plane, and they are the worst when the tensile stress acted on the composite material is normal to the hot pressing plane.

The fabrication of well-interconnected polycaprolactone/hydroxyapatite composite scaffolds, enhancing the exposure of hydroxyapatite using the wire-network molding technique.

Science.gov (United States)

Cho, Yong Sang; Hong, Myoung Wha; Jeong, Hoon-Jin; Lee, Seung-Jae; Kim, Young Yul; Cho, Young-Sam

2017-11-01

In this study, the fabrication method was proposed for the well-interconnected polycaprolactone/hydroxyapatite composite scaffold with exposed hydroxyapatite using modified WNM technique. To characterize well-interconnected scaffolds in terms of hydroxyapatite exposure, several assessments were performed as follows: morphology, mechanical property, wettability, calcium ion release, and cell response assessments. The results of these assessments were compared with those of control scaffolds which were fabricated by precision extruding deposition (PED) apparatus. The control PED scaffolds have interconnected pores with nonexposed hydroxyapatite. Consequently, cell attachment of proposed WNM scaffold was improved by increased hydrophilicity and surface roughness of scaffold surface resulting from the exposure of hydroxyapatite particles and fabrication process using powders. Moreover, cell proliferation and differentiation of WNM scaffold were increased, because the exposure of hydroxyapatite particles may enhance cell adhesion and calcium ion release. © 2016 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 105B: 2315-2325, 2017. © 2016 Wiley Periodicals, Inc.

Near net-shape fabrication of hydroxyapatite glass composites

NARCIS (Netherlands)

Zhu, Q.; With, de G.; Dortmans, L.; Feenstra, F.

2004-01-01

Near net-shape fabrication of hydroxyapatite (HA) glass composites has been attempted by infiltrating a glass into porous HA performs. Main efforts were put to develop glasses that are chemically compatible with HA at elevated temperatures. After extensive investigations in the phosphate and

Preparation of uniform porous hydroxyapatite biomaterials by a new method

International Nuclear Information System (INIS)

Tang Yuejun; Tang Yuefeng; Lv Chuntang; Zhou Zhonghua

2008-01-01

In this paper, a new method of preparation of uniform porous hydroxyapatite biomaterials was reported. In order to obtain uniform porous biomaterials, disk samples were formed by the mixture of hydroxyapatite (HAP) powders and monodispersed polystyrene microspheres, and then HAP uniform porous materials with different diameter and different porosity (diameter: 436 ± 25 nm, 892 ± 20 nm and 1890 ± 20 nm, porosity: 46.5%, 41.3% and 34.7%, respectively) were prepared by sintering these disk samples at 1250 deg. C for 5 h. The pure phase of HAP powders fabricated by the hydrothermal technology was confirmed by X-ray diffraction (XRD). The surface and size distribution of pores in HAP biomaterials were observed by scanning electron microscopy (SEM), and the pore size distribution in porous HAP biomaterials was tested by mercury intrusion method

Preparation of hydroxyapatite nanoparticles facilitated by the presence of {beta}-cyclodextrin

Energy Technology Data Exchange (ETDEWEB)

Martinez-Perez, Carlos A., E-mail: camartin@uacj.mx [Institute of Engineering and Technology, Autonomous University of Juarez, UACJ, Ave. del Charro 610 norte, C.P. 32320, Cd. Juarez, Chihuahua (Mexico); Garcia-Montelongo, Jorge; Garcia Casillas, Perla E.; Farias-Mancilla, Jose R. [Institute of Engineering and Technology, Autonomous University of Juarez, UACJ, Ave. del Charro 610 norte, C.P. 32320, Cd. Juarez, Chihuahua (Mexico); Monreal Romero, Humberto [School of Odontology, Autonomous University of Chihuahua, UACH, Ave. Universidad s/n Campus Universitario I, C.P. 31170, Chihuahua (Mexico)

2012-09-25

Highlights: Black-Right-Pointing-Pointer It was found that {beta}-cyclodextrin can control the particle size in the production of nanohydroxyapatite. Black-Right-Pointing-Pointer Particle size in the range of 30-50 nm was obtained. Black-Right-Pointing-Pointer A new simple methodology for the preparation of hydroxyapatite nanoparticles with a well controlled size and narrow particles size distribution was developed. - Abstract: Hydroxyapatite nanoparticles with uniform morphology have been successfully synthesized by a chemical coprecipitation method and facilitated by the presence of the {beta}-cyclodextrin. X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM); and Fourier Transformed Infrared Spectroscopy (FT-IR) were used in order to characterize the hydroxyapatite samples. The experimental results indicate that the obtained HA is in the range of 20-50 nm. Also it was found that the content of {beta}-CD has an impact on the purity of the HA as well in the particle size of the hydroxyapatite nanoparticles.

Preparation of hydroxyapatite nanoparticles facilitated by the presence of β-cyclodextrin

International Nuclear Information System (INIS)

Martínez-Pérez, Carlos A.; García-Montelongo, Jorge; Garcia Casillas, Perla E.; Farias-Mancilla, José R.; Monreal Romero, Humberto

2012-01-01

Highlights: ► It was found that β-cyclodextrin can control the particle size in the production of nanohydroxyapatite. ► Particle size in the range of 30–50 nm was obtained. ► A new simple methodology for the preparation of hydroxyapatite nanoparticles with a well controlled size and narrow particles size distribution was developed. - Abstract: Hydroxyapatite nanoparticles with uniform morphology have been successfully synthesized by a chemical coprecipitation method and facilitated by the presence of the β-cyclodextrin. X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM); and Fourier Transformed Infrared Spectroscopy (FT-IR) were used in order to characterize the hydroxyapatite samples. The experimental results indicate that the obtained HA is in the range of 20–50 nm. Also it was found that the content of β-CD has an impact on the purity of the HA as well in the particle size of the hydroxyapatite nanoparticles.

Synthesis of hydroxyapatite coatings on metal substrates using a spincasting technique

International Nuclear Information System (INIS)

Yuan Qiuhua; Sahu, Laxmi Kumari; D'Souza, Nandika A.; Golden, Teresa Diane

2009-01-01

Hydroxyapatite coatings on stainless steel substrates were prepared by a simple spincasting technique. Nanosized hydroxyapatite powders were prepared by precipitating in an electrolytic suspension, and then added to a polylactic acid solution for spincasting. The polylactic acid gave enhanced protection from corrosion and inhibited decomposition of the hydroxyapatite coating during the sintering process in air, a significant advantage over other solution processing techniques. Characterization of the phase composition and morphology of the fabricated films on stainless steel was accomplished by X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectroscopy, and Fourier transform infrared spectroscopy.

Mechanical properties of titanium-hydroxyapatite (Ti-HA) composite coating on stainless steel prepared by thermal spraying

Science.gov (United States)

Rosmamuhamadani, R.; Azhar, N. H.; Talari, M. K.; Yahaya, Sabrina M.; Sulaiman, S.; Ismail, M. I. S.

2017-09-01

Addition of hydroxyapatite (HA) can enhance the bioactivity of the common metallic implant due to its similarity with natural bones and teeth. In this investigation, high velocity oxy-fuel (HVOFT) technique was used to deposit titanium-hydroxyapatite (Ti-HA) composite on stainless steel substrate plate with different percentage of HA for biomedical applications. The aim of this research is to investigate the mechanical properties of Ti-HA coating such as hardness, adhesion strength and wear behaviour. The hardness and strength was determined by using SHIMADZU-microhardness Vickers tester and PosiTest AT portable adhesion tester respectively. The wear test was performed by using pin-on-disk equipment and field emission scanning electron microscope (FESEM) used to determine the extent of surface damage. From the results obtained, mechanical properties such as hardness and adhesion strength of titanium (Ti) coating decreased with the increased of HA contents. Meanwhile, the coefficient of friction of Ti-10% HA coating shows the highest value compare to others as three-body abrasion had occurred during the test.

In vitro biomechanical and biocompatible evaluation of natural hydroxyapatite/chitosan composite for bone repair.

Science.gov (United States)

Lü, Xiaoying; Zheng, Buzhong; Tang, Xiaojun; Zhao, Lifeng; Lu, Jieyan; Zhang, Zhiwei; Zhang, Jizhong; Cui, Wei

2011-01-01

To evaluate the biomechanical properties and biocompatibility of natural hydroxyapatite/chitosan (HA/CS) composites. The natural HA/CS composites with a different proportion of HA and CS were prepared by the cross-linking method, and then the compressive strength, microstructure and pH values of extracts from these composites were measured by SEM and pH meter, respectively. Subsequently, the biocompatibility of the composites was evaluated by means of a series of biological tests, including MTT, acute systemic toxicity, heat source, and hemolysis tests in vitro. The chitosan content in the composites had significantly influenced the mechanical properties and microstructure of the composites. The pH value of the composite extract was approximately 7.0, which was very close to that of human plasma. Furthermore, the natural HA/CS composites showed no cytotoxicity, irritation, teratogenicity, carcinogenicity and special pyrogen. These results indicated that the natural HA/CS composite may be a potential bone repair material.

The comparison study of bioactivity between composites containing synthetic non-substituted and carbonate-substituted hydroxyapatite.

Science.gov (United States)

Borkowski, Leszek; Sroka-Bartnicka, Anna; Drączkowski, Piotr; Ptak, Agnieszka; Zięba, Emil; Ślósarczyk, Anna; Ginalska, Grażyna

2016-05-01

Apatite forming ability of hydroxyapatite (HAP) and carbonate hydroxyapatite (CHAP) containing composites was compared. Two composite materials, intended for filling bone defects, were made of polysaccharide polymer and one of two types of hydroxyapatite. The bioactivity of the composites was evaluated in vitro by soaking in a simulated body fluid (SBF), and the formation of the apatite layer was determined by scanning electron microscopy with energy-dispersive spectrometer and Raman spectroscopy. The results showed that both the composites induced the formation of apatite layer on their surface after soaking in SBF. In addition, the sample weight changes and the ion concentration of the SBF were scrutinized. The results showed the weight increase for both materials after SBF treatment, higher weight gain and higher uptake of calcium ions by HAP containing scaffolds. SBF solution analysis indicated loss of calcium and phosphorus ions during experiment. All these results indicate apatite forming ability of both biomaterials and suggest comparable bioactive properties of composite containing pure hydroxyapatite and carbonate-substituted one. Copyright © 2016 Elsevier B.V. All rights reserved.

FIBROUS SILICA-HYDROXYAPATITE COMPOSITE BY ELECTROSPINNING

OpenAIRE

Jesús Alberto Garibay-Alvarado; León Francisco Espinosa-Cristóbal; Simón Yobanny Reyes-López

2017-01-01

New nanocomposite membrane was fabricated by electrospinning. The nanocomposite combines a glass and hydroxyapatite (HA). This research proposed the incorporation of glass to counteract the brittleness of HA in a composite formed by coaxial fibers which will be used for bone replacement. Calcium phosphate ceramics are used widely for dental and orthopedic reasons, because they can join tightly through chemical bonds and promote bone regeneration. Precursors HA and SiO2 were synthetized throug...

Graphene oxide/oxidized carbon nanofiber/mineralized hydroxyapatite based hybrid composite for biomedical applications

Science.gov (United States)

Murugan, N.; Sundaramurthy, Anandhakumar; Chen, Shen-Ming; Sundramoorthy, Ashok K.

2017-12-01

Hydroxyapatite (Ca10(PO4)6(OH)2, HAP), a multi-mineral substituted calcium phosphate is the main mineral component of tooth enamel and bone, has become an important biomaterial for biomedical applications. However, as-synthesized HAP has poor mechanical properties and inferior wear resistance, so it is not suitable to use in bone tissue engineering applications. We report the successful incorporation of oxidized carbon nanofibers (O-CNF) and graphene oxide (GO) into the mineralized hydroxyapatite (M-HAP) which showed excellent mechanical and biological properties. GO improved the high mechanical strength and corrosion protection of the substrate in simulated body fluid (SBF) solution and promoted the viability of osteoblasts MG63 cells. As-prepared M-HAP/O-CNF/GO composite showed materials characteristics that similar to natural bone (M-HAP) with high mechanical strength. The resultant M-HAP/O-CNF/GO composite was characterized out by x-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), and Fourier-transform infrared spectroscopy (FT-IR), respectively. The mechanical strength of the material was determined by Vicker’s micro-hardness method and it was found that M-HAP/O-CNF/GO (468  ±  4 Hv) composite has superior mechanical properties than M-HAP (330  ±  3 Hv) and M-HAP/GO (425  ±  5 Hv) samples. In addition, antibacterial activity of the composite was studied against Staphylococcus aureus and Escherichia coli. Furthermore, the cell viability of the composite was observed in vitro against osteoblast cells. All these studies confirmed that the M-HAP/O-CNF/GO composite can be considered as potential candidate for dental and orthopedic applications.

Effect of Gamma Irradiation on Structural and Biological Properties of a PLGA-PEG-Hydroxyapatite Composite

Science.gov (United States)

Shahabi, Sima; Najafi, Farhood; Majdabadi, Abbas; Hooshmand, Tabassom; Haghbin Nazarpak, Masoumeh; Karimi, Batool

2014-01-01

Gamma irradiation is able to affect various structural and biological properties of biomaterials In this study, a composite of Hap/PLGA-PEG and their ingredients were submitted to gamma irradiation doses of 25 and 50 KGy. Various properties such as molecular weight (GPC), thermal behavior (DSC), wettability (contact angle), cell viability (MTT assay), and alkaline phosphatase activity were studied for the composites and each of their ingredients. The results showed a decrease in molecular weight of copolymer with no change in the glass transition and melting temperatures after gamma irradiation. In general gamma irradiation can increase the activation energy ΔH of the composites and their ingredients. While gamma irradiation had no effect on the wettability of copolymer samples, there was a significant decrease in contact angle of hydroxyapatite and composites with increase in gamma irradiation dose. This study showed an increase in biocompatibility of hydroxyapatite with gamma irradiation with no significant effect on cell viability in copolymer and composite samples. In spite of the fact that no change occurred in alkaline phosphatase activity of composite samples, results indicated a decrease in alkaline phosphatase activity in irradiated hydroxyapatites. These effects on the properties of PLGA-PEG-hydroxyapatite can enhance the composite application as a biomaterial. PMID:25574485

Effect of Gamma Irradiation on Structural and Biological Properties of a PLGA-PEG-Hydroxyapatite Composite

Directory of Open Access Journals (Sweden)

Sima Shahabi

2014-01-01

Full Text Available Gamma irradiation is able to affect various structural and biological properties of biomaterials In this study, a composite of Hap/PLGA-PEG and their ingredients were submitted to gamma irradiation doses of 25 and 50 KGy. Various properties such as molecular weight (GPC, thermal behavior (DSC, wettability (contact angle, cell viability (MTT assay, and alkaline phosphatase activity were studied for the composites and each of their ingredients. The results showed a decrease in molecular weight of copolymer with no change in the glass transition and melting temperatures after gamma irradiation. In general gamma irradiation can increase the activation energy ΔH of the composites and their ingredients. While gamma irradiation had no effect on the wettability of copolymer samples, there was a significant decrease in contact angle of hydroxyapatite and composites with increase in gamma irradiation dose. This study showed an increase in biocompatibility of hydroxyapatite with gamma irradiation with no significant effect on cell viability in copolymer and composite samples. In spite of the fact that no change occurred in alkaline phosphatase activity of composite samples, results indicated a decrease in alkaline phosphatase activity in irradiated hydroxyapatites. These effects on the properties of PLGA-PEG-hydroxyapatite can enhance the composite application as a biomaterial.

Support for the initial attachment, growth and differentiation of MG-63 cells: a comparison between nano-size hydroxyapatite and micro-size hydroxyapatite in composites

Directory of Open Access Journals (Sweden)

Filová E

2014-08-01

Full Text Available Elena Filová,1 Tomáš Suchý,2,3 Zbynek Sucharda,2 Monika Šupová,2 Margit Žaloudková,2 Karel Balík,2 Vera Lisá,1 Miroslav Šlouf,4 Lucie Bacáková11Department of Biomaterials and Tissue Engineering, Institute of Physiology, 2Department of Composite and Carbon Materials, Institute of Rock Structure and Mechanics, Academy of Sciences of the Czech Republic, 3Laboratory of Biomechanics, Department of Mechanics, Biomechanics and Mechatronics, Faculty of Mechanical Engineering, CTU in Prague, 4Department of Morphology and Rheology of Polymer Materials, Institute of Macromolecular Chemistry, Academy of Sciences of the Czech Republic, Prague, Czech RepublicAbstract: Hydroxyapatite (HA is considered to be a bioactive material that favorably influences the adhesion, growth, and osteogenic differentiation of osteoblasts. To optimize the cell response on the hydroxyapatite composite, it is desirable to assess the optimum concentration and also the optimum particle size. The aim of our study was to prepare composite materials made of polydimethylsiloxane, polyamide, and nano-sized (N or micro-sized (M HA, with an HA content of 0%, 2%, 5%, 10%, 15%, 20%, 25% (v/v (referred to as N0–N25 or M0–M25, and to evaluate them in vitro in cultures with human osteoblast-like MG-63 cells. For clinical applications, fast osseointegration of the implant into the bone is essential. We observed the greatest initial cell adhesion on composites M10 and N5. Nano-sized HA supported cell growth, especially during the first 3 days of culture. On composites with micro-size HA (2%–15%, MG-63 cells reached the highest densities on day 7. Samples M20 and M25, however, were toxic for MG-63 cells, although these composites supported the production of osteocalcin in these cells. On N2, a higher concentration of osteopontin was found in MG-63 cells. For biomedical applications, the concentration range of 5%–15% (v/v nano-size or micro-size HA seems to be optimum

Antimicrobial activity of thin solid films of silver doped hydroxyapatite prepared by sol-gel method.

Science.gov (United States)

Iconaru, Simona Liliana; Chapon, Patrick; Le Coustumer, Philippe; Predoi, Daniela

2014-01-01

In this work, the preparation and characterization of silver doped hydroxyapatite thin films were reported and their antimicrobial activity was characterized. Silver doped hydroxyapatite (Ag:HAp) thin films coatings substrate was prepared on commercially pure Si disks by sol-gel method. The silver doped hydroxyapatite thin films were characterized by various techniques such as Scanning electron microscopy (SEM) with energy Dispersive X-ray attachment (X-EDS), Fourier transform infrared spectroscopy (FT-IR), and glow discharge optical emission spectroscopy (GDOES). These techniques have permitted the structural and chemical characterisation of the silver doped hydroxyapatite thin films. The antimicrobial effect of the Ag:HAp thin films on Escherichia coli and Staphylococcus aureus bacteria was then investigated. This is the first study on the antimicrobial effect of Ag:HAp thin films obtained by sol-gel method. The results of this study have shown that the Ag:HAp thin films with x(Ag) = 0.5 are effective against E. coli and S. aureus after 24 h.

Antimicrobial Activity of Thin Solid Films of Silver Doped Hydroxyapatite Prepared by Sol-Gel Method

Directory of Open Access Journals (Sweden)

Simona Liliana Iconaru

2014-01-01

Full Text Available In this work, the preparation and characterization of silver doped hydroxyapatite thin films were reported and their antimicrobial activity was characterized. Silver doped hydroxyapatite (Ag:HAp thin films coatings substrate was prepared on commercially pure Si disks by sol-gel method. The silver doped hydroxyapatite thin films were characterized by various techniques such as Scanning electron microscopy (SEM with energy Dispersive X-ray attachment (X-EDS, Fourier transform infrared spectroscopy (FT-IR, and glow discharge optical emission spectroscopy (GDOES. These techniques have permitted the structural and chemical characterisation of the silver doped hydroxyapatite thin films. The antimicrobial effect of the Ag:HAp thin films on Escherichia coli and Staphylococcus aureus bacteria was then investigated. This is the first study on the antimicrobial effect of Ag:HAp thin films obtained by sol-gel method. The results of this study have shown that the Ag:HAp thin films with xAg=0.5 are effective against E. coli and S. aureus after 24 h.

Antimicrobial Activity of Thin Solid Films of Silver Doped Hydroxyapatite Prepared by Sol-Gel Method

Science.gov (United States)

Iconaru, Simona Liliana; Chapon, Patrick; Le Coustumer, Philippe; Predoi, Daniela

2014-01-01

In this work, the preparation and characterization of silver doped hydroxyapatite thin films were reported and their antimicrobial activity was characterized. Silver doped hydroxyapatite (Ag:HAp) thin films coatings substrate was prepared on commercially pure Si disks by sol-gel method. The silver doped hydroxyapatite thin films were characterized by various techniques such as Scanning electron microscopy (SEM) with energy Dispersive X-ray attachment (X-EDS), Fourier transform infrared spectroscopy (FT-IR), and glow discharge optical emission spectroscopy (GDOES). These techniques have permitted the structural and chemical characterisation of the silver doped hydroxyapatite thin films. The antimicrobial effect of the Ag:HAp thin films on Escherichia coli and Staphylococcus aureus bacteria was then investigated. This is the first study on the antimicrobial effect of Ag:HAp thin films obtained by sol-gel method. The results of this study have shown that the Ag:HAp thin films with x Ag = 0.5 are effective against E. coli and S. aureus after 24 h. PMID:24523630

The comparison study of bioactivity between composites containing synthetic non-substituted and carbonate-substituted hydroxyapatite

International Nuclear Information System (INIS)

Borkowski, Leszek; Sroka-Bartnicka, Anna; Drączkowski, Piotr; Ptak, Agnieszka; Zięba, Emil; Ślósarczyk, Anna; Ginalska, Grażyna

2016-01-01

Apatite forming ability of hydroxyapatite (HAP) and carbonate hydroxyapatite (CHAP) containing composites was compared. Two composite materials, intended for filling bone defects, were made of polysaccharide polymer and one of two types of hydroxyapatite. The bioactivity of the composites was evaluated in vitro by soaking in a simulated body fluid (SBF), and the formation of the apatite layer was determined by scanning electron microscopy with energy-dispersive spectrometer and Raman spectroscopy. The results showed that both the composites induced the formation of apatite layer on their surface after soaking in SBF. In addition, the sample weight changes and the ion concentration of the SBF were scrutinized. The results showed the weight increase for both materials after SBF treatment, higher weight gain and higher uptake of calcium ions by HAP containing scaffolds. SBF solution analysis indicated loss of calcium and phosphorus ions during experiment. All these results indicate apatite forming ability of both biomaterials and suggest comparable bioactive properties of composite containing pure hydroxyapatite and carbonate-substituted one. - Highlights: • Bioactivity of two calcium phosphates (HAP and CHAP) was compared. • Two novel ceramic-polymer composite materials were developed. • We examined apatite forming ability of scaffolds in SBF solution. • We report comparable bioactive properties between both materials.

The comparison study of bioactivity between composites containing synthetic non-substituted and carbonate-substituted hydroxyapatite

Energy Technology Data Exchange (ETDEWEB)

Borkowski, Leszek, E-mail: leszek.borkowski@umlub.pl [Chair and Department of Biochemistry and Biotechnology, Medical University of Lublin, Chodźki 1, 20-093 Lublin (Poland); Sroka-Bartnicka, Anna [Department of Biopharmacy, Medical University of Lublin, Chodźki 4a, 20-093 Lublin (Poland); Drączkowski, Piotr [Department of Synthesis and Chemical Technology of Pharmaceutical Substances, Medical University of Lublin, Chodźki 4a, 20-093 Lublin (Poland); Ptak, Agnieszka [Chair and Department of Biochemistry and Biotechnology, Medical University of Lublin, Chodźki 1, 20-093 Lublin (Poland); Zięba, Emil [SEM Laboratory, Department of Zoology and Ecology, John Paul II Catholic University of Lublin, Al. Kraśnicka 102, 20-718 Lublin (Poland); Ślósarczyk, Anna [Faculty of Materials Science and Ceramics, AGH-University of Science and Technology, Mickiewicza 30, 30-059 Krakow (Poland); Ginalska, Grażyna [Chair and Department of Biochemistry and Biotechnology, Medical University of Lublin, Chodźki 1, 20-093 Lublin (Poland)

2016-05-01

Apatite forming ability of hydroxyapatite (HAP) and carbonate hydroxyapatite (CHAP) containing composites was compared. Two composite materials, intended for filling bone defects, were made of polysaccharide polymer and one of two types of hydroxyapatite. The bioactivity of the composites was evaluated in vitro by soaking in a simulated body fluid (SBF), and the formation of the apatite layer was determined by scanning electron microscopy with energy-dispersive spectrometer and Raman spectroscopy. The results showed that both the composites induced the formation of apatite layer on their surface after soaking in SBF. In addition, the sample weight changes and the ion concentration of the SBF were scrutinized. The results showed the weight increase for both materials after SBF treatment, higher weight gain and higher uptake of calcium ions by HAP containing scaffolds. SBF solution analysis indicated loss of calcium and phosphorus ions during experiment. All these results indicate apatite forming ability of both biomaterials and suggest comparable bioactive properties of composite containing pure hydroxyapatite and carbonate-substituted one. - Highlights: • Bioactivity of two calcium phosphates (HAP and CHAP) was compared. • Two novel ceramic-polymer composite materials were developed. • We examined apatite forming ability of scaffolds in SBF solution. • We report comparable bioactive properties between both materials.

Bioactive glass/hydroxyapatite composites: mechanical properties and biological evaluation.

Science.gov (United States)

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. Copyright © 2015 Elsevier B.V. All rights reserved.

Preparation and biological properties of a novel composite scaffold of nano-hydroxyapatite/chitosan/carboxymethyl cellulose for bone tissue engineering

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Chengdong Xiong

2009-07-01

Full Text Available Abstract In this study, we report the physico-chemical and biological properties of a novel biodegradable composite scaffold made of nano-hydroxyapatite and natural derived polymers of chitosan and carboxymethyl cellulose, namely, n-HA/CS/CMC, which was prepared by freeze-drying method. The physico-chemical properties of n-HA/CS/CMC scaffold were tested by infrared absorption spectra (IR, transmission electron microscope(TEM, scanning electron microscope(SEM, universal material testing machine and phosphate buffer solution (PBS soaking experiment. Besides, the biological properties were evaluated by MG63 cells and Mesenchymal stem cells (MSCs culture experiment in vitro and a short period implantation study in vivo. The results show that the composite scaffold is mainly formed through the ionic crossing-linking of the two polyions between CS and CMC, and n-HA is incorporated into the polyelectrolyte matrix of CS-CMC without agglomeration, which endows the scaffold with good physico-chemical properties such as highly interconnected porous structure, high compressive strength and good structural stability and degradation. More important, the results of cells attached, proliferated on the scaffold indicate that the scaffold is non-toxic and has good cell biocompatibility, and the results of implantation experiment in vivo further confirm that the scaffold has good tissue biocompatibility. All the above results suggest that the novel degradable n-HA/CS/CMC composite scaffold has a great potential to be used as bone tissue engineering material.

Preparation and biological properties of a novel composite scaffold of nano-hydroxyapatite/chitosan/carboxymethyl cellulose for bone tissue engineering

Science.gov (United States)

Liuyun, Jiang; Yubao, Li; Chengdong, Xiong

2009-01-01

In this study, we report the physico-chemical and biological properties of a novel biodegradable composite scaffold made of nano-hydroxyapatite and natural derived polymers of chitosan and carboxymethyl cellulose, namely, n-HA/CS/CMC, which was prepared by freeze-drying method. The physico-chemical properties of n-HA/CS/CMC scaffold were tested by infrared absorption spectra (IR), transmission electron microscope(TEM), scanning electron microscope(SEM), universal material testing machine and phosphate buffer solution (PBS) soaking experiment. Besides, the biological properties were evaluated by MG63 cells and Mesenchymal stem cells (MSCs) culture experiment in vitro and a short period implantation study in vivo. The results show that the composite scaffold is mainly formed through the ionic crossing-linking of the two polyions between CS and CMC, and n-HA is incorporated into the polyelectrolyte matrix of CS-CMC without agglomeration, which endows the scaffold with good physico-chemical properties such as highly interconnected porous structure, high compressive strength and good structural stability and degradation. More important, the results of cells attached, proliferated on the scaffold indicate that the scaffold is non-toxic and has good cell biocompatibility, and the results of implantation experiment in vivo further confirm that the scaffold has good tissue biocompatibility. All the above results suggest that the novel degradable n-HA/CS/CMC composite scaffold has a great potential to be used as bone tissue engineering material. PMID:19594953

Preparation and cellular response of porous A-type carbonated hydroxyapatite nanoceramics

International Nuclear Information System (INIS)

Li Bo; Liao Xiaoling; Zheng Li; He Huawei; Wang Hong; Fan Hongsong; Zhang Xingdong

2012-01-01

Microwave sintering using the activated carbon as embedding material was applied in preparation of porous A-type carbonated hydroxyapatite ceramics with nano(nCHA) and submicron (mCHA) structure. By examining the linear shrinkages and the compressive strengths of samples at different temperatures, a suitable microwave sintering temperature was achieved. The microwave sintering method was successfully used to prepare A-type CHA with nano or submicron structure, and the mechanism of the formation of A-type carbonate groups was discussed also. Compared with the samples prepared by the conventional sintering method (mHA), the nCHA bioceramics synthesized by the microwave sintering approach had smaller grain size and more uniform microstructure, and showed a compressive strength similar to the conventional samples. In vitro dissolution test proved that nCHA exhibits better degradation property in comparison to pure HA. Rat osteoblasts were cultured with nCHA, mCHA and mHA to evaluate their biocompatibility, and nCHA showed significant enhancement of cells in attachment, proliferation and differentiation. In conclusion, carbonate groups can be easily introduced to HA crystal structure using the activated carbon as embedding material, and microwave sintering is an effective and simple method in preparing A-type CHA with a nanostructure. Results from this in vitro biological study suggest that porous A-type carbonated hydroxyapatite nanoceramics may be a much better candidate for clinical use in terms of bioactivity. - Highlights: ► We prepared porous A-type carbonated hydroxyapatite nanoceramics with microwave sintering. ► We examined physico-chemical characterization and osteoblast response. ► The nanoceramics have a comparable compressive strength to samples with conventional sintering method. ► The nanoceramics enhance degradation property, osteoblast proliferation and differentiation. ► The activated carbon is favorable for preheating samples and providing

Simple and Rapid Synthesis of Magnetite/Hydroxyapatite Composites for Hyperthermia Treatments via a Mechanochemical Route

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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

Simple and Rapid Synthesis of Magnetite/Hydroxyapatite Composites for Hyperthermia Treatments via a Mechanochemical Route

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Tomohiro Iwasaki

2013-04-01

Full Text Available 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.

Synthesis and characterization of natural hydroxyapatite (recycled) composites with titania

International Nuclear Information System (INIS)

Mendes Filho, Antonio Alves; Gouveia, Vitor Jose Pinto; Pereira, Renato Alves; Araujo, Fernando Gabriel da Silva; Sousa, Camila Mateus de

2010-01-01

Natural hydroxyapatite biphasic ceramics (recycled) with titania (TiO_2-Hap) were studied in this work. For the formation of such ceramic the powders were mixed natural hydroxyapatite obtained from veal bone by the hydrothermal method with titania (TiO_2), forming the composites H9T1. The powders, manually homogenized, were conformed in pellet and sintered at temperatures between 1200 and 1400 deg C The ceramic bodies were characterized by XRD and SEM/EDS. The initial results were not satisfactory and require new studies. (author)

Design of polymer-biopolymer-hydroxyapatite biomaterials for bone tissue engineering: Through molecular control of interfaces

Science.gov (United States)

Verma, Devendra

In this dissertation, novel biomaterials are designed for bone biomaterials and bone tissue engineering applications. Novel biomaterials of hydroxyapatite with synthetic and natural polymers have been fabricated using a combination of processing routes. Initially, we investigated hydroxyapatite-polycaprolactone-polyacrylic acid composites and observed that minimal interfacial interactions between polymer and mineral led to inadequate improvement in the mechanical properties. Bioactivity experiments on these composites showed that the presence of functional groups, such as carboxylate groups, influence bioactivity of the composites. We have developed and investigated composites of hydroxyapatite with chitosan and polygalacturonic acid (PgA). Chitosan and PgA are biocompatible, biodegradable, and also electrostatically complementary to each other. This strategy led to significant improvement in mechanical properties of new composites. The nanostructure analysis using atomic force microscopy revealed a multilevel organization in these composites. Enhancement in mechanical response was attributed to stronger interfaces due to strong electrostatic interaction between oppositely charged chitosan and PgA. Further analysis using the Rietveld method showed that biopolymers have marked impact on hydroxyapatite crystal growth and also on its crystal structure. Significant changes were observed in the lattice parameters of hydroxyapatite synthesized by following biomineralization method (organics mediated mineralization). For scaffold preparation, chitosan and PgA were mixed first, and then, nano-hydroxyapatite was added. Oppositely charged polyelectrolytes, such as chitosan and PgA, spontaneously form complex upon mixing. The poly-electrolyte complex exists as nano-sized particles. Chitosan/PgA scaffolds with and without hydroxyapatite were prepared by the freeze drying method. By controlling the rate of cooling and concentration, we have produced both fibrous and sheet

Induced wettability and surface-volume correlation of composition for bovine bone derived hydroxyapatite particles

Science.gov (United States)

Maidaniuc, Andreea; Miculescu, Florin; Voicu, Stefan Ioan; Andronescu, Corina; Miculescu, Marian; Matei, Ecaterina; Mocanu, Aura Catalina; Pencea, Ion; Csaki, Ioana; Machedon-Pisu, Teodor; Ciocan, Lucian Toma

2018-04-01

Hydroxyapatite powders characteristics need to be determined both for quality control purposes and for a proper control of microstructural features of bone reconstruction products. This study combines bulk morphological and compositional analysis methods (XRF, SEM-EDS, FT-IR) with surface-related methods (XPS, contact angle measurements) in order to correlate the characteristics of hydroxyapatite powders derived from bovine bone for its use in medical applications. An experimental approach for correlating the surface and volume composition was designed based on the analysis depth of each spectral method involved in the study. Next, the influences of powder particle size and forming method on the contact angle between water drops and ceramic surface were evaluated for identifying suitable strategies of tuning hydroxyapatite's wettability. The results revealed a preferential arrangement of chemical elements at the surface of hydroxyapatite particles which could induce a favourable material behaviour in terms of sinterability and biological performance.

A novel silica nanotube reinforced ionic incorporated hydroxyapatite composite coating on polypyrrole coated 316L SS for implant application

Energy Technology Data Exchange (ETDEWEB)

Prem Ananth, K., E-mail: kpananth01@gmail.com [Department of Nanoscience and Technology, Bharathiar University, Coimbatore – 641 046 (India); Joseph Nathanael, A. [Department of Nano, Medical and Polymer Materials, Yeungnam University, Gyeongsan 712-749 (Korea, Republic of); Jose, Sujin P. [Department of Materials Science and Nano engineering, Rice University, Texas 77005 (United States); School of Physics, Madurai Kamaraj University, Madurai-625021 (India); Oh, Tae Hwan [Department of Nano, Medical and Polymer Materials, Yeungnam University, Gyeongsan 712-749 (Korea, Republic of); Mangalaraj, D. [Department of Nanoscience and Technology, Bharathiar University, Coimbatore – 641 046 (India)

2016-02-01

An attempt has been made to deposit a novel smart ion (Sr, Zn, Mg) substituted hydroxyapatite (I-HAp) and silica nanotube (SiNTs) composite coatings on polypyrrole (PPy) coated surgical grade 316L stainless steel (316L SS) to improve its biocompatibility and corrosion resistance. The I-HAp/SiNTS/PPy bilayer coating on 316L SS was prepared by electrophoretic deposition technique. Potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) studies were carried out. These results confirmed the significant improvement of the corrosion resistance of the 316L SS alloy by the I-HAp/SiNTs/PPy bilayer composite coating. The adhesion strength and hardness test confirmed the anticipated mechanical properties of the composite. A low contact angle value revealed the hydrophilic nature. Inductively coupled plasma-atomic emission spectroscopy (ICP-AES) was used for the leach out analysis of the samples. Added to this, the bioactivity of the composite was analyzed by observing the apatite formation in the SBF solution for 7, 14, 21 and 28 days of incubation. An enhancement of in vitro osteoblast attachment and cell viability was observed, which could lead to the optimistic orthopedic and dental applications. - Highlights: • Polypyrrole (PPy) coated 316L SS substrates were fabricated using electrodeposition method. • A novel silica nanotube (SiNTs) and ionic substituted (Sr, Zn, Mg) hydroxyapatite composite (I-HAp) were prepared. • The composite (I-HAp/SiNTs) was coated on PPy coated 316L SS substrate using electrophoretic deposition. • These results are favorable for corrosion resistance and enhanced osteoblast cell attachment for bone formation.

In vitro study of nano-hydroxyapatite/chitosan–gelatin composites for bio-applications

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Khaled R. Mohamed

2014-03-01

Full Text Available The present work aims to study the in vitro properties of nano-hydroxyapatite/chitosan–gelatin composite materials. In vitro behavior was performed in simulated body fluid (SBF to verify the formation of apatite layer onto the composite surfaces. The in vitro data proved the deposition of calcium and phosphorus ions onto hydroxyapatite /polymeric composite surfaces especially those containing high concentrations of polymer content. The degradation of the composites decreased with increase in the polymeric matrix content and highly decreased in the presence of citric acid (CA, especially these composites which contain 30% polymeric content. The water absorption of the composites increased with increase in the polymeric content and highly increased with CA addition. The Fourier transformed infrared reflectance (FT-IR and scanning electron microscope (SEM for the composites confirmed the formation of bone-like apatite layer on the composite surfaces, especially those containing high content of polymers (30% with 0.2 M of CA. These promising composites have suitable properties for bio-applications such as bone grafting and bone tissue engineering applications in the future.

Phosphonate-hydroxyapatite hybrid compounds prepared by hydrothermal method

Energy Technology Data Exchange (ETDEWEB)

Agougui, H.; Aissa, A. [Laboratoire de Physico-Chimie des Materiaux, Faculte des sciences de Monastir, 5019 Monastir (Tunisia); Maggi, S. [CNR-IC Istituto di Cristallografia, via Amendola 122/O, 70126 Bari (Italy); Debbabi, M., E-mail: m.debbabi@yahoo.fr [Laboratoire de Physico-Chimie des Materiaux, Faculte des sciences de Monastir, 5019 Monastir (Tunisia)

2010-12-15

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 deg. C for 15 h. The modification of hydroxyapatite by grafting organic moieties is confirmed by IR and NMR MAS ({sup 1}H and {sup 31}P) 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{sup -} groups of the apatitic structure.

Phosphonate-hydroxyapatite hybrid compounds prepared by hydrothermal method

International Nuclear Information System (INIS)

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

2010-01-01

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 deg. C for 15 h. The modification of hydroxyapatite by grafting organic moieties is confirmed by IR and NMR MAS ( 1 H and 31 P) 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.

COLOSTRUM-COLLAGEN-HYDROXYAPATITE COMPOSITE, AN EXCELLENT CANDIDATE BIOMATERIAL FOR BONE REPAIR AND BONE INFECTION MANAGEMENT

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Dio Nurdin Setiawan

2014-05-01

Full Text Available In the case ofbone fracture or defect after surgery, which is common in patients with bone cancer (osteosarcoma, it takes a long time for closure and it may cause an infection problem. The use ofcollagen-hydroxyapatite composite with a blend ofcolostrum as a scaffold is aimed to accelerate the process of osteoblast growth, inhibite the emergence of infections, and act as bone tissue repair material. The method used was the hydrogel formation process and freeze dry process to remove the solvent and to form pores. The composition of scaffold composite manufactured was 15% collagen, 75% hydroxyapatite and 10% colostrum. Combination ofscaffold collagen-hydroxyapatite-colostrum has quite reliable properties because SEM test showed that scaffold could bind to both and could bind to both and could form sufficient pores to provide enough place for bone cells (osteoblats to grow. The results of MTT assay revealed percentage of above 60%, which indicates that the material is not toxic. In conclusion, collagen-hydroxyapatite-colostrum combination is an excellent biomaterial candidate for bone repair and bone infection management.

Microwave assisted synthesis of hydroxyapatite - biomass composite sorbent for strontium removal

International Nuclear Information System (INIS)

Parab, Harshala; Shenoy, Niyoti; Kumar, Sanjukta A.; Kumar, Sangita D.; Reddy, A.V.R.

2015-01-01

Radioactive wastes are a cause of concern for the environment; in case of any accidental release or improper storage. 90 Sr is one of the major fission products present in the waste solutions generated during the reprocessing of spent nuclear fuel. Its chemical resemblance to calcium, leads to various health hazards; if there is any discharge/appearance of strontium in the food chain. This necessitates the development of simple and efficient methods of strontium separation from the aqueous solutions. Among various methods used for separation, ion exchange methods are highly efficient but expensive. Recently efforts have been made for development of bioremediation based approach as a viable alternative for such problems. However, the basic requirement for of biomaterials for the use in radionuclides separation is that it should be able to withstand the radiation damage and prevent leaching of sorbed radionuclides with time. In the present studies, authors have developed a composite sorbent comprising of hydroxyapatite and coir pith (HAP-CP) and evaluated its performance for sorption of strontium. Coir pith - an agroindustrial lignocellulosic waste biomass is known for its structural stability due to the large number of aromatic rings in lignin structure. Hydroxyapatite, has also been explored by the researchers for its radiation stability and metal remediation properties. Herein, the HAP-CP composite adsorbent was prepared by microwave heating of a mixture containing phosphoric acid (H 3 PO 4 ) and calcium nitrate tetrahydrate solutions (Ca(NO 3 ) 2 .4H 2 O) in the presence of coir pith at pH 10 until complete dryness

Preparation of the Jaws Damaged Parts from Composite Biopolymers Materials

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Riyam A. Al-husseini

2017-10-01

Full Text Available Composite materials composing of fusing two materials or more are disaccorded in mechanical and physical characteristics, The studied the effect of changing in the reinforcement percentage by Hydroxyapatite Prepared nano world via the size of the nanoscale powder manufacturing manner chemical precipitation and microwave powders were two types their preparations have been from natural sources: the first type of eggshells and the other from the bones of fish in mechanical Properties which include the tensile strength, elastic modulus, elongation, hardness and tear for composite material consisting of Silicone rubber (SIR reinforced by (µ-n-HA, after strengthening silicone rubber Protect proportions (5,10,15,20 wt% of Article achieved results that increase the additive lead to increased hardness while tougher and modulus of elasticity decreases with added as shown in the diagrams.

Development of functionalized hydroxyapatite/poly(vinyl alcohol) composites

Science.gov (United States)

Stipniece, Liga; Salma-Ancane, Kristine; Rjabovs, Vitalijs; Juhnevica, Inna; Turks, Maris; Narkevica, Inga; Berzina-Cimdina, Liga

2016-06-01

Based on the well-known pharmaceutical excipient potential of poly(vinyl alcohol) (PVA) and clinical success of hydroxyapatite (HAp), the objective of this work was to fabricate functionalized composite microgranules. PVA was modified with succinic anhydride to introduce carboxyl groups (-COOH), respectively, by reaction between the -OH groups of PVA and succinic anhydride, for attachment of drug molecules. For the first time, the functionalized composite microgranules containing HAp/PVA in the ratio of 1:1 were prepared through in situ precipitation of HAp in modified PVA aqueous solutions followed by spray drying of obtained suspensions. The microgranules were characterized by Fourier-transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and differential scanning calorimetry (DSC). The presence of -COOH groups was verified by FT-IR, and the amount of functional groups added to PVA molecules (averaging 15 mol%) was determined by nuclear magnetic resonance spectroscopy (NMR). DSC results showed that modification with -COOH groups slightly decreased the thermal stability of PVA. FT-IR and XRD analysis confirmed that the resulting composites contain mainly nanocrystalline HAp and PVA. Moreover, the images taken by FE-SEM revealed that the microgranules consisted of nanosized HAp crystallites homogenously embedded in the PVA matrix. DSC measurements indicated that decomposition mechanism of the HAp/PVA differs from that of pure PVA and occurs at lower temperatures. However, the presence of HAp had minor influence on the thermal decomposition of the PVA modified with succinic anhydride. The investigation of composite microgranules confirmed interaction and integration between the HAp and PVA.

Preparation and cellular response of porous A-type carbonated hydroxyapatite nanoceramics

Energy Technology Data Exchange (ETDEWEB)

Li Bo, E-mail: Leewave@126.com [Institute of Biomaterials and Living Cell Imaging Technology, School of Metallurgy and Materials Engineering, Chongqing University of Science and Technology, Chongqing 401331 (China) and National Engineering Research Center for Biomaterials, Sichuan University, Chengdu 610064 (China); Liao Xiaoling [Institute of Biomaterials and Living Cell Imaging Technology, School of Metallurgy and Materials Engineering, Chongqing University of Science and Technology, Chongqing 401331 (China); Zheng Li [National Engineering Research Center for Biomaterials, Sichuan University, Chengdu 610064 (China); He Huawei [Department of Prosthodontics, Beijing Stomatological Hospital, Capital Medical University, Beijing, 100050 (China); Wang Hong [National Engineering Research Center for Biomaterials, Sichuan University, Chengdu 610064 (China); Fan Hongsong, E-mail: hsfan68@hotmail.com [National Engineering Research Center for Biomaterials, Sichuan University, Chengdu 610064 (China); Zhang Xingdong [National Engineering Research Center for Biomaterials, Sichuan University, Chengdu 610064 (China)

2012-05-01

Microwave sintering using the activated carbon as embedding material was applied in preparation of porous A-type carbonated hydroxyapatite ceramics with nano(nCHA) and submicron (mCHA) structure. By examining the linear shrinkages and the compressive strengths of samples at different temperatures, a suitable microwave sintering temperature was achieved. The microwave sintering method was successfully used to prepare A-type CHA with nano or submicron structure, and the mechanism of the formation of A-type carbonate groups was discussed also. Compared with the samples prepared by the conventional sintering method (mHA), the nCHA bioceramics synthesized by the microwave sintering approach had smaller grain size and more uniform microstructure, and showed a compressive strength similar to the conventional samples. In vitro dissolution test proved that nCHA exhibits better degradation property in comparison to pure HA. Rat osteoblasts were cultured with nCHA, mCHA and mHA to evaluate their biocompatibility, and nCHA showed significant enhancement of cells in attachment, proliferation and differentiation. In conclusion, carbonate groups can be easily introduced to HA crystal structure using the activated carbon as embedding material, and microwave sintering is an effective and simple method in preparing A-type CHA with a nanostructure. Results from this in vitro biological study suggest that porous A-type carbonated hydroxyapatite nanoceramics may be a much better candidate for clinical use in terms of bioactivity. - Highlights: Black-Right-Pointing-Pointer We prepared porous A-type carbonated hydroxyapatite nanoceramics with microwave sintering. Black-Right-Pointing-Pointer We examined physico-chemical characterization and osteoblast response. Black-Right-Pointing-Pointer The nanoceramics have a comparable compressive strength to samples with conventional sintering method. Black-Right-Pointing-Pointer The nanoceramics enhance degradation property, osteoblast

Preparation of hydroxyapatite/poly(lactic acid) hybrid microparticles for local drug delivery

International Nuclear Information System (INIS)

Loca, D; Locs, J; Berzina-Cimdina, L

2013-01-01

Calcium phosphate (CaP) bioceramic is well known as bioactive and biocompatible material in bone tissue regeneration applications. Apatitic CaP, especially nano sized hydroxyapatite (NHAp), is more similar to the natural apatite presented in the bone tissue than CaP bioceramics. In the current research NHAp was modified using biodegradable polymer – poly(lactic acid) (PLA) to develop composites providing bone regeneration and local drug delivery. NHAp/PLA microcapsules were prepared using solid-in-water-in-oil-in-water (s/w 1 /o/w 2 ) encapsulation technology. The impact of primary and secondary emulsion stability on the emulsion droplet and microparticle properties was evaluated. The stability of final emulsion can be increased by varying the process parameters. Stable s/w 1 /o/w 2 emulsion using 3ml of NHAp suspension, not less than 100ml of 4% PVA water solution and 10ml of 10% PLA solution in dichloromethane can be obtained. S/w 1 /o/w 2 microencapuslation method can be effectively used for the preparation of multi-domain microcapsules achieving high NHAp encapsulation efficacy (93%)

Physical characterization of porous hydroxyapatite prepared by slip casting route

International Nuclear Information System (INIS)

Rusnah Mustaffa; Idris Besar; Mohd Reusmaazran Yusof; Che Rohaida Che Hak

2005-01-01

Recent developments have led to an interest in the potential of porous hydroxyapatite (HA) as a synthetic bone graft. The starting material, that is HA powder, was prepared by the precipitation method using calcium hydroxide and ortho-phosporic acid. Through this route, the HA powder was first made into a slip by mixing with binder and then the slip was transferred into a mould. The binder was used as the porosifier where different ratios of HA to binder were studied. The material was then dried in oven followed by burning in furnace and finally the porous product was obtained and ready for characterization after sintering. The paper presents some characterization of porous HA products including chemical composition, density and macrostructure. The pore sizes obtained were in the range 200 mm to 400 mm diameters. From the different HA to binder ratios, variation in apparent densities were observed which is in the range of 2.63 to 2.76 g/cm 3 . The morphology of porous HA was observed by Scanning Electron Microscope (SEM) at 15 KV. The chemical structure and composition were also determined using Fourier Transform Infrared spectroscopy (FTIR) and the SEM EDAX, respectively, and the results will also be discussed. (Author)

Synthesis of Ca,Y-zirconia/hydroxyapatite nanoparticles and composites

Czech Academy of Sciences Publication Activity Database

Částková, K.; Hadraba, Hynek; Matoušek, A.; Roupcová, P.; Chlup, Zdeněk; Novotná, L.; Cihlář, J.

2016-01-01

Roč. 36, č. 12 (2016), s. 2903-2912 ISSN 0955-2219 R&D Projects: GA ČR GA14-11234S; GA MŠk(CZ) LQ1601 Institutional support: RVO:68081723 Keywords : Zirconia * Hydroxyapatite * Composite * Bioactivity * Mechanical properties Subject RIV: JH - Ceramic s, Fire-Resistant Materials and Glass Impact factor: 3.411, year: 2016

Effect of applied voltage on phase components of composite coatings prepared by micro-arc oxidation

Energy Technology Data Exchange (ETDEWEB)

Zhu, Wenjun [Department of Prosthodontics, Guanghua School of Stomatology, Sun Yat-sen University, Guangzhou 510055 (China); Fang, Yu-Jing [Department of Colorectal Surgery, State Key Laboratory of Oncology in South China, Sun Yat-sen University Cancer Center, Guangzhou 510060 (China); Zheng, Huade [College of Materials Science and Engineering, South China University of Technology, Guangzhou 510641 (China); Tan, Guoxin [Guangdong University of Technology, Guangdong Province 510006 (China); Cheng, Haimei [College of Materials Science and Engineering, South China University of Technology, Guangzhou 510641 (China); Ning, Chengyun, E-mail: imcyning@scut.edu.cn [College of Materials Science and Engineering, South China University of Technology, Guangzhou 510641 (China)

2013-10-01

In this report, we present results from our experiments on composite coatings formed on biomedical titanium substrates by micro-arc oxidation (MAO) in constant-voltage mode. The coatings were prepared on the substrates in an aqueous electrolyte containing calcium acetate and β-glycerol phosphate disodium salt pentahydrate (β-GP). We analyzed the element distribution and phase components of the coatings prepared at different voltages by X-ray diffraction, thin-coating X-ray diffraction, electron-probe microanalysis, and Fourier-transform infrared spectroscopy. The results show that the composite coatings formed at 500 V consist of titania (TiO{sub 2}), hydroxylapatite (HA), and calcium carbonate (CaCO{sub 3}). Furthermore, the concentration of Ca, P, and Ti gradually changes with increasing applied voltage, and the phase components of the composite coatings gradually change from the bottom of the coating to the top: the bottom layer consists of TiO{sub 2}, the middle layer consists of TiO{sub 2} and HA, and the top layer consists of HA and a small amount of CaCO{sub 3}. The formation of HA directly on the coating surface by MAO technique can greatly enhance the surface bioactivity. - Highlights: • Coatings prepared on biomedical titanium substrate by micro-arc oxidation • Coatings composed of titania, hydroxyapatite and calcium carbonate • Hydroxyapatite on the coating surface can enhance the surface bioactivity.

Fabrication and Microstructure of Hydroxyapatite Coatings on Zirconia by Room Temperature Spray Process.

Science.gov (United States)

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.

HYDROXYAPATITE THIN FILMS ON TITANIUM DEPOSITED BY KrF LASER

OpenAIRE

QUANHE BAO; CHUANZHONG CHEN; DIANGANG WANG; YAFAN ZHAO; TINGQUAN LEI; JUNMING LIU

2006-01-01

Pulsed laser deposition (PLD) is being investigated as an alternative technique to prepare hydroxyapatite coatings. In this research we studied the microstructure and phase composition of the PLD hydroxyapatite films. The surface morphology of the films is composed of droplets for which size ranges from hundreds of nanometers to a few micrometers. The cross-sectional morphology of the films shows that the films adhere to the substrate well and there are no microcracks, pores and other defects...

Nanoparticle fabrication of hydroxyapatite by laser ablation in water

International Nuclear Information System (INIS)

Musaev, O. R.; Wieliczka, D. M.; Wrobel, J. M.; Kruger, M. B.; Dusevich, V.

2008-01-01

Synthetic polycrystalline hydroxyapatite was ablated in water with 337 nm radiation from a UV nitrogen pulsed laser. According to transmission electron microscopy micrographs, the ablated particles were approximately spherical and had a size of ∼80 nm. Raman spectroscopic analysis demonstrated that particles had the same structure as the original crystal. X-ray photoelectron spectroscopy showed that the surface chemical composition was close to that of the original material. The characteristics of the ablated particles and estimations of the temperature rise of the hydroxyapatite surface under laser irradiation are consistent with the mechanism of explosive boiling being responsible for ablation. The experimental observations offer the basis for preparation of hydroxyapatite nanoparticles by laser ablation in water

Comparative facile methods for preparing graphene oxide-hydroxyapatite for bone tissue engineering.

Science.gov (United States)

Raucci, M G; Giugliano, D; Longo, A; Zeppetelli, S; Carotenuto, G; Ambrosio, L

2017-08-01

Motivated by the success of using graphene oxide (GO) as a nanofiller of composites, there is a drive to search for this new kind of carbon material as a bioactive component in ceramic materials. In the present study, biomineralized GO was prepared by two different approaches, represented by in situ sol-gel synthesis and biomimetic treatment. It was found that in the biocomposites obtained by the sol-gel approach, the spindle-like hydroxyapatite nanoparticles, with a diameter of ca. 5 ± 0.37 nm and a length of ca. 70 ± 2.5 nm, were presented randomly and strongly on the surface. The oxygen-containing functional groups, such as hydroxyl and carbonyl, present on the basal plane and edges of the GO sheets, play an important role in anchoring calcium ions, as demonstrated by FT-IR and TEM investigations. A different result was obtained for biocomposites after biomimetic treatment: an amorphous calcium phosphate on GO sheet was observed after 5 days of treatment. These different approaches resulted in a diverse effect on the proliferation and differentiation of osteogenic mesenchymal stem cells. In fact, in biocomposites prepared by the sol-gel approach the expression of an early marker of osteogenic differentiation, ALP, increases with the amount of GO in the first days of cell culture. Meanwhile, biomimetic materials sustain cell viability and proliferation, even if the expression of alkaline phosphatase activity in a basal medium is delayed. These findings may provide new prospects for utilizing GO-based hydroxyapatite biocomposites in bone repair, bone augmentation and coating of biomedical implants and broaden the application of GO sheets in biological areas. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Preparation of hollow hydroxyapatite microspheres by the conversion of borate glass at near room temperature

International Nuclear Information System (INIS)

Yao, Aihua; Ai, Fanrong; Liu, Xin; Wang, Deping; Huang, Wenhai; Xu, Wei

2010-01-01

Hollow hydroxyapatite microspheres, consisting of a hollow core and a porous shell, were prepared by converting Li 2 O-CaO-B 2 O 3 glass microspheres in dilute phosphate solution at 37 o C. The results confirmed that Li 2 O-CaO-B 2 O 3 glass was transformed to hydroxyapatite without changing the external shape and dimension of the original glass object. Scanning electron microscopy images showed the shell wall of the microsphere was built from hydroxyapatite particles, and these particles spontaneously align with one another to form a porous sphere with an interior cavity. Increase in phosphate concentration resulted in an increase in the reaction rate, which in turn had an effect on shell wall structure of the hollow hydroxyapatite microsphere. For the Li 2 O-CaO-B 2 O 3 glass microspheres reacted in low-concentration K 2 HPO 4 solution, lower reaction rate and a multilayered microstructure were observed. On the other hand, the glass microspheres reacted in higher phosphate solution converted more rapidly and produced a single hydroxyapatite layer. Furthermore, the mechanism of forming hydroxyapatite hollow microsphere was described.

Synthesis of dense nano cobalt-hydroxyapatite by modified electroless deposition technique

Energy Technology Data Exchange (ETDEWEB)

Mohd Zaheruddin, K., E-mail: zaheruddin@unimap.edu.my; Rahmat, A., E-mail: azmirahmat@unimap.edu.my; Shamsul, J. B., E-mail: sbaharin@unimap.edu.my; Mohd Nazree, B. D., E-mail: nazree@unimap.edu.my; Aimi Noorliyana, H., E-mail: aimiliyana@unimap.edu.my [School of Materials Engineering, Universiti Malaysia Perlis, Kompleks Pusat Pengajian Jejawi Universiti Malaysia Perlis, Taman Muhibbah, Jejawi 02600 Arau Perlis (Malaysia)

2016-07-19

Cobalt-hydroxyapatite (Co-HA) composites was successfully prepared by simple electroless deposition process of Co on the surface of hydroxyapatite (HA) particles. Co deposition was carried out in an alkaline bath with sodium hypophosphite as a reducing agent. The electroless process was carried out without sensitization and activation steps. The deposition of Co onto HA was characterized by scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX). The Co-HA composite powder was compacted and sintered at 1250°C. The Co particles were homogeneously dispersed in the HA matrix after sintering and the mechanical properties of composites was enhanced to 100 % with 3 % wt Co and gradually decreased at higher Co content.

Development of dental composites with reactive fillers that promote precipitation of antibacterial-hydroxyapatite layers.

Science.gov (United States)

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. Copyright © 2015 The Authors. Published by Elsevier B.V. All rights reserved.

Biomimetic properties of an injectable chitosan/nano-hydroxyapatite/collagen composite

Energy Technology Data Exchange (ETDEWEB)

Huang Zhi [Laboratory of Advanced Materials, Department of Materials Science and Engineering, Tsinghua University, Beijing 100084 (China); Feng Qingling, E-mail: biomater@mail.tsinghua.edu.cn [Laboratory of Advanced Materials, Department of Materials Science and Engineering, Tsinghua University, Beijing 100084 (China); Yu Bo; Li Songjian [Department of Orthopedics, Zhujiang Hospital of Southern Medical University, Guangzhou 510282 (China)

2011-04-08

To meet the challenges of designing an injectable scaffold and regenerating bone with complex three-dimensional (3D) structures, a biomimetic and injectable hydrogel scaffold based on nano-hydroxyapatite (HA), collagen (Col) and chitosan (Chi) is synthesized. The chitosan/nano-hydroxyapatite/collagen (Chi/HA/Col) solution rapidly forms a stable gel at body temperature. It shows some features of natural bone both in main composition and microstructure. The Chi/HA/Col system can be expected as a candidate for workable systemic minimally invasive scaffolds with surface properties similar to physiological bone based on scanning electron microscopic (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR) results.

Biomimetic properties of an injectable chitosan/nano-hydroxyapatite/collagen composite

International Nuclear Information System (INIS)

Huang Zhi; Feng Qingling; Yu Bo; Li Songjian

2011-01-01

To meet the challenges of designing an injectable scaffold and regenerating bone with complex three-dimensional (3D) structures, a biomimetic and injectable hydrogel scaffold based on nano-hydroxyapatite (HA), collagen (Col) and chitosan (Chi) is synthesized. The chitosan/nano-hydroxyapatite/collagen (Chi/HA/Col) solution rapidly forms a stable gel at body temperature. It shows some features of natural bone both in main composition and microstructure. The Chi/HA/Col system can be expected as a candidate for workable systemic minimally invasive scaffolds with surface properties similar to physiological bone based on scanning electron microscopic (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR) results.

Ionic liquid as a potential solvent for preparation of collagen-alginate-hydroxyapatite beads as bone filler.

Science.gov (United States)

Iqbal, Bushra; Sarfaraz, Zenab; Muhammad, Nawshad; Ahmad, Pervaiz; Iqbal, Jibran; Khan, Zia Ul Haq; Gonfa, Girma; Iqbal, Farasat; Jamal, Arshad; Rahim, Abdur

2018-07-01

In this study, collagen/alginate/hydroxyapatite beads having different proportions were prepared as bone fillers for the restoration of osteological defects. Ionic liquid was used to dissolve the collagen and subsequently the solution was mixed with sodium alginate solution. Hydroxyapatite was added in different proportions, with the rationale to enhance mechanical as well as biological properties. The prepared solutions were given characteristic bead shapes by dropwise addition into calcium chloride solution. The prepared beads were characterized using FTIR, XRD, TGA and SEM analysis. Microhardness testing was used to evaluate the mechanical properties. The prepared beads were investigated for water adsorption behavior to ascertain its ability for body fluid uptake and adjusted accordingly to the bone cavity. Drug loading and subsequently the antibacterial activity was investigated for the prepared beads. The biocompatibility was assessed using the hemolysis testing and cell proliferation assay. The prepared collagen-alginate-HA beads, having biocompatibility and good mechanical properties, have showed an option of promising biologically active bone fillers for bone regeneration.

Fabrication, characterization, and in vitro study of zinc substituted hydroxyapatite/silk fibroin composite coatings on titanium for biomedical applications.

Science.gov (United States)

Zhong, Zhenyu; Ma, Jun

2017-09-01

Zinc substituted hydroxyapatite/silk fibroin composite coatings were deposited on titanium substrates at room temperature by electrophoretic deposition. Microscopic characterization of the synthesized composite nanoparticles revealed that the particle size ranged 50-200 nm, which increased a little after zinc substitution. The obtained coatings maintained the phase of hydroxyapatite and they could induce fast apatite formation in simulated body fluid, indicating high bone activity. The cell culturing results showed that the biomimetic hydroxyapatite coatings could regulate adhesion, spreading, and proliferation of osteoblastic cells. Furthermore, the biological behavior of the zinc substituted hydroxyapatite coatings was found to be better than the bare titanium without coatings and hydroxyapatite coatings without zinc, increasing MC3T1-E1 cell differentiation in alkaline phosphatase expression.

Hydroxyapatite-silver nanoparticles coatings on porous polyurethane scaffold.

Science.gov (United States)

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. © 2013.

Preparation and characterization of multi-walled carbon nanotube/hydroxyapatite nanocomposite film dip coated on Ti–6Al–4V by sol–gel method for biomedical applications: An in vitro study

International Nuclear Information System (INIS)

Abrishamchian, Alireza; Hooshmand, Tabassom; Mohammadi, Mohammadreza; Najafi, Farhood

2013-01-01

In the present research, the introduction of multi-walled carbon nanotubes (MWCNTs) into the hydroxyapatite (HA) matrix and dip coating of nanocomposite on titanium alloy (Ti–6Al–4V) plate was conducted in order to improve the performance of the HA-coated implant via the sol–gel method. The structural characterization and electron microscopy results confirmed well crystallized HA–MWCNT coating and homogenous dispersion of carbon nanotubes in the ceramic matrix at temperatures as low as 500 °C. The evaluation of the mechanical properties of HA and HA/MWCNT composite coatings with different weight percentages of MWCNTs showed that the addition of low concentrations of MWCNTs (0.5 and 1 wt.%) had improved effect on the mechanical properties of nanocomposite coatings. Moreover, this in vitro study ascertained the biocompatibility of the prepared sol–gel-derived HA/MWCNT composite coatings. - Highlights: ► Carbon nanotube/hydroxyapatite composite was successfully dip-coated on Ti by sol–gel. ► Well-crystallized HA–MWCNT and homogenous dispersion of nanotubes were obtained. ► Low concentration of CNTs improved the mechanical properties of composite coating. ► Biocompatibility of the prepared sol–gel-derived HA/MWCNT films was ascertained

Preparation and characterization of multi-walled carbon nanotube/hydroxyapatite nanocomposite film dip coated on Ti–6Al–4V by sol–gel method for biomedical applications: An in vitro study

Energy Technology Data Exchange (ETDEWEB)

Abrishamchian, Alireza [Department of Dental Biomaterials, School of Dentistry/Research Center for Science and Technology in Medicine, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of); Hooshmand, Tabassom, E-mail: hoshmand@sina.tums.ac.ir [Department of Dental Biomaterials, School of Dentistry/Research Center for Science and Technology in Medicine, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of); Mohammadi, Mohammadreza [Department of Materials Science and Engineering, Sharif University of Technology, Tehran (Iran, Islamic Republic of); Najafi, Farhood [Department of Resin and Additives, Institute for Color Science and Technology, Tehran (Iran, Islamic Republic of)

2013-05-01

In the present research, the introduction of multi-walled carbon nanotubes (MWCNTs) into the hydroxyapatite (HA) matrix and dip coating of nanocomposite on titanium alloy (Ti–6Al–4V) plate was conducted in order to improve the performance of the HA-coated implant via the sol–gel method. The structural characterization and electron microscopy results confirmed well crystallized HA–MWCNT coating and homogenous dispersion of carbon nanotubes in the ceramic matrix at temperatures as low as 500 °C. The evaluation of the mechanical properties of HA and HA/MWCNT composite coatings with different weight percentages of MWCNTs showed that the addition of low concentrations of MWCNTs (0.5 and 1 wt.%) had improved effect on the mechanical properties of nanocomposite coatings. Moreover, this in vitro study ascertained the biocompatibility of the prepared sol–gel-derived HA/MWCNT composite coatings. - Highlights: ► Carbon nanotube/hydroxyapatite composite was successfully dip-coated on Ti by sol–gel. ► Well-crystallized HA–MWCNT and homogenous dispersion of nanotubes were obtained. ► Low concentration of CNTs improved the mechanical properties of composite coating. ► Biocompatibility of the prepared sol–gel-derived HA/MWCNT films was ascertained.

Mechanical properties and crystallization behavior of hydroxyapatite/poly(butylenes succinate) composites.

Science.gov (United States)

Guo, Wenmin; Zhang, Yihe; Zhang, Wei

2013-09-01

Biodegradable synthetic polymers have attracted much attention nowadays, and more and more researches have been done on biodegradable polymers due to their excellent mechanical properties, biocompatibility, and biodegradability. In this work, hydroxyapatite (HA) particles were melt-mixing with poly (butylenes succinate) (PBS) to prepare the material, which could be used in the biomedical industry. To develop high-performance PBS for cryogenic engineering applications, it is necessary to investigate the cryogenic mechanical properties and crystallization behavior of HA/PBS composites. Cryogenic mechanical behaviors of the composites were studied in terms of tensile and impact strength at the glass transition temperature (-30°C) and compared to their corresponding behaviors at room temperature. With the increase of HA content, the crystallization of HA/PBS composites decreased and crystallization onset temperature shifted to a lower temperature. The diameter of spherulites increased at first and decreased with a further HA content. At the same time, the crystallization rate became slow when the HA content was no more than 15wt% and increased when HA content reached 20wt%. In all, the results we obtained demonstrate that HA/PBS composites reveal a better tensile strength at -30°C in contrast to the strength at room temperature. HA particles with different amount affect the crystallization of PBS in different ways. Copyright © 2013 Wiley Periodicals, Inc.

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

Science.gov (United States)

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.

The coprecipitation of strontium with hydroxyapatite

International Nuclear Information System (INIS)

Fujino, Osamu

1975-01-01

The distribution behavior of the strontium ion between hydroxyapatite and the parent solution was investigated. The hydroxyapatite was formed by the extremely slow addition of diammonium hydrogenphosphate to solutions of calcium and strontium nitrate buffered with ethylenediamine at 80 0 C. The precipitate yielded a typical X-ray diffraction pattern of hydroxyapatite and had a composition in which the Ca/P molar ratio was 1.67 at pH 6.80. The strontium ion was coprecipitated in the apatite, obeying the Doerner and Hoskins logarithnmic distribution law. The distribution coefficient was scarcely affected by the strontium concentration on the pH value in the parent solution, and had a value of 0.26+-0.02 at 80 0 C. On the other hand, the apparent distribution coefficient was a little affected by such organic anions as acetate, citrate, lactate, glycinate, and glutamate ions. The lattice constants of the precipitates prepared in the research were measured in order to confirm the formation of the solid solutions. (auth.)

Formation of nano-hydroxyapatite crystal in situ in chitosan-pectin polyelectrolyte complex network

International Nuclear Information System (INIS)

Li Junjie; Zhu Dunwan; Yin Jianwei; Liu Yuxi; Yao Fanglian; Yao Kangde

2010-01-01

Hydroxyapatite (HA)/polysaccharide composites have been widely used in bone tissue engineering due to their chemical similarity to natural bone. Polymer matrix-mediated synthesis of nano-hydroxyapatite is one of the simplest models for biomimetic. In this article, the nano-hydroxyapatite/chitosan-pectin (nHCP) composites were prepared through in situ mineralization of hydroxyapatite in chitosan-pectin polyelectrolyte complex (PEC) network. The formation processes of nHCP were investigated by X-ray diffraction (XRD) analysis. The interactions between nHA crystal and chitosan-pectin PEC networks were studied using Fourier Transform Infrared Spectroscopy (FTIR) and Differential Scanning Calorimetry (DSC). The morphology and structure of nHA crystal were characterized by XRD and Transmission Electron Microscope (TEM). Results suggested that the interfacial interactions between nano-hydroxyapatite crystal and chitosan-pectin PEC network assist the site specific nucleation and growth of nHA nanoparticles. The nHA crystals grow along the c-axis. In this process, pH value is the main factor to control the nucleation and growth of nHA crystal in chitosan-pectin PEC networks, because both the interactions' strength between nHA crystal and chitosan-pectin and diffusion rate of inorganic ions depend on the pH value of the reaction system. Apart from the pH value, the chitosan/pectin ratio and [Ca 2+ ] also take important effects on the formation of nHA crystal. An effective way to control the size of nHA crystal is to adjust the content of pectin and [Ca 2+ ]. It is interesting that the Zeta potential of nHCP composites is about - 30 mV when the chitosan/pectin ratio ≤ 1:1, and the dispersion solution of nHCP composites has higher stability, which provides the possibility to prepare 3D porous scaffolds with nHCP for bone tissue engineering.

Formation of nano-hydroxyapatite crystal in situ in chitosan-pectin polyelectrolyte complex network

Energy Technology Data Exchange (ETDEWEB)

Li Junjie [Department of Polymer Science and Key Laboratory of Systems Bioengineering of Ministry of Education, School of Chemical Engineering and Technology, Tianjin University, Tianjin, 300072 (China); Research Institute of Polymeric Materials, Tianjin University, Tianjin, 300072 (China); Zhu Dunwan [Institute of Biomedical Engineering, Chinese Academy of Medical Sciences and Peking Union Medical College, Tianjin, 300072 (China); Yin Jianwei; Liu Yuxi [Department of Polymer Science and Key Laboratory of Systems Bioengineering of Ministry of Education, School of Chemical Engineering and Technology, Tianjin University, Tianjin, 300072 (China); Yao Fanglian, E-mail: yaofanglian@tju.edu.cn [Department of Polymer Science and Key Laboratory of Systems Bioengineering of Ministry of Education, School of Chemical Engineering and Technology, Tianjin University, Tianjin, 300072 (China); Yao Kangde [Research Institute of Polymeric Materials, Tianjin University, Tianjin, 300072 (China)

2010-07-20

Hydroxyapatite (HA)/polysaccharide composites have been widely used in bone tissue engineering due to their chemical similarity to natural bone. Polymer matrix-mediated synthesis of nano-hydroxyapatite is one of the simplest models for biomimetic. In this article, the nano-hydroxyapatite/chitosan-pectin (nHCP) composites were prepared through in situ mineralization of hydroxyapatite in chitosan-pectin polyelectrolyte complex (PEC) network. The formation processes of nHCP were investigated by X-ray diffraction (XRD) analysis. The interactions between nHA crystal and chitosan-pectin PEC networks were studied using Fourier Transform Infrared Spectroscopy (FTIR) and Differential Scanning Calorimetry (DSC). The morphology and structure of nHA crystal were characterized by XRD and Transmission Electron Microscope (TEM). Results suggested that the interfacial interactions between nano-hydroxyapatite crystal and chitosan-pectin PEC network assist the site specific nucleation and growth of nHA nanoparticles. The nHA crystals grow along the c-axis. In this process, pH value is the main factor to control the nucleation and growth of nHA crystal in chitosan-pectin PEC networks, because both the interactions' strength between nHA crystal and chitosan-pectin and diffusion rate of inorganic ions depend on the pH value of the reaction system. Apart from the pH value, the chitosan/pectin ratio and [Ca{sup 2+}] also take important effects on the formation of nHA crystal. An effective way to control the size of nHA crystal is to adjust the content of pectin and [Ca{sup 2+}]. It is interesting that the Zeta potential of nHCP composites is about - 30 mV when the chitosan/pectin ratio {<=} 1:1, and the dispersion solution of nHCP composites has higher stability, which provides the possibility to prepare 3D porous scaffolds with nHCP for bone tissue engineering.

Intercalated chitosan/hydroxyapatite nanocomposites: Promising materials for bone tissue engineering applications.

Science.gov (United States)

Nazeer, Muhammad Anwaar; Yilgör, Emel; Yilgör, Iskender

2017-11-01

Preparation and characterization of chitosan/hydroxyapatite (CS/HA) nanocomposites displaying an intercalated structure is reported. Hydroxyapatite was synthesized through sol-gel process. Formic acid was introduced as a new solvent to obtain stable dispersions of nano-sized HA particles in polymer solution. CS/HA dispersions with HA contents of 5, 10 and 20% by weight were prepared. Self-assembling of HA nanoparticles during the drying of the solvent cast films led to the formation of homogeneous CS/HA nanocomposites. Composite films were analyzed by scanning electron microscopy (SEM), atomic force microscopy (AFM), energy dispersive X-rays (EDX) analysis, Fourier transform infrared (FTIR) spectroscopy, X-rays diffraction (XRD) analysis and thermogravimetric analysis (TGA). SEM and AFM confirmed the presence of uniformly distributed HA nanoparticles on the chitosan matrix surface. XRD patterns and cross-sectional SEM images showed the formation of layered nanocomposites. Complete degradation of chitosan matrix in TGA experiments, led to the formation of nanoporous 3D scaffolds containing hydroxyapatite, β-tricalcium phosphate and calcium pyrophosphate. CS/HA composites can be considered as promising materials for bone tissue engineering applications. Copyright © 2017 Elsevier Ltd. All rights reserved.

Bone regeneration based on nano-hydroxyapatite and hydroxyapatite/chitosan nanocomposites: an in vitro and in vivo comparative study

International Nuclear Information System (INIS)

Tavakol, S.; Nikpour, M. R.; Amani, A.; Soltani, M.; Rabiee, S. M.; Rezayat, S. M.; Chen, P.; Jahanshahi, M.

2013-01-01

Surface morphology, surface wettability, and size distribution of biomaterials affect their in vitro and in vivo bone regeneration potential. Since nano-hydroxyapatite has a great chemical and structural similarity to natural bone and dental tissues, incorporated biomaterial of such products could improve bioactivity and bone bonding ability. In this research, nano-hydroxyapatite (23 ± 0.09 nm) and its composites with variety of chitosan content [2, 4, and 6 g (45 ± 0.19, 32 ± 0.12, and 28 ± 0.12 nm, respectively)] were prepared via an in situ hybridization route. Size distribution of the particles, protein adsorption, and calcium deposition of powders by the osteoblast cells, gene expression and percentage of new bone formation area were investigated. The highest degree of bone regeneration potential was observed in nano-hydroxyapatite powder, while the bone regeneration was lowest in nano-hydroxyapatite with 6 g of chitosan. Regarding these data, suitable size distribution next to size distribution of hydroxyapatite in bone, smaller size, higher wettability, lower surface roughness of the nano-hydroxyapatite particles and homogeneity in surface resulted in higher protein adsorption, cell differentiation and percentage of bone formation area. Results obtained from in vivo and in vitro tests confirmed the role of surface morphology, surface wettability, mean size and size distribution of biomaterial besides surface chemistry as a temporary bone substitute.

Hydroxyapatite-silver nanoparticles coatings on porous polyurethane scaffold

International Nuclear Information System (INIS)

Ciobanu, Gabriela; Ilisei, Simona; Luca, Constantin

2014-01-01

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 AgNO 3 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. - Highlights: • The hydroxyapatite and silver nanoparticles were grown on the polyurethane scaffold • The hydroxyapatite/polyurethane acts as reducing agent, stabilizer and matrix for Ag • The samples were well characterized by SEM-EDX, XRD, XPS, UV-visible spectroscopy • The hydroxyapatite/silver polyurethane scaffold shows antibacterial property

Scaffolds for bone regeneration made of hydroxyapatite microspheres in a collagen matrix

Energy Technology Data Exchange (ETDEWEB)

Cholas, Rahmatullah, E-mail: rahmat.cholas@gmail.com; Kunjalukkal Padmanabhan, Sanosh, E-mail: sanosh2001@gmail.com; Gervaso, Francesca; Udayan, Gayatri; Monaco, Graziana; Sannino, Alessandro; Licciulli, Antonio

2016-06-01

Biomimetic scaffolds with a structural and chemical composition similar to native bone tissue may be promising for bone tissue regeneration. In the present work hydroxyapatite mesoporous microspheres (mHA) were incorporated into collagen scaffolds containing an ordered interconnected macroporosity. The mHA were obtained by spray drying of a nano hydroxyapatite slurry prepared by the precipitation technique. X-ray diffraction (XRD) analysis revealed that the microspheres were composed only of hydroxyapatite (HA) phase, and energy-dispersive x-ray spectroscopy (EDS) analysis revealed the Ca/P ratio to be 1.69 which is near the value for pure HA. The obtained microspheres had an average diameter of 6 μm, a specific surface area of 40 m{sup 2}/g as measured by Brunauer-Emmett-Teller (BET) analysis, and Barrett-Joyner-Halenda (BJH) analysis showed a mesoporous structure with an average pore diameter of 16 nm. Collagen/HA-microsphere (Col/mHA) composite scaffolds were prepared by freeze-drying followed by dehydrothermal crosslinking. SEM observations of Col/mHA scaffolds revealed HA microspheres embedded within a porous collagen matrix with a pore size ranging from a few microns up to 200 μm, which was also confirmed by histological staining of sections of paraffin embedded scaffolds. The compressive modulus of the composite scaffold at low and high strain values was 1.7 and 2.8 times, respectively, that of pure collagen scaffolds. Cell proliferation measured by the MTT assay showed more than a 3-fold increase in cell number within the scaffolds after 15 days of culture for both pure collagen scaffolds and Col/mHA composite scaffolds. Attractive properties of this composite scaffold include the potential to load the microspheres for drug delivery and the controllability of the pore structure at various length scales. - Highlights: • Mesoporous hydroxyapatite microsphere(mHA) synthesized by spray drying method • Porous collagen/mHA composite scaffold made by freeze

Effect of the addition of collagen in the preparation of hydroxyapatite, aiming the application of pulp capping; Efeito da adicao de colageno na preparacao de hidroxiapatita visando a aplicacao como capeador pulpar

Energy Technology Data Exchange (ETDEWEB)

Ribeiro, Geysy L.; Mendes, Luis C., E-mail: geysylopes@ima.ufrj.br [Instituto de Macromoleculas Professora Eloisa Mano (IMA) - Universidade Federal do Rio de Janeiro, UFRJ. Centro de Tecnologia, RJ (Brazil)

2011-07-01

This work studied the action of collagen (COLL) in the hydroxyapatite (HA) synthesis, produced through sol-gel process, in order to mimetize the chemical composition of dental tissue. The resulting material was characterized by energy dispersive X-ray spectroscopy (EDX), Fourier transform infrared spectroscopy (FT-IR), wide-angle X-ray diffraction (WAXD) and scanning electron microscopy (SEM). The Ca/P ratio was determined through EDX - 1,89 e 2,38, with and without collagen, respectively. The FT-IR analysis showed no significant interaction between the constituents of the composite. The R-ray diffractograms indicated an increase of the resolution and intensity of the HA peak. The photomicrographies showed that the preparation method exhibited significantly influence onto the hydroxyapatite morphology, as well as resulted in a homogeneously dispersed composite. (author)

Development and characterization of poli composites (ether ether ketone)(PEEK)(Hydroxyapatite(HA)

International Nuclear Information System (INIS)

Ferreira, V.P.; Santos, F.S.F.; Sa, M.D. de; Fook, M.V.L.

2016-01-01

The objective of this work was to develop PEEK / HA composites, combining the biological activity of the ceramic phase with the properties of the polymer phase, the materials used in this research were Poly (ether-ether-ketone) (PEEK) and Hydroxyapatite (HA) (50, 60, 70 and 80% m / v HA), this material was subjected to a load of two tons followed by a thermal treatment at 390 ° for a period of 30 minutes. Then they were characterized by FTIR, DRX and MO. In the physical-chemical characterization of FTIR and XRD, it was not possible to identify significant alterations. In the FTIR spectra of the composites, there is no formation of new identifiable chemical bonds. In the composites XRD diffractograms a profile similar to the ceramic phase was observed, with peaks increasing in intensity and narrowing proportional to the increase of the hydroxyapatite concentration in the composites. In optical microscopy it is possible to observe surfaces with heterogeneous morphology, with signs of roughness and in the cross section we observe a heterogeneous aspect, rich in regions with large agglomerates and lighter particles. Considering the processing aspects, the technique proved to be effective for the development of PEEK /HA composites. (author)

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

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L. T. Bang

2014-01-01

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

Synthesis and characterization of 64SiO2-26CaO-5P2O5-5CuO bioactive composition for the growth of hydroxyapatite layer by XRD, Raman and pH studies

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Kaur, Pardeep; Singh, K. J.

2016-05-01

Bioactive sample with the nominal composition of 64SiO2-26CaO-5P2O5-5CuO has been prepared in the laboratory by using the sol-gel technique. The bioactivity of the prepared sample has been analyzed by using the Tris Simulated Body Fluid which has also been prepared in the laboratory. XRD and Raman techniques have been employedto probe the formation of hydroxyapatite layer. pH studies has also been undertaken to check the acidic/non-acidic behavior of sample. Growth of hydroxyapatite layer has been observed after one day on the surface of the sample. Moreover, sample has been observed to be non-acidic in nature.

Development of Antibiotics Impregnated Nanosized Silver Phosphate-Doped Hydroxyapatite Bone Graft

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Waraporn Suvannapruk

2013-01-01

Full Text Available Nanosized Ag3PO4 loaded hydroxyapatite which was prepared by a novel low temperature phosphorization of 3D printed calcium sulfate dihydrate at the nominal silver concentration of 0.001 M and 0.005 M was impregnated by two antibiotics including gentamicin and vancomycin. Phase composition, microstructure, antibiotics loading, silver content, antimicrobial performance, and cytotoxic potential of the prepared samples were characterized. It was found that the fabricated sample consisted of hydroxyapatite as a main phase and spherical-shaped silver phosphate nanoparticles distributing within the cluster of hydroxyapatite crystals. Antibacterial activity of the samples against two bacterial strains (gram negative P. aeruginosa and gram positive S. aureus was carried out. It was found that the combination of antibiotics and nanosized Ag3PO4 in hydroxyapatite could enhance the antibacterial performance of the samples by increasing the duration in which the materials exhibited antibacterial property and the size of the inhibition zone depending on the type of antibiotics and bacterial strains compared to those contained antibiotics or nanosilver phosphate alone. Cytotoxic potential against osteoblasts of antibiotics impregnated nanosilver phosphate hydroxyapatite was found to depend on the combination of antibiotics content, type of antibiotics, and nanosilver phosphate content.

Bioactivity of thermal plasma synthesized bovine hydroxyapatite/glass ceramic composites

International Nuclear Information System (INIS)

Yoganand, C P; Selvarajan, V; Rouabhia, Mahmoud; Cannillo, Valeria; Sola, Antonella

2010-01-01

Bone injuries and failures often require the inception of implant biomaterials. Research in this area is receiving increasing attention worldwide. A variety of artificial bone materials, such as metals, polymeric materials, composites and ceramics, are being explored to replace diseased bones. Calcium phosphate ceramics are currently used as biomaterials for many applications in both dentistry and orthopedics. Bioactive silicate-based glasses show a higher bioactive behaviour than calcium phosphate materials. It is very interesting to study the mixtures of HA and silicate-based glasses. In the present study; natural bovine hydroxyapatite / SiO 2 -CaO-MgO glass composites were produced using the Transferred arc plasma (TAP) melting method. TAP melting route is a brisk process of preparation of glass-ceramics in which the raw materials are melted in the plasma and crystallization of the melt occurs while cooling down at a much faster rate in relatively short processing times compared to the conventional methods of manufacture of glass ceramics/composites. It is well known that; one essential step to the understanding of the biological events occurring at the bone tissue/material interface is the biological investigation by in vitro tests. Cell lines are commonly used for biocompatibility tests, and are very efficient because of their reproducibility and culture facility. In this study, we report the results of a study on the response of primary cultures of human fibroblast cells to TAP melted bioactive glass ceramics.

[Effect of nano-hydroxyapatite to glass ionomer cement].

Science.gov (United States)

Mu, Ya-Bing; Zang, Guang-Xiang; Sun, Hong-Chen; Wang, Cheng-Kun

2007-12-01

To investigate the mechanical character, microleakage and mineralizing potential of nano-hydroxyapatite (nano-HAP)-added glass ionomer cement(GIC). 8% nano-HAP were incorporated into GIC as composite, and pure GIC as control. Both types of material were used to make 20 cylinders respectively in order to detect three-point flexural strength and compressive strength. Class V cavities were prepared in 120 molars extracted for orthodontic treatment, then were filled by two kinds of material. The microleakage at the composite-dentine interface was observed with confocal laser scanning microscope (CLSM) after stained with 1% rhodamin-B-isothiocyanate for 24 hours. Class V cavities were prepared in the molars of 4 healthy dogs, filled with composite, and the same molars in the other side were filled with GIC as control. The teeth were extracted to observe the mineralizing property with polarimetric microscope in 8 weeks after filling. Three-point flexural strength and compressive of nano-HAP-added GIC were increased compared with pure GIC (P nano-HAP-added GIC, while there was no hydroxyapatite crystals formed at the interface of tooth and pure GIC. 8% nano-HAP-added GIC can tightly fill tooth and have mineralizing potential, and can be used as liner or filling material for prevention.

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

Science.gov (United States)

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

Evaluation of the Antimicrobial Activity of Different Antibiotics Enhanced with Silver-Doped Hydroxyapatite Thin Films

Directory of Open Access Journals (Sweden)

Daniela Predoi

2016-09-01

Full Text Available The inhibitory and antimicrobial effects of silver particles have been known since ancient times. In the last few years, a major health problem has arisen due to pathogenic bacteria resistance to antimicrobial agents. The antibacterial activities of new materials including hydroxyapatite (HAp, silver-doped hydroxyapatite (Ag:HAp and various types of antibiotics such as tetracycline (T-HAp and T-Ag:HAp or ciprofloxacin (C-HAp and C-Ag:HAp have not been studied so far. In this study we reported, for the first time, the preparation and characterization of various thin films based on hydroxyapatite and silver-doped hydroxyapatite combined with tetracycline or ciprofloxacin. The structural and chemical characterization of hydroxyapatite and silver-doped hydroxyapatite thin films has been evaluated by X-ray diffraction (XRD and Fourier transform infrared spectroscopy (FTIR. The morphological studies of the HAp, Ag:HAp, T-HAp, T-Ag:HAp, C-HAp and C-Ag:HAp thin solid films were performed using scanning electron microscopy (SEM. In order to study the chemical composition of the coatings, energy dispersive X-ray analysis (EDX and glow discharge optical emission spectroscopy (GDOES measurements have been used, obtaining information on the distribution of the elements throughout the film. These studies have confirmed the purity of the prepared hydroxyapatite and silver-doped hydroxyapatite thin films obtained from composite targets containing Ca10−xAgx(PO46(OH2 with xAg = 0 (HAp and xAg = 0.2 (Ag:HAp. On the other hand, the major aim of this study was the evaluation of the antibacterial activities of ciprofloxacin and tetracycline in the presence of HAp and Ag:HAp thin layers against Staphylococcus aureus and Escherichia coli strains. The antibacterial activities of ciprofloxacin and tetracycline against Staphylococcus aureus and Escherichia coli test strains increased in the presence of HAp and Ag:HAp thin layers.

Preparation and Luminescent Properties of the antibacterial materials of the La3+ Doped Sm3+-Hydroxyapatite

Science.gov (United States)

Lv, Yuguang; Shi, Qi; Jin, Yuling; Ren, Hengxin; Qin, Yushan; Wang, Bo; Song, Shanshan

2018-03-01

In this paper, the La3+-doped Sm3+ hydroxyapatite (La/Sm/HAP) complexes were prepared by a precipitation method. The sample was defined by IR spectra, fluorescence spectra and X ray diffraction analysis et al. The structure of complexes were discussed. The emission wavelength of heat treatment of Sm3+ do not change, but will affect the intensity of the peak Sm3+ luminescence properties and the occupy hydroxyapatite in the lattice Ca( II )and Ca( I ) loci with Sm3+ doped concentration and the proportion of the sintering temperature change and change: The nano hydroxyapatite complex of the La3+ doped samarium obtain the good fluorescence intensity, by La3+ doping content of Sm3+ were hydroxyapatite 6% (La3+, Sm3+ mole ratio) device. The complex of La3+ doped samarium HAP have Stable chemical property, fluorescence property and excellent biological activity. The ligand HAP absorbs energy or captures an electron-hole pair and then transfers it to the lanthanide ions. The catalytic activity influence of the La3+-doped Sm3+hydroxyapatite was discussed, the La/Sm/HAP had excellent antibacterial property, which used as potential biological antibacterial material.

Electrochemical corrosion and bioactivity of Ti-Nb-Sn-hydroxyapatite composites fabricated by pulse current activated sintering.

Science.gov (United States)

Xiaopeng, Wang; Fantao, Kong; Biqing, Han; Yuyong, Chen

2017-11-01

Ti-Nb-Sn-hydroxyapatite (HA) composites were prepared by mechanical alloying for different times (unmilled, 4, 8 and 12h), followed by pulse current activated sintering. The effects of the milling time on the electrochemical corrosion resistance and bioactivity of the sintered Ti-35Nb-2.5Sn-15HA composites were investigated. Potentiodynamic polarization test results indicated that the sintered Ti-35Nb-2.5Sn-15HA composites exhibited higher corrosion resistance with increasing milling time. The corrosion potential and current of the Ti-35Nb-2.5Sn-15HA composite sintered by 12h milled powders were - 0.261V and 0.18μA/cm 2 , respectively, and this sintered composite showed a stable and wide passivation region. The hemolysis rate of the sintered Ti-35Nb-2.5Sn-15HA composites reduced with increasing milling time and the lowest hemolytic rate of the composites was 0.87%. In addition, the in vitro cell culture results indicated that the composite sintered by 12h milled powders had good biocompatibility. These results indicate the significant potential of Ti-35Nb-2.5Sn/xHA composites for biomedical implant applications. Copyright © 2017 Elsevier Ltd. All rights reserved.

Hydroxyapatite-diamondlike carbon nanocomposite films

International Nuclear Information System (INIS)

Narayan, Roger J.

2005-01-01

Hydroxyapatite is a bioactive ceramic that mimics the mineral composition of natural bone. Conventional plasma-sprayed hydroxyapatite coatings demonstrate poor adhesion and poor mechanical integrity. We have developed hydroxyapatite-diamondlike carbon bilayer film. The diamondlike carbon interlayer serves to prevent metal ion release and improve adhesion of the hydroxyapatite film. These films were characterized using X-ray photoelectron spectroscopy, scanning electron microscopy, transmission electron microscopy, X-ray diffraction, Raman spectroscopy, nanoindentation, and microscratch adhesion testing. Based on the results of this study, hydroxyapatite-diamondlike carbon bilayers demonstrate promise for use in several orthopedic implants

Hydroxyapatite-diamondlike carbon nanocomposite films

Energy Technology Data Exchange (ETDEWEB)

Narayan, Roger J. [School of Materials Science and Engineering, Georgia Institute of Technology, Atlanta, GA 30332-0245 (United States)]. E-mail: roger.narayan@mse.gatech.edu

2005-05-15

Hydroxyapatite is a bioactive ceramic that mimics the mineral composition of natural bone. Conventional plasma-sprayed hydroxyapatite coatings demonstrate poor adhesion and poor mechanical integrity. We have developed hydroxyapatite-diamondlike carbon bilayer film. The diamondlike carbon interlayer serves to prevent metal ion release and improve adhesion of the hydroxyapatite film. These films were characterized using X-ray photoelectron spectroscopy, scanning electron microscopy, transmission electron microscopy, X-ray diffraction, Raman spectroscopy, nanoindentation, and microscratch adhesion testing. Based on the results of this study, hydroxyapatite-diamondlike carbon bilayers demonstrate promise for use in several orthopedic implants.

Preparation of bone-implants by coating hydroxyapatite nanoparticles on self-formed titanium dioxide thin-layers on titanium metal surfaces

Energy Technology Data Exchange (ETDEWEB)

Wijesinghe, W.P.S.L.; Mantilaka, M.M.M.G.P.G.; Chathuranga Senarathna, K.G. [Department of Chemistry, Faculty of Science, University of Peradeniya, 20400 Peradeniya (Sri Lanka); Postgraduate Institute of Science, University of Peradeniya, 20400 Peradeniya (Sri Lanka); Herath, H.M.T.U. [Postgraduate Institute of Science, University of Peradeniya, 20400 Peradeniya (Sri Lanka); Department of Medical Laboratory Science, Faculty of Allied Health Sciences, University of Peradeniya, 20400 Peradeniya (Sri Lanka); Premachandra, T.N. [Department of Veterinary Pathobiology, Faculty of Veterinary Medicine, University of Peradeniya, 20400 Peradeniya (Sri Lanka); Ranasinghe, C.S.K. [Department of Chemistry, Faculty of Science, University of Peradeniya, 20400 Peradeniya (Sri Lanka); Postgraduate Institute of Science, University of Peradeniya, 20400 Peradeniya (Sri Lanka); Rajapakse, R.P.V.J. [Postgraduate Institute of Science, University of Peradeniya, 20400 Peradeniya (Sri Lanka); Department of Veterinary Pathobiology, Faculty of Veterinary Medicine, University of Peradeniya, 20400 Peradeniya (Sri Lanka); Rajapakse, R.M.G., E-mail: rmgr@pdn.ac.lk [Department of Chemistry, Faculty of Science, University of Peradeniya, 20400 Peradeniya (Sri Lanka); Postgraduate Institute of Science, University of Peradeniya, 20400 Peradeniya (Sri Lanka); Edirisinghe, Mohan; Mahalingam, S. [Department of Mechanical Engineering, University College London, London WC1E 7JE (United Kingdom); Bandara, I.M.C.C.D. [School of Chemistry, Physics and Mechanical Engineering, Queensland University of Technology, 2 George Street, Brisbane 4001, QLD (Australia); Singh, Sanjleena [Central Analytical Research Facility, Institute of Future Environments, Queensland University of Technology, 2 George Street, Brisbane 4001, QLD (Australia)

2016-06-01

Preparation of hydroxyapatite coated custom-made metallic bone-implants is very important for the replacement of injured bones of the body. Furthermore, these bone-implants are more stable under the corrosive environment of the body and biocompatible than bone-implants made up of pure metals and metal alloys. Herein, we describe a novel, simple and low-cost technique to prepare biocompatible hydroxyapatite coated titanium metal (TiM) implants through growth of self-formed TiO{sub 2} thin-layer (SFTL) on TiM via a heat treatment process. SFTL acts as a surface binder of HA nanoparticles in order to produce HA coated implants. Colloidal HA nanorods prepared by a novel surfactant-assisted synthesis method, have been coated on SFTL via atomized spray pyrolysis (ASP) technique. The corrosion behavior of the bare and surface-modified TiM (SMTiM) in a simulated body fluid (SBF) medium is also studied. The highest corrosion rate is found to be for the bare TiM plate, but the corrosion rate has been reduced with the heat-treatment of TiM due to the formation of SFTL. The lowest corrosion rate is recorded for the implant prepared by heat treatment of TiM at 700 °C. The HA-coating further assists in the passivation of the TiM in the SBF medium. Both SMTiM and HA coated SMTiM are noncytotoxic against osteoblast-like (HOS) cells and are in high-bioactivity. The overall production process of bone-implant described in this paper is in high economic value. - Highlights: • Colloidal hydroxyapatite nanorods are prepared by a novel method. • Surfaces of titanium metal plates are modified by self-forming TiO{sub 2} thin-films. • Prostheses are prepared by coating hydroxyapatite on surface modified Ti metal. • Bioactivity and noncytotoxicity are increased with surface modifications.

Preparation of bone-implants by coating hydroxyapatite nanoparticles on self-formed titanium dioxide thin-layers on titanium metal surfaces

International Nuclear Information System (INIS)

Wijesinghe, W.P.S.L.; Mantilaka, M.M.M.G.P.G.; Chathuranga Senarathna, K.G.; Herath, H.M.T.U.; Premachandra, T.N.; Ranasinghe, C.S.K.; Rajapakse, R.P.V.J.; Rajapakse, R.M.G.; Edirisinghe, Mohan; Mahalingam, S.; Bandara, I.M.C.C.D.; Singh, Sanjleena

2016-01-01

Preparation of hydroxyapatite coated custom-made metallic bone-implants is very important for the replacement of injured bones of the body. Furthermore, these bone-implants are more stable under the corrosive environment of the body and biocompatible than bone-implants made up of pure metals and metal alloys. Herein, we describe a novel, simple and low-cost technique to prepare biocompatible hydroxyapatite coated titanium metal (TiM) implants through growth of self-formed TiO_2 thin-layer (SFTL) on TiM via a heat treatment process. SFTL acts as a surface binder of HA nanoparticles in order to produce HA coated implants. Colloidal HA nanorods prepared by a novel surfactant-assisted synthesis method, have been coated on SFTL via atomized spray pyrolysis (ASP) technique. The corrosion behavior of the bare and surface-modified TiM (SMTiM) in a simulated body fluid (SBF) medium is also studied. The highest corrosion rate is found to be for the bare TiM plate, but the corrosion rate has been reduced with the heat-treatment of TiM due to the formation of SFTL. The lowest corrosion rate is recorded for the implant prepared by heat treatment of TiM at 700 °C. The HA-coating further assists in the passivation of the TiM in the SBF medium. Both SMTiM and HA coated SMTiM are noncytotoxic against osteoblast-like (HOS) cells and are in high-bioactivity. The overall production process of bone-implant described in this paper is in high economic value. - Highlights: • Colloidal hydroxyapatite nanorods are prepared by a novel method. • Surfaces of titanium metal plates are modified by self-forming TiO_2 thin-films. • Prostheses are prepared by coating hydroxyapatite on surface modified Ti metal. • Bioactivity and noncytotoxicity are increased with surface modifications.

Onlay bone augmentation on mouse calvarial bone using a hydroxyapatite/collagen composite material with total blood or platelet-rich plasma.

Science.gov (United States)

Ohba, Seigo; Sumita, Yoshinori; Umebayashi, Mayumi; Yoshimura, Hitoshi; Yoshida, Hisato; Matsuda, Shinpei; Kimura, Hideki; Asahina, Izumi; Sano, Kazuo

2016-01-01

The aim of this study was to assess newly formed onlay bone on mouse calvarial bone using a new artificial bone material, a hydroxyapatite/collagen composite, with total blood or platelet-rich plasma. The hydroxyapatite/collagen composite material with normal saline, total blood or platelet-rich plasma was transplanted on mouse calvarial bone. The mice were sacrificed and the specimens were harvested four weeks after surgery. The newly formed bone area was measured on hematoxylin and eosin stained specimens using Image J software. The hydroxyapatite/collagen composite materials with total blood or platelet-rich plasma induced a significantly greater amount of newly formed bone than that with normal saline. Moreover, bone marrow was observed four weeks after surgery in the transplanted materials with total blood or platelet-rich plasma but not with normal saline. However, there were no significant differences in the amount of newly formed bone between materials used with total blood versus platelet-rich plasma. The hydroxyapatite/collagen composite material was valid for onlay bone augmentation and this material should be soaked in total blood or platelet-rich plasma prior to transplantation. Copyright © 2015 Elsevier Ltd. All rights reserved.

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

Science.gov (United States)

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.

Electrochemical performance of an air-breathing direct methanol fuel cell using poly(vinyl alcohol)/hydroxyapatite composite polymer membrane

Science.gov (United States)

Yang, Chun-Chen; Chiu, Shwu-Jer; Lin, Che-Tseng

A novel composite polymer membrane based on poly(vinyl alcohol)/hydroxyapatite (PVA/HAP) was successfully prepared by a solution casting method. The characteristic properties of the PVA/HAP composite polymer membranes were examined by thermal gravimetric analysis (TGA), X-ray diffraction (XRD), scanning electron microscopy (SEM), micro-Raman spectroscopy and AC impedance method. An air-breathing DMFC, comprised of an air cathode electrode with MnO 2/BP2000 carbon inks on Ni-foam, an anode electrode with PtRu black on Ti-mesh, and the PVA/HAP composite polymer membrane, was assembled and studied. It was found that this alkaline DMFC showed an improved electrochemical performance at ambient temperature and pressure; the maximum peak power density of an air-breathing DMFC in 8 M KOH + 2 M CH 3OH solution is about 11.48 mW cm -2. From the application point of view, these composite polymer membranes show a high potential for the DMFC applications.

Electrochemical performance of an air-breathing direct methanol fuel cell using poly(vinyl alcohol)/hydroxyapatite composite polymer membrane

Energy Technology Data Exchange (ETDEWEB)

Yang, Chun-Chen; Chiu, Shwu-Jer; Lin, Che-Tseng [Department of Chemical Engineering, Mingchi University of Technology, Taipei Hsien 243 (China)

2008-02-15

A novel composite polymer membrane based on poly(vinyl alcohol)/hydroxyapatite (PVA/HAP) was successfully prepared by a solution casting method. The characteristic properties of the PVA/HAP composite polymer membranes were examined by thermal gravimetric analysis (TGA), X-ray diffraction (XRD), scanning electron microscopy (SEM), micro-Raman spectroscopy and AC impedance method. An air-breathing DMFC, comprised of an air cathode electrode with MnO{sub 2}/BP2000 carbon inks on Ni-foam, an anode electrode with PtRu black on Ti-mesh, and the PVA/HAP composite polymer membrane, was assembled and studied. It was found that this alkaline DMFC showed an improved electrochemical performance at ambient temperature and pressure; the maximum peak power density of an air-breathing DMFC in 8 M KOH + 2 M CH{sub 3}OH solution is about 11.48 mW cm{sup -2}. From the application point of view, these composite polymer membranes show a high potential for the DMFC applications. (author)

Adhesion of composite carbon/hydroxyapatite coatings on AISI 316L medical steel

Directory of Open Access Journals (Sweden)

J. Gawroński

2009-07-01

Full Text Available In this paper are contains the results of studies concerning the problems associated with increased of hydroxyapatite (HAp adhesion, manufactured by using Pulse Laser Deposition (PLD method, to the austenitic steel (AISI 316L through the coating of carbon interlayer on it. Carbon coating was deposited by Radio Frequency Plasma Assisted Chemical Vapour Deposition (RF PACVD method.Test results unequivocally showed that the intermediate carbon layer in a determined manner increase the adhesion of hydroxyapatite to the metallic substrate. Obtained results give rise to deal with issues of manufacturing composite bilayer – carbon film/HAp – on ready implants, casted from austenitic cast steel by lost-wax process method as well as in gypsum forms.

XPS and XANES studies of biomimetic composites based on B-type nano-hydroxyapatite

Science.gov (United States)

Goloshchapov, D. L.; Gushchin, M. S.; Kashkarov, V. M.; Seredin, P. V.; Ippolitov, Y. A.; Khmelevsky, N. O.; Aksenenko, A. Yu.

2018-06-01

The paper presents an investigation of the local atomic structure of nanocrystalline carbonate-substituted hydroxyapatite (CHAP) contained in biomimetic composites - analogues of intact human tooth tissues. Using the XPS technique, the presence of impurity Mg and F atoms and structurally bound carbon in CHAP, at the concentrations typical of apatite enamel and dentine was determined. The XANES method was used to study the changes occurring in P L2,3 spectra of biocomposites with CHAP, depending on the percentage of the amino acid matrix. The appearance of maxima in the spectra of XANES P L2,3 near 135.7 eV for the samples with the composition of amino acid complex/hydroxyapatite - 5/95, 25/75 and the splitting of a broad peak of 146.9 eV in the spectrum of a biocomposite with a composition of 40/60 indicates at the interaction of molecular complex of amino acids with atomic environment of phosphorus. This fact can be used in the fundamental medicine for synthesizing of new biomaterials in dentistry.

Effects of sterilisation by high-energy radiation on biomedical poly-(epsilon-caprolactone)/hydroxyapatite composites.

Science.gov (United States)

Di Foggia, Michele; Corda, Ugo; Plescia, Elena; Taddei, Paola; Torreggiani, Armida

2010-06-01

The effects of a high energy sterilization treatment on poly-epsilon-caprolactone/carbonated hydroxyapatite composites have been investigated. Poly-epsilon-caprolactone is a biodegradable polymer used as long-term bioresorbable scaffold for bone tissue engineering and carbonated hydroxyapatite is a bioactive material able to promote bone growth. The composites were gamma-irradiated in air or under nitrogen atmosphere with doses ranging from 10 to 50 kGy (i.e. to a value higher than that recommended for sterilization). The effects of the irradiation treatment were evaluated by vibrational spectroscopy (IR and Raman spectroscopies) coupled to thermal analysis (Differential Scanning Calorimetry and Thermogravimetry) and Electron Paramagnetic Resonance spectroscopy. Irradiation with the doses required for sterilization induced acceptable structural changes and damaging effects: only a very slight fragmentation of the polymeric chains and some defects in the inorganic component were observed. Moreover, the radiation sensitivity of the composites proved almost the same under the two different atmospheres.

Continuous microwave flow synthesis of mesoporous hydroxyapatite

International Nuclear Information System (INIS)

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

2015-01-01

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 2.45 GHz 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. - Highlights: • Continuous microwave flow synthesis method was used to prepare hydroxyapatite. • Increase in microwave power enhanced the degree of crystallinity. • TEM images confirmed the presence of mesopores on the surface of HA

Continuous microwave flow synthesis of mesoporous hydroxyapatite

Energy Technology Data Exchange (ETDEWEB)

Akram, Muhammad; Alshemary, Ammar Z.; Goh, Yi-Fan; Wan Ibrahim, Wan Aini [Department of Chemistry, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor (Malaysia); Lintang, Hendrik O. [Centre for Sustainable Nanomaterials (CSNano), Ibnu Sina Institute for Scientific and Industrial Research, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor (Malaysia); Hussain, Rafaqat, E-mail: rafaqat@kimia.fs.utm.my [Centre for Sustainable Nanomaterials (CSNano), Ibnu Sina Institute for Scientific and Industrial Research, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor (Malaysia)

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 2.45 GHz 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{sup 2+} ion released in SBF solution. - Highlights: • Continuous microwave flow synthesis method was used to prepare hydroxyapatite. • Increase in microwave power enhanced the degree of crystallinity. • TEM images confirmed the presence of mesopores on the surface of HA.

Greener synthesis of electrospun collagen/hydroxyapatite composite fibers with an excellent microstructure for bone tissue engineering

Directory of Open Access Journals (Sweden)

Zhou YY

2015-04-01

Full Text Available Yuanyuan Zhou,1,2 Hongchang Yao,1 Jianshe Wang,1 Dalu Wang,1 Qian Liu,1 Zhongjun Li11College of Chemistry and Molecular Engineering, Zhengzhou University, Zhengzhou, People’s Republic of China; 2Institute of Enviromental and Municipal Engineering, North China University of Water Resources and Electric Power, Zhengzhou, People’s Republic of ChinaAbstract: In bone tissue engineering, collagen/hydroxyapatite (HAP fibrous composite obtained via electrospinning method has been demonstrated to support the cells’ adhesion and bone regeneration. However, electrospinning of natural collagen often requires the use of cytotoxic organic solvents, and the HAP crystals were usually aggregated and randomly distributed within a fibrous matrix of collagen, limiting their clinical potential. Here, an effective and greener method for the preparation of collagen/HAP composite fibers was developed for the first time, and this green product not only had 40 times higher mechanical properties than that previously reported, but also had an excellent microstructure similar to that of natural bone. By dissolving type I collagen in environmentally friendly phosphate buffered saline/ethanol solution instead of the frequently-used cytotoxic organic solvents, followed with the key step of desalination, co-electrospinning the collagen solution with the HAP sol, generates a collagen/HAP composite with a uniform and continuous fibrous morphology. Interestingly, the nano-HAP needles were found to preferentially orient along the longitudinal direction of the collagen fibers, which mimicked the nanostructure of natural bones. Based on the characterization of the related products, the formation mechanism for this novel phenomenon was proposed. After cross-linking with 1-ethyl-3-(3-dimethyl-aminopropyl-1-carbodiimide hydrochloride/N-hydroxysuccinimide, the obtained composite exhibited a significant enhancement in mechanical properties. In addition, the biocompatibility of the

Minocycline-released hydroxyapatite-gelatin nanocomposite and its cytocompatibility in vitro

Energy Technology Data Exchange (ETDEWEB)

Dou Xiaochen; Zhu Xiaopeng; Zhou Jian; Cai Huaqiong; Li Quanli [Key Laboratory of Oral Disease Research of Anhui Province, Stomatologic Hospital and Collage, Anhui Medical University, Hefei (China); Tang Jian, E-mail: ql-li@126.com [Department of Orthopedic Surgery, The First Hospital of Anhui Medical University, Hefei (China)

2011-04-15

The incorporation of antibacterial agents into biomaterials is extremely desirable for repairing bone defects. Minocycline, a semi-synthetic tetracycline antibiotic, is active against aerobic, anaerobic, Gram-positive and Gram-negative bacteria, and can enhance bone formation, decrease connective tissue breakdown and diminish bone resorption. In this study, a novel minocycline-releasing biomaterial was synthesized using a biomimetic method. A measured amount of an acidic hydroxyapatite and minocycline solution was respectively added to a gelatin solution and kept at 40 deg. C and pH 7-8 for 2 h. The mixture was aged overnight, lyophilized and a hydroxyapatite-gelatin-minocycline composite was obtained. The composite was co-cultured with rat bone marrow stromal cells (BMSCs) in vitro. Our results show that nanohydroxyapatite was distributed evenly in the fibrils of the gelatin. Minocycline was incorporated into the composite and could be released from the composite particles slowly over 2 weeks in vitro. The composite promoted BMSC adhesion, proliferation and differentiation in vitro. The approach described here may provide a basis for the preparation of an antibacterial biomaterial for bone regeneration.

Minocycline-released hydroxyapatite-gelatin nanocomposite and its cytocompatibility in vitro

International Nuclear Information System (INIS)

Dou Xiaochen; Zhu Xiaopeng; Zhou Jian; Cai Huaqiong; Li Quanli; Tang Jian

2011-01-01

The incorporation of antibacterial agents into biomaterials is extremely desirable for repairing bone defects. Minocycline, a semi-synthetic tetracycline antibiotic, is active against aerobic, anaerobic, Gram-positive and Gram-negative bacteria, and can enhance bone formation, decrease connective tissue breakdown and diminish bone resorption. In this study, a novel minocycline-releasing biomaterial was synthesized using a biomimetic method. A measured amount of an acidic hydroxyapatite and minocycline solution was respectively added to a gelatin solution and kept at 40 deg. C and pH 7-8 for 2 h. The mixture was aged overnight, lyophilized and a hydroxyapatite-gelatin-minocycline composite was obtained. The composite was co-cultured with rat bone marrow stromal cells (BMSCs) in vitro. Our results show that nanohydroxyapatite was distributed evenly in the fibrils of the gelatin. Minocycline was incorporated into the composite and could be released from the composite particles slowly over 2 weeks in vitro. The composite promoted BMSC adhesion, proliferation and differentiation in vitro. The approach described here may provide a basis for the preparation of an antibacterial biomaterial for bone regeneration.

Physical-mechanical characterization of hydroxyapatite-titanium oxide composites made by the polymeric sponge method

International Nuclear Information System (INIS)

Galdino, A.G.S.; Zavaglia, C.A.C.

2011-01-01

Bioceramics have been used as bone reconstruction materials since last decades, where hydroxyapatite is one of the most used for this purpose. However, hydroxyapatite's mechanical strength is not so high when compared to other bioceramics. This work aimed on characterizing physically and mechanically composites of HA-TiO_2. Samples were made by the polymeric sponge method with 70% - 30% wt., 60% - 40% wt. and 50% - 50% wt. of HA - TiO_2, calcined at 550 deg C for sponge burning and sintered at 1250 deg C, 1300 deg C and 1350 deg C. Samples were submitted to mechanical essays of compression and Hardness Vickers and to physical essays of water absorption, apparent density, burning linear retraction and apparent density. Results showed relatively better than those of pure hydroxyapatite and they are in accordance with the literature. (author)

Polymer-Ceramic Composite Scaffolds: The Effect of Hydroxyapatite and β-tri-Calcium Phosphate

OpenAIRE

Boyang Huang; Guilherme Caetano; Cian Vyas; Jonny James Blaker; Carl Diver; Paulo Bártolo

2018-01-01

The design of bioactive scaffolds with improved mechanical and biological properties is an important topic of research. This paper investigates the use of polymer-ceramic composite scaffolds for bone tissue engineering. Different ceramic materials (hydroxyapatite (HA) and β-tri-calcium phosphate (TCP)) were mixed with poly-ε-caprolactone (PCL). Scaffolds with different material compositions were produced using an extrusion-based additive manufacturing system. The produced scaffolds were physi...

[Biomimetic nanohydroxyapatite/gelatin composite material preparation and in vitro study].

Science.gov (United States)

Li, Siriguleng; Hu, Xiaowen

2014-09-01

To prepare nHA/gelatin porous scaffold and to evaluate its physical and chemical properties and biocompatibility. We used nano-powders of HA and gelatin to prepare 3D porous composite scaffold by freeze-drying technique, and used scanning electron microscope, fourier transform infrared spectroscopy and universal testing machine to characterize the composite material. Osteoblasts were primarily cultured, and the third-passage osteoblasts were co-cultured with the composite material. The cell adhesion and morphology were examined under scanning electron microscope. The cell viability analysis was performed by MTT assay, and the alkaline phosphatase activity was measured with alkaline phosphatase kit. Scanning electron microscope showed that the scaffold possessed a 3-dimensional interconnected homogenous porous structure with pore sizes ranging from 150 to 400 μm. Fourier transform infrared spectroscopy showed that the composite material had a strong chemical bond between the inorganic phase and organic phase. The scaffold presented the compressive strength of (3.28 ± 0.51) MPa and porosities of (80.6 ± 4.1)%. Composite materials showed features of had good biocompatibility. Mouse osteoblasts were well adhered and spread on the materials. The grade of the cell toxicity ranged from I to II. On the 5th and 7th day the proliferative rate of osteoblasts on scaffolds in the composite materials was significantly higher than that in the control group. The activity of alkaline phosphatase was obviously higher than that in the control group on Day 1 and 3. Nano-hydroxyapatite and gelatin in certain proportions and under certain conditions can be prepared into a composite biomimetic porous scaffolds with high porosity and three-dimensional structure using freeze-drying method. The scaffold shows good biocompatibility with mouse osteoblasts and may be a novel scaffolds for bone tissue engineering.

A novel squid pen chitosan/hydroxyapatite/β-tricalcium phosphate composite for bone tissue engineering

Energy Technology Data Exchange (ETDEWEB)

Shavandi, Amin, E-mail: amin.shavandi@postgrad.otago.ac.nz [Department of Food Sciences, University of Otago, Dunedin (New Zealand); Department of Applied Sciences, University of Otago, Dunedin (New Zealand); Bekhit, Alaa El-Din A. [Department of Food Sciences, University of Otago, Dunedin (New Zealand); Sun, Zhifa; Ali, Azam [Department of Physics, University of Otago, Dunedin (New Zealand); Gould, Maree [Department of Anatomy, University of Otago, Dunedin (New Zealand)

2015-10-01

Squid pen chitosan was used in the fabrication of biocomposite scaffolds for bone tissue engineering. Hydroxyapatite (HA) and beta-tricalcium phosphate (β-TCP) obtained from waste mussel shells were used as the calcium phosphate source. The composite was prepared using 2.5% tripolyphosphate (TPP) and 1% glycerol as a cross-linker and plasticizer, respectively. The weight percent (wt.%) ratios of the ceramic components in the composite were 20/10/70, 30/20/50 and 40/30/30 (HA/β-TCP/Chi). The biodegradation rate and structural properties of the scaffolds were investigated. Scanning electron microscopy (SEM) and microCT(μCT) results indicated that the composites have a well defined lamellar structure with an average pore size of 200 μm. The porosity of the composites decreased from 88 to 56% by increasing the ratio of HA/β-TCP from 30 to 70%. After 28 days of incubation in a physiological solution, the scaffolds were degraded by approximately 30%. In vitro investigations showed that the composites were cytocompatible and supported the growth of L929 and Saos-2 cells. The obtained data suggests that the squid pen chitosan composites are potential candidates for bone regeneration. - Highlights: • Biocomposite scaffolds were made from mussel shells HA and β-TCP, and squid pin chitosan. • The porosity of the composites decreased with an increase in HA/β-TCP ratio. • Composites were cytocompatible and supported the growth of L929 and Saos-2 cells. • Composite containing 50% HA and β-TCP had the best mechanical properties.

Preparation and characterization of chitosan-natural nano hydroxyapatite-fucoidan nanocomposites for bone tissue engineering.

Science.gov (United States)

Lowe, Baboucarr; Venkatesan, Jayachandran; Anil, Sukumaran; Shim, Min Suk; Kim, Se-Kwon

2016-12-01

Solid three dimensional (3D) composite scaffolds for bone tissue engineering were prepared using the freeze-drying method. The scaffolds were composed of chitosan, natural nano-hydroxyapatite (nHA) and fucoidan in the following combinations: chitosan, chitosan-fucoidan, chitosan-nHA, and chitosan-nHA-fucoidan. Fourier transform infrared spectroscopy (FT-IR), thermal gravimetric analysis (TGA), X-ray diffraction analysis (XRD), scanning electron microscopy (SEM), and optical microscopy (OM) were used to determine the physiochemical constituents and the morphology of the scaffolds. The addition of nHA into the chitosan-fucoidan composite scaffold reduced the water uptake and water retention. FT-IR analysis confirmed the presence of a phosphate group in the chitosan-nHA-fucoidan scaffold. This group is present because of the presence of nHA (isolated via alkaline hydrolysis from salmon fish bones). Microscopic results indicated that the dispersion of nHA and fucoidan in the chitosan matrix was uniform with a pore size of 10-400μm. The composite demonstrated a suitable micro architecture for cell growth and nutrient supplementation. This compatibility was further elucidated in vitro using periosteum-derived mesenchymal stem cells (PMSCs). The cells demonstrated high biocompatibility and excellent mineralization for the chitosan-nHA-fucoidan scaffold. We believe that a chitosan-nHA-fucoidan composite is a promising biomaterial for the scaffold that can be used for bone tissue regeneration. Copyright © 2016 Elsevier B.V. All rights reserved.

Hydroxyapatite nanocrystals: simple preparation, characterization and formation mechanism.

Science.gov (United States)

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. Copyright © 2014 Elsevier B.V. All rights reserved.

Study of sorption processes of strontium on the synthetic hydroxyapatite

International Nuclear Information System (INIS)

Rosskopfova, O.; Galambos, M.; Rajec, P.

2011-01-01

The sorption of strontium on synthetic hydroxyapatite was investigated using batch method and radiotracer technique. The hydroxyapatite samples were prepared by a wet precipitation process followed by calcination of calcium phosphate that precipitated from aqueous solution. Also, commercial hydroxyapatites were used. The sorption of strontium on hydroxyapatite depended on the method of preparation and it was pH independent ranging from 4 to 9 as a result of buffering properties of hydroxyapatite. The distribution coefficient K d was significantly decreased with increasing concentration of Sr 2+ and Ca 2+ ions in solution with concentration above 1 x 10 -3 mol dm -3 . The percentage strontium sorption for commercial and by wet method prepared hydroxyapatite was in the range of 83-96%, while calcined hydroxyapatite was ranging from 10 to 30%. The experimental data for sorption of strontium have been interpreted in the term of Langmuir isotherm. The sorption of Sr 2+ ions was performed by ion-exchange with Ca 2+ cations on the crystal surface of hydroxyapatite. Although calcined hydroxyapatite is successfully used as biomaterial for hard tissues repair, it is not used for the treatment of liquid wastes. (author)

Improved osteoblasts growth on osteomimetic hydroxyapatite/BaTiO_3 composites with aligned lamellar porous structure

International Nuclear Information System (INIS)

Liu, Beilei; Chen, Liangjian; Shao, Chunsheng; Zhang, Fuqiang; Zhou, Kechao; Cao, Jun; Zhang, Dou

2016-01-01

Osteoblasts growing into bone substitute is an important step of bone regeneration. This study prepared porous hydroxyapatite (HA)/BaTiO_3 piezoelectric composites with porosity of 40%, 50% and 60% by ice-templating method. Effects of HA/BaTiO_3 composites with different porosities, with and without polarizing treatment on adhesion, proliferation and differentiation of osteoblasts were investigated in vitro. Results revealed that cell densities of the porous groups were significantly higher than those of the dense group (p 0.05). The absence of mechanical loading on the polarized samples may account for this. The results indicated that hierarchically porous HA/BaTiO_3 played a favorable part in osteoblasts proliferation, differentiation and adhesion process and is a promising bone substitute material. - Graphical abstract: Aligned porous structure of HA/BaTiO_3 piezoelectric composites prepared by ice-templating method was similar to the lamellar Haversian system in bone tissue. When co-cultured with human osteosarcoma cells (MG63), porous HA/BaTiO_3 composites exhibited remarkable biological activity in promoting proliferation, differentiation and adhesion of MG63 cells. - Highlights: • The aligned porous structure of HA/BaTiO_3 composite was similar to the lamellar Haversian system in bone tissue. • The piezoelectric d_3_3 coefficient of HA/BaTiO_3 with porosity of 50% was 5.0 pC/N, much higher than that of natural bone. • HA/BaTiO_3 with porosity of 50% promoted proliferation, differentiation and adhesion of MG63 cells remarkably.

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

Science.gov (United States)

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.

Composite biomaterials with chemical bonding between hydroxyapatite filler particles and PEG/PBT copolymer matrix

NARCIS (Netherlands)

Liu, Qing; de Wijn, J.R.; van Blitterswijk, Clemens

1998-01-01

In an effort to make composites from hydroxyapatite and a PEG/PBT copolymer (PolyactiveTM 70/30), chemical linkages were introduced between the filler particles and polymer matrix using hexamethylene diisocyanate as a coupling agent. Infrared spectra (IR) and thermal gravimetric analysis (TGA)

Mechanical properties and in vivo study of modified-hydroxyapatite/polyetheretherketone biocomposites

Energy Technology Data Exchange (ETDEWEB)

Ma, Rui [College of Chemistry and Environmental Engineering, Shenzhen University, Shenzhen 518060, China, (China); Li, Qiankuan [Harbin Institute of Technology Shenzhen Graduate School, Shenzhen 518060 (China); Wang, Lin, E-mail: wanglinhitsz@163.com [Shenzhen Institute of Geriatrics, Shenzhen 518020 (China); Zhang, Xianghua [College of Chemistry and Environmental Engineering, Shenzhen University, Shenzhen 518060, China, (China); Laboratory of Glasses and Ceramics, Institute of Chemical Science, University of Rennes 1, Rennes 35042 (France); Fang, Lin; Luo, Zhongkuan; Xue, Bai [College of Chemistry and Environmental Engineering, Shenzhen University, Shenzhen 518060, China, (China); Ma, Lei, E-mail: leima@szu.edu.cn [College of Chemistry and Environmental Engineering, Shenzhen University, Shenzhen 518060, China, (China)

2017-04-01

Polyether ether ketone (PEEK) has received much attention for its excellent mechanical properties and biocompatibility. Here, the silane coupling agent KH560 [γ-(2,3-epoxypropoxy)propyltrimethoxysilane] is used for graft modification of bioactive HA (hydroxyapatite) particles and for preparing HA/PEEK composites via a hot-press molding method. The prepared HA/PEEK composites were tested for their mechanical properties with SEM (scanning electron microscopy), infrared spectroscopy, and thermo-analysis. The results show that silane coupling KH-560 modifies HA successfully and that the tensile strengths of HA/PEEK and m-HA/PEEK composites indicate an increasing and then a decreasing tendency with increasing HA contents. The non-modified HA/PEEK composites display the same trend as the modified specimens with lower tensile strength and consist of sharp points. When the HA content is 5 wt.%, the tensile strength of m-HA/PEEK composite reaches its maximum, which is 23% higher than that of pure PEEK specimens. The in vivo experiments of m-HA/PEEK used a biomechanical push-out test, SEM, optical microscopy, and an Image-Pro Express C image analysis system. The growth of the bone tissues around the m-HA/PEEK composites with an HA content of 5 wt.% is better than that of specimens with different HA contents. This finding shows the nano-scale effect of the bioactive filler HA in PEEK substrates, which obviously contributes to the growth of the surrounding bone issues in vivo. This study could provide theoretical support for the further promotion and application of high-performance engineering plastics such as PEEK in biomedical fields. - Highlight: • The modification of hydroxyapatite with KH-560 can increase the efficient dispersion of hydroxyapatite in PEEK substrates. • When the HA content is 5 wt. %, the tensile strength of modified-HA/PEEK composite reaches its maximum. • The nano-scale effect of HA fillers in PEEK substrates contributes to the growth of the

Mechanical properties and in vivo study of modified-hydroxyapatite/polyetheretherketone biocomposites

International Nuclear Information System (INIS)

Ma, Rui; Li, Qiankuan; Wang, Lin; Zhang, Xianghua; Fang, Lin; Luo, Zhongkuan; Xue, Bai; Ma, Lei

2017-01-01

Polyether ether ketone (PEEK) has received much attention for its excellent mechanical properties and biocompatibility. Here, the silane coupling agent KH560 [γ-(2,3-epoxypropoxy)propyltrimethoxysilane] is used for graft modification of bioactive HA (hydroxyapatite) particles and for preparing HA/PEEK composites via a hot-press molding method. The prepared HA/PEEK composites were tested for their mechanical properties with SEM (scanning electron microscopy), infrared spectroscopy, and thermo-analysis. The results show that silane coupling KH-560 modifies HA successfully and that the tensile strengths of HA/PEEK and m-HA/PEEK composites indicate an increasing and then a decreasing tendency with increasing HA contents. The non-modified HA/PEEK composites display the same trend as the modified specimens with lower tensile strength and consist of sharp points. When the HA content is 5 wt.%, the tensile strength of m-HA/PEEK composite reaches its maximum, which is 23% higher than that of pure PEEK specimens. The in vivo experiments of m-HA/PEEK used a biomechanical push-out test, SEM, optical microscopy, and an Image-Pro Express C image analysis system. The growth of the bone tissues around the m-HA/PEEK composites with an HA content of 5 wt.% is better than that of specimens with different HA contents. This finding shows the nano-scale effect of the bioactive filler HA in PEEK substrates, which obviously contributes to the growth of the surrounding bone issues in vivo. This study could provide theoretical support for the further promotion and application of high-performance engineering plastics such as PEEK in biomedical fields. - Highlight: • The modification of hydroxyapatite with KH-560 can increase the efficient dispersion of hydroxyapatite in PEEK substrates. • When the HA content is 5 wt. %, the tensile strength of modified-HA/PEEK composite reaches its maximum. • The nano-scale effect of HA fillers in PEEK substrates contributes to the growth of the

Evaluating morphology and mechanical properties of glass-reinforced natural hydroxyapatite composites.

Science.gov (United States)

Yazdanpanah, Z; Bahrololoom, M E; Hashemi, B

2015-01-01

Hydroxyapatite has been used in a wide variety of biomedical applications and it can be produced from natural resources such as bovine bone. This material does not have acceptable mechanical properties by itself. In the present work, hydroxyapatite composites with different weight percentages of sodalime glass were made and sintered at different temperatures (800-1200°C). Eventually the properties such as density, micro hardness, compressive strength and wear of specimens were evaluated. Specific percentages of glass additive increased the density and hardness of specimens due to increasing the sintering temperature. The hardness and density of specimens were decreased with higher percentage of glass additive. Moreover, the results of compressive test showed that increasing the glass addition increases the compressive performance. Furthermore, the SEM micrographs on worn specimens showed that the mechanism of wear was abrasive. Copyright © 2014 Elsevier Ltd. All rights reserved.

A novel electrospun silk fibroin/hydroxyapatite hybrid nanofibers

International Nuclear Information System (INIS)

Ming, Jinfa; Zuo, Baoqi

2012-01-01

A novel electrospinning of silk fibroin/hydroxyapatite hybrid nanofibers with different composition ratios was performed with methanoic acid as a spinning solvent. The silk fibroin/hydroxyapatite hybrids containing up to 30% hydroxyapatite nanoparticles could be electrospun into the continuous fibrous structure. The electrospun silk fibroin/hydroxyapatite hybrid nanofibers showed bigger diameter and wider diameter distribution than pure silk fibroin nanofibers, and the average diameter gradually increased from 95 to 582 nm. At the same time, the secondary structure of silk fibroin/hydroxyapatite nanofibers was characterized by X-ray diffraction, Fourier transform infrared analysis, and DSC measurement. Comparing with the pure silk fibroin nanofibers, the crystal structure of silk fibroin was mainly amorphous structure in the hybrid nanofibers. X-ray diffraction results demonstrated the hydroxyapatite crystalline nature remained as evidenced from the diffraction planes (002), (211), (300), and (202) of the hydroxyapatite crystallites, which was also confirmed by Fourier transform infrared analysis. The thermal behavior of hybrid nanofibers exhibited the endothermic peak of moisture evaporation ranging from 86 to 113 °C, and the degradation peak at 286 °C appeared. The SF/HAp nanofibers mats containing 30% HAp nanoparticles showed higher breaking tenacity and extension at break for 1.1688 ± 0.0398 MPa and 6.55 ± 1.95%, respectively. Therefore, the electrospun silk fibroin/hydroxyapatite hybrid nanofibers should be provided potentially useful options for the fabrication of biomaterial scaffolds for bone tissue engineering. -- Highlights: ► The novel SF/HAp nanofibers were directly prepared by electrospinning method. ► The nanofiber diameter had significant related to the content of HAp. ► The crystal structure of silk fibroin was mainly amorphous structure in the hybrid nanofibers. ► The HAp crystals existing in the hybrid nanofibers were characterized

In situ synthesis of bilayered gradient poly(vinyl alcohol)/hydroxyapatite composite hydrogel by directional freezing-thawing and electrophoresis method.

Science.gov (United States)

Su, Cui; Su, Yunlan; Li, Zhiyong; Haq, Muhammad Abdul; Zhou, Yong; Wang, Dujin

2017-08-01

Bilayered poly(vinyl alcohol) (PVA)/hydroxyapatite (HA) composite hydrogels with anisotropic and gradient mechanical properties were prepared by the combination of directional freezing-thawing (DFT) and electrophoresis method. Firstly, PVA hydrogels with aligned channel structure were prepared by the DFT method. Then, HA nanoparticles were in situ synthesized within the PVA hydrogels via electrophoresis. By controlling the time of the electrophoresis process, a bilayered gradient hydrogel containing HA particles in only half of the gel region was obtained. The PVA/HA composite hydrogel exhibited gradient mechanical strength depending on the distance to the cathode. The gradient initial tensile modulus ranging from 0.18MPa to 0.27MPa and the gradient initial compressive modulus from 0.33MPa to 0.51MPa were achieved. The binding strength of the two regions was relatively high and no apparent internal stress or defect was observed at the boundary. The two regions of the bilayered hydrogel also showed different osteoblast cell adhesion properties. Copyright © 2017 Elsevier B.V. All rights reserved.

Preliminary biocompatible evaluation of nano-hydroxyapatite/polyamide 66 composite porous membrane

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Yili Qu

2010-06-01

Full Text Available Yili Qu1,3, Ping Wang1,3, Yi Man1, Yubao Li2, Yi Zuo2, Jidong Li21State Key Laboratory of Oral Diseases, Sichuan University, Chengdu 610064, China; 2Research Center for Nano-Biomaterials, Analytical and Testing Center, Sichuan University, Chengdu 610064, China; 3These authors contributed equally to this workAbstract: Nano-hydroxyapatite/polyamide 66 (nHA/PA66 composite with good bioactivity and osteoconductivity was employed to develop a novel porous membrane with asymmetric structure for guided bone regeneration (GBR. In order to test material cytotoxicity and to investigate surface-dependent responses of bone-forming cells, the morphology, proliferation, and cell cycle of bone marrow stromal cells (BMSCs of rats cultured on the prepared membrane were determined. The polygonal and fusiform shape of BMSCs was observed by scanning electronic microscopy (SEM. The proliferation of BMSCs cultured on nHA/PA66 membrane tested by the MTT method (MTT: [3-{4,5-dimethylthiazol-2yl}-2,5-diphenyl-2H-tetrazoliumbromide] was higher than that of negative control groups for 1 and 4 days’ incubation and had no significant difference for 7 and 11 days’ culture. The results of cell cycle also suggested that the membrane has no negative influence on cell division. The nHA/PA66 membranes were then implanted into subcutaneous sites of nine Sprague Dawley rats. The wounds and implant sites were free from suppuration and necrosis in all periods. All nHA/PA66 membranes were surrounded by a fibrous capsule with decreasing thickness 1 to 8 weeks postoperatively. In conclusion, the results of the in vitro and in vivo studies reveal that nHA/PA66 membrane has excellent biocompatibility and indicate its use in guided tissue regeneration (GTR or GBR.Keywords: hydroxyapatite/polyamide, barrier membrane, biocompatibility, guided bone regeneration

Preparation and characterization of carbon nanofibrous/hydroxyapatite sheets for bone tissue engineering.

Science.gov (United States)

Abd El-Aziz, A M; El Backly, Rania M; Taha, Nahla A; El-Maghraby, Azza; Kandil, Sherif H

2017-07-01

Critical size bone defects are orthopedic defects that will not heal without intervention or that will not completely heal over the natural life time of the animal. Although bone generally has the ability to regenerate completely however, critical defects require some sort of scaffold to do so. In the current study we proposed a method to obtain a carbon nanofibrous/Hydroxyapatite (HA) bioactive scaffold. The carbon nanofibrous (CNF) nonwoven fabrics were obtained by the use of the electrospinning process of the polymeric solution of poly acrylonitrile "PAN" and subsequent stabilization and carbonization processes. The CNFs sheets were functionalized by both hydroxyapatite (HA) and bovine serum albumin (BSA). The HA was added to the electrospun solution, but in case of (BSA), it was adsorbed after the carbonization process. The changes in the properties taking place in the precursor sheets were investigated using the characterization methods (SEM, FT-IR, TGA and EDX). The prepared materials were tested for biocompatibility via subcutaneous implantation in New Zealand white rabbits. We successfully prepared biocompatible functionalized sheets, which have been modified with HA or HA and BSA. The sheets that were functionalized by both HA and BSA are more biocompatible with fewer inflammatory cells of (neutrophils and lymphocytes) than ones with only HA over the period of 3weeks. Copyright © 2017 Elsevier B.V. All rights reserved.

Hard tissue compatibility of natural hydroxyapatite/chitosan composite

International Nuclear Information System (INIS)

Tang Xiaojun; Gui Lai; Lue Xiaoying

2008-01-01

The natural hydroxyapatite/chitosan (NHC) composite is a new synthesized material. The aim of this experiment was to assess the bone tissue compatibility of this NHC composite in vivo. Twenty-four healthy New Zealand rabbits were included in this study. Of those, 20 were used as the experimental group and four as the control group. In the experimental group, animals receive a cranium defect procedure and NHC composite repair. In the control group, animals underwent the cranium defect procedure without NHC composite repair. At 1, 4, 12, 24, and 40 weeks after surgery, the animals were sacrificed and samples were taken and assessed by gross observation, three-dimensional (3D) computerized tomographic (CT) reconstruction, histology and scanning electron microscope. Our results showed that at 1 week after repairing the bone defect with the NHC composite in the experimental group, new bone appeared around the composite and matured gradually. At 24 weeks after surgery, there were little collagenous tissues present between the material and surrounding bones. At 40 weeks after surgery, new bone had grown into the mature bone and total osseointegration had occurred. In the control group, however, no bone defect healing was observed at 40 weeks after surgery. All these results of the present in vivo work suggest that the NHC composite has a good hard tissue biocompatibility and an excellent osteoconductivity. It is suitable for artificial bone implants and frame materials of tissue engineering.

Hard tissue compatibility of natural hydroxyapatite/chitosan composite

Energy Technology Data Exchange (ETDEWEB)

Tang Xiaojun; Gui Lai [Department of Cranio-maxillofacial Surgery, Plastic Surgery Hospital, Chinese Academy of Medical Sciences and Peking Union Medical College, 33 Ba-Da-Chu Road, Beijing, 100144 (China); Lue Xiaoying [State Key Laboratory of Bioelectronics, School of Biological Science and Medical Engineering, Southeast University, Nanjing, 210096 (China)], E-mail: laiguiplastic@tom.com, E-mail: luxy@seu.edu.cn

2008-12-15

The natural hydroxyapatite/chitosan (NHC) composite is a new synthesized material. The aim of this experiment was to assess the bone tissue compatibility of this NHC composite in vivo. Twenty-four healthy New Zealand rabbits were included in this study. Of those, 20 were used as the experimental group and four as the control group. In the experimental group, animals receive a cranium defect procedure and NHC composite repair. In the control group, animals underwent the cranium defect procedure without NHC composite repair. At 1, 4, 12, 24, and 40 weeks after surgery, the animals were sacrificed and samples were taken and assessed by gross observation, three-dimensional (3D) computerized tomographic (CT) reconstruction, histology and scanning electron microscope. Our results showed that at 1 week after repairing the bone defect with the NHC composite in the experimental group, new bone appeared around the composite and matured gradually. At 24 weeks after surgery, there were little collagenous tissues present between the material and surrounding bones. At 40 weeks after surgery, new bone had grown into the mature bone and total osseointegration had occurred. In the control group, however, no bone defect healing was observed at 40 weeks after surgery. All these results of the present in vivo work suggest that the NHC composite has a good hard tissue biocompatibility and an excellent osteoconductivity. It is suitable for artificial bone implants and frame materials of tissue engineering.

Obtaining of biodegradable polylactide films and fibers filled hydroxyapatite for medical purposes

Energy Technology Data Exchange (ETDEWEB)

Lytkina, D. N., E-mail: darya-lytkina@yandex.ru; Shapovalova, Y. G., E-mail: elena.shapovalova@ro.ru; Rasskazova, L. A., E-mail: ly-2207@mail.ru; Kurzina, I. A., E-mail: kurzina99@mail.ru; Filimoshkin, A. G., E-mail: filag05@rambler.ru [National Research Tomsk State University 36, Lenina Avenue, Tomsk, 634050 (Russian Federation)

2015-11-17

Relevance of the work is due to the need for new materials that are used in medicine (orthopedics, surgery, dentistry, and others) as a substitute for natural bone tissue injuries, fractures, etc. The aim of presented work is developing of a method of producing biocompatible materials based on polyesters of hydroxycarboxylic acids and calcium phosphate ceramic (hydroxyapatite, HA) with homogeneous distribution of the inorganic component. Bioactive composites based on poly-L-lactide (PL) and hydroxyapatite with homogeneous distribution were prepared. The results of scanning electron microscopy confirm homogeneous distribution of the inorganic filler in the polymer matrix. The positive effect of ultrasound on the homogeneity of the composites was determined. The rate of hydrolysis of composites was evaluated. The rate of hydrolysis of polylactide as an individual substance is 7 times lower than the rate of hydrolysis of the polylactide as a part of the composite. It was found that materials submarines HA composite and do not cause a negative response in the cells of the immune system, while contributing to anti-inflammatory cytokines released by cells.

The influence of phosphorylation and freezing temperature on the mechanical properties of hydroxyapatite/chitosan composite as bone scaffold biomaterial

Science.gov (United States)

Albab, Muh Fadhil; Giovani, Nicholas; Yuwono, Akhmad Herman; Sofyan, Nofrijon; Ramahdita, Ghiska; Whulanza, Yudan

2018-02-01

Biomaterials composite of hydroxyapatite/chitosan is a preeminent material for medical applications including bone scaffold. To improve its mechanical properties, the chitosan as the matrix needs to be modified with particular chemical agents. One of the methods is phosphorylation of chitosan by using orthophosphoric acid prior to the biomaterials fabrication. In the current study, biomaterials with the weight composition of 70% hydroxyapatite (HA) and 30% phosphorylated chitosan have been fabricated using thermally induced phase separation (TIPS) method with freezing temperature variation of -20, -30, -40 and -80°C prior to three day-freeze drying. The results obtained by this work showed that the highest compression modulus of 376.9 kPa, highest compressive strength of 38.4 kPa and biggest pore size of 48.24 µm were achieved in the freezing temperature of -20°C. In comparison to non-phosphorylated chitosan/hydroxyapatite, the modification of chitosan using orthophosphoric acid in this work has been found to increase the compressive strength of composite up to 5.5 times.

Biomorphous porous hydroxyapatite-ceramics from rattan (Calamus Rotang).

Science.gov (United States)

Eichenseer, Christiane; Will, Julia; Rampf, Markus; Wend, Süsen; Greil, Peter

2010-01-01

The three-dimensional, highly oriented pore channel anatomy of native rattan (Calamus rotang) was used as a template to fabricate biomorphous hydroxyapatite (Ca(5)(PO(4))(3)OH) ceramics designed for bone regeneration scaffolds. A low viscous hydroxyapatite-sol was prepared from triethyl phosphite and calcium nitrate tetrahydrate and repeatedly vacuum infiltrated into the native template. The template was subsequently pyrolysed at 800 degrees C to form a biocarbon replica of the native tissue. Heat treatment at 1,300 degrees C in air atmosphere caused oxidation of the carbon skeleton and sintering of the hydroxyapatite. SEM analysis confirmed detailed replication of rattan anatomy. Porosity of the samples measured by mercury porosimetry showed a multimodal pore size distribution in the range of 300 nm to 300 microm. Phase composition was determined by XRD and FT-IR revealing hydroxyapatite as the dominant phase with minimum fractions of CaO and Ca(3)(PO(4))(2). The biomorphous scaffolds with a total porosity of 70-80% obtained a compressive strength of 3-5 MPa in axial direction and 1-2 MPa in radial direction of the pore channel orientation. Bending strength was determined in a coaxial double ring test resulting in a maximum bending strength of approximately 2 MPa.

Characterization of fabricated cobalt-based alloy/nano bioactive glass composites

Energy Technology Data Exchange (ETDEWEB)

Bafandeh, Mohammad Reza, E-mail: mr.bafandeh@gmail.com [Department of Materials Science and Engineering, Faculty of Engineering, University of Kashan, Kashan (Iran, Islamic Republic of); Gharahkhani, Raziyeh; Fathi, Mohammad Hossein [Department of Materials Engineering, Isfahan University of Technology (IUT), Isfahan 84156-83111 (Iran, Islamic Republic of)

2016-12-01

In this work, cobalt-based alloy/nano bioactive glass (NBG) composites with 10, 15 and 20 wt% NBG were prepared and their bioactivity after immersion in simulated body fluid (SBF) for 1 to 4 weeks was studied. Scanning electron microscopy images of two- step sintered composites revealed relatively dense microstructure. The results showed that density of composite samples decreased with increase in NBG amount. The microstructure analysis as well as energy dispersive X-ray analysis (EDX) revealed that small amount of calcium phosphate phases precipitates on the surface of composite samples after 1 week immersion in SBF. After 2 weeks immersion, considerable amounts of cauliflower-like shaped precipitations were seen on the surface of the composites. Based on EDX analysis, these precipitations were composed mainly from Ca, P and Si. The observed bands in the Fourier transform infrared spectroscopy of immersed composites samples for 4 weeks in SBF, were characteristic bands of hydroxyapatite. Therefore it is possible to form hydroxyapatite layer on the surface of composite samples during immersion in SBF. The results indicated that prepared composites unlike cobalt-based alloy are bioactive, promising their possibility for implant applications. - Highlights: • Co-based alloy/nano bioactive glass (NBG) composites with 10, 15 and 20 wt% NBG were prepared. • In order to study their bioactivity, composite samples were immersed in SBF solution for 1 to 4 weeks. • Immersion in SBF accompanied with precipitation of hydroxyapatite on surface of samples. • Prepared composite samples unlike cobalt-based alloy were bioactive.

Characterization of fabricated cobalt-based alloy/nano bioactive glass composites

International Nuclear Information System (INIS)

Bafandeh, Mohammad Reza; Gharahkhani, Raziyeh; Fathi, Mohammad Hossein

2016-01-01

In this work, cobalt-based alloy/nano bioactive glass (NBG) composites with 10, 15 and 20 wt% NBG were prepared and their bioactivity after immersion in simulated body fluid (SBF) for 1 to 4 weeks was studied. Scanning electron microscopy images of two- step sintered composites revealed relatively dense microstructure. The results showed that density of composite samples decreased with increase in NBG amount. The microstructure analysis as well as energy dispersive X-ray analysis (EDX) revealed that small amount of calcium phosphate phases precipitates on the surface of composite samples after 1 week immersion in SBF. After 2 weeks immersion, considerable amounts of cauliflower-like shaped precipitations were seen on the surface of the composites. Based on EDX analysis, these precipitations were composed mainly from Ca, P and Si. The observed bands in the Fourier transform infrared spectroscopy of immersed composites samples for 4 weeks in SBF, were characteristic bands of hydroxyapatite. Therefore it is possible to form hydroxyapatite layer on the surface of composite samples during immersion in SBF. The results indicated that prepared composites unlike cobalt-based alloy are bioactive, promising their possibility for implant applications. - Highlights: • Co-based alloy/nano bioactive glass (NBG) composites with 10, 15 and 20 wt% NBG were prepared. • In order to study their bioactivity, composite samples were immersed in SBF solution for 1 to 4 weeks. • Immersion in SBF accompanied with precipitation of hydroxyapatite on surface of samples. • Prepared composite samples unlike cobalt-based alloy were bioactive.

A process for the development of strontium hydroxyapatite

International Nuclear Information System (INIS)

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

2014-01-01

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% Sr 2 + 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

A process for the development of strontium hydroxyapatite

Science.gov (United States)

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.

A process for the development of strontium hydroxyapatite

International Nuclear Information System (INIS)

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

2013-01-01

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 percentage 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. (author)

Mechanical properties and biocompatibility of the sputtered Ti doped hydroxyapatite.

Science.gov (United States)

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

2016-10-01

The hydroxyapatite enriched with Ti were prepared as possible candidates for biomedical applications especially for implantable devices that are in direct contact to the bone. The hydroxyapatites with different Ti content were prepared by RF magnetron sputtering on Ti-6Al-4V alloy using pure hydroxyapatite and TiO2 targets. The content of Ti was modified by changing the RF power fed on TiO2 target. The XPS and FTIR analyses revealed the presence of hydroxyapatite structure. The hardness and elastic modulus of the hydroxyapatite were increased by Ti addition. After 5 days of culture, the cell viability of the Ti-6Al-4V was enhanced by depositing with undoped or doped hydroxyapatite. The Ti additions led to an increase in cell viability of hydroxyapatite, after 5 days of culture. The electron microscopy showed the presence of more cells on the surface of Ti-enriched hydroxyapatite than those observed on the surface of the uncoated alloys or undoped hydroxyapatite. Copyright © 2016 Elsevier Ltd. All rights reserved.

Polyurethane/nano-hydroxyapatite composite films as osteogenic platforms.

Science.gov (United States)

Jackson, Bailey K; Bow, Austin J; Kannarpady, Ganesh; Biris, Alexandru S; Anderson, David E; Dhar, Madhu; Bourdo, Shawn E

2018-05-02

A wide variety of biomaterials are utilized in tissue engineering to promote cell proliferations in vitro or tissue growth in vivo. The combination of cells, extracellular matrices, and biocompatible materials may make it possible to grow functional living tissues ranging from bone to nerve cells. In bone regeneration, polymeric scaffolds can be enhanced by the addition of bioactive materials. To this end, this study designed several ratios of polyurethane (PU) and nano-hydroxyapatite (nHA) composites (PU-nHA ratios: 100/0, 90/10, 80/20, 70/30, 60/40 w/w). The physical and mechanical properties of these composites and their relative cellular compatibility in vitro were determined. The chemical composition and crystallinity of the composites were confirmed using X-ray diffraction, X-ray photoelectron spectroscopy, and thermogravimetric analyses. Atomic force microscopy, nano-indentation, and contact angle measurements were used to evaluate surface properties. The results showed a significant increase in surface roughness and a decrease in contact angle when the nHA concentration increased above 20%, resulting in a significant increase in hydrophilicity. These surface property changes influenced cellular behavior when MC 3T3-E1 cells were seeded on the composites. All composites were cytocompatible. There was a linear increase in cell proliferation on the 80/20 and 70/30 composites only, whereas subjective evaluation demonstrated noticeable clusters or nodules of cells (considered hallmarks of osteogenic differentiation) in the absence of any osteogenic inducers only on the 90/10 and 80/20 composites. Cellular data suggests that the 80/20 composite was an optimal environment for cell adhesion, proliferation, and, potentially, osteogenic differentiation in vitro.

Preparation of Gelatin coated hydroxyapatite nanorods and the stability of its aqueous colloidal

International Nuclear Information System (INIS)

Chen Minfang; Tan Junjun; Lian Yuying; Liu Debao

2008-01-01

This paper describes a novel process for preparing Gelatin coated hydroxyapatite (HAp) nanorods to improve the stability of its aqueous colloid. As Gelatin is a typical protein with abundant hydroxyls, carboxys and imines, it is a very effective functional group to attach onto the surfaces of the HAp particles. Our data show that the Gelatin layer firmly coated on the hydroxyapatite nanorods, and their structure and interfacial chemical bonding have been studied using various techniques, such as X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), high-resolution transmission electron microscopy (HRTEM), differential thermal analysis (DTA) and thermal gravimetric analysis (TGA). The reaction temperature, pH, amount of Gelatin, and Ca/P molar ratio in the material determine the quality of Gelatin coating and the stability of the HAp in aqueous solution. Moreover, an interesting phenomenon was found that the Gelatin coated HAp sediment separated by centrifugal was easily dispersed in water and forms HAp aqueous suspension. The suspension was stable for more than 24 h

In vitro degradation of porous nano-hydroxyapatite/collagen/PLLA scaffold reinforced by chitin fibres

International Nuclear Information System (INIS)

Li Xiaoming; Feng Qingling; Cui Fuzhai

2006-01-01

In this paper, a novel porous scaffold for bone tissue engineering was prepared with nano-hydroxyapatite/collagen/Poly-L-lactic acid (PLLA) composite reinforced by chitin fibres. To enhance the strength of the scaffold further, PLLA was linked with chitin fibres by Dicyclohexylcarbodimide (DCC). The structures of the reinforced scaffold with and without linking were characterized by Scanning Electron Microscopy (SEM). The chemical characteristics of the chitin fibres with and without linking were evaluated by Fourier-transformed infrared (FTIR) spectroscopy. The mechanical performance during degradation in vitro was investigated. The results indicated that the nano-hydroxyapatite/collagen/PLLA composite reinforced by chitin fibres with linking kept better mechanical properties than that of the composite without linking. These results denoted that the stronger interfacial bonding strength of the scaffold with linking could decrease the degradation rate in vitro. The reinforced composite with the link-treatment can be severed as a scaffold for bone tissue engineering

Study of mixed Ca-Zn hydroxyapatite surface modified by lactic acid

Science.gov (United States)

Turki, Thouraya; Aissa, Abdallah; Bac, Christophe Goze; Rachdi, Férid; Debbabi, Mongi

2012-07-01

The new hybrid inorganic-organic composites, Ca(10-x)Znx(PO4)6(OH)2-lactic acid, at different amounts of zinc and lactic acid were prepared by dissolution of the organic compound in an hydroxyapatite suspension. They were characterized by XRD, IR, MAS NMR (13C and 1H) and chemical analysis. The crystallinity was slightly affected by the presence of organic fragments. IR and (13C and 1H) MAS NMR measurements indicate that the carboxylic groups of the acid interact with calcium and zinc ions of hydroxyapatite surface. Chemical analysis displays that zinc promotes the acid grafting. A mechanism of surface modification is proposed based on the obtained results.

Study of mixed Ca-Zn hydroxyapatite surface modified by lactic acid

International Nuclear Information System (INIS)

Turki, Thouraya; Aissa, Abdallah; Bac, Christophe Goze; Rachdi, Férid; Debbabi, Mongi

2012-01-01

The new hybrid inorganic-organic composites, Ca (10-x) Zn x (PO 4 ) 6 (OH) 2 -lactic acid, at different amounts of zinc and lactic acid were prepared by dissolution of the organic compound in an hydroxyapatite suspension. They were characterized by XRD, IR, MAS NMR ( 13 C and 1 H) and chemical analysis. The crystallinity was slightly affected by the presence of organic fragments. IR and ( 13 C and 1 H) MAS NMR measurements indicate that the carboxylic groups of the acid interact with calcium and zinc ions of hydroxyapatite surface. Chemical analysis displays that zinc promotes the acid grafting. A mechanism of surface modification is proposed based on the obtained results.

Mechanical, Rheological, and Bioactivity Properties of Ultra High-Molecular-Weight Polyethylene Bioactive Composites Containing Polyethylene Glycol and Hydroxyapatite

Directory of Open Access Journals (Sweden)

Mazatusziha Ahmad

2012-01-01

Full Text Available Ultrahigh-molecular-weight polyethylene/high-density polyethylene (UHMWPE/HDPE blends prepared using polyethylene glycol PEG as the processing aid and hydroxyapatite (HA as the reinforcing filler were found to be highly processable using conventional melt blending technique. It was demonstrated that PEG reduced the melt viscosity of UHMWPE/HDPE blend significantly, thus improving the extrudability. The mechanical and bioactive properties were improved with incorporation of HA. Inclusion of HA from 10 to 50 phr resulted in a progressive increase in flexural strength and modulus of the composites. The strength increment is due to the improvement on surface contact between the irregular shape of HA and polymer matrix by formation of mechanical interlock. The HA particles were homogenously distributed even at higher percentage showed improvement in wetting ability between the polymer matrix and HA. The inclusion of HA enhanced the bioactivity properties of the composite by the formation of calcium phosphate (Ca-P precipitates on the composite surface as proven from SEM and XRD analysis.

Porous stable poly(lactic acid)/ethyl cellulose/hydroxyapatite composite scaffolds prepared by a combined method for bone regeneration.

Science.gov (United States)

Mao, Daoyong; Li, Qing; Bai, Ningning; Dong, Hongzhou; Li, Daikun

2018-01-15

A major challenge in bone tissue engineering is the development of biomimetic scaffolds which should simultaneously meet mechanical strength and pore structure requirements. Herein, we combined technologies of high concentration solvent casting, particulate leaching, and room temperature compression molding to prepare a novel poly(lactic acid)/ethyl cellulose/hydroxyapatite (PLA/EC/HA) scaffold. The functional, structural and mechanical properties of the obtained porous scaffolds were characterized. The results indicated that the PLA/EC/HA scaffolds at the 20wt% HA loading level showed optimal mechanical properties and desired porous structure. Its porosity, contact angle, compressive yield strength and weight loss after 56days were 84.28±7.04%, 45.13±2.40°, 1.57±0.09MPa and 4.77±0.32%, respectively, which could satisfy the physiological demands to guide bone regeneration. Thus, the developed scaffolds have potential to be used as a bone substitute material for bone tissue engineering application. Copyright © 2017. Published by Elsevier Ltd.

Crystallization of modified hydroxyapatite on titanium implants

International Nuclear Information System (INIS)

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

2016-01-01

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

Adsorption of nickel on synthetic hydroxyapatite from aqueous solutions

International Nuclear Information System (INIS)

Rosskopfova, O.; Galambos, M.; Pivarciova, L.; Rajec, P.; Caplovicova, M.

2013-01-01

The sorption of nickel on synthetic hydroxyapatite was investigated using a batch method and radiotracer technique. The hydroxyapatite samples used in experiments were a commercial hydroxyapatite and hydroxyapatite of high crystallinity with Ca/P ratio of 1.563 and 1.688, respectively, prepared by a wet precipitation process. The sorption of nickel on hydroxyapatite was pH independent ranging from 4.5 to 6.5 as a result of buffering properties of hydroxyapatite. The adsorption of nickel was rapid and the percentage of Ni sorption on both samples of hydroxyapatite was >98 % during the first 15-30 min of the contact time for initial Ni 2+ concentration of 1 x 10 -4 mol dm -3 . The experimental data for sorption of nickel have been interpreted in the term of Langmuir isotherm and the value of maximum sorption capacity of nickel on a commercial hydroxyapatite and hydroxyapatite prepared by wet precipitation process was calculated to be 0.184 and 0.247 mmol g -1 , respectively. The sorption of Ni 2+ ions was performed by ion-exchange with Ca 2+ cations on the crystal surface of hydroxyapatite under experimental conditions. The competition effect of Co 2+ and Fe 2+ towards Ni 2+ sorption was stronger than that of Ca 2+ ions. NH 4 + ions have no apparent effect on nickel sorption. (author)

Clinical and radiographic evaluation of citric acid-based nano hydroxyapatite composite graft in the regeneration of intrabony defects - A randomized controlled trial

Directory of Open Access Journals (Sweden)

Chaurasia Priya Dayashankar

2017-01-01

Full Text Available Background: Conventional periodontal therapy with various bone grafts has limited scope and the results are not predictable. To improve their utility, the hybridization of bioceramics and biodegradable polymers has been widely adopted to reform the mechanical properties of bone grafts. One such biodegradable polymer is POC (Poly 1,8 octanediol. Secondly, citric acid is considered as the key material in bone mineralization, which is related to the overall stability, strength and fracture resistance of bone. Hence citric acid is incorporated in a polymer and Nano hydroxyapatite to form a composite graft, for periodontal bone regeneration. This study attempts to evaluate the efficacy of citric acid based Nano-hydroxyapatite composite graft for the treatment of intrabony defects in chronic periodontitis patients over 12 months. Methods: A split mouth study, which consists of 10 systemically healthy patients, were randomly treated with Citric acid based Nano hydroxyapatite composite graft (test sites, n=18 or with Nano hydroxyapatite alone (control sites, n=15. Plaque index, gingival index, gingival bleeding index, probing pocket depth (PPD, clinical attachment level (CAL, bone probing depth (BPD and hard tissue parameters such as amount of defect fill, percentage of defect fill, and changes in alveolar crest were assessed over a period of 12 months. Statistical analysis used was student's t-test and One-Way ANOVA. Results: Both test and control sites demonstrated statistically significant reduction of PD, BPD, gain in CAL and radiographic bone fill. Nevertheless the test sites showed Statistically significant improvements in all the parameters as compared to control sites at 12 months. Conclusion: Citric acid based Nano hydroxyapatite composite graft can be considered as a newer material for periodontal regeneration.

In-vitro bioactivity, biocorrosion and antibacterial activity of silicon integrated hydroxyapatite/chitosan composite coating on 316 L stainless steel implants

Energy Technology Data Exchange (ETDEWEB)

Sutha, S.; Kavitha, K.; Karunakaran, G.; Rajendran, V., E-mail: veerajendran@gmail.com

2013-10-15

A simple and effective ultrasonication method was applied for the preparation of 0, 0.4, 0.8, 1.0 and 1.6 wt% silicon substituted hydroxyapatite (HAp) (SH). The Ca/P ratio of the synthesised SH nanoparticles were in the range of 1.58–1.70. Morphological changes were noticed in HAp with respect to the amount of Si from 0 to 1.6 wt%. The morphology of the particles changed from spherical shape to rod-like morphology with respect to the amount of Si which was confirmed using transmission electron microscopy. X-ray diffraction studies confirm the formation of phase pure SH nanoparticles without any secondary phase. Chitosan (CTS) blended SH nanocomposites coating on surgical grade 316 L stainless steel (316 L SS) implant was made by spin coating technique. The surface of the coated implant was characterised using scanning electron microscopy which confirms the uniform coating without cracks and pores. The increased corrosion resistance of the 1.6 wt% of SH/CTS-coated SS implant in the simulated body fluid (SBF) indicates the long-term biostability of SH composite-coated ceramics in vitro than the 0 wt% SH/CTS. The testing of SH/CTS nanocomposites with gram-positive and gram-negative bacterial strains confirms that the antibacterial ability improves with the higher substitution of Si. In addition, formation of bone-like apatite layer on the SH/CTS-coated implant in SBF was studied through SEM analysis and it confirms the ability to increase the HAp formation on the surface of 1.0 wt% SH/CTS-coated 316 L SS implant. Highlights: • Hydroxyapatite particles are prepared with various silicon concentration • Prepared composites are blended with chitosan and coated on the implant • Corrosion resistance in simulated body fluid improves its stability • Increase in silicon concentration improves the antibacterial activity • Coated plate exhibit high in-vitro bioactivity in simulated body fluid.

In-vitro bioactivity, biocorrosion and antibacterial activity of silicon integrated hydroxyapatite/chitosan composite coating on 316 L stainless steel implants

International Nuclear Information System (INIS)

Sutha, S.; Kavitha, K.; Karunakaran, G.; Rajendran, V.

2013-01-01

A simple and effective ultrasonication method was applied for the preparation of 0, 0.4, 0.8, 1.0 and 1.6 wt% silicon substituted hydroxyapatite (HAp) (SH). The Ca/P ratio of the synthesised SH nanoparticles were in the range of 1.58–1.70. Morphological changes were noticed in HAp with respect to the amount of Si from 0 to 1.6 wt%. The morphology of the particles changed from spherical shape to rod-like morphology with respect to the amount of Si which was confirmed using transmission electron microscopy. X-ray diffraction studies confirm the formation of phase pure SH nanoparticles without any secondary phase. Chitosan (CTS) blended SH nanocomposites coating on surgical grade 316 L stainless steel (316 L SS) implant was made by spin coating technique. The surface of the coated implant was characterised using scanning electron microscopy which confirms the uniform coating without cracks and pores. The increased corrosion resistance of the 1.6 wt% of SH/CTS-coated SS implant in the simulated body fluid (SBF) indicates the long-term biostability of SH composite-coated ceramics in vitro than the 0 wt% SH/CTS. The testing of SH/CTS nanocomposites with gram-positive and gram-negative bacterial strains confirms that the antibacterial ability improves with the higher substitution of Si. In addition, formation of bone-like apatite layer on the SH/CTS-coated implant in SBF was studied through SEM analysis and it confirms the ability to increase the HAp formation on the surface of 1.0 wt% SH/CTS-coated 316 L SS implant. Highlights: • Hydroxyapatite particles are prepared with various silicon concentration • Prepared composites are blended with chitosan and coated on the implant • Corrosion resistance in simulated body fluid improves its stability • Increase in silicon concentration improves the antibacterial activity • Coated plate exhibit high in-vitro bioactivity in simulated body fluid

Tensile properties and microstructural analysis of spheroidized hydroxyapatite-poly (etheretherketone) biocomposites

International Nuclear Information System (INIS)

Abu Bakar, M.S.; Cheang, P.; Khor, K.A.

2003-01-01

Poly(etheretherketone) or PEEK, is a high performance thermoplastic possessing exceptional mechanical properties, high temperature durability, good chemical and fatigue resistance. These coupled with its ability to withstand sterilization treatment, make it a preferred material for biomedical applications. This study examines the benefit of incorporating hydroxyapatite particulates in poly(etheretherketone) for possible usage as bone analogue materials. Flame spheroidized hydroxyapatite (FSHA) were incorporated into semi-crystalline poly(etheretherketone) polymer through a series of processes comprising melt compounding, granulating and injection molding. Biocomposites with high hydroxyapatite loading of up to 40 vol.% were processed successfully using this technique. Scanning electron microscopy (SEM) revealed fair dispersion and distribution of hydroxyapatite particles within the polymer matrix. The series of composites were characterized in terms of tensile and microhardness properties. Microstructural analysis was also carried out to correlate the structure-property relationship of the composite. The dependency of tensile properties such as modulus, strength and strain to fracture as well as the micro-hardness on the volume percentage of hydroxyapatite were investigated. By varying the amount of hydroxyapatite particles in the composite, a wide range of mechanical properties were obtained. In general, the tensile modulus and microhardness increased, while strength and strain to fracture decreased correspondingly with progressive addition of hydroxyapatite particles. The composite system under investigation also exhibited mechanical properties matching those of human bone. With hydroxyapatite loading beyond 30 vol.%, the modulus were within the bounds of the human cortical bone. Findings from this study suggest that this bioactive composite system have the potential as an alternative implant material for orthopaedic application

Characterization of mechanical properties of hydroxyapatite-silicon-multi walled carbon nano tubes composite coatings synthesized by EPD on NiTi alloys for biomedical application.

Science.gov (United States)

Khalili, Vida; Khalil-Allafi, Jafar; Sengstock, Christina; Motemani, Yahya; Paulsen, Alexander; Frenzel, Jan; Eggeler, Gunther; Köller, Manfred

2016-06-01

Release of Ni(1+) ions from NiTi alloy into tissue environment, biological response on the surface of NiTi and the allergic reaction of atopic people towards Ni are challengeable issues for biomedical application. In this study, composite coatings of hydroxyapatite-silicon multi walled carbon nano-tubes with 20wt% Silicon and 1wt% multi walled carbon nano-tubes of HA were deposited on a NiTi substrate using electrophoretic methods. The SEM images of coated samples exhibit a continuous and compact morphology for hydroxyapatite-silicon and hydroxyapatite-silicon-multi walled carbon nano-tubes coatings. Nano-indentation analysis on different locations of coatings represents the highest elastic modulus (45.8GPa) for HA-Si-MWCNTs which is between the elastic modulus of NiTi substrate (66.5GPa) and bone tissue (≈30GPa). This results in decrease of stress gradient on coating-substrate-bone interfaces during performance. The results of nano-scratch analysis show the highest critical distance of delamination (2.5mm) and normal load before failure (837mN) as well as highest critical contact pressure for hydroxyapatite-silicon-multi walled carbon nano-tubes coating. The cell culture results show that human mesenchymal stem cells are able to adhere and proliferate on the pure hydroxyapatite and composite coatings. The presence of both silicon and multi walled carbon nano-tubes (CS3) in the hydroxyapatite coating induce more adherence of viable human mesenchymal stem cells in contrast to the HA coated samples with only silicon (CS2). These results make hydroxyapatite-silicon-multi walled carbon nano-tubes a promising composite coating for future bone implant application. Copyright © 2016 Elsevier Ltd. All rights reserved.

Biomimetic composite microspheres of collagen/chitosan/nano-hydroxyapatite: In-situ synthesis and characterization.

Science.gov (United States)

Teng, Shu-Hua; Liang, Mian-Hui; Wang, Peng; Luo, Yong

2016-01-01

The collagen/chitosan/hydroxyapatite (COL/CS/HA) composite microspheres with a good spherical form and a high dispersity were successfully obtained using an in-situ synthesis method. The FT-IR and XRD results revealed that the inorganic phase in the microspheres was crystalline HA containing carbonate ions. The morphology of the composite microspheres was dependent on the HA content, and a more desirable morphology was achieved when 20 wt.% HA was contained. The composite microspheres exhibited a narrow particle distribution, most of which ranged from 5 to 10 μm. In addition, the needle-like HA nano-particles were uniformly distributed in the composite microspheres, and their crystallinity and crystal size decreased with the HA content. Copyright © 2015 Elsevier B.V. All rights reserved.

Bioactivity of cellulose acetate/hydroxyapatite nanoparticle composite fiber by an electro-spinning process.

Science.gov (United States)

Kwak, Dae Hyun; Lee, Eun Ju; Kim, Deug Joong

2014-11-01

Hydroxyapatite/cellulose acetate composite webs were fabricated by an electro-spinning process. This electro-spinning process makes it possible to fabricate complex three-dimensional shapes. Nano fibrous web consisting of cellulose acetate and hydroxyapatite was produced from their mixture solution by using an electro-spinning process under high voltage. The surface of the electro-spun fiber was modified by a plasma and alkaline solution in order to increase its bioactivity. The structure, morphology and properties of the electro-spun fibers were investigated and an in-vitro bioactivity test was evaluated in simulated body fluid (SBF). Bioactivity of the electro-spun web was enhanced with the filler concentration and surface treatment. The surface changes of electro-spun fibers modified by plasma and alkaline solution were investigated by FT-IR (Fourier Transform Infrared Spectroscopy) and XPS (X-ray Photoelectron Spectroscopy).

Preparation and structure of carbonated calcium hydroxyapatite substituted with heavy rare earth ions

Energy Technology Data Exchange (ETDEWEB)

Yasukawa, Akemi, E-mail: yasukawa@cc.hirosaki-u.ac.jp [School of Home Economics, Faculty of Education, Hirosaki University, 1-bunkyo, Hirosaki, Aomori 036-8560 (Japan); Kandori, Kazuhiko [School of Chemistry, Osaka University of Education, 4-698-1 Asahigaoka, Kashiwara, Osaka 582-8582 (Japan); Tanaka, Hidekazu [Department of Material Science, Faculty of Science and Engineering, Shimane University, 1060 Nishikawatsu, Matsue, Shimane 690-8504 (Japan); Gotoh, Keiko [Faculty of Human Life and Environment, Nara Women' s University, Kita-uoya-nishi, Nara 630-8506 (Japan)

2012-05-15

Highlights: Black-Right-Pointing-Pointer LnCaHap solid solution particles were prepared using five types of heavy rare earth ions by a precipitation method. Black-Right-Pointing-Pointer The length and the crystallinity of the LnCaHap particles first increased and then decreased with increasing Ln{sup 3+} contents. Black-Right-Pointing-Pointer A series of YCaHap solid solution particles formed with Y/(Y + Ca) = 0-0.10 were investigated using various methods in detail. -- Abstract: Calcium hydroxyapatite (CaHap) particles substituted five types of heavy rare earth ions (Ln: Y{sup 3+}, Gd{sup 3+}, Dy{sup 3+}, Er{sup 3+} and Yb{sup 3+}) were synthesized using a precipitation method and characterized using various means. These Ln ions strongly affected the crystal phases and the structures of the products. With increasing Ln/(Ln + Ca) in the starting solution ([X{sub Ln}]), the length and the crystallinity of the particles first increased and then decreased. The rare earth metal-calcium hydroxyapatite (LnCaHap) solid solution particles were obtained at [X{sub Y}] {<=} 0.10 for substituting Y system and at [X{sub Ln}] {<=} 0.01-0.03 for substituting the other Ln systems. LnPO{sub 4} was mixed with LnCaHap at higher [X{sub Ln}] for all Ln systems. A series of yttrium-calcium hydroxyapatite (YCaHap) solid solutions with [X{sub Y}] = 0-0.10 were investigated using XRD, TEM, ICP-AES, IR and TG-DTA in detail.

Preparation and structure of carbonated calcium hydroxyapatite substituted with heavy rare earth ions

International Nuclear Information System (INIS)

Yasukawa, Akemi; Kandori, Kazuhiko; Tanaka, Hidekazu; Gotoh, Keiko

2012-01-01

Highlights: ► LnCaHap solid solution particles were prepared using five types of heavy rare earth ions by a precipitation method. ► The length and the crystallinity of the LnCaHap particles first increased and then decreased with increasing Ln 3+ contents. ► A series of YCaHap solid solution particles formed with Y/(Y + Ca) = 0–0.10 were investigated using various methods in detail. -- Abstract: Calcium hydroxyapatite (CaHap) particles substituted five types of heavy rare earth ions (Ln: Y 3+ , Gd 3+ , Dy 3+ , Er 3+ and Yb 3+ ) were synthesized using a precipitation method and characterized using various means. These Ln ions strongly affected the crystal phases and the structures of the products. With increasing Ln/(Ln + Ca) in the starting solution ([X Ln ]), the length and the crystallinity of the particles first increased and then decreased. The rare earth metal-calcium hydroxyapatite (LnCaHap) solid solution particles were obtained at [X Y ] ≤ 0.10 for substituting Y system and at [X Ln ] ≤ 0.01–0.03 for substituting the other Ln systems. LnPO 4 was mixed with LnCaHap at higher [X Ln ] for all Ln systems. A series of yttrium-calcium hydroxyapatite (YCaHap) solid solutions with [X Y ] = 0–0.10 were investigated using XRD, TEM, ICP-AES, IR and TG–DTA in detail.

Fibrous hydroxyapatite-carbon nanotube composites by chemical vapor deposition : In situ fabrication, structural and morphological characterization

NARCIS (Netherlands)

Kosma, Vassiliki; Tsoufis, Theodoros; Koliou, Theodora; Kazantzis, Antonios; Beltsios, Konstantinos; De Hosson, Jeff Th. M.; Gournis, Dimitrios

2013-01-01

Fibrous hydroxyapatite (HA)-carbon nanotube composites were synthesized by the catalytic decomposition of acetylene over Fe-Co bimetallic catalysts supported on the fibrous HA. Two forms of fibrous HA (distinct needle-like monocrystals and spherulitic aggregates of needles) were synthesized using a

Production of zirconia - hydroxyapatite (Z Ha) by using the co-precipitation method and studies of densification

International Nuclear Information System (INIS)

Silva, Viviane V.; Domingues, Rosana Z.

1997-01-01

Hydroxyapatite (Ha) is one of the materials most bio compatible with human bones and teeth, but its mechanical properties, especially toughness, are insufficient for hard tissue. Recent studies demonstrated that ceramics can be toughened by zirconium particles disperse in them, due to transformation, microcracking, and/or crack diffraction toughening mechanisms. The objective of this study is to characterize zirconia-toughened hydroxy apatite powders prepared by precipitation method by XRD, IR spectroscopy, TEM, TAG, DTA and BET analysis. The density of their ceramics was determined by mercury picnometry method. It was discussed the influence of addition of zirconium in different compositions and phases (Zr O 2 or Zr(OH) 4 ), compacting pressure and sintering temperature on zirconia - hydroxyapatite composites (ZHA). The results show that there is not any kind of reaction or chemical interaction between both phases of the composite materials. (author)

Study of mixed Ca-Zn hydroxyapatite surface modified by lactic acid

Energy Technology Data Exchange (ETDEWEB)

Turki, Thouraya; Aissa, Abdallah [Laboratoire de Physico-Chimie des Materiaux, Faculte des Sciences de Monastir, 5019 Monastir (Tunisia); Bac, Christophe Goze [Laboratoire Charles Coulomb, UMR 5221 CNRS/UM2, Universite Montpellier 2, Place E. Bataillon, 34095 Montpellier (France); Rachdi, Ferid, E-mail: Ferid.Rachdi@univ-montp2.fr [Laboratoire Charles Coulomb, UMR 5221 CNRS/UM2, Universite Montpellier 2, Place E. Bataillon, 34095 Montpellier (France); Debbabi, Mongi [Laboratoire de Physico-Chimie des Materiaux, Faculte des Sciences de Monastir, 5019 Monastir (Tunisia)

2012-07-01

The new hybrid inorganic-organic composites, Ca{sub (10-x)}Zn{sub x}(PO{sub 4}){sub 6}(OH){sub 2}-lactic acid, at different amounts of zinc and lactic acid were prepared by dissolution of the organic compound in an hydroxyapatite suspension. They were characterized by XRD, IR, MAS NMR ({sup 13}C and {sup 1}H) and chemical analysis. The crystallinity was slightly affected by the presence of organic fragments. IR and ({sup 13}C and {sup 1}H) MAS NMR measurements indicate that the carboxylic groups of the acid interact with calcium and zinc ions of hydroxyapatite surface. Chemical analysis displays that zinc promotes the acid grafting. A mechanism of surface modification is proposed based on the obtained results.

Surface modification of calcium-copper hydroxyapatites using polyaspartic acid

Science.gov (United States)

Othmani, Masseoud; Aissa, Abdallah; Bachoua, Hassen; Debbabi, Mongi

2013-01-01

Mixed calcium-copper hydroxyapatite (Ca-CuHAp), with general formula Ca(10-x)Cux(PO4)6(OH)2, where 0 ≤ x ≤ 0.75 was prepared in aqueous medium in the presence of different concentrations of poly-L-aspartic acid (PASP). XRD, IR, TG-DTA, TEM-EDX, AFM and chemical analyses were used to characterize the structure, morphology and composition of the products. All techniques show the formation of new hybrid compounds Ca-CuHAp-PASP. The presence of the grafting moiety on the apatitic material is more significant with increasing of copper amount and/or organic concentration in the starting solution. These increases lead to the affectation of apatite crystallinity. The IR spectroscopy shows the conservation of (Psbnd OH) band of (HPO4)2- groups, suggesting that PASP acid was interacted only with metallic cations of hydroxyapatite.

Use of agroindustrial waste in the preparation of nanocomposites based on bacterial cellulose and hydroxyapatite

International Nuclear Information System (INIS)

Duarte, Eden B.; Chagas, Bruna S. das; Feitosa, Judith P.A.; Andrade, Fabia K.; Borges, Maria F.; Muniz, Celli R.; Souza Filho, Men de Sa M.; Rosa, Morsyleide F.; Brigida, Ana I.; Morais, Joao P.S.

2015-01-01

Environmental issues have supported the interest in renewable sources and agroindustrial residues became a significant resource for the production of new materials. The present work presents the use of agroindustrial residues to obtain bacterial cellulose (BC) for further elaboration of nanocomposites with hydroxyapatite (HA). The production of BC membranes occurred in Hestrin & Schramm medium, cashew juice and sisal liquid waste cultivated under static conditions. After the incubation period, the BC membranes were purified and nanocomposites prepared by successive immersion of the purified membranes in solutions of Calcium Chloride (CaCl_2), and Sodium Phosphate (Na_2HPO_4), followed by drying and subsequent characterization. The materials obtained were characterized by Thermogravimetric Analysis (TGA) and X-ray Diffraction (XRD). Additionally, in vitro tests were performed for nanocomposites. The results showed the production of cellulose from the three substrates studied, without the need for further supplementation or pH change. In all characterizations, structure and typical behavior of bacterial cellulose were found. The composites showed bioactivity and the adsorption capacity of proteins, which lead to potential biocompatibility of these materials. (author)

Characteristics of porous zirconia coated with hydroxyapatite

Indian Academy of Sciences (India)

However, porous hydroxyapatite bodies are mechanically weak and brittle, which makes shaping and implantation difficult. One way to solve this problem is to introduce a strong porous network onto which hydroxyapatite coating is applied. In this study, porous zirconia and alumina-added zirconia ceramics were prepared ...

Surface modification of calcium hydroxyapatite by grafting of etidronic acid

Science.gov (United States)

Othmani, Masseoud; Aissa, Abdallah; Bac, Christophe Goze; Rachdi, Férid; Debbabi, Mongi

2013-06-01

The surface of prepared calcium hydroxyapatite CaHAp has been modified by grafting the etidronic acid (ETD). For that purpose, CaHAp powders have been suspended in an aqueous etidronate solution with different concentrations. The obtained composites CaHAp-(ETD) were characterized by TEM and AFM techniques to determinate morphological properties and were also characterized by XRD, IR, NMR and chemical and thermal analysis to determinate their physico-chemical properties and essentially the nature of the interaction between the inorganic support and the grafted organic ETD. After reaction with ETD, XRD powder analysis shows that the apatitic structure remains unchanged with slight affectation of its crystallinity. The presence of etidronate fragment bounded to hydroxyapatite was confirmed by IR and solid-state NMR spectroscopy. TEM and AFM techniques indicate that the presence of etidronate changes the morphology of the particles. Basing on the obtained results, a reactional mechanism was proposed to explain the formation of covalent Casbnd Osbnd Porg bonds on the hydroxyapatite surface between the superficial hydroxyl groups (tbnd Casbnd OH) of the apatite and phosphonate group (Psbnd OH) of etidronate.

Valorization of Bone Waste of Saudi Arabia by Synthesizing Hydroxyapatite.

Science.gov (United States)

Amna, Touseef

2018-05-09

At present, hydroxyapatite is being frequently used for diverse biomedical applications as it possesses excellent biocompatibility, osteoconductivity, and non-immunogenic characteristics. The aim of the present work was to recycle bone waste for synthesis of hydroxyapatite nanoparticles to be used as bone extracellular matrix. For this reason, we for the first time utilized bio-waste of cow bones of Albaha city. The residual bones were utilized for the extraction of natural bone precursor hydroxyapatite. A facile scientific technique has been used to synthesize hydroxyapatite nanoparticles through calcinations of wasted cow bones without further supplementation of chemicals/compounds. The obtained hydroxyapatite powder was ascertained using physicochemical techniques such as XRD, SEM, FTIR, and EDX. These analyses clearly show that hydroxyapatite from native cow bone wastes is biologically and physicochemically comparable to standard hydroxyapatite, commonly used for biomedical functions. The cell viability and proliferation over the prepared hydroxyapatite was confirmed with CCk-8 colorimetric assay. The morphology of the cells growing over the nano-hydroxyapatite shows that natural hydroxyapatite promotes cellular attachment and proliferation. Hence, the as-prepared nano-hydroxyapatite can be considered as cost-effective source of bone precursor hydroxyapatite for bone tissue engineering. Taking into account the projected demand for reliable bone implants, the present research work suggested using environment friendly methods to convert waste of Albaha city into nano-hydroxyapatite scaffolds. Therefore, besides being an initial step towards accomplishment of projected demands of bone implants in Saudi Arabia, our study will also help in reducing the environmental burden by recycling of bone wastes of Albaha city.

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

International Nuclear Information System (INIS)

De Araujo, T S; De Souza, S O; De Sousa, E M B; Araujo, M S

2010-01-01

Hydroxyapatite (HAP) have been used as starting material for biomedical applications. The pure and Cr 3+ -doped hydroxyapatite were prepared by chemical precipitation reactions at 100, 500 e 800 0 C in order to investigate the thermal stability of these materials. The characterization of the thermal behavior of this phosphate, especially on the structural changes with heating, is very important for production of sunscreens The powders were characterized using chemical analysis: X-ray diffraction (XRD) and thermal analysis. The present study was successful in the preparation of pure hydroxyapatite and chromium substituted hydroxyapatites with good thermal stability and nanoparticles formation.

Characterisation of Suspension Precipitated Nanocrystalline Hydroxyapatite Powders

International Nuclear Information System (INIS)

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

2016-01-01

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. (paper)

[Study on biocompatibility of hydroxyapatite/high density polyethylene (HA/HDPE) nano-composites artificial ossicle].

Science.gov (United States)

Wang, Guohui; Zhu, Shaihong; Tan, Guolin; Zhou, Kechao; Huang, Suping; Zhao, Yanzhong; Li, Zhiyou; Huang, Boyun

2008-06-01

This study was aimed to evaluate the biocompatibility of Hydroxyapatite/High density polyethylene (HA/ HDPE) nano-composites artificial ossicle. The percentage of S-period cells were detected by flow cytometry after L929 cells being incubated with extraction of the HA/HDPE nano-composites; the titanium materials for clinical application served as the contrast. In addition, both materials were implanted in animals and the histopathological evaluations were conducted. There were no statistically significant differences between the two groups (P >0.05). The results demonstrated that the HA/HDPE nano-composite artificial ossicle made by our laboratory is of a good biocompatibility and clinical application outlook.

Preparation of zeolite-A/chitosan hybrid composites and their bioactivities and antimicrobial activities

International Nuclear Information System (INIS)

Yu, Liang; Gong, Jie; Zeng, Changfeng; Zhang, Lixiong

2013-01-01

Zeolite-A/chitosan hybrid composites with zeolite contents of 20–55 wt.% were prepared by in situ transformation of silica/chitosan mixtures in a sodium aluminate alkaline solution through impregnation–gelation–hydrothermal synthesis. The products were characterized by X-ray diffraction, diffuse reflectance infrared Fourier transform spectroscopy, scanning electron microscopy, thermogravimetric analysis, and mercury penetration porosimetry. Their in vitro bioactivities were examined using as-synthesized and Ca 2+ -exchanged hybrid composites in simulated body fluid (SBF) for hydroxyapatite (HAP) growth. Their antimicrobial activities for Escherichia coli (E. coli) in trypticase soy broth (TSB) were evaluated using Ag + -exchanged hybrid composites. The zeolite-A/chitosan hybrid composites could be prepared as various shapes, including cylinders, plates and thin films. They possessed macropores with pore sizes ranging from 100 to 300 μm and showed compressive mechanical strength as high as 3.2 MPa when the zeolite content was 35 wt.%. Fast growth on the Ca 2+ -exchanged hybrid composites was observed with the highest weight gain of 51.4% in 30 days. The 35 wt.% Ag + -exchanged hybrid composite showed the highest antimicrobial activity, which could reduce the 9 × 10 6 CFU mL −1 E. coli concentration to zero within 4 h of incubation time with the Ag + -exchanged hybrid composite amount of 0.4 g L −1 . The bioactivity and antimicrobial activity could be combined by ion-exchanging the composites first with Ca 2+ and then with Ag + . These zeolite-A/chitosan hybrid composites have potential applications on tissue engineering and antimicrobial food packaging. - Graphical abstract: Zeolite A/chitosan hybrid composites were prepared by in situ transformation of precursors in the chitosan matrix, which possess macroporous structures and exhibit superior bioactivity and antimicrobial activity and potential biomedical application. Highlights: • Zeolite A

Preparation of zeolite-A/chitosan hybrid composites and their bioactivities and antimicrobial activities

Energy Technology Data Exchange (ETDEWEB)

Yu, Liang; Gong, Jie [State Key Laboratory of Materials-Oriented Chemical Engineering, College of Chemistry and Chemical Engineering, Nanjing University of Technology, Nanjing 210009 (China); Zeng, Changfeng [College of Mechanic and Power Engineering, Nanjing University of Technology, Nanjing 210009 (China); Zhang, Lixiong, E-mail: lixiongzhang@yahoo.com [State Key Laboratory of Materials-Oriented Chemical Engineering, College of Chemistry and Chemical Engineering, Nanjing University of Technology, Nanjing 210009 (China)

2013-10-15

Zeolite-A/chitosan hybrid composites with zeolite contents of 20–55 wt.% were prepared by in situ transformation of silica/chitosan mixtures in a sodium aluminate alkaline solution through impregnation–gelation–hydrothermal synthesis. The products were characterized by X-ray diffraction, diffuse reflectance infrared Fourier transform spectroscopy, scanning electron microscopy, thermogravimetric analysis, and mercury penetration porosimetry. Their in vitro bioactivities were examined using as-synthesized and Ca{sup 2+}-exchanged hybrid composites in simulated body fluid (SBF) for hydroxyapatite (HAP) growth. Their antimicrobial activities for Escherichia coli (E. coli) in trypticase soy broth (TSB) were evaluated using Ag{sup +}-exchanged hybrid composites. The zeolite-A/chitosan hybrid composites could be prepared as various shapes, including cylinders, plates and thin films. They possessed macropores with pore sizes ranging from 100 to 300 μm and showed compressive mechanical strength as high as 3.2 MPa when the zeolite content was 35 wt.%. Fast growth on the Ca{sup 2+}-exchanged hybrid composites was observed with the highest weight gain of 51.4% in 30 days. The 35 wt.% Ag{sup +}-exchanged hybrid composite showed the highest antimicrobial activity, which could reduce the 9 × 10{sup 6} CFU mL{sup −1}E. coli concentration to zero within 4 h of incubation time with the Ag{sup +}-exchanged hybrid composite amount of 0.4 g L{sup −1}. The bioactivity and antimicrobial activity could be combined by ion-exchanging the composites first with Ca{sup 2+} and then with Ag{sup +}. These zeolite-A/chitosan hybrid composites have potential applications on tissue engineering and antimicrobial food packaging. - Graphical abstract: Zeolite A/chitosan hybrid composites were prepared by in situ transformation of precursors in the chitosan matrix, which possess macroporous structures and exhibit superior bioactivity and antimicrobial activity and potential biomedical

Facile synthesis of both needle-like and spherical hydroxyapatite nanoparticles: Effect of synthetic temperature and calcination on morphology, crystallite size and crystallinity

International Nuclear Information System (INIS)

Wijesinghe, W.P.S.L.; Mantilaka, M.M.M.G.P.G.; Premalal, E.V.A.; Herath, H.M.T.U.; Mahalingam, S.; Edirisinghe, M.; Rajapakse, R.P.V.J.; Rajapakse, R.M.G.

2014-01-01

Synthetic hydroxyapatite (HA) nanoparticles, that mimic natural HA, are widely used as biocompatible coatings on prostheses to repair and substitute human bones. In this study, HA nanoparticles are prepared by precipitating them from a precursor solution containing calcium sucrate and ammonium dihydrogen orthophosphate, at a Ca/P mole ratio of 1.67:1, at temperatures, ranging from 10 °C to 95 °C. A set of products, prepared at different temperatures, is analyzed for their crystallinity, crystallite size, morphology, thermal stability and composition, by X-ray diffraction (XRD), scanning electron microscopy (SEM), thermogravimetric analysis (TGA) and Fourier transform infrared (FT-IR) spectroscopic techniques, while the other set is analyzed after calcining the respective products, soon after their synthesis, for 3 h, at 700 °C. The as-prepared products, after 2 h of drying, without any calcination, are not crystalline, but they grow very slowly into needle-like morphologies, as they are ripened with time. The percentage crystallinity of the final products increases from 15% to 52%, with increasing the preparative temperature. The calcined samples always produce spherical nanoparticles of essentially the same diameter, between 90 nm and 100 nm, which does not change due to aging and preparative temperatures. Therefore, the same method can be utilized to synthesize both spherical and needle-like nanoparticles of hydroxyapatite, with well-defined sizes and shapes. The ability to use readily available cheap raw materials, for the synthesis of such well-defined crystallites of hydroxyapatite, is an added advantage of this method, which may be explored further for the scaling up of the procedures to suit to industrial scale synthesis of such hydroxyapatite nanoparticles. - Highlights: • Hydroxyapatite nanoparticles are synthesized using a simple precipitation method. • Both needle-like and spherical hydroxyapatite nanoparticles are synthesized. • The prepared

Facile synthesis of both needle-like and spherical hydroxyapatite nanoparticles: Effect of synthetic temperature and calcination on morphology, crystallite size and crystallinity

Energy Technology Data Exchange (ETDEWEB)

Wijesinghe, W.P.S.L.; Mantilaka, M.M.M.G.P.G. [Department of Chemistry, Faculty of Science, University of Peradeniya, Peradeniya 20400 (Sri Lanka); Post-graduate Institute of Science, P.O. Box: 25, University of Peradeniya, Peradeniya 20400 (Sri Lanka); Premalal, E.V.A. [Department of Materials Science, Shizuoka University, Johoku, Naka-ku Hamamatsu, 432-8011 (Japan); Herath, H.M.T.U. [Department of Medical Laboratory Science, Faculty of Allied Health Sciences, University of Peradeniya, Peradeniya 20400 (Sri Lanka); Mahalingam, S.; Edirisinghe, M. [Department of Mechanical Engineering, University College London, London WC1E 7JE (United Kingdom); Rajapakse, R.P.V.J. [Department of Veterinary Pathobiology, Faculty of Veterinary, University of Peradeniya, Peradeniya 20400 (Sri Lanka); Rajapakse, R.M.G., E-mail: rmgr@pdn.ac.lk [Department of Chemistry, Faculty of Science, University of Peradeniya, Peradeniya 20400 (Sri Lanka); Post-graduate Institute of Science, P.O. Box: 25, University of Peradeniya, Peradeniya 20400 (Sri Lanka)

2014-09-01

Synthetic hydroxyapatite (HA) nanoparticles, that mimic natural HA, are widely used as biocompatible coatings on prostheses to repair and substitute human bones. In this study, HA nanoparticles are prepared by precipitating them from a precursor solution containing calcium sucrate and ammonium dihydrogen orthophosphate, at a Ca/P mole ratio of 1.67:1, at temperatures, ranging from 10 °C to 95 °C. A set of products, prepared at different temperatures, is analyzed for their crystallinity, crystallite size, morphology, thermal stability and composition, by X-ray diffraction (XRD), scanning electron microscopy (SEM), thermogravimetric analysis (TGA) and Fourier transform infrared (FT-IR) spectroscopic techniques, while the other set is analyzed after calcining the respective products, soon after their synthesis, for 3 h, at 700 °C. The as-prepared products, after 2 h of drying, without any calcination, are not crystalline, but they grow very slowly into needle-like morphologies, as they are ripened with time. The percentage crystallinity of the final products increases from 15% to 52%, with increasing the preparative temperature. The calcined samples always produce spherical nanoparticles of essentially the same diameter, between 90 nm and 100 nm, which does not change due to aging and preparative temperatures. Therefore, the same method can be utilized to synthesize both spherical and needle-like nanoparticles of hydroxyapatite, with well-defined sizes and shapes. The ability to use readily available cheap raw materials, for the synthesis of such well-defined crystallites of hydroxyapatite, is an added advantage of this method, which may be explored further for the scaling up of the procedures to suit to industrial scale synthesis of such hydroxyapatite nanoparticles. - Highlights: • Hydroxyapatite nanoparticles are synthesized using a simple precipitation method. • Both needle-like and spherical hydroxyapatite nanoparticles are synthesized. • The prepared

Hydroxyapatite-chitosan based bioactive hybrid biomaterials with improved mechanical strength

Science.gov (United States)

Zima, A.

2018-03-01

Composites consisting of hydroxyapatite (HA) and chitosan (CTS) have recently been intensively studied. In this work, a novel inorganic-organic (I/O) HA/CTS materials in the form of granules were prepared through a simple solution-based chemical method. During the synthesis of these hybrids, the electrostatic complexes between positively charged, protonated amine groups of chitosan and the negative phosphate species (HPO42 - and H2PO4-) were formed. Our biocomposites belong to the class I of hybrids, which was confirmed by FTIR studies. XRD analysis revealed that the obtained materials consisted of hydroxyapatite as the only crystalline phase. Homogeneous dispersion of the components in HA/CTS composites was confirmed. The use of 17 wt% and 23 wt% of chitosan resulted in approximately 12-fold and 16-fold increase in the compressive strength of HA/CTS as compared to the non-modified HA material. During incubation of the studied materials in SBF, pH of the solution remained close to the physiological one. Formation of apatite layer on their surfaces indicated bioactive nature of the developed biomaterials.

A simple route to prepare stable hydroxyapatite nanoparticles suspension

International Nuclear Information System (INIS)

Han Yingchao; Wang Xinyu; Li Shipu

2009-01-01

A simple ultrasound assisted precipitation method with addition of glycosaminoglycans (GAGs) is proposed to prepare stable hydroxyapatite (HAP) nanoparticles suspension from the mixture of Ca(H 2 PO 4 ) 2 solution and Ca(OH) 2 solution. The product was characterized by XRD, FT-IR, TEM, HRTEM and particle size, and zeta potential analyzer. TEM observation shows that the suspension is composed of 10-20 nm x 20-50 nm short rod-like and 10-30 nm similar spherical HAP nanoparticles. The number-averaged particle size of stable suspension is about 30 nm between 11.6 and 110.5 nm and the zeta potential is -60.9 mV. The increase of stability of HAP nanoparticles suspension mainly depends on the electrostatic effect and steric effect of GAGs. The HAP nanoparticles can be easily transported into the cancer cells and exhibit good potential as gene or drug carrier system.

Modified composite microspheres of hydroxyapatite and poly(lactide-co-glycolide) as an injectable scaffold

Energy Technology Data Exchange (ETDEWEB)

Hu, Xixue [BNLMS, State Key Laboratory of Polymer Physics and Chemistry, Institute of Chemistry, Chinese Academy of Sciences, Beijing 100190 (China); CAS Key Laboratory for Biomedical Effects of Nanomaterials and Nanosafety, National Center for Nanoscience and Technology, Beijing 100190 (China); Shen, Hong, E-mail: shenhong516@iccas.ac.cn [BNLMS, State Key Laboratory of Polymer Physics and Chemistry, Institute of Chemistry, Chinese Academy of Sciences, Beijing 100190 (China); Yang, Fei [BNLMS, State Key Laboratory of Polymer Physics and Chemistry, Institute of Chemistry, Chinese Academy of Sciences, Beijing 100190 (China); Liang, Xinjie [CAS Key Laboratory for Biomedical Effects of Nanomaterials and Nanosafety, National Center for Nanoscience and Technology, Beijing 100190 (China); Wang, Shenguo, E-mail: wangsg@iccas.ac.cn [BNLMS, State Key Laboratory of Polymer Physics and Chemistry, Institute of Chemistry, Chinese Academy of Sciences, Beijing 100190 (China); Wu, Decheng, E-mail: dcwu@iccas.ac.cn [BNLMS, State Key Laboratory of Polymer Physics and Chemistry, Institute of Chemistry, Chinese Academy of Sciences, Beijing 100190 (China)

2014-02-15

The compound of hydroxyapatite-poly(lactide-co-glycolide) (HA-PLGA) was prepared by ionic bond between HA and PLGA. HA-PLGA was more stable than the simple physical blend of hydroxyapatite and poly(lactide-co-glycolide) (HA/PLGA). The surface of HA-PLGA microsphere fabricated by an emulsion–solvent evaporation method was rougher than that of HA/PLGA microspheres. Moreover, surface HA content of HA-PLGA microspheres was more than that of HA/PLGA microspheres. In vitro mouse OCT-1 osteoblast-like cell culture results showed that the HA-PLGA microspheres clearly promoted osteoblast attachment, proliferation and alkaline phosphatase activity. It was considered that surface rich HA component and rough surface of HA-PLGA microsphere enhanced cell growth and differentiation. The good cell affinity of the HA-PLGA microspheres indicated that they could be used as an injectable scaffold for bone tissue engineering.

Modified composite microspheres of hydroxyapatite and poly(lactide-co-glycolide) as an injectable scaffold

International Nuclear Information System (INIS)

Hu, Xixue; Shen, Hong; Yang, Fei; Liang, Xinjie; Wang, Shenguo; Wu, Decheng

2014-01-01

The compound of hydroxyapatite-poly(lactide-co-glycolide) (HA-PLGA) was prepared by ionic bond between HA and PLGA. HA-PLGA was more stable than the simple physical blend of hydroxyapatite and poly(lactide-co-glycolide) (HA/PLGA). The surface of HA-PLGA microsphere fabricated by an emulsion–solvent evaporation method was rougher than that of HA/PLGA microspheres. Moreover, surface HA content of HA-PLGA microspheres was more than that of HA/PLGA microspheres. In vitro mouse OCT-1 osteoblast-like cell culture results showed that the HA-PLGA microspheres clearly promoted osteoblast attachment, proliferation and alkaline phosphatase activity. It was considered that surface rich HA component and rough surface of HA-PLGA microsphere enhanced cell growth and differentiation. The good cell affinity of the HA-PLGA microspheres indicated that they could be used as an injectable scaffold for bone tissue engineering.

Hydroxyapatite Reinforced Coatings with Incorporated Detonationally Generated Nanodiamonds

International Nuclear Information System (INIS)

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

2010-01-01

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

In situ annealing of hydroxyapatite thin films

International Nuclear Information System (INIS)

Johnson, Shevon; Haluska, Michael; Narayan, Roger J.; Snyder, Robert L.

2006-01-01

Hydroxyapatite is a bioactive ceramic that mimics the mineral composition of natural bone. Unfortunately, problems with adhesion, poor mechanical integrity, and incomplete bone ingrowth limit the use of many conventional hydroxyapatite surfaces. In this work, we have developed a novel technique to produce crystalline hydroxyapatite thin films involving pulsed laser deposition and postdeposition annealing. Hydroxyapatite films were deposited on Ti-6Al-4V alloy and Si (100) using pulsed laser deposition, and annealed within a high temperature X-ray diffraction system. The transformation from amorphous to crystalline hydroxyapatite was observed at 340 deg. C. Mechanical and adhesive properties were examined using nanoindentation and scratch adhesion testing, respectively. Nanohardness and Young's modulus values of 3.48 and 91.24 GPa were realized in unannealed hydroxyapatite films. Unannealed and 350 deg. C annealed hydroxyapatite films exhibited excellent adhesion to Ti-6Al-4V alloy substrates. We anticipate that the adhesion and biological properties of crystalline hydroxyapatite thin films may be enhanced by further consideration of deposition and annealing parameters

Surface modification of calcium–copper hydroxyapatites using polyaspartic acid

International Nuclear Information System (INIS)

Othmani, Masseoud; Aissa, Abdallah; Bachoua, Hassen; Debbabi, Mongi

2013-01-01

Highlights: ► The reaction of polyaspartic acid with calcium hydroxyapatite and mixed calcium–copper hydroxyapatite is tested. ► Chemical analysis shows that the presence of copper in the apatitic structure increases the reactivity of the apatite surface. ► X-ray powder analysis shows the conservation of unique crystalline phase of hydroxyapatite after copper incorporation and/or PASP acid reacting. ► IR spectra show the formation of the formation of organometallic bond M-O-C (M=Ca or Cu) on the apatitic surface. ► Transmission electron microscopy (TEM) micrographs and atomic force microscopy (AFM) indicated that the texture surface was changed by the grafting. - Abstract: Mixed calcium–copper hydroxyapatite (Ca–CuHAp), with general formula Ca (10−x) Cu x (PO 4 ) 6 (OH) 2 , where 0 ≤ x ≤ 0.75 was prepared in aqueous medium in the presence of different concentrations of poly-L-aspartic acid (PASP). XRD, IR, TG-DTA, TEM-EDX, AFM and chemical analyses were used to characterize the structure, morphology and composition of the products. All techniques show the formation of new hybrid compounds Ca–CuHAp–PASP. The presence of the grafting moiety on the apatitic material is more significant with increasing of copper amount and/or organic concentration in the starting solution. These increases lead to the affectation of apatite crystallinity. The IR spectroscopy shows the conservation of (P-OH) band of (HPO 4 ) 2− groups, suggesting that PASP acid was interacted only with metallic cations of hydroxyapatite.

Preparation of zeolite-A/chitosan hybrid composites and their bioactivities and antimicrobial activities.

Science.gov (United States)

Yu, Liang; Gong, Jie; Zeng, Changfeng; Zhang, Lixiong

2013-10-01

Zeolite-A/chitosan hybrid composites with zeolite contents of 20-55 wt.% were prepared by in situ transformation of silica/chitosan mixtures in a sodium aluminate alkaline solution through impregnation-gelation-hydrothermal synthesis. The products were characterized by X-ray diffraction, diffuse reflectance infrared Fourier transform spectroscopy, scanning electron microscopy, thermogravimetric analysis, and mercury penetration porosimetry. Their in vitro bioactivities were examined using as-synthesized and Ca(2+)-exchanged hybrid composites in simulated body fluid (SBF) for hydroxyapatite (HAP) growth. Their antimicrobial activities for Escherichia coli (E. coli) in trypticase soy broth (TSB) were evaluated using Ag(+)-exchanged hybrid composites. The zeolite-A/chitosan hybrid composites could be prepared as various shapes, including cylinders, plates and thin films. They possessed macropores with pore sizes ranging from 100 to 300 μm and showed compressive mechanical strength as high as 3.2 MPa when the zeolite content was 35 wt.%. Fast growth on the Ca(2+)-exchanged hybrid composites was observed with the highest weight gain of 51.4% in 30 days. The 35 wt.% Ag(+)-exchanged hybrid composite showed the highest antimicrobial activity, which could reduce the 9×10(6) CFU mL(-1)E. coli concentration to zero within 4h of incubation time with the Ag(+)-exchanged hybrid composite amount of 0.4 g L(-1). The bioactivity and antimicrobial activity could be combined by ion-exchanging the composites first with Ca(2+) and then with Ag(+). These zeolite-A/chitosan hybrid composites have potential applications on tissue engineering and antimicrobial food packaging. Copyright © 2013 Elsevier B.V. All rights reserved.

Hydroxyapatite supported Ag3PO4 nanoparticles with higher visible light photocatalytic activity

International Nuclear Information System (INIS)

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

2012-01-01

Hydroxyapatite supported Ag 3 PO 4 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 Ag 3 PO 4 nanoparticles (6-17 nm in diameter) are well dispersed on the hydroxyapatite support and Ag 3 PO 4 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 Ag 3 PO 4 and the accelerated electron/hole separation resulting from the photoinduced electrons captured by the slow-released Ag + at the interface of Ag 3 PO 4 and hydroxyapatite is proposed for the nanocomposites on the enhancement of photocatalytic performance in comparison to that of pure Ag 3 PO 4 nanoparticles. The support of hydroxyapatite may also act as an absorbent which favors the mass transfer in heterogeneous photocatalysis reaction.

Degradation and biocompatibility of porous nano-hydroxyapatite/polyurethane composite scaffold for bone tissue engineering

Energy Technology Data Exchange (ETDEWEB)

Dong Zhihong [Research Center for Nano-Biomaterials, Analytical and Testing Center, Sichuan University, Chengdu 610064 (China); Shanghai Institute of Ceramics, Chinese Academy of Sciences, 1295 Dingxi Road, Shanghai 200050 (China); Li Yubao, E-mail: nic7504@scu.edu.cn [Research Center for Nano-Biomaterials, Analytical and Testing Center, Sichuan University, Chengdu 610064 (China); Zou Qin [Research Center for Nano-Biomaterials, Analytical and Testing Center, Sichuan University, Chengdu 610064 (China)

2009-04-01

Porous scaffold containing 30 wt% nano-hydroxyapatite (n-HA) and 70 wt% polyurethane (PU) from castor oil was prepared by a foaming method and investigated by X-ray diffraction (XRD), Fourier transform infrared absorption (FTIR), scanning electron microscopy (SEM) techniques. The results show that n-HA particles disperse homogeneously in the PU matrix. The porous scaffold has not only macropores of 100-800 {mu}m in size but also a lot of micropores on the walls of macropores. The porosity and compressive strength of scaffold are 80% and 271 kPa, respectively. After soaking in simulated body fluid (SBF), hydrolysis and deposition partly occur on the scaffold. The biological evaluation in vitro and in vivo shows that the n-HA/PU scaffold is non-cytotoxic and degradable. The porous structure provides a good microenvironment for cell adherence, growth and proliferation. The n-HA/PU composite scaffold can be satisfied with the basic requirement for tissue engineering, and has the potential to be applied in repair and substitute of human menisci of the knee-joint and articular cartilage.

Biocompatibility of sol-gel hydroxyapatite-titania composite and bilayer coatings

Energy Technology Data Exchange (ETDEWEB)

Sidane, D., E-mail: dj.sidane@yahoo.fr [Laboratoire de Génie de l' Environnement (LGE), Faculté de Technologie, Université de Bejaia, 06000, Bejaia (Algeria); Rammal, H. [Equipe d' Accueil 4691 Biomatériaux et Inflammation en Site Osseux, SFR-CAP Santé (FED 4231), Université de Reims Champagne Ardenne, 1 Avenue du Maréchal Juin, 51100 Reims (France); Beljebbar, A. [UMR CNRS 7369, Equipe MéDIAN Biophotonique et Technologies pour la Santé, UFR de Pharmacie, SFR-CAP Santé (FED 4231), Université de Reims Champagne Ardenne, 51 rue Cognacq-Jay, 51096 Reims (France); Gangloff, S.C. [Equipe d' Accueil 4691 Biomatériaux et Inflammation en Site Osseux, SFR-CAP Santé (FED 4231), Université de Reims Champagne Ardenne, 1 Avenue du Maréchal Juin, 51100 Reims (France); Chicot, D. [FRE 3723 - LML - Laboratoire de Mécanique de Lille, Univ. Lille, 59000 Lille (France); Velard, F. [Equipe d' Accueil 4691 Biomatériaux et Inflammation en Site Osseux, SFR-CAP Santé (FED 4231), Université de Reims Champagne Ardenne, 1 Avenue du Maréchal Juin, 51100 Reims (France); Khireddine, H. [Laboratoire de Génie de l' Environnement (LGE), Faculté de Technologie, Université de Bejaia, 06000, Bejaia (Algeria); and others

2017-03-01

Titania-Hydroxyapatite (TiO{sub 2}/HAP) reinforced coatings are proposed to enhance the bioactivity and corrosion resistance of 316L stainless steel (316L SS). Herein, spin- and dip-coating sol-gel processes were investigated to construct two kinds of coatings: TiO{sub 2}/HAP composite and TiO{sub 2}/HAP bilayer. Physicochemical characterization highlighted the bioactivity response of the TiO{sub 2}/HAP composite once incubated in physiological conditions for 7 days whereas the TiO{sub 2}/HAP bilayer showed instability and dissolution. Biological analysis revealed a failure in human stem cells adhesion on TiO{sub 2}/HAP bilayer whereas on TiO{sub 2}/HAP composite the presence of polygonal shaped cells, possessing good behaviour attested a good biocompatibility of the composite coating. Finally, TiO{sub 2}/HAP composite with hardness up to 0.6 GPa and elastic modulus up to 18 GPa, showed an increased corrosion resistance of 316L SS. In conclusion, the user-friendly sol-gel processes led to bioactive TiO{sub 2}/HAP composite buildup suitable for biomedical applications. - Highlights: • 316L SS implant TiO{sub 2} reinforced HAP coatings were investigated and compared. • TiO{sub 2}/HAP composite had better structural features and biocompatible properties. • Improvement of 316L SS implants corrosion resistance. • TiO{sub 2}/HAP composite mechanical properties close to bone tissue • Low cost and desired material for hard tissue applications.

Biocompatibility of sol-gel hydroxyapatite-titania composite and bilayer coatings

International Nuclear Information System (INIS)

Sidane, D.; Rammal, H.; Beljebbar, A.; Gangloff, S.C.; Chicot, D.; Velard, F.; Khireddine, H.

2017-01-01

Titania-Hydroxyapatite (TiO 2 /HAP) reinforced coatings are proposed to enhance the bioactivity and corrosion resistance of 316L stainless steel (316L SS). Herein, spin- and dip-coating sol-gel processes were investigated to construct two kinds of coatings: TiO 2 /HAP composite and TiO 2 /HAP bilayer. Physicochemical characterization highlighted the bioactivity response of the TiO 2 /HAP composite once incubated in physiological conditions for 7 days whereas the TiO 2 /HAP bilayer showed instability and dissolution. Biological analysis revealed a failure in human stem cells adhesion on TiO 2 /HAP bilayer whereas on TiO 2 /HAP composite the presence of polygonal shaped cells, possessing good behaviour attested a good biocompatibility of the composite coating. Finally, TiO 2 /HAP composite with hardness up to 0.6 GPa and elastic modulus up to 18 GPa, showed an increased corrosion resistance of 316L SS. In conclusion, the user-friendly sol-gel processes led to bioactive TiO 2 /HAP composite buildup suitable for biomedical applications. - Highlights: • 316L SS implant TiO 2 reinforced HAP coatings were investigated and compared. • TiO 2 /HAP composite had better structural features and biocompatible properties. • Improvement of 316L SS implants corrosion resistance. • TiO 2 /HAP composite mechanical properties close to bone tissue • Low cost and desired material for hard tissue applications

Hydroxyapatite coatings with oriented nanoplate and nanorod arrays: Fabrication, morphology, cytocompatibility and osteogenic differentiation

Energy Technology Data Exchange (ETDEWEB)

Chen, Wei [The Education Ministry Key Lab of Resource Chemistry and Shanghai Key Laboratory of Rare Earth Functional Materials, Shanghai Normal University, Shanghai 200234 (China); Tian, Bo [Shanghai Key Laboratory of Orthopedic Implant, Department of Orthopedic Surgery, Shanghai Ninth People' s Hospital, Shanghai Jiao Tong University School of Medicine, Shanghai 200011 (China); Lei, Yong; Ke, Qin-Fei [The Education Ministry Key Lab of Resource Chemistry and Shanghai Key Laboratory of Rare Earth Functional Materials, Shanghai Normal University, Shanghai 200234 (China); Zhu, Zhen-An, E-mail: zhuzhenan2006@126.com [Shanghai Key Laboratory of Orthopedic Implant, Department of Orthopedic Surgery, Shanghai Ninth People' s Hospital, Shanghai Jiao Tong University School of Medicine, Shanghai 200011 (China); Guo, Ya-Ping, E-mail: ypguo@shnu.edu.cn [The Education Ministry Key Lab of Resource Chemistry and Shanghai Key Laboratory of Rare Earth Functional Materials, Shanghai Normal University, Shanghai 200234 (China)

2016-10-01

Hydroxyapatite (HA) crystals exhibit rod-like shape with c-axis orientation and plate-like shape with a(b)-axis orientation in vertebrate bones and tooth enamel surfaces, respectively. Herein, we report the synthesis of HA coatings with the oriented nanorod arrays (RHACs) and HA coatings with oriented nanoplate arrays (PHACs) by using bioglass coatings as sacrificial templates. After soaking in simulated body fluid (SBF) at 120 °C, the bioglass coatings are hydrothermally converted into the HA coatings via a dissolution-precipitation reaction. If the Ca/P ratios in SBF are 2.50 and 1.25, the HA crystals on the coatings are oriented nanorod arrays and oriented nanoplate arrays, respectively. Moreover, the bioglass coatings are treated with SBF at 37 °C, plate-like HA coatings with a low crystallinity (SHACs) are prepared. As compared with the Ti6Al4V and SHACs, the human bone marrow stromal cells (hBMSCs) on the RHACs and PHACs have better cell adhesion, spreading, proliferation and osteogenic differentiation because of their moderately hydrophilic surfaces and similar chemical composition, morphology and crystal orientation to human hard tissues. Notably, the morphologies of HA crystals have no obvious effects on cytocompatibility and osteogenic differentiation. Hence, the HA coatings with oriented nanoplate arrays or oriented nanorod arrays have a great potential for orthopedic applications. - Highlights: • We prepare hydroxyapatite coatings with oriented nanoplate and nanorod arrays. • Hydroxyapatite coatings are in situ converted from bioglass coatings. • Hydroxyapatite coatings have good cytocompatibility and osteogenic differentiation. • Oriented hydroxyapatite coatings are used for orthopedic implants.

Hydroxyapatite coatings with oriented nanoplate and nanorod arrays: Fabrication, morphology, cytocompatibility and osteogenic differentiation

International Nuclear Information System (INIS)

Chen, Wei; Tian, Bo; Lei, Yong; Ke, Qin-Fei; Zhu, Zhen-An; Guo, Ya-Ping

2016-01-01

Hydroxyapatite (HA) crystals exhibit rod-like shape with c-axis orientation and plate-like shape with a(b)-axis orientation in vertebrate bones and tooth enamel surfaces, respectively. Herein, we report the synthesis of HA coatings with the oriented nanorod arrays (RHACs) and HA coatings with oriented nanoplate arrays (PHACs) by using bioglass coatings as sacrificial templates. After soaking in simulated body fluid (SBF) at 120 °C, the bioglass coatings are hydrothermally converted into the HA coatings via a dissolution-precipitation reaction. If the Ca/P ratios in SBF are 2.50 and 1.25, the HA crystals on the coatings are oriented nanorod arrays and oriented nanoplate arrays, respectively. Moreover, the bioglass coatings are treated with SBF at 37 °C, plate-like HA coatings with a low crystallinity (SHACs) are prepared. As compared with the Ti6Al4V and SHACs, the human bone marrow stromal cells (hBMSCs) on the RHACs and PHACs have better cell adhesion, spreading, proliferation and osteogenic differentiation because of their moderately hydrophilic surfaces and similar chemical composition, morphology and crystal orientation to human hard tissues. Notably, the morphologies of HA crystals have no obvious effects on cytocompatibility and osteogenic differentiation. Hence, the HA coatings with oriented nanoplate arrays or oriented nanorod arrays have a great potential for orthopedic applications. - Highlights: • We prepare hydroxyapatite coatings with oriented nanoplate and nanorod arrays. • Hydroxyapatite coatings are in situ converted from bioglass coatings. • Hydroxyapatite coatings have good cytocompatibility and osteogenic differentiation. • Oriented hydroxyapatite coatings are used for orthopedic implants.

Development of hydroxyapatite bone cement for controlled drug ...

Indian Academy of Sciences (India)

The purpose of this work was to study the preparation and characterization of drug–hydroxyapatite cement. The hydroxyapatite (HA) cement has been synthesized by using tricalcium phosphate, calcium carbonate and dicalcium phosphate anhydrous with sodium hydrogen phosphate as liquid phase. The effect of added ...

Zirconia-hydroxyapatite composite material with micro porous structure.

Science.gov (United States)

Matsumoto, Takuya Junior; An, Sang-Hyun; Ishimoto, Takuya; Nakano, Takayoshi; Matsumoto, Takuya; Imazato, Satoshi

2011-11-01

Titanium plates and apatite blocks are commonly used for restoring large osseous defects in dental and orthopedic surgery. However, several cases of allergies against titanium have been recently reported. Also, sintered apatite block does not possess sufficient mechanical strength. In this study, we attempted to fabricate a composite material that has mechanical properties similar to biocortical bone and high bioaffinity by compounding hydroxyapatite (HAp) with the base material zirconia (ZrO(2)), which possesses high mechanical properties and low toxicity toward living organisms. After mixing the raw material powders at several different ZrO(2)/HAp mixing ratios, the material was compressed in a metal mold (8 mm in diameter) at 5 MPa. Subsequently, it was sintered for 5 h at 1500°C to obtain the ZrO(2)/HAp composite. The mechanical property and biocompatibility of materials were investigated. Furthermore, osteoconductivity of materials was investigated by animal studies. A composite material with a minute porous structure was successfully created using ZrO(2)/HAp powders, having different particle sizes, as the starting material. The material also showed high protein adsorption and a favorable cellular affinity. When the mixing ratio was ZrO(2)/HAp=70/30, the strength was equal to cortical bone. Furthermore, in vivo experiments confirmed its high osteoconductivity. The composite material had strength similar to biocortical bones with high cell and tissue affinities by compounding ZrO(2) and HAp. The ZrO(2)/HAp composite material having micro porous structure would be a promising bone restorative material. Copyright © 2011 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

The effect of Hydroxyapatite/collagen I composites, bone marrow aspirate and bone graft on fixation of bone implants in sheep

DEFF Research Database (Denmark)

Babiker, Hassan

  The effect of Hydroxyapatite/collagen I composites, bone marrow aspirate and bone graft on fixation of bone implants IN SHEEP   Ph.D. Student, Hassan Babiker; Associate Professor, Ph.D. Ming Ding; Professor, dr.med., Soren Overgaard. Department of Orthopaedic Surgery, Odense University Hospital......, Odense, Denmark   Background: Hydroxyapatite and collagen composites (HA/coll) have the potential in mimicking and replacing skeletal bones. This study attempted to determine the effect of newly developed HA/coll-composites with and without bone marrow aspirate (BMA) in order to enhance the fixation...... of bone implants.   Materials and Methods: Titanium alloy implants were inserted into bilateral femoral condyles of 8 skeletally mature sheep, four in each sheep. The implant has a circumferential gap of 2 mm. The gap was filled with: HA/coll; HA/coll-BMA; autograft or allograft. Allograft was served...

Mechanical characterisation of porous glass reinforced hydroxyapatite ceramics: Bonelike®

Directory of Open Access Journals (Sweden)

Marcelo Henrique Prado da Silva

2003-06-01

Full Text Available In the present study, mechanical properties of porous glass reinforced hydroxyapatite bioceramics were assessed by microhardness, bending and compression tests and fracture toughness determination. Porous discs were produced by a dry method using wax spheres as pore formers. Green bodies were sintered and the final microstructure of the composites consists of hydroxyapatite, alpha and beta tricalcium phosphate (alpha and b-Ca3(PO42due to the reaction between the glassy phase and the hydroxyapatite matrix. The results of the mechanical tests showed that the glassy phase yielded higher fracture toughness and bending strength when comparing with literature data for single hydroxyapatite. There is a compromise between mechanical properties and the porosity level for bioceramics: for example, according to Weibull statistics for composites with 65% porosity the maximum bending stress level is 0.2 MPa for 100% survival probability whereas this stress level increases to 2.5 MPa for composites with 40%. However, only the 65% porosity composite samples seem to have the complete adequate morphology for bone ingrowth.

Bioactivity and electrochemical behavior of hydroxyapatite-silicon-multi walled carbon nano-tubes composite coatings synthesized by EPD on NiTi alloys in simulated body fluid

Energy Technology Data Exchange (ETDEWEB)

Khalili, V., E-mail: V_khalili@sut.ac.ir [Department of Materials Engineering, Engineering Faculty, University of Bonab, Bonab (Iran, Islamic Republic of); Khalil-Allafi, J. [Research Center for Advanced Materials and Mineral Processing, Faculty of Materials Engineering, Sahand University of Technology, Tabriz (Iran, Islamic Republic of); Frenzel, J.; Eggeler, G. [Institute for Materials, Faculty of Mechanical Engineering, Ruhr-University Bochum, 44801 Bochum (Germany)

2017-02-01

In order to improve the surface bioactivity of NiTi bone implant and corrosion resistance, hydroxyapatite coating with addition of 20 wt% silicon, 1 wt% multi walled carbon nano-tubes and both of them were deposited on a NiTi substrate using a cathodic electrophoretic method. The apatite formation ability was estimated using immersion test in the simulated body fluid for 10 days. The SEM images of the surface of coatings after immersion in simulated body fluid show that the presence of silicon in the hydroxyapatite coatings accelerates in vitro growth of apatite layer on the coatings. The Open-circuit potential and electrochemical impedance spectroscopy were measured to evaluate the electrochemical behavior of the coatings in the simulated body fluid at 37 °C. The results indicate that the compact structure of hydroxyapatite-20 wt% silicon and hydroxyapatite-20 wt% silicon-1 wt% multi walled carbon nano-tubes coatings could efficiently increase the corrosion resistance of NiTi substrate. - Highlights: • The composite coatings of HA, Si and MWCNTs was prepared using electrophoretic deposition. • The presence of 1 wt.% MWCNTs in the HA coating provides more nucleation cites of apatite crystallites in SBF. • The presence of Si in HA coating increases the growth rate of apatite crystallites with the Ca/P atomic ratio of 1.67. • The EIS indicate the compact HA-20%Si and HA-20%Si-1%MWCNTs coatings efficiently increase corrosion resistance of NiTi. • The porous HA and HA-1%MWCNTs do not increase significantly corrosion resistance due to the easy diffusion path.

In vitro and in vivo study to the biocompatibility and biodegradation of hydroxyapatite/poly(vinyl alcohol)/gelatin composite.

NARCIS (Netherlands)

Wang, M.; Li, Y.; Wu, J.; Xu, F.; Zuo, Y.; Jansen, J.A.

2008-01-01

A novel porous composite material composed of hydroxyapatite, poly(vinyl alcohol) (PVA), and gelatin (Gel) was fabricated by emulsification. Scanning electron microscopy showed that the material had a well-interconnected porous structure including many macropores (100-500 microm) and micropores

Electrochemical properties of Ti3+ doped Ag-Ti nanotube arrays coated with hydroxyapatite

Science.gov (United States)

Zhang, Hangzhou; Shi, Xiaoguo; Tian, Ang; Wang, Li; Liu, Chuangwei

2018-04-01

Ag-Ti nanotube array was prepared by simple anodic oxidation method and uniform hydroxyapatite were electrochemically deposited on the nanotubes, and then characterized by SEM, XRD, XPS and EIS. In order to investigate the influence of Ti3+ on the electrochemical deposition of hydroxyapatite on the nanotubes, the Ag-Ti nanotube array self-doped with Ti3+ was prepared by one step reduction method. The experiment results revealed that the Ti3+ can promote the grow rate of hydroxyapatite coatings on nanotube surface. The hydroxyapatite coated Ag-Ti nanotube arrays with Ti3+ exhibit excellent stability and higher corrosion resistance. Moreover, the compact and dense hydroxyapatite coating can also prevent the Ag atom erosion from the Ag-Ti nanotube.

Micro-tribological properties of hydroxyapatite-based composites in dry sliding

International Nuclear Information System (INIS)

Lu, Zhi; Liu, Yong; Liu, Bowei; Liu, Meiling

2013-01-01

Highlights: ► The micro-tribological properties of HA-based composites were investigated. ► The micro-scale test is greatly benefits to the analyses of the wear mechanism. ► A higher speed benefits the formation of the lubricating layer, when high in Cu. ► With increasing Cu, the wear mechanism shift from abrasive wear to adhesive wear. - Abstract: The micro-tribological properties of hydroxyapatite-based composites sliding against alumina balls were investigated by a ball-on-block tribometer. Surface properties of the HA-based composites were measured and examined by using atomic force microscopy and scanning electron microscopy. Running-in behavior during sliding tests was studied as a function of surface properties. The effects of copper fibers, initial surface roughness, and sliding velocity on the friction coefficient and the wear resistance were discussed. Results show that a lubricant layer benefits the tribological properties of the composites. With the increasing of Cu, the lubricant layer is more stable, and resistant to increase of the sliding velocity. At a Cu content of 15%, the wear curve is very stable even at a velocity of 900 rpm. The wear mechanism also changes from abrasive wear to adhesive wear. A model was quoted to describe the relationship between the wear resistant and the load

Influence of preparation method on hydroxyapatite porous scaffolds

Indian Academy of Sciences (India)

Administrator

Hydroxyapatite (HA) is extensively used in medical applications as an artificial bone because of its similarity to ... system, have been applied to fabricate HA porous scaffolds. In this work .... ceramic structured by the colloidal processing was.

In situ ring-opening polymerization of hydroxyapatite/poly (ethylene ...

Indian Academy of Sciences (India)

2016-08-26

Aug 26, 2016 ... Hydroxyapatite/poly(ethylene adipate)--poly(ethylene terephthalate) biomaterials (HAp/PEA--PET) have been prepared by ring opening polymerization (ROP) of cyclic oligo(ethylene adipate)--oligo(ethylene terephthalate) (C-OEA--C-OET) in the porous hydroxyapatite (HAp) scaffolds at 250 ...

Surface modification of calcium-copper hydroxyapatites using polyaspartic acid

Energy Technology Data Exchange (ETDEWEB)

Othmani, Masseoud; Aissa, Abdallah; Bachoua, Hassen [Laboratoire de Physico-Chimie des Materiaux, Faculte des Sciences de Monastir, 5019 Monastir (Tunisia); Debbabi, Mongi, E-mail: m.debbabi@yahoo.fr [Laboratoire de Physico-Chimie des Materiaux, Faculte des Sciences de Monastir, 5019 Monastir (Tunisia)

2013-01-01

Highlights: Black-Right-Pointing-Pointer The reaction of polyaspartic acid with calcium hydroxyapatite and mixed calcium-copper hydroxyapatite is tested. Black-Right-Pointing-Pointer Chemical analysis shows that the presence of copper in the apatitic structure increases the reactivity of the apatite surface. Black-Right-Pointing-Pointer X-ray powder analysis shows the conservation of unique crystalline phase of hydroxyapatite after copper incorporation and/or PASP acid reacting. Black-Right-Pointing-Pointer IR spectra show the formation of the formation of organometallic bond M-O-C (M=Ca or Cu) on the apatitic surface. Black-Right-Pointing-Pointer Transmission electron microscopy (TEM) micrographs and atomic force microscopy (AFM) indicated that the texture surface was changed by the grafting. - Abstract: Mixed calcium-copper hydroxyapatite (Ca-CuHAp), with general formula Ca{sub (10-x)}Cu{sub x}(PO{sub 4}){sub 6}(OH){sub 2}, where 0 {<=} x {<=} 0.75 was prepared in aqueous medium in the presence of different concentrations of poly-L-aspartic acid (PASP). XRD, IR, TG-DTA, TEM-EDX, AFM and chemical analyses were used to characterize the structure, morphology and composition of the products. All techniques show the formation of new hybrid compounds Ca-CuHAp-PASP. The presence of the grafting moiety on the apatitic material is more significant with increasing of copper amount and/or organic concentration in the starting solution. These increases lead to the affectation of apatite crystallinity. The IR spectroscopy shows the conservation of (P-OH) band of (HPO{sub 4}){sup 2-} groups, suggesting that PASP acid was interacted only with metallic cations of hydroxyapatite.

Zirconia/Hydroxyapatite Composites Synthesized Via Sol-Gel: Influence of Hydroxyapatite Content and Heating on Their Biological Properties

Science.gov (United States)

Bollino, Flavia; Armenia, Emilia; Tranquillo, Elisabetta

2017-01-01

Zirconia (ZrO2) and zirconia-based glasses and ceramics are materials proposed for use in the dental and orthopedic fields. In this work, ZrO2 glass was modified by adding different amounts of bioactive and biocompatible hydroxyapatite (HAp). ZrO2/HAp composites were synthesized via the sol-gel method and heated to different temperatures to induce modifications of their chemical structure, as ascertained by Fourier transform infrared spectroscopy (FTIR) analysis. The aim was to investigate the effect of both HAp content and heating on the biological performances of ZrO2. The materials’ bioactivity was studied by soaking samples in a simulated body fluid (SBF). FTIR and scanning electron microscopy (SEM)) analyses carried out after exposure to SBF showed that all materials are bioactive, i.e., they are able to form a hydroxyapatite layer on their surface. Moreover, the samples were soaked in a solution containing bovine serum albumin (BSA). FTIR analysis proved that the synthesized materials are able to adsorb the blood protein, the first step of cell adhesion. WST-8 ([2-(2-methoxy-4-nitrophenyl)-3-(4-nitrophenyl)-5-(2,4-disulfophenyl)-2H-tetrazolium, monosodium salt]) assay showed that no cytotoxicity effects were induced by the materials’ extract. However, the results proved that bioactivity increases with both the HAp content and the temperature used for the thermal treatment, whereas biocompatibility increases with heating but is not affected by the HAp content. PMID:28773116

Effects of increased collagen-matrix density on the mechanical properties and in vivo absorbability of hydroxyapatite-collagen composites as artificial bone materials

Energy Technology Data Exchange (ETDEWEB)

Yunoki, Shunji [Life Science Group, Tokyo Metropolitan Industrial Technology Research Institute, 2-11-1 Fukasawa, Setagaya-ku, Tokyo 158-0081 (Japan); Sugiura, Hiroaki; Kondo, Eiji; Yasuda, Kazunori [Department of Sports Medicine and Joint Surgery, Graduate School of Medicine, Hokkaido University, Kita-15 Nishi-7, Sapporo, Hokkaido 060-8638 Japan (Japan); Ikoma, Toshiyuki; Tanaka, Junzo, E-mail: yunoki.shunji@iri-tokyo.jp [Department of Metallurgy and Ceramics Science, 2-12-1-S7-1, Ookayama, Meguro-ku, Tokyo 152-8550 (Japan)

2011-02-15

The aim of this study was to evaluate the effects of increased collagen-matrix density on the mechanical properties and in vivo absorbability of porous hydroxyapatite (HAp)-collagen composites as artificial bone materials. Seven types of porous HAp-collagen composites were prepared from HAp nanocrystals and dense collagen fibrils. Their densities and HAp/collagen weight ratios ranged from 122 to 331 mg cm{sup -3} and from 20/80 to 80/20, respectively. The flexural modulus and strength increased with an increase in density, reaching 2.46 {+-} 0.48 and 0.651 {+-} 0.103 MPa, respectively. The porous composites with a higher collagen-matrix density exhibited much higher mechanical properties at the same densities, suggesting that increasing the collagen-matrix density is an effective way of improving the mechanical properties. It was also suggested that other structural factors in addition to collagen-matrix density are required to achieve bone-like mechanical properties. The in vivo absorbability of the composites was investigated in bone defects of rabbit femurs, demonstrating that the absorption rate decreased with increases in the composite density. An exhaustive increase in density is probably limited by decreases in absorbability as artificial bones.

Effects of increased collagen-matrix density on the mechanical properties and in vivo absorbability of hydroxyapatite-collagen composites as artificial bone materials

International Nuclear Information System (INIS)

Yunoki, Shunji; Sugiura, Hiroaki; Kondo, Eiji; Yasuda, Kazunori; Ikoma, Toshiyuki; Tanaka, Junzo

2011-01-01

The aim of this study was to evaluate the effects of increased collagen-matrix density on the mechanical properties and in vivo absorbability of porous hydroxyapatite (HAp)-collagen composites as artificial bone materials. Seven types of porous HAp-collagen composites were prepared from HAp nanocrystals and dense collagen fibrils. Their densities and HAp/collagen weight ratios ranged from 122 to 331 mg cm -3 and from 20/80 to 80/20, respectively. The flexural modulus and strength increased with an increase in density, reaching 2.46 ± 0.48 and 0.651 ± 0.103 MPa, respectively. The porous composites with a higher collagen-matrix density exhibited much higher mechanical properties at the same densities, suggesting that increasing the collagen-matrix density is an effective way of improving the mechanical properties. It was also suggested that other structural factors in addition to collagen-matrix density are required to achieve bone-like mechanical properties. The in vivo absorbability of the composites was investigated in bone defects of rabbit femurs, demonstrating that the absorption rate decreased with increases in the composite density. An exhaustive increase in density is probably limited by decreases in absorbability as artificial bones.

Greener synthesis of electrospun collagen/hydroxyapatite composite fibers with an excellent microstructure for bone tissue engineering

Science.gov (United States)

Zhou, Yuanyuan; Yao, Hongchang; Wang, Jianshe; Wang, Dalu; Liu, Qian; Li, Zhongjun

2015-01-01

In bone tissue engineering, collagen/hydroxyapatite (HAP) fibrous composite obtained via electrospinning method has been demonstrated to support the cells’ adhesion and bone regeneration. However, electrospinning of natural collagen often requires the use of cytotoxic organic solvents, and the HAP crystals were usually aggregated and randomly distributed within a fibrous matrix of collagen, limiting their clinical potential. Here, an effective and greener method for the preparation of collagen/HAP composite fibers was developed for the first time, and this green product not only had 40 times higher mechanical properties than that previously reported, but also had an excellent microstructure similar to that of natural bone. By dissolving type I collagen in environmentally friendly phosphate buffered saline/ethanol solution instead of the frequently-used cytotoxic organic solvents, followed with the key step of desalination, co-electrospinning the collagen solution with the HAP sol, generates a collagen/HAP composite with a uniform and continuous fibrous morphology. Interestingly, the nano-HAP needles were found to preferentially orient along the longitudinal direction of the collagen fibers, which mimicked the nanostructure of natural bones. Based on the characterization of the related products, the formation mechanism for this novel phenomenon was proposed. After cross-linking with 1-ethyl-3-(3-dimethyl-aminopropyl)-1-carbodiimide hydrochloride/N-hydroxysuccinimide, the obtained composite exhibited a significant enhancement in mechanical properties. In addition, the biocompatibility of the obtained composite fibers was evaluated by in vitro culture of the human myeloma cells (U2-OS). Taken together, the process outlined herein provides an effective, non-toxic approach for the fabrication of collagen/HAP composite nanofibers that could be good candidates for bone tissue engineering. PMID:25995630

Microstructure and Mechanical Properties of Graphene-Reinforced Titanium Matrix/Nano-Hydroxyapatite Nanocomposites.

Science.gov (United States)

Li, Feng; Jiang, Xiaosong; Shao, Zhenyi; Zhu, Degui; Zhu, Minhao

2018-04-16

Biomaterial composites made of titanium and hydroxyapatite (HA) powder are among the most important biomedicalmaterials due to their good mechanical properties and biocompatibility. In this work, graphene-reinforced titanium matrix/nano-hydroxyapatite nanocomposites were prepared by vacuum hot-pressing sintering. The microstructure and mechanical properties of graphene-reinforced titanium matrix/nano-hydroxyapatite nanocomposites with different graphene content were systematically investigated. Microstructures of the nanocomposites were examined by X-ray diffraction (XRD), back scattered electron imaging (BSE), scanning electron microscope (SEM) equipped with energy dispersive spectrometer (EDS), electron probe microanalyzer (EPMA), and transmission electron microscope (TEM). The mechanical properties were determined from microhardness, shear strength, and compressive strength. Results showed that during the high-temperature sintering process, complex chemical reactions occurred, resulting in new phases of nucleation such as Ca₃(PO₄)₂, Ti x P y , and Ti₃O.The new phases, which easily dropped off under the action of external force, could hinder the densification of sintering and increase the brittleness of the nanocomposites. Results demonstrated that graphene had an impact on the microstructure and mechanical properties of the nanocomposites. Based on the mechanical properties and microstructure of the nanocomposites, the strengthening and fracture mechanisms of the graphene-reinforced titanium matrix/nano-hydroxyapatite nanocomposites with different graphene content were analyzed.

Microstructure and Mechanical Properties of Graphene-Reinforced Titanium Matrix/Nano-Hydroxyapatite Nanocomposites

Directory of Open Access Journals (Sweden)

Feng Li

2018-04-01

Full Text Available Biomaterial composites made of titanium and hydroxyapatite (HA powder are among the most important biomedicalmaterials due to their good mechanical properties and biocompatibility. In this work, graphene-reinforced titanium matrix/nano-hydroxyapatite nanocomposites were prepared by vacuum hot-pressing sintering. The microstructure and mechanical properties of graphene-reinforced titanium matrix/nano-hydroxyapatite nanocomposites with different graphene content were systematically investigated. Microstructures of the nanocomposites were examined by X-ray diffraction (XRD, back scattered electron imaging (BSE, scanning electron microscope (SEM equipped with energy dispersive spectrometer (EDS, electron probe microanalyzer (EPMA, and transmission electron microscope (TEM. The mechanical properties were determined from microhardness, shear strength, and compressive strength. Results showed that during the high-temperature sintering process, complex chemical reactions occurred, resulting in new phases of nucleation such as Ca3(PO42, TixPy, and Ti3O.The new phases, which easily dropped off under the action of external force, could hinder the densification of sintering and increase the brittleness of the nanocomposites. Results demonstrated that graphene had an impact on the microstructure and mechanical properties of the nanocomposites. Based on the mechanical properties and microstructure of the nanocomposites, the strengthening and fracture mechanisms of the graphene-reinforced titanium matrix/nano-hydroxyapatite nanocomposites with different graphene content were analyzed.

Enhanced osteoconductivity of sodium-substituted hydroxyapatite by system instability.

Science.gov (United States)

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. © 2013 Wiley Periodicals, Inc.

Preparation Of Porous And Dense Bodies From Hydroxyapatite Powders Prepared Via Sol-Gel Technique

International Nuclear Information System (INIS)

Sopyan, Lis

2001-01-01

Hydroxyapatite (HA) ceramics is clinically proven and, thus, a reliable material for medical applications, that is, for use in dental and orthopedical surgery to fill cavities in bones. In this paper, we report a preliminary study on development of HA porous and dense materials manufactured using fine HA powders prepared via a sol-gel technique. In the preparation of HA porous bodies, slurries of the as-prepared powder were prepared with an adjusted loading ofHA, using Duramax of 0-3021 type as dispersant. After soaking cellulosic sponges into the slurry, the sponges were dried and then subjected to heat-treatment at 600 o C, followed by sintering at 1250 o C for I h. The apparent density of the porous bodies is 1.290 g/cm 3 , with a porosity of 59%. The sintering shrinkage is about 20% (in respect of dimension) and 44 % (in respect of volume). Morphological evaluation of the porous bodies showed that the samples contained macropores of 1-2 mm diameter and micropores of 1-2 μm diameter. The measurement of mechanical strength provided 1.31 ± 0.30 MPa. Subsequently, dense samples were prepared from the as-prepared powder. In this case, the powder was mixed with poly(vinyl alcohol) and distilled water to make a slurry. The mixture was mixed using Zirconia balls as the crusher for 2h. The suspension was then spray-dried, and well-dispersed powder was obtained. The powder was compressed uniaxially using cold pressing technique at 800 kglcm2 and the pellets obtained were sintered in air at : 250 o C for I h. The sintered dense bodies have apparent density of 2.855 g/cm 3 , with a 10% porosity. The flexural strength of the dense bodies measured on the specimens of riimension 2 mm x 2.5 mm gave rise to the considerable value of 57.7 MPa

N-Lauroyl sarcosine sodium salt mediated formation of hydroxyapatite microspheres via a hydrothermal route

International Nuclear Information System (INIS)

Xiao Xiufeng; Zheng Xuan; Liu Rongfang; Lu Yihua; Wu Shanshan

2012-01-01

Dandelion-like hydroxyapatite (HA) microspheres were successfully prepared using Ca(NO 3 ) 2 ·4H 2 O and (NH 4 ) 3 PO 4 ·3H 2 O as raw materials and N-Lauroyl sarcosine sodium salt (Sar-Na) as template via a hydrothermal route. The chemical composition, structure, morphology and thermal properties of the samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscope (FTIR), Scanning electron microscope (SEM) and Thermal gravimetric analysis (TG), respectively. The results demonstrate that, Sar-Na has great impact on the morphology of HA. With increasing the amount of Sar-Na, the morphology of HA varies from nanograins to nanorods, finally grows into dandelion-like microstructure. The obtained dandelion-like HA microspheres about 6 μm in diameter are composed of radially oriented nanorods. Furthermore, the possible formation mechanism of morphology change is also discussed. - Highlights: ► N-Lauroyl sarcosine sodium salt is firstly used to control the morphology of hydroxyapatite. ► The mechanism of Sar-Na on the morphology of hydroxyapatite are discussed in this paper. ► The dandelion-like microsphere hydroxyapatite are obtained at suitable conditions.

The Development of Biomimetic Spherical Hydroxyapatite/Polyamide 66 Biocomposites as Bone Repair Materials

Directory of Open Access Journals (Sweden)

Xuesong Zhang

2014-01-01

Full Text Available A novel biomedical material composed of spherical hydroxyapatite (s-HA and polyamide 66 (PA biocomposite (s-HA/PA was prepared, and its composition, mechanical properties, and cytocompatibility were characterized and evaluated. The results showed that HA distributed uniformly in the s-HA/PA matrix. Strong molecule interactions and chemical bonds were presented between the s-HA and PA in the composites confirmed by IR and XRD. The composite had excellent compressive strength in the range between 95 and 132 MPa, close to that of natural bone. In vitro experiments showed the s-HA/PA composite could improve cell growth, proliferation, and differentiation. Therefore, the developed s-HA/PA composites in this study might be used for tissue engineering and bone repair.

Molecular modeling, FTIR spectral characterization and mechanical properties of carbonated-hydroxyapatite prepared by mechanochemical synthesis

International Nuclear Information System (INIS)

Youness, Rasha A.; Taha, Mohammed A.; Elhaes, Hanan; Ibrahim, Medhat

2017-01-01

Nanocrystalline B-type carbonate substituted hydroxyapatite (B-CHA) powder has been successively synthesized by mechanochemical method. The effect of milling times on the formation of B-CHA was investigated by Fourier transform infrared spectroscopy, X-ray diffraction technique and scanning electron microscopy. Moreover, physical as well as mechanical properties were examined as a function of milling time. Furthermore, theoretical model was presented for hydroxyapatite (HA). Semiempirical calculations at PM6 level were used to calculate thermal parameters including entropy; enthalpy; heat capacity; free energy and heat of formation in the temperature range from 200 up to 500 k. The results revealed that single phase B-CHA was successfully formed after 8 h of milling when Ball to Powder Ratio (BPR) equals to 10:1. Results revealed that entropy; enthalpy and heat capacity gradually increased as a function of temperature while, free energy and heat of formation decreased with the increasing of temperature. Comparison with higher level of theory was conducted at HF and DFT using the models HF/3-21g**; B3LYP/6-31G(d,p) and B3LYP/LANL2DZ, respectively and indicated that PM6 could be utilized with appropriate accuracy and time to study physical and thermochemical parameters for HA. - Highlights: • Preparation of Nanocrystalline B-type carbonate substituted hydroxyapatite (B-CHA) powder by mechanochemical method. • Characterization of CHA. • Semiemperical and DFT models for CHA.

Molecular modeling, FTIR spectral characterization and mechanical properties of carbonated-hydroxyapatite prepared by mechanochemical synthesis

Energy Technology Data Exchange (ETDEWEB)

Youness, Rasha A. [Spectroscopy Department, National Research Centre, El-Bohouth Str., 12622, Dokki, Giza (Egypt); Taha, Mohammed A. [Solid-State Physics Department, National Research Centre, El-Bohouth Str., 12622, Dokki, Giza (Egypt); Elhaes, Hanan [Physics Department, Faculty of Women for Arts, Science, and Education, Ain Shams University, 11757 Cairo (Egypt); Ibrahim, Medhat, E-mail: medahmed6@yahoo.com [Spectroscopy Department, National Research Centre, El-Bohouth Str., 12622, Dokki, Giza (Egypt)

2017-04-01

Nanocrystalline B-type carbonate substituted hydroxyapatite (B-CHA) powder has been successively synthesized by mechanochemical method. The effect of milling times on the formation of B-CHA was investigated by Fourier transform infrared spectroscopy, X-ray diffraction technique and scanning electron microscopy. Moreover, physical as well as mechanical properties were examined as a function of milling time. Furthermore, theoretical model was presented for hydroxyapatite (HA). Semiempirical calculations at PM6 level were used to calculate thermal parameters including entropy; enthalpy; heat capacity; free energy and heat of formation in the temperature range from 200 up to 500 k. The results revealed that single phase B-CHA was successfully formed after 8 h of milling when Ball to Powder Ratio (BPR) equals to 10:1. Results revealed that entropy; enthalpy and heat capacity gradually increased as a function of temperature while, free energy and heat of formation decreased with the increasing of temperature. Comparison with higher level of theory was conducted at HF and DFT using the models HF/3-21g**; B3LYP/6-31G(d,p) and B3LYP/LANL2DZ, respectively and indicated that PM6 could be utilized with appropriate accuracy and time to study physical and thermochemical parameters for HA. - Highlights: • Preparation of Nanocrystalline B-type carbonate substituted hydroxyapatite (B-CHA) powder by mechanochemical method. • Characterization of CHA. • Semiemperical and DFT models for CHA.

In situ ring-opening polymerization of hydroxyapatite/poly (ethylene ...

Indian Academy of Sciences (India)

Hydroxyapatite/poly(ethylene adipate)--poly(ethylene terephthalate) biomaterials (HAp/PEA--PET) have been prepared by ring opening polymerization (ROP) of cyclic oligo(ethylene adipate)--oligo(ethylene terephthalate) (C-OEA--C-OET) in the porous hydroxyapatite (HAp) scaffolds at 250 °C for 24 h under ...

Characterization of dicalcium phosphate dihydrate cements prepared using a novel hydroxyapatite-based formulation

International Nuclear Information System (INIS)

Alge, Daniel L; Cruz, Grace Santa; Chu, Tien-Min Gabriel; Goebel, W Scott

2009-01-01

Dicalcium phosphate dihydrate (DCPD) cements are typically prepared using β-tricalcium phosphate (β-TCP) as the base component. However, hydroxyapatite (HA) is an interesting alternative because of its potential for reducing cement acidity, as well as modulating cement properties via ionic substitutions. In the present study, we have characterized DCPD cements prepared with a novel formulation based on monocalcium phosphate monohydrate (MCPM) and HA. Cements were prepared using a 4:1 MCPM:HA molar ratio. The reactivity of HA in this system was verified by showing DCPD formation using poorly crystalline HA, as well as highly crystalline HA. Evaluation of cements prepared with poorly crystalline HA revealed that setting occurs rapidly in the MCPM/HA system, and that the use of a setting regulator is necessary to maintain workability of the cement paste. Compressive testing showed that MCPM/HA cements have strengths comparable to what has previously been published for DCPD cements. However, preliminary in vitro analysis of cement degradation revealed that conversion of DCPD to HA may occur much more rapidly in the MCPM/HA system compared to cements prepared with β-TCP. Future studies should investigate this property further, as it could have important implications for the use of HA-based DCPD cement formulations.

Fibronectin-calcium phosphate composite layer on hydroxyapatite to enhance adhesion, cell spread and osteogenic differentiation of human mesenchymal stem cells in vitro

International Nuclear Information System (INIS)

Sogo, Yu; Ito, Atsuo; Matsuno, Tomonori; Oyane, Ayako; Tamazawa, Gaku; Satoh, Tazuko; Yamazaki, Atsushi; Uchimura, Eiji; Ohno, Tadao

2007-01-01

Fibronectin (Fn) and type I collagen (Col) were immobilized on a surface of a hydroxyapatite (HAP) ceramic by coprecipitation with calcium phosphate in a supersaturated calcium phosphate solution prepared by mixing clinically approved infusion fluids. These proteins and the calcium phosphate precipitate formed a composite surface layer. As a result, the proteins were immobilized firmly as not to be released completely for 3 d in a physiological salt solution. When human mesenchymal stem cells (hMSCs) were cultured on a HAP ceramic in a differentiation medium supplemented with dexamethasone, β-glycerophosphate and ascorbic acid, hMSCs spread well within 1 h. The alkaline phosphatase (ALP) activity of hMSCs cultured on the Fn-calcium phosphate composite layer significantly increased compared with that of hMSCs cultured on the untreated HAP ceramic. On the other hand, Col did not increase the ALP activity of hMSCs and no synergy between Fn and Col was observed. Therefore, the Fn-calcium phosphate composite layer formed on the HAP is useful for the enhancement of the spreading and osteogenic differentiation of hMSCs in vitro

Development of a composite based on hydroxyapatite and magnesium and zinc‐containing sol–gel-derived bioactive glass for bone substitute applications

International Nuclear Information System (INIS)

Ashuri, Maziar; Moztarzadeh, Fathollah; Nezafati, Nader; Ansari Hamedani, Ali; Tahriri, Mohammadreza

2012-01-01

In the present study, a bioceramic-based composite was prepared by sintering compacts made up of mixtures of hydroxyapatite (HA) and sol–gel-derived bioactive glass (64SiO 2 -26CaO-5MgO-5ZnO) (based on mol%) powders. HA powder was mixed with different concentrations of the glass powders up to 30 wt.%. The effect of adding bioactive glass powder to HA matrix, on the mechanical properties of the composite was assessed by compression test. The specimen with the highest compressive strength was chosen to be immersed in simulated body fluid (SBF) to study apatite forming ability and dissolution behavior. It was found that compressive strength of the specimen was decreased 65% after maintaining in the SBF for 14 days. X-ray diffraction (XRD) showed prevalence of HA and β-TCP related peaks. Also, the surface morphology of the composite was observed using scanning electron microscopy (SEM). The study of degradation behavior revealed Si release capability of this composite. Biological evaluations in vitro confirmed the composite studied could induce osteoblast-like cells' activities. - Highlights: ► A novel composite based on HA/bioactive glass for bone substitutes was developed. ► Evaluations in vitro confirmed the composites induce bone-like cells' activities. ► A successful compromise of bioactivity and cytocompatibility was observed.

Electrospun composites of PHBV, silk fibroin and nano-hydroxyapatite for bone tissue engineering

Energy Technology Data Exchange (ETDEWEB)

Paşcu, Elena I.; Stokes, Joseph; McGuinness, Garrett B., E-mail: garrett.mcguinness@dcu.ie

2013-12-01

prepared with 5 (w/vol) % each of nHAp and SF did not show a similar improvement. - Highlights: • Electrospinning of PHBV/nHAp composites was first achieved using silk fibroin (SF). • Smooth, uniform, continuous fibres with diameters between 10 and 15 μm were deposited. • Bioactivity was confirmed by surface apatite formation in Simulated Body Fluid. • Tensile modulus was increased for 2% nHAp and SF relative to 0% and 5% cases. • PHBV/nHAp/SF composites support initial osteoblast attachment and proliferation.

Electrospun composites of PHBV, silk fibroin and nano-hydroxyapatite for bone tissue engineering

International Nuclear Information System (INIS)

Paşcu, Elena I.; Stokes, Joseph; McGuinness, Garrett B.

2013-01-01

prepared with 5 (w/vol) % each of nHAp and SF did not show a similar improvement. - Highlights: • Electrospinning of PHBV/nHAp composites was first achieved using silk fibroin (SF). • Smooth, uniform, continuous fibres with diameters between 10 and 15 μm were deposited. • Bioactivity was confirmed by surface apatite formation in Simulated Body Fluid. • Tensile modulus was increased for 2% nHAp and SF relative to 0% and 5% cases. • PHBV/nHAp/SF composites support initial osteoblast attachment and proliferation

Lecithin-based wet chemical precipitation of hydroxyapatite nanoparticles.

Science.gov (United States)

Michał, Wojasiński; Ewa, Duszyńska; Tomasz, Ciach

Hydroxyapatite Ca 10 (PO 4 ) 6 (OH) 2 nanoparticles have been successfully synthesized by the wet chemical precipitation method at 60 °C in the presence of biocompatible natural surfactant-lecithin. The composition and morphology of nanoparticles of hydroxyapatite synthesized with lecithin (nHAp-PC) was studied by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM). Size distribution for nanoparticles was measured by nanoparticle tracking analysis in NanoSight system. We discuss in details influence of lecithin concentration in reaction system on nHAp-PC morphology, as well as on size distributions and suspendability of nanoparticles. Product exhibits crystalline structure and chemical composition of hydroxyapatite, with visible traces of lecithin. Difference in surfactant amounts results in changes in particles morphology and their average size.

Gamma irradiation processing of Hydroxyapatite/poly-L-lactide composite biomaterial

International Nuclear Information System (INIS)

Suljovrujic, E.; Ignjatovic, N.; Uskokovic, D.

2002-01-01

Complete text of publication follows. As is well known, Hydroxyapatite/poly-L-lactide (HAp/PLLA) is a composite biomaterial, used for substitution and repair of hard bone tissue. It consists of a non-bioresorptive ceramic (HAp) and a bioresorptive polymer PLLA component, with mechanical properties similar to those of bones can be produced. On the other hand, a radiation processing is a main wide used step in certain modern technologies, and can be utilized for sterilization of implants based on sensitive polymers and composites. In this paper, the relation between the structure and properties is investigated for the case of HAp/PLLA composite where structure changes are created by gamma irradiation. The irradiation, to various absorbed doses (10, 25, 50, 100 and 300 KGy) of gamma radiation, was performed in a 60 Co radiation facility, in air at room temperature, at a dose rate of 9 kGy/h. Since the morphology of Hap/PLLA composite biomaterial is very sensitive to these procedures, surface microstructure was analyzed by scanning electronic microscopy (SEM). Structural changes occurring in the material, mostly changes in PLLA, which is more sensitive to irradiation than HAp, were studied by wade angle X-ray structural analyses (WAXS) and infrared (IR) spectroscopy. Differential scanning calorimetry measurements (DSC) were used to study the changes in thermal behaviour and crystallinity. Effects of radiation on the HAp/PLLA composite thermal stability were determined by thermogravimetric analysis (TGA). Conclusions derived using different methods were compared

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

International Nuclear Information System (INIS)

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

2003-01-01

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 10 (PO 4 ) 6 (OH) 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 sp > 10 -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.

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

International Nuclear Information System (INIS)

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

2004-01-01

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 10 (PO 4 ) 6 (OH) 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 sp >10 -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

Fabrication and Physical Properties of Titanium Nitride/Hydroxyapatite Composites on Polyether Ether Ketone by RF Magnetron Sputtering Technique

Science.gov (United States)

Nupangtha, W.; Boonyawan, D.

2017-09-01

Titanium nitride (TiN) coatings have been used very successfully in a variety of applications because of their excellent properties, such as the high hardness meaning good wear resistance and also used for covering medical implants. Hydroxyapatite is a bioactive ceramic that contributes to the restoration of bone tissue, which together with titanium nitride may contribute to obtaining a superior composite in terms of mechanical and bone tissue interaction matters. This paper aims to explain how to optimize deposition conditions for films synthesis on PEEK by varying sputtering parameters such as nitrogen flow rate and direction, deposition time, d-s (target-to-substrate distance) and 13.56 MHz RF power. The plasma conditions used to deposit films were monitored by the optical emission spectroscopy (OES). Titanium nitride/Hydroxyapatite composite films were performed by gas mixture with nitrogen and argon ratio of 1:3 and target-to-substrate distance at 8 cm. The gold colour, as-deposited film was found on PEEK with high hardness and higher surface energy than uncoated PEEK. X-ray diffraction characterization study was carried to study the crystal structural properties of these composites.

Optical characterization of infrared emitting Nd3+ doped hydroxyapatite nanoparticles prepared by hydrothermal method

International Nuclear Information System (INIS)

Gayathri, K.; Kumar, G.A.; Manrique, Solange Ivette Rivera; Santhosh, C.; Sardar, Dhiraj K.

2017-01-01

Trivalent Nd doped hydroxyapatite (HAp) nanoparticles were prepared by a hydrothermal method using calcium nitrate and diammonium phosphate as precursors. Well crystallized nanoparticles of size less than 200 nm with hexagonal plate and rod morphologies were obtained at a reaction temperature of 180 °C. Under 808 nm excitation the nanoparticles exhibit strong near infrared emission at 1064 nm. All the emission spectral properties such as emission intensity and fluorescence decay time are found to decrease with Nd 3+ concentration. In Hap 0.5% Nd shows the highest decay time of 159 μs and highest emission at 1064 nm emission.

Synthesis and characterization of Poly(2-hydroxyethylmethacrylate-hydroxyapatite) a novel composite for the removal of Lead(II) from aqueous solutions

Energy Technology Data Exchange (ETDEWEB)

Akkaya, Recep [Vocational School of Health Services, Cumhuriyet University, Sivas (Turkey)

2012-11-15

In the present study, a novel adsorbent, poly (2-hydroxyethylmethacrylate-hydroxyapatite) [P(HEMA-Hap)], was prepared and characterized. The synthesis was achieved by means of free-radical polymerization and a number of structural characterization methods, including FT-IR, XRD, TGA, SEM, BET-porosity, and swelling tests. Pb{sup 2+} adsorption was performed using a series of pH, time, and temperature ranges. The reusability of the composite was also tested. The results obtained indicated that the novel adsorbent is able to bind Pb{sup 2+} ions with strong chemical affinity. The adsorption results were fitted to the classic Langmuir, Freundlich, and Dubinin-Radushkevich (D-R) sorption models. Thermodynamic parameters obtained demonstrated that the sorption process was spontaneous ({Delta}G < 0), endothermic ({Delta}H > 0), as expected. The process was also consistent with the pseudo-second-order model, and chemical adsorption was determined to be the rate-controlling step. It was also shown that the composite could be used for five consecutive adsorption processes. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

Coupling of HDPE/hydroxyapatite composites by silane-based methodologies.

Science.gov (United States)

Sousa, R A; Reis, R L; Cunha, A M; Bevis, M J

2003-06-01

Several coupling treatments based on silane chemicals were investigated for the development of high density (HDPE)/hydroxyapatite (HA) composites. Two HA powders, sintered HA (HAs) and non sintered HA (HAns), were studied in combination with five silanes, namely y-methacryloxy propyltrimethoxy silane (MEMO), 3-(2-aminoethyl)aminopropyltrimethoxy silane (DAMO), vinyltrimethoxy silane (VTMO), 3-aminopropyltriethoxy silane (AMEO) and trimethoxypropyl silane (PTMO). The HA particles were treated by a dipping in method or by spraying with silane solutions. After drying, the treated powders were compounded with HDPE or HDPE with acrylic acid and/or organic peroxide and subsequently compression molded. The tensile test specimens obtained from the molded plates were tensile tested and their fracture surfaces were observed by scanning electron microscopy (SEM). For the sintered HA (HAs) composites, the most effective coupling treatments concerning stiffness are those based on MEMO and AMEO. The low influence of these coupling procedures on strength is believed to be associated to the low volume fraction and the relatively smooth surface of the used HA particles. For the non-sintered HA (HAns) composites, it was possible to improve significantly both the stiffness and the strength. Amino silanes demonstrated to be highly efficient concerning strength enhancement. The higher effectiveness of the coupling treatments for HAns filled composites is attributed to their higher particle surface area, smaller particle size distribution and expected higher chemical reactivity. For both cases, the improvement in mechanical performance after the coupling treatment is consistent with the enhancement in interfacial adhesion observed by SEM.

Preparation of nano-hydroxyapatite particles with different morphology and their response to highly malignant melanoma cells in vitro

Energy Technology Data Exchange (ETDEWEB)

Li Bo [National Engineering Research Center for Biomaterial, Sichuan University, Chengdu 610064 (China); Guo Bo [National Engineering Research Center for Biomaterial, Sichuan University, Chengdu 610064 (China); West China Eye Center of Huaxi Hospital, Sichuan University, Chengdu 610064 (China); Fan Hongsong [National Engineering Research Center for Biomaterial, Sichuan University, Chengdu 610064 (China)], E-mail: leewave@126.com; Zhang Xingdong [National Engineering Research Center for Biomaterial, Sichuan University, Chengdu 610064 (China)

2008-11-15

To investigate the effects of nano-hydroxyapatite (HA) particles with different morphology on highly malignant melanoma cells, three kinds of HA particles with different morphology were synthesized and co-cultured with highly malignant melanoma cells using phosphate-buffered saline (PBS) as control. A precipitation method with or without citric acid addition as surfactant was used to produce rod-like hydroxyapatite (HA) particles with nano- and micron size, respectively, and a novel oil-in-water emulsion method was employed to prepare ellipse-like nano-HA particles. Particle morphology and size distribution of the as prepared HA powders were characterized by transmission electron microscope (TEM) and dynamic light scattering technique. The nano- and micron HA particles with different morphology were co-cultured with highly malignant melanoma cells. Immunofluorescence analysis and MTT assay were employed to evaluate morphological change of nucleolus and proliferation of tumour cells, respectively. To compare the effects of HA particles on cell response, the PBS without HA particles was used as control. The experiment results indicated that particle nanoscale effect rather than particle morphology of HA was more effective for the inhibition on highly malignant melanoma cells proliferation.

Development of hydroxyapatite/polyvinyl alcohol bionanocomposite for prosthesis implants

Science.gov (United States)

Karthik, V.; Pabi, S. K.; Chowdhury, S. K. Roy

2018-02-01

Hydroxyapatite (Ca10(PO4)6(OH)2) has similar structural and chemical properties of natural bone mineral and hence widely used as a bone replacement substitute. Natural bone consists of hydroxyapatite and collagen. For mimicking the natural, in the present work, a sintered porous hydroxyapatite component has been vacuum impregnated with Polyvinyl alcohol (PVA), which has better properties like biocompatibility, biodegradability and water- solubility. Hydroxyapatite powders have been made into nanosize to reduce the melting point and hence the sintering temperature. In the present investigation high energy ball mill is used to produce nano-hydroxyapatite powders in bulk quantity by optimizing the milling parameters using stainless steel grinding media. Pellets of 10 mm diameter have been produced from nano- hydroxyapatite powders under different uniaxial compaction pressures. The pellets have been sintered to form porous compacts. The vacuum impregnation of sintered pallets with PVA solution of different strength has been done to find the optimum impregnation condition. Microhardness, compressive strength, wear loss and haemocompatibility of hydroxyapatite ceramics have been studied before and after impregnation of PVA. The nano- hydroxyapatite/PVA composites have superior mechanical properties and reduced wear loss than the non-impregnated porous nano-hydroxyapatite ceramics.

Poly(dimethylsiloxane) / tetraethyl orthosilicate modified hydroxyapatite composites: mechanical properties and biocompatibility evaluation

International Nuclear Information System (INIS)

Bareiro, O.; Santos, L. A.

2012-01-01

A composite of poly(dimethylsiloxane)/hydroxyapatite (PDMS/HAp) has been developed and its mechanical properties and biocompatibility were assessed. The processing of the composite involved the surface modification of HAp with 5 or 10 %(wt/wt) tetraethyl orthosilicate (TEOS) solutions, followed by mixing in a two roll open mixer with the silicone. The energy dispersive spectroscopy (EDS) spectra indicated evidence of a silane layer in the HAp modified surface. In tensile property measurement, the PDMS/modified-HAp composite showed higher values of tensile strength (2.41 MPa) and lower elongation at break (73.44 %) than the PDMS/unmodified HAp composite, 2.26 MPa and 365.58 % respectively. In both cases, the composites showed higher values of tensile strength than the original silicone (1.97 MPa). Scanning electron microscopy (SEM) micrographs of the PDMS/unmodified-HAp composite exhibited debonding of the HAp particles from the elastomeric matrix at the fracture surface. On the other hand, HAp particles remained well attached to the matrix in the PDMS/modified-HAp composite. The presence of HAp improved the biocompatibility of the silicone. The soaking of the composites for 7 days in a simulated body fluid (SBF) formed a dense and homogeneous layer of HAp like crystals in the surface of the composites. The surface modification of HAp powders with TEOS solutions formed a strong interface PDMS/HAp, this enhanced the tensile strength of the composite. (author)

Study of the effects of heat-treatment of hydroxyapatite synthesized in gelatin matrix

Science.gov (United States)

Zaits, A. V.; Golovanova, O. A.; Kuimova, M. V.

2017-01-01

In the study, the isothermal thermogravimetric analysis (TGA) of hydroxyapatite synthesized in gelatin matrix (HAG) has been performed. 3 wt.% HAG samples were synthesized from the solution simulating the human extracellular fluid (SBF). X-ray diffraction and IR spectroscopy were used to determine the composition. During the experiment, increase in the calcination temperature up to 200°C-800°C was found to cause weight loss. The study of phase composition revealed that heat treatment does not affect the phase composition of the solid phase, which is composed of hydroxylapatite (HA). The prepared HAG (3 wt.% gelatin) samples are shown to have low thermal stability; the degradation of the samples occurs at 400°C.

Hydroxyapatite/gelatin functionalized graphene oxide composite coatings deposited on TiO2 nanotube by electrochemical deposition for biomedical applications

International Nuclear Information System (INIS)

Yan, Yajing; Zhang, Xuejiao; Mao, Huanhuan; Huang, Yong; Ding, Qiongqiong; Pang, Xiaofeng

2015-01-01

Highlights: • Graphene oxide cross-linked gelatin was firstly employed as reinforcement fillers in hydroxyapatite coatings by electrochemical deposition process on TiO 2 nanotube arrays. • Gelatin functionalized graphene oxide induced the formation of hydroxyapatite coatings. • The success of gelatin and graphene oxide incorporation was evidenced with FTIR and XPS. • The synthesized composite coatings showed good biocompatibility and no adverse effect in cell culture tests. - Abstract: Graphene oxide cross-linked gelatin was employed as reinforcement fillers in hydroxyapatite coatings by electrochemical deposition process on TiO 2 nanotube arrays (TNs). The TNs were grown on titanium by electrochemical anodization in hydrofluoric electrolyte using constant voltage. Fourier transform infrared spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy, Field emission scanning electron microscopy equipped with energy dispersive X-ray analysis and biological studies were used to characterize the coatings. The corrosion resistance of the coatings was also investigated by electrochemical method in simulated body fluid solution

Degradable biocomposite of nano calcium- deficient hydroxyapatite-multi(amino acid copolymer

Directory of Open Access Journals (Sweden)

Li XD

2012-03-01

Full Text Available Hong Li1, Min Gong1, Aiping Yang1, Jian Ma2, Xiangde Li3, Yonggang Yan11School of Physical Science and Technology, Sichuan University, Chengdu People’s Republic of China; 2Hospital of Stomatology, Tongji University, ShanghaiPeople’s Republic of China; 3Key Laboratory for Ultrafine Materials of Ministry of Education, East China University of Science and Technology, Shanghai, People’s Republic of ChinaBackground and methods: A nano calcium-deficient hydroxyapatite (n-CDHA-multi(amino acid copolymer (MAC composite bone substitute biomaterial was prepared using an in situ polymerization method. The composition, structure, and compressive strength of the composite was characterized, and the in vitro degradability in phosphate-buffered solution and preliminary cell responses to the composite were investigated.Results: The composite comprised n-CDHA and an amide linkage copolymer. The compressive strength of the composite was in the range of 88–129 MPa, varying with the amount of n-CDHA in the MAC (ranging from 10 wt% to 50 wt%. Weight loss from the composite increased (from 32.2 wt% to 44.3 wt% with increasing n-CDHA content (from 10 wt% to 40 wt% in the MAC after the composite was soaked in phosphate-buffered solution for 12 weeks. The pH of the soaking medium varied from 6.9 to 7.5. MG-63 cells with an osteogenic phenotype were well adhered and spread on the composite surface. Viability and differentiation increased with time, indicating that the composite had no negative effects on MG-63 cells.Conclusion: The n-CDHA-MAC composite had good cytocompatibility and has potential to be used as a bone substitute.Keywords: calcium deficient hydroxyapatite, multi(amino acid copolymer, biocomposite, degradability, cytocompatibility

Hydroxyapatite-ciprofloxacin delivery system: Synthesis, characterisation and antibacterial activity

Directory of Open Access Journals (Sweden)

Ciocilteu Maria-Viorica

2018-06-01

Full Text Available The main objective of this study was to synthesize hydroxyapatite-ciprofloxacin composites using a chemical precipitation method and to evaluate the properties and in vitro release profile of the drug from the hydroxyapatite-ciprofloxacin composites. Composite characterization was achieved by FT-IR, XRD and DLS. Ciprofloxacin determination was accomplished by HPLC, resulting in good incorporation efficiency of the drug (18.13 %. The in vitro release study (Higuchi model C = K t1/2 and Ritger-Peppas model, C = K t0.6 showed a diffusion-controlled mechanism. The antibacterial activity showed that the bacterial growth inhibition zones were approximately equal for the synthesis composites and for the mechanical mixture on the Staphylococcus aureus germ.

Properties and in vitro biological evaluation of nano-hydroxyapatite/chitosan membranes for bone guided regeneration

Energy Technology Data Exchange (ETDEWEB)

Cheng Xianmiao [Research Center for Nano-Biomaterials, Analytical and Testing Center, Sichuan University, 610064 Chengdu (China); Department of Chemistry, Sichuan University, 610064 Chengdu (China); Li Yubao [Research Center for Nano-Biomaterials, Analytical and Testing Center, Sichuan University, 610064 Chengdu (China)], E-mail: nic7504@scu.edu.cn; Zuo Yi; Zhang Li [Research Center for Nano-Biomaterials, Analytical and Testing Center, Sichuan University, 610064 Chengdu (China); Li Jidong [Research Center for Nano-Biomaterials, Analytical and Testing Center, Sichuan University, 610064 Chengdu (China); Department of Chemistry, Sichuan University, 610064 Chengdu (China); Wang Huanan [Research Center for Nano-Biomaterials, Analytical and Testing Center, Sichuan University, 610064 Chengdu (China)

2009-01-01

Nano-hydroxyapatite(n-HA)/chitosan(CS) composite membranes were prepared by solvent casting and evaporation methods for the function of guided bone regeneration (GBR). The effect of n-HA content and solvent evaporation temperature on the properties of the composite membranes was studied. The n-HA/CS membranes were analyzed by scanning electron microscopy, Fourier transformed infrared spectroscopy, X-ray diffraction, swelling measurement, mechanical test, cell culture and MTT (3-[4,5-dimethylthiazol-2-yl]-2,5-diphenylte-2H-tetrazolium bromide) assay. The results show that the surface roughness and micropores of the composite membranes increase with the rise of n-HA content, suitable for adhesion, crawl and growth of cells. The hydroxyapatite holds nano size and distributes uniformly in the composite membranes. Chemical bond interaction exists between Ca ions and -OH groups of n-HA and -NH{sub 2} or -OH groups of CS. The n-HA content and solvent evaporation temperature have obvious influence on the swelling ratio, tensile strength and elongation rate of the composite membranes. Cell culture and MTT assays show that n-HA and its content can affect the proliferation of cells. The n-HA/CS composite membranes have no negative effect on the cell morphology, viability and proliferation and possess good biocompatibility. This study makes the n-HA/CS composite membrane be a prospective biodegradable GBR membrane for future applications.

Properties and in vitro biological evaluation of nano-hydroxyapatite/chitosan membranes for bone guided regeneration

International Nuclear Information System (INIS)

Cheng Xianmiao; Li Yubao; Zuo Yi; Zhang Li; Li Jidong; Wang Huanan

2009-01-01

Nano-hydroxyapatite(n-HA)/chitosan(CS) composite membranes were prepared by solvent casting and evaporation methods for the function of guided bone regeneration (GBR). The effect of n-HA content and solvent evaporation temperature on the properties of the composite membranes was studied. The n-HA/CS membranes were analyzed by scanning electron microscopy, Fourier transformed infrared spectroscopy, X-ray diffraction, swelling measurement, mechanical test, cell culture and MTT (3-[4,5-dimethylthiazol-2-yl]-2,5-diphenylte-2H-tetrazolium bromide) assay. The results show that the surface roughness and micropores of the composite membranes increase with the rise of n-HA content, suitable for adhesion, crawl and growth of cells. The hydroxyapatite holds nano size and distributes uniformly in the composite membranes. Chemical bond interaction exists between Ca ions and -OH groups of n-HA and -NH 2 or -OH groups of CS. The n-HA content and solvent evaporation temperature have obvious influence on the swelling ratio, tensile strength and elongation rate of the composite membranes. Cell culture and MTT assays show that n-HA and its content can affect the proliferation of cells. The n-HA/CS composite membranes have no negative effect on the cell morphology, viability and proliferation and possess good biocompatibility. This study makes the n-HA/CS composite membrane be a prospective biodegradable GBR membrane for future applications

Structure and characteristics of the hot pressed hydroxyapatite/poly-L-lactide composite

Directory of Open Access Journals (Sweden)

Ignjatović Nenad L.

2002-01-01

Full Text Available Hydroxyapatite/poly-L-lactide (HAp/PLL composite biomaterial can be obtained by different processing methods. Three-dimensional blocks of HAp/PLLA composite biomaterial with mechanical characteristics close to the natural bone tissue can be obtained by hot pressing procedure. Effects of synthesis and compacting on the structure and characteristics of the HAp/PLLA composite biomaterial were studied in this work. Using wade angle X-ray structural analyses (WAXS, differentially scanning calorimetry (DSC, thermogravimetric analysis (TGA and infrared (IR spectroscopy, the changes occurring in the material during synthesis and hot pressing were monitored. Surface microstructure was analyzed by scanning electronic microscopy (SEM coupled with electron-dispersion analysis (EDX. The results obtained indicate a possible decrease in the degree of crystallinity with hot pressing time increase. A block of HAp/PLLA composite biomaterial with 1.6 times lower crystallinity of the polymer phase was obtained by hot pressing in a given time interval with a maximum of 60 minutes. Results of TG analysis show that PLLA stability decreases with increasing hot pressing time, and vice versa. IR study proved that neither destructive changes in constituents nor formation of new phases occurred during hot pressing.

Polymer-Ceramic Composite Scaffolds: The Effect of Hydroxyapatite and β-tri-Calcium Phosphate.

Science.gov (United States)

Huang, Boyang; Caetano, Guilherme; Vyas, Cian; Blaker, Jonny James; Diver, Carl; Bártolo, Paulo

2018-01-14

The design of bioactive scaffolds with improved mechanical and biological properties is an important topic of research. This paper investigates the use of polymer-ceramic composite scaffolds for bone tissue engineering. Different ceramic materials (hydroxyapatite (HA) and β-tri-calcium phosphate (TCP)) were mixed with poly-ε-caprolactone (PCL). Scaffolds with different material compositions were produced using an extrusion-based additive manufacturing system. The produced scaffolds were physically and chemically assessed, considering mechanical, wettability, scanning electron microscopy and thermal gravimetric tests. Cell viability, attachment and proliferation tests were performed using human adipose derived stem cells (hADSCs). Results show that scaffolds containing HA present better biological properties and TCP scaffolds present improved mechanical properties. It was also possible to observe that the addition of ceramic particles had no effect on the wettability of the scaffolds.

Preparation of chitosan/nano hydroxyapatite organic-inorganic hybrid microspheres for bone repair.

Science.gov (United States)

Chen, Jingdi; Pan, Panpan; Zhang, Yujue; Zhong, Shengnan; Zhang, Qiqing

2015-10-01

In this work, we encapsulated icariin (ICA) into chitosan (CS)/nano hydroxyapatite (nHAP) composite microspheres to form organic-inorganic hybrid microspheres for drug delivery carrier. The composition and morphology of composite microspheres were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) and differential scanning calorimetry- thermogravimetric analysis (DSC-TGA). Moreover, we further studied the performance of swelling properties, degradation properties and drug release behavior of the microspheres. ICA, the extract of traditional Chinese medicine-epimedium, was combined to study drug release properties of the microspheres. ICA loaded microspheres take on a sustained release behavior, which can be not only ascribed to electrostatic interaction between reactive negative hydroxyl (OH) of ICA and positive amine groups (NH₂) of CS, but also depended on the homogeneous dispersion of HAP nanoparticles inside CS organic matrix. In addition, the adhesion and morphology of osteoblasts were detected by inverted fluorescence microscopy. The biocompatibility of CS/nHAP/ICA microspheres was evaluated by the MTT cytotoxicity assay, Hoechst 33258 and PI fluorescence staining. These studies demonstrate that composite microspheres provide a suitable microenvironment for osteoblast attachment and proliferation. It can be speculated that the ICA loaded CS-based organic-inorganic hybrid microspheres might have potential applications in drug delivery systems. Copyright © 2015 Elsevier B.V. All rights reserved.

Mechanical response and multilevel structure of biomimetic hydroxyapatite/polygalacturonic/chitosan nanocomposites

International Nuclear Information System (INIS)

Verma, Devendra; Katti, Kalpana S.; Katti, Dinesh R.; Mohanty, Bedabibhas

2008-01-01

Using an in situ mineralization process that is biomimetic we have synthesized new nanocomposites of chitosan/hydroxyapatite in 50-50 ratio(ChiHAP50), polygalacturonic acid/hydroxyapatite in 50-50 ratio (PgAHAP50) and Chitosan/hydroxyapatite/Polygalacturonic acid (ChiPgAHAP50). Polygalacturonic acid (PgA) is electrostatically complementary to chitosan, and thus is expected to provide stronger interfacial interactions and improve mechanical response. Atomic force imaging of fractured and polished surfaces suggests a multilevel organization in the hydroxyapatite/biopolymer nanocomposite. The AFM images of ChiPgAHAP50 nanocomposite display presence of chitosan rich and polygalacturonic rich domains. These chitosan rich and PgA rich domains are made of smaller globular shaped particles in which, hydroxyapatite nano-particles are embedded in the biopolymer matrix. The average size of the hydroxyapatite particles in PgAHAP50, ChiHAP50 and ChiPgAHAP50 were found to be 25, 42 and 34 nm respectively. The elastic moduli determined from nanoindentation of PgAHAP50, ChiHAP50 and ChiPgAHAP50 composites are 29.81, 17.56 and 23.62 GPa respectively. Hardness values of the three composites in the same order were found to be 1.56, 0.65 and 1.14 GPa respectively. Macro-mechanical tests showed significant enhancement in elastic moduli, strain to failure and compressive strength of ChiPgAHAP50 composites over ChiHAP50 and PgAHAP50

Cobalt doped proangiogenic hydroxyapatite for bone tissue engineering application

International Nuclear Information System (INIS)

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

2016-01-01

ABSTRACT: 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. - Highlights: • Cobalt (Co"+"2) doped hydroxyapatite (Co-HAp) can be prepared by the wet chemical method. • The concentration of Co"+"2 influences the physico-chemical properties of HAp. • Co-HAp was found to be biocompatible and osteogenic. • Co-HAp enhanced cellular VEGF secretion through HIF-1α stabilization. • The optimum biological performance of Co-HAp was achieved for 0.33% (w/w) Co"+"2 doping.

[Remediation Pb, Cd contaminated soil in lead-zinc mining areas by hydroxyapatite and potassium chloride composites].

Science.gov (United States)

Wang, Li; Li, Yong-Hua; Ji, Yan-Fang; Yang, Lin-Sheng; Li, Hai-Rong; Zhang, Xiu-Wu; Yu, Jiang-Ping

2011-07-01

The composite agents containing potassium chloride (KCl) and Hydroxyapatite (HA) were used to remediate the lead and cadmium contaminated soil in Fenghuang lead-zinc mining-smelting areas, Hunan province. The objective of this study was to identify and evaluate the influence of Cl- to the fixing efficiency of Pb and Cd by HA. Two types of contaminated soil (HF-1, HF-2) were chosen and forty treatments were set by five different Hydroxyapatite (HA) dosages and four different Cl- dosages. The toxicity characteristic leaching procedure (TCLP) was used to evaluate the results. It showed that HA could efficiently fix the Pb and Cd from TCLP form. The maximum Pb-fixing efficiency and Cd-fixing efficiency of two types of soil were 83.3%, 97.27% and 35.96%, 57.82% when the HA: Pb: KCl molar ratio was 8: 1: 2. Compared to the fixing efficiency without KCl, KCl at the KCl: Pb molar ratio of 2 improved Pb-fixing efficiency and Cd-fixing efficiency by 6.26%, 0.33% and 7.74%, 0.83% respectively when the HA: Pb molar ratio was 8. Generally, Cl- can improve the Pb/Cd-fixing efficiency in heavy metal contaminated soil by Hydroxyapatite.

Nanostructure of plasma-sprayed hydroxyapatite coating

International Nuclear Information System (INIS)

Suvorova, E.I.; Klechkovskaya, V.V.; Bobrovsky, V.V.; Khamchukov, Yu.D.; Klubovich, V.V.

2003-01-01

Calcium phosphate coatings were studied by high-resolution transmission microscopy, microdiffraction, and X-ray energy-dispersive spectroscopy. Coatings were prepared by spraying hydroxyapatite targets onto copper, nickel, and chromium substrates and onto NaCl and BaF 2 single crystals in an argon plasma at a gas pressure of ∼1 Pa; the sputter power was about 200 W; and the RF-generator frequency was 13.56 MHz. Under the conditions used, thin layers of nanocrystalline hydroxyapatite were formed regardless of the nature of the substrate

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

International Nuclear Information System (INIS)

Mendez-Gonzalez, M.

2004-01-01

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

Preparation, characterization and properties of nano-hydroxyapatite/polypropylene carbonate biocomposite

Energy Technology Data Exchange (ETDEWEB)

Liao, Jianguo, E-mail: liaojianguo10@hpu.edu.cn [School of Materials Science and Engineering, Henan Polytechnic University, Jiaozuo 454000 (China); Li, Yanqun [School of Materials Science and Engineering, Henan Polytechnic University, Jiaozuo 454000 (China); Zou, Qin [Analytical & Testing Center, Sichuan University, Chengdu 610064 (China); Duan, Xingze; Yang, Zhengpeng; Xie, Yufen [School of Materials Science and Engineering, Henan Polytechnic University, Jiaozuo 454000 (China); Liu, Haohuai [School of Chemistry and Chemical Engineering, Analytical and Testing Center, Guangzhou University, Guangzhou 510006 (China)

2016-06-01

The combination of nano-hydroxyapatite (n-HA) and polypropylene carbonate (PPC) was used to make a composite materials by a coprecipitation method. The physical and chemical properties of the composite were tested. Scanning electron microscope (SEM) observation indicated that the biomimetic n-HA crystals were uniformly distributed in the polymer matrix. As the n-HA content increased in the composite, the fracture mechanism of the composites changes from gliding fracture to gliding and brittle fracture. Furthermore, the chemical interaction between inorganic n-HA and polypropylene carbonate was also investigated and discussed in detail. The hydrogen bonds might be formed between –OH/CO{sub 3}{sup 2−} of n-HA crystal and the ester group (–COO–) of PPC. The tensile strength of n-HA/PPC (40/60) was similar to that of the cancellous bone, and reached ca 58 MPa. The osteoblasts were cultured for up to 7 days, and then the adhesion and proliferation of osteoblasts were measured by Methyl thiazolyl tetrazolium (MTT) colorimetry assay and SEM. The cells proliferated, grew normally in fusiform shape and well attached. The in vitro test confirmed that the n-HA/PPC composites were biocompatible and showed undetectable negative effect on osteoblasts. In vivo implantation of the composite in New Zealand white rabbits was performed. It can stimulate the growth of a new bone, and at the same time the material begins to degrade. These results suggested that the composite may be suitable for the reparation or replacement of bone defects and possessed the potential for clinical applications. - Graphical abstract: SEM micrographs of the induced osteoblasts cultured on the n-HA/PC (40/60) composite. After 2 day cell culture (a), after 4 days (b) hematoxylin/eosin-stained sections of n-HA/PPC (40/60) composite materials. In the photos, M denotes n-HA/PPC (40/60) composite materials, B denotes bone, while NB denotes newly formed bone tissue. - Highlights: • A novel method, co

Biomedical properties of laser prepared silver-doped hydroxyapatite

Czech Academy of Sciences Publication Activity Database

Jelínek, Miroslav; Weiserová, Marie; Kocourek, Tomáš; Zezulová, Markéta; Strnad, D.

2011-01-01

Roč. 21, č. 7 (2011), 1265-1269 ISSN 1054-660X R&D Projects: GA ČR GA204/07/0325 Institutional research plan: CEZ:AV0Z10100522; CEZ:AV0Z50200510 Keywords : silver -doped hydroxyapatite * PLD * layers * antibacterial properties Subject RIV: BH - Optics, Masers, Lasers Impact factor: 3.605, year: 2011

Lithium-doped hydroxyapatite nano-composites: Synthesis, characterization, gamma attenuation coefficient and dielectric properties

Science.gov (United States)

Badran, H.; Yahia, I. S.; Hamdy, Mohamed S.; Awwad, N. S.

2017-01-01

Lithium-hydroxyapatite (0, 1, 5, 10, 20, 30 and 40 wt% Li-HAp) nano-composites were synthesized by sol-gel technique followed by microwave-hydrothermal treatment. The composites were characterized by X-ray diffraction (XRD), Field emission scanning electron microscope (FE-SEM), energy dispersive spectroscopy (EDS), Fourier transform infrared (FTIR) and Raman techniques. Gamma attenuation coefficient and the dielectric properties for all composites were investigated. The crystallinity degree of Li-doped HAp was higher than that of un-doped HAp. Gamma attenuation coefficient values increased from 0.562 cm-1 for 0 wt% Li-HAp to 2.190 cm-1 for 40 wt% Li-HAp. The alternating current conductivity increased with increasing frequency. The concentration of Li affect the values of dielectric constant where Li doped HAp of low dielectric constant can have an advantage for healing in bone fractures. The calcium to phosphorus ratio decreased from 1.43 to 1.37 with the addition of lithium indicating the Ca deficiency in the studied composites. Our findings lead to the conclusion that Li-HAp is a new nano-composite useful for medical applications and could be doped with gamma shield materials.

A Novel Method to Improve the Anticancer Activity of Natural-Based Hydroxyapatite against the Liver Cancer Cell Line HepG2 Using Mesoporous Magnesia as a Micro-Carrier

OpenAIRE

Nasser S. Awwad; Ali M. Alshahrani; Kamel A. Saleh; Mohamed S. Hamdy

2017-01-01

Micro-carriers are the best known vehicles to transport different kinds of drugs to achieve high impact. In this study, mesoporous magnesium oxide has been harnessed as a micro-carrier to encapsulate the anticancer candidate drug natural-based cubic hydroxyapatite (HAP). HAP@MgO composites with different HAP loading (0–60 wt %), were prepared by a hydrothermal treatment method using triethanol amine as a template. The characterization of the prepared composites were achieved by using XRD, Ram...

Innovative biodegradable poly(L-lactide/collagen/hydroxyapatite composite fibrous scaffolds promote osteoblastic proliferation and differentiation

Directory of Open Access Journals (Sweden)

Zhou GQ

2017-10-01

Full Text Available Guoqiang Zhou,1–3 Sudan Liu,1 Yanyan Ma,1 Wenshi Xu,1 Wei Meng,1 Xue Lin,1 Wenying Wang,1,3 Shuxiang Wang,1–3 Jinchao Zhang1–3 1College of Chemistry and Environmental Science, 2Key Laboratory of Medicinal Chemistry and Molecular Diagnosis of Ministry of Education, 3Key Laboratory of Chemical Biology of Hebei Province, Hebei University, Baoding, Hebei, People’s Republic of China Abstract: The development of an artificial bone graft which can promote the regeneration of fractures or diseased bones is currently the most challenging aspect in bone tissue engineering. To achieve the purpose of promoting bone proliferation and differentiation, the artificial graft needs have a similar structure and composition of extracellular matrix. One-step electrospinning method of biocomposite nanofibers containing hydroxyapatite (HA nanoparticles and collagen (Coll were developed for potential application in bone tissue engineering. Nanocomposite scaffolds of poly(L-lactide (PLLA, PLLA/HA, PLLA/Coll, and PLLA/Coll/HA were fabricated by electrospinning. The morphology, diameter, elements, hydrophilicity, and biodegradability of the composite scaffolds have been investigated. The biocompatibility of different nanocomposite scaffolds was assessed using mouse osteoblasts MC3T3-E1 in vitro, and the proliferation, differentiation, and mineralization of cells on different nanofibrous scaffolds were investigated. The results showed that PLLA/Coll/HA nanofiber scaffolds enhanced cell adhesion, spreading, proliferation, differentiation, mineralization, and gene expression of osteogenic markers compared to other scaffolds. In addition, the nanofibrous scaffolds maintained a stable composition at the beginning of the degradation period and morphology wastage and weight loss were observed when incubated for up to 80 days in physiological simulated conditions. The PLLA/Coll/HA composite nanofibrous scaffolds could be a potential material for guided bone regeneration

Optical characterization of infrared emitting Nd{sup 3+} doped hydroxyapatite nanoparticles prepared by hydrothermal method

Energy Technology Data Exchange (ETDEWEB)

Gayathri, K. [Department of Physics and Astronomy, University of Texas at San Antonio, San Antonio, TX 78249 (United States); Kumar, G.A., E-mail: ajith@gakumar.net [Department of Physics and Astronomy, University of Texas at San Antonio, San Antonio, TX 78249 (United States); Department of Atomic and Molecular Spectroscopy, Manipal University, Manipal 576104 (India); Northwest Vista College, 3535 N Ellison Dr, San Antonio, TX 78251 (United States); Manrique, Solange Ivette Rivera [Instituto Politécnico Nacional (IPN), Av. Luis Enrique Erro S/N, Unidad Profesional Adolfo López Mateos, Zacatenco, Delegación Gustavo A. Madero, C.P. 07738, Ciudad de México 2009-2010 (Mexico); Santhosh, C. [Department of Atomic and Molecular Spectroscopy, Manipal University, Manipal 576104 (India); Sardar, Dhiraj K. [Department of Physics and Astronomy, University of Texas at San Antonio, San Antonio, TX 78249 (United States)

2017-05-15

Trivalent Nd doped hydroxyapatite (HAp) nanoparticles were prepared by a hydrothermal method using calcium nitrate and diammonium phosphate as precursors. Well crystallized nanoparticles of size less than 200 nm with hexagonal plate and rod morphologies were obtained at a reaction temperature of 180 °C. Under 808 nm excitation the nanoparticles exhibit strong near infrared emission at 1064 nm. All the emission spectral properties such as emission intensity and fluorescence decay time are found to decrease with Nd{sup 3+} concentration. In Hap 0.5% Nd shows the highest decay time of 159 μs and highest emission at 1064 nm emission.

Use of hydroxyapatite prepared by sol-gel method for gamma ray and electron beam dosimetry

International Nuclear Information System (INIS)

Hajiloo, N.; Ziaie, F.; Hesami, M.

2011-01-01

In this research, radiation dosimetry was made through measuring free radicals induced in synthetic hydroxyapatite using EPR spectroscopy. At the first step, the hydroxyapatite nano-powders were synthesized via sol-gel method. The produced powders were passed through a thermal treatment, weighted and packed. Then, the samples were irradiated at different dose rates using 60 Co γ-ray and 10 MeV electron beam radiation at a high dose range. The hydroxyapatite signal intensity of hydroxyapatite samples were measured at room temperature in the air. Subsequently, the variations of the EPR signal intensities were constructed as peak-to-peak signal amplitude and were compared with alanine and bone powder samples. The results showed that the EPR signal intensity of the hydroxyapatite samples are several times higher than alanine and bone powder and are saturated at the higher dose rates in comparison with other species.

Sorption of fission nuclides on model milk components. I. Sorption of radiostrontium on hydroxyapatite in aqueous solutions

International Nuclear Information System (INIS)

Rosskopfova, O.; Kopunec, R.; Matel, L.; Macasek, F.; Kristin, J.

1999-01-01

Hydroxyapatite, Ca 10 (PO 4 ) 6 (OH) 2 is a mineral widely spread in nature as a main constituent of phosphate rocks, and also as the major inorganic component of bones and teeth. It was found that sorption process occurs by an ion exchange reaction mechanism between strontium ions in solution and calcium ions in apatite. Ca 2+ → Sr 2+ substitution in hydroxyapatite is important since it explains the mechanism of incorporation of beta-active Sr-90 of atomic debris into the human skeletal system. The strontium uptake at 100 grad C is done by adsorption and diffusion while at 25 grad C it is done by the process of adsorption only. The hydroxyapatite was prepared from aqueous solutions and characterized by standard analytical methods. Some samples of hydroxyapatite were modified by heating after its precipitation from aqueous solution. The sample obtained had characteristics of well crystallized stoichiometric hydroxyapatite. Also, commercial hydroxy-apatites were used. Sorption of strontium ions on synthetic hydroxyapatite was examined using batch method and sorption depends on the method of preparation of hydroxyapatite. In generally, sorption of strontium decreases with the increase in the particle size of hydroxyapatite and decreases with the increase in the pH ( hydroxyapatite surface is amphoteric and acts as a buffer in a wide pH range). The sorption of strontium increases with the increase in [Sr 2+ ] or [Ca 2+ ] in solution to ∼ 10 -5 mol · dm -3 for the hydroxyapatite prepared by heating. The experimental data for sorption of strontium has been fitted with Langmuir-adsorption isotherm. (authors)

A novel method to reduce postoperative sensitivity after composite restoration: A triple-blinded in-vivo study

Directory of Open Access Journals (Sweden)

Chitra Janardhanan Vejai Vekaash

2018-01-01

Full Text Available Objective: To evaluate the efficacy of Zinc-carbonated hydroxyapatite in the reduction of postoperative sensitivity during composite placement. Context: Postoperative sensitivity after composite restoration still remains a major clinical challenge. Materials and Methods: Sixty class I cavities were prepared in 60 patients by the same operator with the following inclusion and exclusion criteria: The patients selected for the study were between 20–45 years with vital pulp and having remaining dentin thickness of 1mm. Previously restored, nonvital and tooth with periodical changes were excluded. Patients were randomly divided into two groups of 30 each—Group I self-etch and Group II selective-etch with Subgroup A- zinc-carbonated hydroxyapatite applied and Subgroup B- zinc-carbonated hydroxyapatite not applied. After the surface treatment, the teeth were restored with composite resin. The patients were evaluated with visual analogue scale (VAS at the end of one week and one month. Statistical Analysis: Data were analyzed using Kruskal–Wallis one-way analysis. Results: Comparing within groups, Group I self-etch mean values showed statistically significant lower values compared with Group II selective-etch (P < 0.01. Zinc-carbonated hydroxyapatite Subgroup A showed statistically significant lower values compared with Subgroup B where zinc-carbonated hydroxyapatite was not applied (P < 0.01. Conclusion: Application of zinc-carbonated hydroxyapatite showed significant reduction in postoperative sensitivity after composite placement.

Self-assembled high-strength hydroxyapatite/graphene oxide/chitosan composite hydrogel for bone tissue engineering.

Science.gov (United States)

Yu, Peng; Bao, Rui-Ying; Shi, Xiao-Jun; Yang, Wei; Yang, Ming-Bo

2017-01-02

Graphene hydrogel has shown greatly potentials in bone tissue engineering recently, but it is relatively weak in the practical use. Here we report a facile method to synthesize high strength composite graphene hydrogel. Graphene oxide (GO), hydroxyapatite (HA) nanoparticles (NPs) and chitosan (CS) self-assemble into a 3-dimensional hydrogel with the assistance of crosslinking agent genipin (GNP) for CS and reducing agent sodium ascorbate (NaVC) for GO simultaneously. The dense and oriented microstructure of the resulted composite gel endows it with high mechanical strength, high fixing capacity of HA and high porosity. These properties together with the good biocompatibility make the ternary composite gel a promising material for bone tissue engineering. Such a simultaneous crosslinking and reduction strategy can also be applied to produce a variety of 3D graphene-polymer based nanocomposites for biomaterials, energy storage materials and adsorbent materials. Copyright © 2016 Elsevier Ltd. All rights reserved.

Synthesis and Characterization of Nano-Hydroxyapatite/mPEG-b-PCL Composite Coating on Nitinol Alloy

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Mohamadreza Etminanfar

2017-12-01

Full Text Available In this study the bioactivity of hydroxyapatite/poly(ε-caprolactone–poly(ethylene glycol bilayer coatings on Nitinol superelastic alloy was investigated. The surface of Nitinol alloy was activated by a thermo-chemical treatment and hydroxyapatite coating was electrodeposited on the alloy, followed by applying the polymer coating. The surface morphology of coatings was studied using FE-SEM and SEM. The data revealed that the hydroxyapatite coating is composed of one-dimensional nano sized flakes and the polymer coating is uniformly covered the sublayer. Also, High resolution TEM studies on the hydroxyapatite samples revealed that each flake contains nano-crystalline grains with a diameter of about 15 nm. The hydroxyapatite monolayer coating was rapidly covered by calcium phosphate crystals (Ca/P=1.7 after immersion in simulated body fluid confirming the bioactivity of the nanostructured flakes. However, the flakes were weak against applied external forces because of their ultra-fine thickness. Scratch test was applied on hydroxyapatite/polymer coating to evaluate delamination of the coating from substrate. It was shown that, the polymer coating has a great influence on toughening the hydroxyapatite coating. To assess the degradation effect of the polymer layer on hydroxyapatite coating, samples were immersed in phosphate-buffered saline at 37 ᵒC. SEM studies on the samples revealed that the beneath layer of hydroxyapatite appears after 72 h without any visible change in morphology. It seems that, application of a biodegradable polymer film on the nanostructured hydroxyapatite coating is a good way to support the coating during implantation processes

COMPARISON OF REACTIVITY OF SYNTHETIC AND BOVINE HYDROXYAPATITE IN VITRO UNDER DYNAMIC CONDITIONS

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DIANA HORKAVCOVÁ

2014-03-01

Full Text Available Hydroxyapatite materials prepared by two methods: synthetic (HA–S and bovine (HA-B granules were exposed to a longterm in vitro test under dynamic conditions. Testing cells, filled up to one fourth (¼V of their volume with the tested material, were exposed to continuous flow of simulated body fluid (SBF for 56 days. The objective of the experiment was to determine whether reactivity of the biomaterials (hydroxyapatites, prepared by different methods but identical in terms of their chemical and phase composition, in SBF were comparable. Analyses of the solutions proved that both materials were highly reactive from the very beginning of interaction with SBF (significant decrease of Ca2+ and (PO43- concentrations in the leachate. SEM/EDS images have shown that the surface of bovine HA-B was covered with a new hydroxyapatite (HAp phase in the first two weeks of the test while synthetic HA–S was covered after two weeks of the immersion in SBF. At the end of the test, day 56, both materials were completely covered with well developed porous HAp phase in form of nano-plates. A calculation of the rate of HAp formation from the concentration of (PO43- ions in SBF leachates confirmed that all removed ions were consumed for the formation of the HAp phase throughout the entire testing time for bovine HA–B and only during the second half of the testing time for synthetic HA–S.

Preferential Alignment of Hydroxyapatite Crystallites in Nanocomposites with Chemically Disintegrated Silk Fibroin

International Nuclear Information System (INIS)

Nemoto, Rei; Wang Li; Ikoma, Toshiyuki; Tanaka, Junzo; Senna, Mamoru

2004-01-01

Hydroxyapatite (HAp) nanocrystals were prepared at room temperature by a coprecipitation method from Ca(OH) 2 and H 3 PO 4 , in the presence of chemically disintegrated silk fibroin (SF). Adsorbed amounts of cations on SF and crystallinity of HAp in the composite were increased by the chemical disintegration of SF higher order structure. Preferential alignment of c-axis of HAp crystallites along the longitudinal direction of ca. 150nm SF fibril was observed. These changes due to disintegration of SF were discussed in terms of the chemical interaction between HAp and SF. The resulted composite with preferential alignment of HAp nanocrystals is a good candidate as a starting material for bone substitutes

Polymer-Ceramic Composite Scaffolds: The Effect of Hydroxyapatite and β-tri-Calcium Phosphate

Directory of Open Access Journals (Sweden)

Boyang Huang

2018-01-01

Full Text Available The design of bioactive scaffolds with improved mechanical and biological properties is an important topic of research. This paper investigates the use of polymer-ceramic composite scaffolds for bone tissue engineering. Different ceramic materials (hydroxyapatite (HA and β-tri-calcium phosphate (TCP were mixed with poly-ε-caprolactone (PCL. Scaffolds with different material compositions were produced using an extrusion-based additive manufacturing system. The produced scaffolds were physically and chemically assessed, considering mechanical, wettability, scanning electron microscopy and thermal gravimetric tests. Cell viability, attachment and proliferation tests were performed using human adipose derived stem cells (hADSCs. Results show that scaffolds containing HA present better biological properties and TCP scaffolds present improved mechanical properties. It was also possible to observe that the addition of ceramic particles had no effect on the wettability of the scaffolds.

A novel self-catalyzed photoATRP strategy for preparation of fluorescent hydroxyapatite nanoparticles and their biological imaging

Science.gov (United States)

Jiang, Ruming; Liu, Meiying; Huang, Hongye; Huang, Long; Huang, Qiang; Wen, Yuanqing; Cao, Qian-yong; Tian, Jianwen; Zhang, Xiaoyong; Wei, Yen

2018-03-01

Hydroxyapatite (HAp), as an important biomaterial for the regeneration and reconstruction of bone tissue, has attracted more and more attention of researchers and scientists due to its unique structure and compositions. However, the preparation of fluorescent HAp with controllable morphology has achieved only limited success. In this work, we reported a novel strategy to construct the water dispersible fluorescent HAp nanorods via the combination of ligand exchange and metal-free atom transfer radical polymerization (ATRP). The Br-containing fluorescent HAp nanorods with controllable size and morphology were first prepared through hydrothermal treatment. A multifunctional organic molecule (named as PTH-Br) with aggregation-induced emission feature was immobilized on the surface of hydrophobic HAp nanorods through ligand exchange reaction. The PTH-Br could be used as the initiator and catalyst for surface-initiated metal-free ATRP using poly(ethylene glycol) methacrylate as monomer to obtain hydrophilic fluorescent HAp polymer nanoparticles. This strategy successfully endowed HAp nanorods excellent fluorescence properties and favorable water dispersibility but well preserved their regular morphology. Biological assays demonstrated that the HAp-PTH-poly(PEGMA) nanoparticles exhibited good biocompatibility and efficient cell uptake performance. Taken together, we have developed a rather facile strategy based on the surface ligand exchange reaction and metal-free photoATRP to fabricate fluorescent HAp with controllable size and morphology, high water dispersibility and biological properties. These HAp-PTH-poly(PEGMA) nanoparticles should be novel and promising candidates for biomedical applications.

Preparation of bone-implants by coating hydroxyapatite nanoparticles on self-formed titanium dioxide thin-layers on titanium metal surfaces.

Science.gov (United States)

Wijesinghe, W P S L; Mantilaka, M M M G P G; Chathuranga Senarathna, K G; Herath, H M T U; Premachandra, T N; Ranasinghe, C S K; Rajapakse, R P V J; Rajapakse, R M G; Edirisinghe, Mohan; Mahalingam, S; Bandara, I M C C D; Singh, Sanjleena

2016-06-01

Preparation of hydroxyapatite coated custom-made metallic bone-implants is very important for the replacement of injured bones of the body. Furthermore, these bone-implants are more stable under the corrosive environment of the body and biocompatible than bone-implants made up of pure metals and metal alloys. Herein, we describe a novel, simple and low-cost technique to prepare biocompatible hydroxyapatite coated titanium metal (TiM) implants through growth of self-formed TiO2 thin-layer (SFTL) on TiM via a heat treatment process. SFTL acts as a surface binder of HA nanoparticles in order to produce HA coated implants. Colloidal HA nanorods prepared by a novel surfactant-assisted synthesis method, have been coated on SFTL via atomized spray pyrolysis (ASP) technique. The corrosion behavior of the bare and surface-modified TiM (SMTiM) in a simulated body fluid (SBF) medium is also studied. The highest corrosion rate is found to be for the bare TiM plate, but the corrosion rate has been reduced with the heat-treatment of TiM due to the formation of SFTL. The lowest corrosion rate is recorded for the implant prepared by heat treatment of TiM at 700 °C. The HA-coating further assists in the passivation of the TiM in the SBF medium. Both SMTiM and HA coated SMTiM are noncytotoxic against osteoblast-like (HOS) cells and are in high-bioactivity. The overall production process of bone-implant described in this paper is in high economic value. Copyright © 2016 Elsevier B.V. All rights reserved.

Cobalt doped proangiogenic hydroxyapatite for bone tissue engineering application

Energy Technology Data Exchange (ETDEWEB)

Kulanthaivel, Senthilguru [Department of Biotechnology and Medical Engineering, National Institute of Technology, Rourkela, Odisha 769008 (India); Roy, Bibhas [Department of Biotechnology, Indian Institute of Technology Kharagpur, Kharagpur, West Bengal 721302 (India); Agarwal, Tarun [Department of Biotechnology and Medical Engineering, National Institute of Technology, Rourkela, Odisha 769008 (India); Giri, Supratim [Department of Chemistry, National Institute of Technology, Rourkela, Odisha 769008 (India); Pramanik, Krishna; Pal, Kunal; Ray, Sirsendu S. [Department of Biotechnology and Medical Engineering, National Institute of Technology, Rourkela, Odisha 769008 (India); Maiti, Tapas K. [Department of Biotechnology, Indian Institute of Technology Kharagpur, Kharagpur, West Bengal 721302 (India); Banerjee, Indranil, E-mail: indraniliit@gmail.com [Department of Biotechnology and Medical Engineering, National Institute of Technology, Rourkela, Odisha 769008 (India)

2016-01-01

ABSTRACT: The present study delineates the synthesis and characterization of cobalt doped proangiogenic–osteogenic hydroxyapatite. Hydroxyapatite samples, doped with varying concentrations of bivalent cobalt (Co{sup 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. - Highlights: • Cobalt (Co{sup +2}) doped hydroxyapatite (Co-HAp) can be prepared by the wet chemical method. • The concentration of Co{sup +2} influences the physico-chemical properties of HAp. • Co-HAp was found to be biocompatible and osteogenic. • Co-HAp enhanced cellular VEGF secretion through HIF-1α stabilization. • The optimum biological performance of Co-HAp was achieved for 0.33% (w/w) Co{sup +2} doping.

Structural Properties and Antifungal Activity against Candida albicans Biofilm of Different Composite Layers Based on Ag/Zn Doped Hydroxyapatite-Polydimethylsiloxanes

Directory of Open Access Journals (Sweden)

Andreea Groza

2016-04-01

Full Text Available Modern medicine is still struggling to find new and more effective methods for fighting off viruses, bacteria and fungi. Among the most dangerous and at times life-threatening fungi is Candida albicans. Our work is focused on surface and structural characterization of hydroxyapatite, silver doped hydroxyapatite and zinc doped hydroxyapatite deposited on a titanium substrate previously coated with polydimethylsiloxane (HAp-PDMS, Ag:HAp-PDMS, Zn:HAp-PDMS by different techniques: Scanning Electron Microscopy (SEM, Glow Discharge Optical Emission Spectroscopy (GDOES and Fourier Transform Infrared Spectroscopy (FTIR. The morphological studies revealed that the use of the PDMS polymer as an interlayer improves the quality of the coatings. The structural characterizations of the thin films revealed the basic constituents of both apatitic and PDMS structure. In addition, the GD depth profiles indicated the formation of a composite material as well as the successful embedding of the HAp, Zn:HAp and Ag:HAp into the polymer. On the other hand, in vitro evaluation of the antifungal properties of Ag:HAp-PDMS and Zn:HAp-PDMS demonstrated the fungicidal effects of Ag:HAp-PDMS and the potential antifungal effect of Zn:HAp-PDMS composite layers against C. albicans biofilm. The results acquired in this research complete previous research on the potential use of new complex materials produced by nanotechnology in biomedicine.

Ion exchange of strontium on synthetic hydroxyapatite

International Nuclear Information System (INIS)

Lazic, S.; Vukovic, Z.

1991-01-01

Adsorption of strontium ions on synthetic hydroxyapatite was examined using both batch and column methods. The apatite was prepared from aqueous solutions and characterized by standard analytical methods. The sample obtained had characteristics of well crystallized stoichiometric hydroxyapatite. The experimental data for sorption of strontium can be very well fitted with Langmuir's adsorption isotherm. It was found that sorption occurs by an ion exchange reaction between strontium ions in solution and calcium ions in apatite. (author) 14 refs.; 5 figs.; 1 tab

Bioinspired Hydroxyapatite/Poly(methyl methacrylate) Composite with a Nacre-Mimetic Architecture by a Bidirectional Freezing Method.

Science.gov (United States)

Bai, Hao; Walsh, Flynn; Gludovatz, Bernd; Delattre, Benjamin; Huang, Caili; Chen, Yuan; Tomsia, Antoni P; Ritchie, Robert O

2016-01-06

Using a bidirectional freezing technique, combined with uniaxial pressing and in situ polymerization, "nacre-mimetic" hydroxyapatite/poly(methyl methacrylate) (PMMA) composites are developed by processing large-scale aligned lamellar ceramic scaffolds. Structural and mechanical characterization shows "brick-and-mortar" structures, akin to nacre, with interesting combinations of strength, stiffness, and work of fracture, which provide a pathway to making strong and tough lightweight materials. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Study of sorption processes of copper on synthetic hydroxyapatite

International Nuclear Information System (INIS)

Rosskopfova, O.; Galambos, M.; Ometakova, J.; Rajec, P.; Caplovicova, M.

2012-01-01

The sorption of copper on synthetic hydroxyapatite was investigated using a batch method and radiotracer technique. The hydroxyapatite sample prepared by a wet precipitation process was of high crystallinity with Ca/P ratio of 1.688. The sorption of copper on hydroxyapatite was pH independent ranging from 4 to 6 as a result of buffering properties of hydroxyapatite. The adsorption of copper was rapid and the percentage of Cu sorption was >98% during the first 15-30 min of the contact time. The experimental data for sorption of copper have been interpreted in the term of Langmuir isotherm. The sorption of Cu 2+ ions was performed by ion-exchange with Ca 2+ cations on the crystal surface of hydroxyapatite under experimental conditions. The competition effect of Zn 2+ , Fe 2+ and Pb 2+ towards Cu 2+ sorption was stronger than that of Co 2+ , Ni 2+ and Ca 2+ ions. The ability of the bivalent cations to depress the sorption of copper on hydroxyapatite was in the following order Pb 2+ > Fe 2+ > Zn 2+ > Co 2+ ∼ Ni 2+ . (author)

Surface characteristics of hydroxyapatite-coated layer prepared on nanotubular Ti–35Ta–xHf alloys by EB-PVD

Energy Technology Data Exchange (ETDEWEB)

Jeong, Yong-Hoon [Department of Dental Materials and Research Center of Nano-Interface Activation for Biomaterials, School of Dentistry, Chosun University, Gwangju (Korea, Republic of); Biomechanics and Tissue Engineering Laboratory, Division of Orthodontics, College of Dentistry, The Ohio State University, Columbus, OH (United States); Moon, Byung-Hak [Department of Dental Materials and Research Center of Nano-Interface Activation for Biomaterials, School of Dentistry, Chosun University, Gwangju (Korea, Republic of); Choe, Han-Cheol, E-mail: hcchoe@chosun.ac.kr [Department of Dental Materials and Research Center of Nano-Interface Activation for Biomaterials, School of Dentistry, Chosun University, Gwangju (Korea, Republic of); Brantley, William A. [Division of Restorative, Prosthetic and Primary Care Dentistry, College of Dentistry, The Ohio State University, Columbus, OH (United States)

2013-12-31

In this study, we investigated the surface characteristics of hydroxyapatite (HA)-coated layers prepared by electron-beam physical vapor deposition (EB-PVD) on nanotubular Ti–35Ta–xHf alloys (x = 3, 7, and 15 wt.%). Ti–35Ta–xHf alloys were first prepared by arc melting. Formation of a nanotube structure on these alloys was achieved by an electrochemical method in 1 M H{sub 3}PO{sub 4} + 0.8 wt.% NaF electrolytes. The HA coatings were then deposited on the nanotubular surface by an EB-PVD method. The surface characteristics were analyzed by field-emission scanning electron microscopy, energy-dispersive X-ray spectroscopy, and X-ray diffraction (XRD). The electrochemical behavior was examined using a potentiodynamic polarization test in 0.9% NaCl solution. The Ti–35Ta–xHf alloys had an equiaxed grain structure with α″ + β phases, and the α″ phase disappeared with increases in Hf content. The Ti–35Ta–15Hf alloy showed higher β-phase peak intensity in the XRD patterns than that for the lower Hf-content alloys. A highly ordered nanotubular oxide layer was formed on the Ti–35Ta–15Hf alloy, and the tube length depended on Hf content. The HA coating surface formed at traces of the nanotubular titanium oxide layer and completely covered the tips of the nanotubes with a cluster shape. From the potentiodynamic polarization tests, the incorporation of Hf element and formation of the nanotubular structure were the main factors for achieving lower current density. In particular, the surface of the HA coating on the nanotubular structure exhibited higher corrosion resistance than that of the nanotubular titanium oxide structure without an HA coating. - Highlights: • Hydroxyapatite (HA) was coated on nanotubular Ti–35Ta–xHf alloys, using EB-PVD. • Increasing the Hf content reduced the relative proportion of α″ martensite to β-Ti in the microstructures. • The detailed nanotubular structure formed by anodization depended on alloy composition

Surface characteristics of hydroxyapatite-coated layer prepared on nanotubular Ti–35Ta–xHf alloys by EB-PVD

International Nuclear Information System (INIS)

Jeong, Yong-Hoon; Moon, Byung-Hak; Choe, Han-Cheol; Brantley, William A.

2013-01-01

In this study, we investigated the surface characteristics of hydroxyapatite (HA)-coated layers prepared by electron-beam physical vapor deposition (EB-PVD) on nanotubular Ti–35Ta–xHf alloys (x = 3, 7, and 15 wt.%). Ti–35Ta–xHf alloys were first prepared by arc melting. Formation of a nanotube structure on these alloys was achieved by an electrochemical method in 1 M H 3 PO 4 + 0.8 wt.% NaF electrolytes. The HA coatings were then deposited on the nanotubular surface by an EB-PVD method. The surface characteristics were analyzed by field-emission scanning electron microscopy, energy-dispersive X-ray spectroscopy, and X-ray diffraction (XRD). The electrochemical behavior was examined using a potentiodynamic polarization test in 0.9% NaCl solution. The Ti–35Ta–xHf alloys had an equiaxed grain structure with α″ + β phases, and the α″ phase disappeared with increases in Hf content. The Ti–35Ta–15Hf alloy showed higher β-phase peak intensity in the XRD patterns than that for the lower Hf-content alloys. A highly ordered nanotubular oxide layer was formed on the Ti–35Ta–15Hf alloy, and the tube length depended on Hf content. The HA coating surface formed at traces of the nanotubular titanium oxide layer and completely covered the tips of the nanotubes with a cluster shape. From the potentiodynamic polarization tests, the incorporation of Hf element and formation of the nanotubular structure were the main factors for achieving lower current density. In particular, the surface of the HA coating on the nanotubular structure exhibited higher corrosion resistance than that of the nanotubular titanium oxide structure without an HA coating. - Highlights: • Hydroxyapatite (HA) was coated on nanotubular Ti–35Ta–xHf alloys, using EB-PVD. • Increasing the Hf content reduced the relative proportion of α″ martensite to β-Ti in the microstructures. • The detailed nanotubular structure formed by anodization depended on alloy composition. • The

Multifunctional nano-hydroxyapatite and alginate/gelatin based sticky gel composites for potential bone regeneration

International Nuclear Information System (INIS)

Cai, Yurong; Yu, Juhong; Kundu, Subhas C.; Yao, Juming

2016-01-01

To improve the fixations of the implant and implant-bone integration after joint arthroplasty from locally preventing inflammation and promoting the bone regeneration, we design a multifunctional biomaterial consisting of recombinant human bone morphogenetic protein 2 (rhBMP-2) and antibiotic loaded nano-hydroxyapatite with an alginate/gelatin sticky gel. We investigate its role for the prevention of the inflammation and possibility of inducing a new bone growth along with its adhesive ability. The stickiness exists in the composite, which may help to fix itself on the bone fracture surface. The composite sustains the antibacterial effect and promotes the proliferation and differentiation of MG63 cells in vitro. In vivo experimentation also shows that the composite gel has a role for the reduction of inflammation. It enhances the formation of new bone and blood vessels compared to both the sole rhBMP-2 and non-rhBMP-2/antibiotic loaded composite gels. The multifunctional composite provides a promising material for the prosthetic and bone tissue regeneration. - Highlights: • Multifunctional nanohydroxyapatite composite is fabricated. • The composite consists of nHAP, growth factor, antibiotic and alginate/gelatin gel. • The composite shows antibacterial effect and good cytocompatibility. • No adverse effect to the cells tested in vitro and in vivo.

Multifunctional nano-hydroxyapatite and alginate/gelatin based sticky gel composites for potential bone regeneration

Energy Technology Data Exchange (ETDEWEB)

Cai, Yurong; Yu, Juhong [The Key Laboratory of Advanced Textile Materials and Manufacturing Technology of Ministry of Education, National Engineering Lab of Textile Fiber Materials & Processing Technology, College of Materials and Textile, Zhejiang Sci-Tech University, Hangzhou 310018 (China); Kundu, Subhas C. [Department of Biotechnology, Indian Institute of Technology (IIT) Kharagpur, West Bengal 721302 (India); Institute of Tissue Regeneration Engineering (ITREN), Dankook University, Cheonan 330-714 (Korea, Republic of); Yao, Juming, E-mail: yaoj@zstu.edu.cn [The Key Laboratory of Advanced Textile Materials and Manufacturing Technology of Ministry of Education, National Engineering Lab of Textile Fiber Materials & Processing Technology, College of Materials and Textile, Zhejiang Sci-Tech University, Hangzhou 310018 (China)

2016-09-15

To improve the fixations of the implant and implant-bone integration after joint arthroplasty from locally preventing inflammation and promoting the bone regeneration, we design a multifunctional biomaterial consisting of recombinant human bone morphogenetic protein 2 (rhBMP-2) and antibiotic loaded nano-hydroxyapatite with an alginate/gelatin sticky gel. We investigate its role for the prevention of the inflammation and possibility of inducing a new bone growth along with its adhesive ability. The stickiness exists in the composite, which may help to fix itself on the bone fracture surface. The composite sustains the antibacterial effect and promotes the proliferation and differentiation of MG63 cells in vitro. In vivo experimentation also shows that the composite gel has a role for the reduction of inflammation. It enhances the formation of new bone and blood vessels compared to both the sole rhBMP-2 and non-rhBMP-2/antibiotic loaded composite gels. The multifunctional composite provides a promising material for the prosthetic and bone tissue regeneration. - Highlights: • Multifunctional nanohydroxyapatite composite is fabricated. • The composite consists of nHAP, growth factor, antibiotic and alginate/gelatin gel. • The composite shows antibacterial effect and good cytocompatibility. • No adverse effect to the cells tested in vitro and in vivo.

Improved osteoblasts growth on osteomimetic hydroxyapatite/BaTiO{sub 3} composites with aligned lamellar porous structure

Energy Technology Data Exchange (ETDEWEB)

Liu, Beilei [Department of Stomatology, Third Xiangya Hospital, Central South University, Changsha, Hunan 410013 (China); Chen, Liangjian, E-mail: jian007040@sina.com [Department of Stomatology, Third Xiangya Hospital, Central South University, Changsha, Hunan 410013 (China); State Key Laboratory of Powder Metallurgy, Central South University, Changsha, Hunan 410083 (China); Shao, Chunsheng [Department of Stomatology, Third Xiangya Hospital, Central South University, Changsha, Hunan 410013 (China); Zhang, Fuqiang; Zhou, Kechao [State Key Laboratory of Powder Metallurgy, Central South University, Changsha, Hunan 410083 (China); Cao, Jun [Department of Stomatology, Third Xiangya Hospital, Central South University, Changsha, Hunan 410013 (China); Zhang, Dou, E-mail: dzhang@csu.edu.cn [State Key Laboratory of Powder Metallurgy, Central South University, Changsha, Hunan 410083 (China)

2016-04-01

Osteoblasts growing into bone substitute is an important step of bone regeneration. This study prepared porous hydroxyapatite (HA)/BaTiO{sub 3} piezoelectric composites with porosity of 40%, 50% and 60% by ice-templating method. Effects of HA/BaTiO{sub 3} composites with different porosities, with and without polarizing treatment on adhesion, proliferation and differentiation of osteoblasts were investigated in vitro. Results revealed that cell densities of the porous groups were significantly higher than those of the dense group (p < 0.05), so did the alkaline phosphate (ALP) and bone gla protein (BGP) activities. Porosity of 50% group exhibited higher ALP activity and BGP activity than those of the 40% and 60% groups. Scanning electron microscopy (SEM) observations revealed that osteoblasts adhered and stretched better on porous HA/BaTiO{sub 3} than on the dense one, especially HA/BaTiO{sub 3} with porosity of 50% and 60%. However, there was no significant difference in the cell morphology, cell densities, ALP and BGP activities between the polarized group and the non-polarized group (p > 0.05). The absence of mechanical loading on the polarized samples may account for this. The results indicated that hierarchically porous HA/BaTiO{sub 3} played a favorable part in osteoblasts proliferation, differentiation and adhesion process and is a promising bone substitute material. - Graphical abstract: Aligned porous structure of HA/BaTiO{sub 3} piezoelectric composites prepared by ice-templating method was similar to the lamellar Haversian system in bone tissue. When co-cultured with human osteosarcoma cells (MG63), porous HA/BaTiO{sub 3} composites exhibited remarkable biological activity in promoting proliferation, differentiation and adhesion of MG63 cells. - Highlights: • The aligned porous structure of HA/BaTiO{sub 3} composite was similar to the lamellar Haversian system in bone tissue. • The piezoelectric d{sub 33} coefficient of HA/BaTiO{sub 3} with porosity

Vancomycin–chitosan composite deposited on post porous hydroxyapatite coated Ti6Al4V implant for drug controlled release

Energy Technology Data Exchange (ETDEWEB)

Yang, Chi-Chuan [Department of Materials Science and Engineering, National Chung Hsing, University 250, Kuo-Kuang Road, Taichung 40227, Taiwan (China); Lin, Chien-Chung [Department of Materials Science and Engineering, National Chung Hsing, University 250, Kuo-Kuang Road, Taichung 40227, Taiwan (China); Department of Orthopaedic Surgery, Taichung Armed Force General Hospital, 348, Sec. 2, Jhongshan Road, Taiping City, Taichung 411, Taiwan (China); Liao, Jiunn-Wang [Graduate Institute of Veterinary Pathobiology, National Chung Hsing, University 250, Kuo-Kuang Road, Taichung 40227, Taiwan (China); Yen, Shiow-Kang, E-mail: skyen@dragon.nchu.edu.tw [Department of Materials Science and Engineering, National Chung Hsing, University 250, Kuo-Kuang Road, Taichung 40227, Taiwan (China)

2013-05-01

Through the hydrogen bonds and the deprotonation, the vancomycin–chitosan composite has been originally deposited on Ti4Al4V by electrochemical technology. However, the rapid destruction of the hydrogen bonding between them by polar water molecules during immersion tests revealed 80% drug burst in a few hours. In this study, the post porous hydroxyapatite (HA) coated Ti4Al4V is prepared for the subsequent electrolytic deposition of vancomycin–chitosan composite to control the drug release. As expected, the initial burst is reduced to 55%, followed by a steady release about 20% from day 1 to day 5 and a slower release of the retained 25% after day 6, resulting in bacterial inhibition zone diameter of 30 mm which can last for more than a month in antibacterial tests, compared with the coated specimen without HA gradually loosing inhibition zone after 21 days. Besides, the cell culture indicates that the vancomycin–chitosan/HA composite coated has enhanced the proliferation, the differentiation and the mineralization of the osteoblast-like cell. In general, it is helpful for the osteointegration on permanent implants. Consistently, it effectively provides the prophylaxis and therapy of osteomyelitis according to the results of the rabbit infection animal model. - Highlights: ► The releasing curve of the vancomycin–chitosan/HA composite revealed three periods. ► The drug release sustained one month due to the effect of post porous HA coating. ► The composite coating could treat the osteomyelitis in the rabbit infection model.

Structural characteristics of porous hydroxyapatite coating on CaO-SiO{sub 2} system glass

Energy Technology Data Exchange (ETDEWEB)

Zhang Hongquan; Yan Yuhua; Li Shipu [Wuhan Univ. of Technology (China). Biomedical and Engineering Research Center

2001-07-01

Hydroxyapatite(HA) coated CaO-SiO{sub 2} system glass composites were prepared successfully by the hydrothermal coating method at the temperature of 250 to 350 C and at pH of 7 to 9. The microstructure and phase composition were identified by XRD, FT-IR, SEM, EPMA and TEM. It is shown that HA coating possessed a porous gradient construction in the interface; HA coating and glass substrate were tightly bonded by an obvious transition. HA coating had a well-distributed porous construction on the surface layer. The interface structure, phase composition and the stability of HA coated glass composites were related with its forming process. These kinds of structure will benefit to the interface bonging strength and bone bonding strength. (orig.)

Mesoporous hydroxyapatite: Preparation, drug adsorption, and release properties

Energy Technology Data Exchange (ETDEWEB)

Gu, Lina; He, Xiaomei; Wu, Zhenyu, E-mail: zhenyuwuhn@sina.com

2014-11-14

Mesoporous hydroxyapatite (HA) was synthesized through gas–liquid chemical precipitation method at ambient temperature without any template. Structure, morphology and pore size distribution of HA were analyzed via X-ray powder diffraction, scanning electron microscopy, transmission electron microscopy, high-resolution electron microscopy and N{sub 2} adsorption/desorption. The chemotherapeutic agent doxorubicin (DOX) was used to investigate the drug adsorption and release behavior of HA. The kinetics of DOX adsorption on HA followed the pseudo-second-order rate expression. Adsorption isotherms at various temperatures were obtained, and the equilibrium data fitted the Langmuir model. The values of thermodynamic parameters (Gibbs free energy, entropy, and enthalpy changes) demonstrated that the adsorption process was spontaneous and endothermic. In vitro pH-responsive (pH = 7.4, 5.8) controlled release was investigated. DOX-loaded HA showed a slow, long-term, and steady release rate. The release rate at pH5.8 was larger than that at pH7.4. Consequently, the as-prepared mesoporous HA has potential applications in controlled drug delivery systems. - Highlights: • Mesoporous HA was synthesized by a simple precipitation method without any template. • The kinetics of adsorption followed the pseudo-second-order rate expression. • Thermodynamics investigation showed that adsorption was spontaneous and endothermic. • DOX-loaded HA showed a long-term, steady, and pH-controlled release rate.

Cadmium immobilization by hydroxyapatite

Directory of Open Access Journals (Sweden)

Smičiklas Ivana D.

2003-01-01

Full Text Available The contamination of air, soil and water by cadmium is a great environmental problem. If cadmium occurs in nature in ionic form, soluble in water, it easily enters into the food chain. Hydroxyapatite (HAP, Ca-o(POAe(OH2 is a sparingly soluble salt and an excellent matrix for the removal of heavy metals from solutions. Considerable research attention has been paid to the bond between Cc/2+ ions and synthetic hydroxyapatite of known composition. The sorption mechanism is complex. The dominant process is ion exchange, but surface adsorption, surface complexation and coprecipitation can also contribute to the overall mechanism. The sorption capacity depends on the characteristics of hydroxyapatite itself and on the experimental conditions. Under optimum conditions a maximum capacity of 0.8 mol Cd2+/mol HAP can be achieved. HAP is a potential sorbent for the remediation of contaminated water and soil, for industrial waste treatment, and it is also referenced as a material that can be used as a barrier around waste depositories.

Differentiation study of porous hydroxyapatite body fabricated by using three different additives

International Nuclear Information System (INIS)

Cik Rohaida Che Hak; Idris Besar; Rusnah Mustaffa; Mohd Reusmaazran Yusof

2005-01-01

Porous hydroxyapatite is suitable for bone surgery applications because it allows bone ingrowth and promotes faster healing. In this study, a porous hydroxyapatite body was fabricated by slip casting route, followed by a comprehensive investigation of its physical properties. The porous body was prepared by mixing the hydroxyapatite slurry with three different additives namely; sago beads, potassium oleate and sodium dodecyl sulphate (SDS). The mixture of slurry and additives was then casted in plaster mold before it was dried and sintered at high temperature. The structure of the porous body could be tailored by using different composition and parameters of the additives; sago beads (pore former agent), potassium oleate (foaming agent) and SDS (foaming agent). The role of these three additives was investigated by several chemical, physical and mechanical evaluations method. The identification of additives was determined by FTIR, the porosity of porous hydroxyapatite was measured by Densitometer and the morphology of the porous structure was observed under Scanning Electron Microscopy and Image Analyzer. The results showed that potassium oleate contribute significantly towards porosity. However the resulting porosity would actually very dependent on the proportions of the additives, the more additives being added, the higher the porosity. All three additives produced macrostructure with pores larger than 100 mm, however the one produced by using sago beads showed a less pore interconnection structure compared to those obtained by both foaming agent. Playing with different proportions of these additives, it was possible to improve the foam stability, size of pores and pore connectivity in order to reproduce the porous hydroxyapatite body that having a similar pore structure of the natural bone. (Author)

Determination of Microstructural Parameters of Nanocrystalline Hydroxyapatite Prepared by Mechanical Alloying Method

Science.gov (United States)

Joughehdoust, Sedigheh; Manafi, Sahebali

2011-12-01

Hydroxyapatite [HA, Ca10(PO4)6(OH)2] is chemically similar to the mineral component of bones and hard tissues. HA can support bone ingrowth and osseointegration when used in orthopaedic, dental and maxillofacial applications. In this research, HA nanostructure was synthesized by mechanical alloying method. Phase development, particle size and morphology of HA were investigated by X-ray diffraction (XRD) pattern, zetasizer instrument, scanning electron microscopy (SEM), respectively. XRD pattern has been used to determination of the microstructural parameters (crystallite size, lattice parameters and crystallinity percent) by Williamson-Hall equation, Nelson-Riley method and calculating the areas under the peaks, respectively. The crystallite size and particle size of HA powders were in nanometric scales. SEM images showed that some parts of HA particles have agglomerates. The ratio of lattice parameters of synthetic hydroxyapatite (c/a = 0.73) was determined in this study is the same as natural hydroxyapatite structure.

Preparation and labelling hydroxyapatite with 223Ra and 99mTc

International Nuclear Information System (INIS)

Malkova, E.; Micolova, P.; Vlk, M.; Kozempel, J.; Rabyk, M.

2015-01-01

The aim of this study was the preparation, studies and investigation of novel nanoparticles suitable for targeted delivery of 223 Ra and 99 mTc. Preliminary experiments were focused on the synthesis of hydroxyapatite nanoparticles (HANPs) and their affinity to 223 Ra and 99m Tc. Technetium-99m ( 99 mTc, T 1 /2 = 6.0 h) is the most commonly used medical radionuclide for diagnostic procedures. Radium-223 is the first -emitting radionuclide approved for targeted radionuclide therapy. The physical half-life of 223 Ra of 11.4 days is providing sufficient time for the synthesis, distribution and administration of the radiopharmaceutical to patients. HANPs labelling yields with 223 Ra were 95 - 100 % and with 99m Tc were 93 - 94 % depending on the reaction conditions. HANPs were studied on FT-IR (Fourier transform infrared spectroscopy), XRPD (X-Ray Powder Diffraction), DLS (Dynamic Light Scattering), and the sizes of nanoparticles were studied at temperatures 80, 120 and 200 grad C. (authors)

Preparation of micro-porous bioceramic containing silicon-substituted hydroxyapatite and beta-tricalcium phosphate.

Science.gov (United States)

Fuh, Lih-Jyh; Huang, Ya-Jing; Chen, Wen-Cheng; Lin, Dan-Jae

2017-06-01

Dimensional instability caused by sintering shrinkage is an inevitable drawback for conventional processing of hydroxyapatite (HA). A new preparation method for biphasic calcium phosphates was developed to increase micro pores and biodegradation without significant dimensional change. Powder pressed HA discs, under 100MPa, were immersed in a colloidal mixture of tetraethoxysilane (TEOS) and ammonium hydroxide for 10min, followed by drying, and then were sintered at 900°C, 1050°C, and 1200°C, respectively. Comparing with pure HA discs, the newly prepared product sintered up to 1200°C contained silicon substituted HA, beta-tricalcium phosphate, and calcium silicate with better micro-porosity, high specific surface area, less sintering shrinkage and the strength maintained. The cytocompatibility test demonstrated a better viability for D1 mice stem cells cultured on TEOS treated HA for 14days compared to the pure HA. This simple TEOS sol-gel pretreatment has the potential to be applied to any existing manufacturing process of HA scaffold for better control of sintering shrinkage, create micropores, and increase biodegradation. Copyright © 2017 Elsevier B.V. All rights reserved.

Preparation and antibacterial effect of silver-hydroxyapatite/titania nanocomposite thin film on titanium

Energy Technology Data Exchange (ETDEWEB)

Mo Anchun [West China College of Stomatology, Sichuan University, Chengdu 610041 (China)], E-mail: moanchun@163.com; Liao Juan [West China College of Stomatology, Sichuan University, Chengdu 610041 (China); Xu Wei [West China College of Stomatology, Sichuan University, Chengdu 610041 (China); Arrail-Dental, Shanghai 200122 (China); Xian Suqin [West China College of Stomatology, Sichuan University, Chengdu 610041 (China); Li Yubao [Research Center for Nano-Biomaterials, Sichuan University, Chengdu 610064 (China); Bai Shi [West China College of Stomatology, Sichuan University, Chengdu 610041 (China)

2008-11-15

The composite which contains Ag{sup +} and nanosized hydroxyapatite with TiO{sub 2} was deposited onto titanium by dipping method. The morphology, chemical components and structures of the thin film were characterized by XRD, scanning electronic microscope (SEM) and energy dispersive X-ray analysis (EDX). Staphylococcus aureus and Escherichia coli were utilized to test the antibacterial effect. XRD results demonstrated that the films have characteristic diffraction peaks of pure HA. EDX results showed that the deposited films consisted of Ca, P, Ti, O and Ag, all of which distribute uniformly. With regard to the antibacterial effect, 98% of S. aureus and more than 99% of E. coli were killed after 24 h incubation and pictures of SEM showed obviously fewer cells on the surface with coating.

Lead and copper removal from aqueous solutions by porous glass derived calcium hydroxyapatite

International Nuclear Information System (INIS)

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

2011-01-01

Graphical abstract: . Adsorption of Pb 2+ increases with the increase in NaCl volume percentage (1:0%, 2:30%, 3:40%, 4:40%) of the Glass Derived Hydroxyapatite and reaches equilibrium after 24 h. Highlights: → Novel porous glass derived hydroxyapatite matrix is prepared. → Glass derived hydroxyapatite matrix adsorbs lead and copper ions in solutions effectively. → Two adsorption mechanisms including ion exchange theory and the dissolution and precipitation theory are involved in removal of the heavy metal ions from the solutions. - Abstract: A porous glass was prepared by sintering Na 2 O-CaO-B 2 O 3 glass powder with powdered sodium chloride. Subsequently, the sodium chloride was dissolved in water resulting in a highly porous material. A sample was prepared consisting of 60 vol% glass and 40 vol% salt which both had particle sizes 2 HPO 4 solutions at room temperature for 1 day. The porous glass derived hydroxyapatite matrix was then processed for removing lead and copper ions from aqueous solutions. The results showed that the glass derived calcium hydroxyapatite matrix effectively immobilizes lead and copper ions in solution. The adsorption mechanism was investigated by the X-ray Diffraction (XRD) and Scanning Electron Microscopy including Energy Dispersive X-Ray Spectrometry (SEM-EDX).

Fabrication of polylactic acid/hydroxyapatite/graphene oxide composite and their thermal stability, hydrophobic and mechanical properties

Directory of Open Access Journals (Sweden)

Ming Gong

2017-06-01

Full Text Available A series of polylactic acid/hydroxyapatite/graphene oxide composite (PLA/HA/GO were fabricated via solution blending and casting method using N,N-dimethyl-formamide (DMF and CH2Cl2 as mutual solvents. The physicochemical properties of the resulting composites were characterized by means of FT-IR, SEM, TEM, Raman spectra, XRD and N2-physisorption. Particularly, the thermal stabilities, hydrophobic and mechanical properties of PLA/HA/GO composites were systematically investigated. The influences of GO content on thermal stabilities, hydrophobic and mechanical properties of the composites were also evaluated. The results showed that the addition of GO and HA not only improved the thermal stability of PLA, but also improved the hydrophobic property of PLA-based composites. By compared with the PLA/HA/GO composite, the tensile strength of pristine PLA is slight high. The tensile strength and hardness of PLA/HA/GO composites increased with the increase of GO content. The obtained PLA/HA/GO composite may be a promising material for load-bearing orthopedic implants.

Hydroxyapatite fiber reinforced poly(alpha-hydroxy ester) foams for bone regeneration

Science.gov (United States)

Thomson, R. C.; Yaszemski, M. J.; Powers, J. M.; Mikos, A. G.; McIntire, L. V. (Principal Investigator)

1998-01-01

A process has been developed to manufacture biodegradable composite foams of poly(DL-lactic-co-glycolic acid) (PLGA) and hydroxyapatite short fibers for use in bone regeneration. The processing technique allows the manufacture of three-dimensional foam scaffolds and involves the formation of a composite material consisting of a porogen material (either gelatin microspheres or salt particles) and hydroxyapatite short fibers embedded in a PLGA matrix. After the porogen is leached out, an open-cell composite foam remains which has a pore size and morphology defined by the porogen. By changing the weight fraction of the leachable component it was possible to produce composite foams with controlled porosities ranging from 0.47 +/- 0.02 to 0.85 +/- 0.01 (n = 3). Up to a polymer:fiber ratio of 7:6, short hydroxyapatite fibers served to reinforce low-porosity PLGA foams manufactured using gelatin microspheres as a porogen. Foams with a compressive yield strength up to 2.82 +/- 0.63 MPa (n = 3) and a porosity of 0.47 +/- 0.02 (n = 3) were manufactured using a polymer:fiber weight ratio of 7:6. In contrast, high-porosity composite foams (up to 0.81 +/- 0.02, n = 3) suitable for cell seeding were not reinforced by the introduction of increasing quantities of hydroxyapatite short fibers. We were therefore able to manufacture high-porosity foams which may be seeded with cells but which have minimal compressive yield strength, or low porosity foams with enhanced osteoconductivity and compressive yield strength.

Hydroxyapatite-lignin composite as a metallic implant-bone tissue osseointegration improver: experimental study in dogs

Directory of Open Access Journals (Sweden)

Fabrício Luciani Valente

2015-01-01

Full Text Available The study aimed to evaluate biocompatibility, osteoconduction and osseointegration of a pasty composite of hydroxyapatite (20% and lignin (80% as a promoter of metal implant and bone tissue integration. An intramedullary Schanz pin was implanted in both tibias of fifteen bitches. In the left tibia, the pin was coated with the biomaterial at the time of surgery. Marrow cavity was also filled with the biomaterial. Right limb did not receive the biomaterial, then constituting the control group. Tibias were harvested from five animals at 8, 60 and 150 days after surgery; three of them were analyzed by histological and biomechanical assessment and the two remaining tibias by X-ray diffraction. Results showed that the biomaterial is biocompatible, with osteoconductivity and osseointegration properties. Histological analysis and diffractograms showed the presence of hydroxyapatite in samples in all periods, although the presence of organic material of low crystallinity was variable. There was no statistical difference in the forces required for removal of the biocompatibility, osteoconductivity and osseointegration, it was not able to promote a better intramedullary pin anchorage.

Structure of Biocompatible Coatings Produced from Hydroxyapatite Nanoparticles by Detonation Spraying

Science.gov (United States)

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.

Preparation of silicon-substituted hydroxyapatite coatings on Ti–30Nb–xTa alloys using cyclic electrochemical deposition method

International Nuclear Information System (INIS)

Kim, Eun-Sil; Jeong, Yong-Hoon; Choe, Han-Cheol; Brantley, William A.

2014-01-01

Silicon-substituted hydroxyapatite coatings on Ti–30Nb–xTa alloys, prepared using a cyclic electrochemical deposition method, have been investigated using a variety of surface analytical experimental methods. The silicon-substituted hydroxyapatite (Si-HA) coatings were prepared by electrolytic deposition in electrolytes containing Ca 2+ , PO 4 3− and SiO 3 2− ions. The deposited layers were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDS), and a wettability test. Phase transformation from (α″ + β) to largely β occurred with increasing Ta content in the Ti –30Nb–xTa alloys, yielding larger grain size. The morphology of the Si-HA coatings was changed by increasing the number of deposition cycles, with the initial plate-like structures changing to mixed rod-like and plate-like shapes, and finally to a rod-like structure. From the ATR-FTIR spectra, Si existed in the form of SiO 4 4− groups in Si-HA coating layer. The lowest aqueous contact angles and best wettability were found for the Si-HA coatings prepared with 30 deposition cycles. - Highlights: • Electrochemically deposited Si-HA coatings on Ti –30Nb–xTa alloys were investigated. • The Si-HA coatings were initially precipitated along the martensitic structure. • The morphology of the Si-HA coating changed with the deposition cycles. • Si existed in the form of SiO 4 4− groups in the Si-HA coating

Bio resorbability of the modified hydroxyapatite in Tris-HCL buffer

International Nuclear Information System (INIS)

Golovanova, O A; Izmailov, R R; Ghyngazov, S A

2016-01-01

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. (paper)

Preparation, characterization and biological test of 3D-scaffolds based on chitosan, fibroin and hydroxyapatite for bone tissue engineering

International Nuclear Information System (INIS)

Lima, Paulo Autran Leite; Resende, Cristiane Xavier; Dulce de Almeida Soares, Glória; Anselme, Karine; Almeida, Luís Eduardo

2013-01-01

This work describes the preparation and characterization of porous 3D-scaffolds based on chitosan (CHI), chitosan/silk fibroin (CHI/SF) and chitosan/silk fibroin/hydroxyapatite (CHI/SF/HA) by freeze drying. The biomaterials were characterized by X-ray diffraction, attenuated total reflection Fourier transform infrared spectroscopy, thermogravimetric analysis, differential scanning calorimetry, scanning electron microscopy and energy dispersive spectroscopy. In addition, studies of porosity, pore size, contact angle and biological response of SaOs-2osteoblastic cells were performed. The CHI scaffolds have a porosity of 94.2 ± 0.9%, which is statistically higher than the one presented by CHI/SF/HA scaffolds, 89.7 ± 2.6%. Although all scaffolds were able to promote adhesion, growth and maintenance of osteogenic differentiation of SaOs-2 cells, the new 3D-scaffold based on CHI/SF/HA showed a significantly higher cell growth at 7 days and 21 days and the level of alkaline phosphatase at 14 and 21 days was statistically superior compared to other tested materials. - Highlights: • Preparation of 3D-scaffolds based on CHI, with or without addition of SF and HA. • Scaffolds exhibited interconnected porous structure (pore size superior to 50 μm). • The tripolyphosphate did not induce any significant cytotoxic response. • The CHI/SF/HA composite showed a higher cell growth and ALP activity

Preparation of bioactive porous HA/PCL composite scaffolds

Energy Technology Data Exchange (ETDEWEB)

Zhao, J.; Guo, L.Y.; Yang, X.B. [Key Laboratory of Advanced Technologies of Materials (Ministry of Education), School of Materials Science and Engineering, Southwest Jiaotong University, Chengdu 610031 (China); Weng, J. [Key Laboratory of Advanced Technologies of Materials (Ministry of Education), School of Materials Science and Engineering, Southwest Jiaotong University, Chengdu 610031 (China)], E-mail: jweng@swjtu.cn

2008-12-30

Porous hydroxyapatite (HA) bioceramic scaffold has been widely attracted the attention to act as a three-dimensional (3D) template for cell adhesion, proliferation, differentiation and thus promoting bone and cartilage regeneration because of its osteoinduction. However, the porous bioceramic scaffold is fragile so that it is not suitable to be applied in clinic for bone repair or replacement. Therefore, it is significant to improve the mechanical property of porous HA bioceramics while the interconnected structure is maintained for tissue ingrowth in vivo. In the present research, a porous composite scaffold composed of HA scaffold and polycaprolactone (PCL) lining was fabricated by the method of polymer impregnating to produce HA scaffold coated with PCL lining. Subsequently, the composite scaffolds were deposited with biomimetic coating for improving the bioactivity. The HA/PCL composite scaffolds with improved mechanical property and bioactivity is expected to be a promising bone substitute in tissue engineering applications.

Preparation of bioactive porous HA/PCL composite scaffolds

International Nuclear Information System (INIS)

Zhao, J.; Guo, L.Y.; Yang, X.B.; Weng, J.

2008-01-01

Porous hydroxyapatite (HA) bioceramic scaffold has been widely attracted the attention to act as a three-dimensional (3D) template for cell adhesion, proliferation, differentiation and thus promoting bone and cartilage regeneration because of its osteoinduction. However, the porous bioceramic scaffold is fragile so that it is not suitable to be applied in clinic for bone repair or replacement. Therefore, it is significant to improve the mechanical property of porous HA bioceramics while the interconnected structure is maintained for tissue ingrowth in vivo. In the present research, a porous composite scaffold composed of HA scaffold and polycaprolactone (PCL) lining was fabricated by the method of polymer impregnating to produce HA scaffold coated with PCL lining. Subsequently, the composite scaffolds were deposited with biomimetic coating for improving the bioactivity. The HA/PCL composite scaffolds with improved mechanical property and bioactivity is expected to be a promising bone substitute in tissue engineering applications

Composite biocompatible hydroxyapatite-silk fibroin coatings for medical implants obtained by Matrix Assisted Pulsed Laser Evaporation

International Nuclear Information System (INIS)

Miroiu, F.M.; Socol, G.; Visan, A.; Stefan, N.; Craciun, D.; Craciun, V.; Dorcioman, G.; Mihailescu, I.N.; Sima, L.E.; Petrescu, S.M.; Andronie, A.; Stamatin, I.; Moga, S.; Ducu, C.

2010-01-01

The aim of this study was to obtain biomimetic inorganic-organic thin films as coatings for metallic medical implants. These contain hydroxyapatite, the inorganic component of the bony tissues, and a natural biopolymer - silk fibroin - added in view to induce the surface functionalization. Hydroxyapatite (HA), silk fibroin (FIB) and composite HA-FIB films were obtained by Matrix Assisted Pulsed Laser Evaporation (MAPLE) in order to compare their physical and biological performances as coatings on metallic prostheses. We used an excimer laser source (KrF*, λ = 248 nm, τ = 25 ns) operated at 10 Hz repetition rate. Coatings were deposited on quartz, Si and Ti substrates and then subjected to physical (FTIR, XRD, AFM, SEM) analyses, correlated with the results of the cytocompatibility in vitro tests. The hybrid films were synthesized from frozen targets of aqueous suspensions with 3:2 or 3:4 weight ratio of HA:FIB. An appropriate stoichiometric and functional transfer was obtained for 0.4-0.5 J/cm 2 laser fluence. FTIR spectra of FIB and HA-FIB films exhibited distinctive absorption maxima, in specific positions of FIB random coil form: 1540 cm -1 amide II, 1654 cm -1 amide I, 1243 cm -1 amide III, while the peak from 1027 cm -1 appeared only for HA and composite films. Osteosarcoma SaOs2 cells cultured 72 h on FIB and HA-FIB films showed increased viability, good spreading and normal cell morphology. The well-elongated, flattened cells are a sign of an appropriate interaction with the MAPLE FIB and composite HA-FIB coatings.

Composite biocompatible hydroxyapatite-silk fibroin coatings for medical implants obtained by Matrix Assisted Pulsed Laser Evaporation

Energy Technology Data Exchange (ETDEWEB)

Miroiu, F.M., E-mail: marimona.miroiu@inflpr.ro [National Institute for Lasers, Plasma, and Radiation Physics, 409 Atomistilor Street, RO-77125, MG-36, Magurele-Ilfov (Romania); Socol, G.; Visan, A.; Stefan, N.; Craciun, D.; Craciun, V.; Dorcioman, G.; Mihailescu, I.N. [National Institute for Lasers, Plasma, and Radiation Physics, 409 Atomistilor Street, RO-77125, MG-36, Magurele-Ilfov (Romania); Sima, L.E.; Petrescu, S.M. [Institute of Biochemistry, Romanian Academy, 296 Splaiul Independentei, 060031 Bucharest (Romania); Andronie, A.; Stamatin, I. [3Nano-SAE Alternative Energy Sources-University of Bucharest, Faculty of Physics, 409 Atomistilor Street, RO-77125, Magurele-Ilfov (Romania); Moga, S.; Ducu, C. [University of Pitesti, Targul din Vale Str, no. 1, 110040 Pitesti (Romania)

2010-05-25

The aim of this study was to obtain biomimetic inorganic-organic thin films as coatings for metallic medical implants. These contain hydroxyapatite, the inorganic component of the bony tissues, and a natural biopolymer - silk fibroin - added in view to induce the surface functionalization. Hydroxyapatite (HA), silk fibroin (FIB) and composite HA-FIB films were obtained by Matrix Assisted Pulsed Laser Evaporation (MAPLE) in order to compare their physical and biological performances as coatings on metallic prostheses. We used an excimer laser source (KrF*, {lambda} = 248 nm, {tau} = 25 ns) operated at 10 Hz repetition rate. Coatings were deposited on quartz, Si and Ti substrates and then subjected to physical (FTIR, XRD, AFM, SEM) analyses, correlated with the results of the cytocompatibility in vitro tests. The hybrid films were synthesized from frozen targets of aqueous suspensions with 3:2 or 3:4 weight ratio of HA:FIB. An appropriate stoichiometric and functional transfer was obtained for 0.4-0.5 J/cm{sup 2} laser fluence. FTIR spectra of FIB and HA-FIB films exhibited distinctive absorption maxima, in specific positions of FIB random coil form: 1540 cm{sup -1} amide II, 1654 cm{sup -1} amide I, 1243 cm{sup -1} amide III, while the peak from 1027 cm{sup -1} appeared only for HA and composite films. Osteosarcoma SaOs2 cells cultured 72 h on FIB and HA-FIB films showed increased viability, good spreading and normal cell morphology. The well-elongated, flattened cells are a sign of an appropriate interaction with the MAPLE FIB and composite HA-FIB coatings.

Preparation of magnetic and bioactive calcium zinc iron silicon oxide composite for hyperthermia treatment of bone cancer and repair of bone defects.

Science.gov (United States)

Jiang, Yumin; Ou, Jun; Zhang, Zhanhe; Qin, Qing-Hua

2011-03-01

In this paper, a calcium zinc iron silicon oxide composite (CZIS) was prepared using the sol-gel method. X-ray diffraction (XRD) was then employed to test the CZIS composite. The results from the test showed that the CZIS had three prominent crystalline phases: Ca(2)Fe(1.7)Zn(0.15)Si(0.15)O(5), Ca(2)SiO(4), and ZnFe(2)O(4). Calorimetric measurements were then performed using a magnetic induction furnace. Scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) analysis were conducted to confirm the growth of a precipitated hydroxyapatite phase after immersion in simulated body fluid (SBF). Cell culture experiments were also carried out, showing that the CZIS composite more visibly promoted osteoblast proliferation than ZnFe(2)O(4) glass ceramic and HA, and osteoblasts adhered and spread well on the surfaces of composite samples.

Adsorptive features of poli(acrylic acid-co-hydroxyapatite) composite for UO22+

International Nuclear Information System (INIS)

Liu Tonghuan; Xu Zhen; Tan Yinping; Zhong Qiangqiang; Wu Wangsuo

2016-01-01

The copolymer of poli(acrylic acid-co-hydroxyapatite) (PAA-HAP) was prepared and characterized by means of FT-IR and SEM analysis. The adsorptive features of PAA-HAP for UO 2 2+ was studied as a function of pH, adsorbent dosage, initial metal ion concentration and temperature. The adsorption isotherm data fitted well to the Langmuir isotherm model. The adsorbed UO 2 2+ can be desorbed effectively by 0.1 M HNO 3 . The maximum adsorption capacities for UO 2 2+ of the dry PAA-HAP was 1.86 x 10 -4 mol/g. The high adsorption capacity and kinetics results indicate that PAA-HAP can be used as an alternative adsorbent to remove UO 2 2+ from aqueous solution. (author)

Facile synthesis of both needle-like and spherical hydroxyapatite nanoparticles: effect of synthetic temperature and calcination on morphology, crystallite size and crystallinity.

Science.gov (United States)

Wijesinghe, W P S L; Mantilaka, M M M G P G; Premalal, E V A; Herath, H M T U; Mahalingam, S; Edirisinghe, M; Rajapakse, R P V J; Rajapakse, R M G

2014-09-01

Synthetic hydroxyapatite (HA) nanoparticles, that mimic natural HA, are widely used as biocompatible coatings on prostheses to repair and substitute human bones. In this study, HA nanoparticles are prepared by precipitating them from a precursor solution containing calcium sucrate and ammonium dihydrogen orthophosphate, at a Ca/P mole ratio of 1.67:1, at temperatures, ranging from 10°C to 95°C. A set of products, prepared at different temperatures, is analyzed for their crystallinity, crystallite size, morphology, thermal stability and composition, by X-ray diffraction (XRD), scanning electron microscopy (SEM), thermogravimetric analysis (TGA) and Fourier transform infrared (FT-IR) spectroscopic techniques, while the other set is analyzed after calcining the respective products, soon after their synthesis, for 3h, at 700°C. The as-prepared products, after 2h of drying, without any calcination, are not crystalline, but they grow very slowly into needle-like morphologies, as they are ripened with time. The percentage crystallinity of the final products increases from 15% to 52%, with increasing the preparative temperature. The calcined samples always produce spherical nanoparticles of essentially the same diameter, between 90 nm and 100 nm, which does not change due to aging and preparative temperatures. Therefore, the same method can be utilized to synthesize both spherical and needle-like nanoparticles of hydroxyapatite, with well-defined sizes and shapes. The ability to use readily available cheap raw materials, for the synthesis of such well-defined crystallites of hydroxyapatite, is an added advantage of this method, which may be explored further for the scaling up of the procedures to suit to industrial scale synthesis of such hydroxyapatite nanoparticles. Copyright © 2014 Elsevier B.V. All rights reserved.

Response of Human Osteoblast to n-HA/PEEK—Quantitative Proteomic Study of Bio-effects of Nano-Hydroxyapatite Composite

Science.gov (United States)

Zhao, Minzhi; Li, Haiyun; Liu, Xiaochen; Wei, Jie; Ji, Jianguo; Yang, Shu; Hu, Zhiyuan; Wei, Shicheng

2016-03-01

Nano-sized hydroxyapatite (n-HA) is considered as a bio-active material, which is often mixed into bone implant material, polyetheretherketone (PEEK). To reveal the global protein expression modulations of osteoblast in response to direct contact with the PEEK composite containing high level (40%) nano-sized hydroxyapatite (n-HA/PEEK) and explain its comprehensive bio-effects, quantitative proteomic analysis was conducted on human osteoblast-like cells MG-63 cultured on n-HA/PEEK in comparison with pure PEEK. Results from quantitative proteomic analysis showed that the most enriched categories in the up-regulated proteins were related to calcium ion processes and associated functions while the most enriched categories in the down-regulated proteins were related to RNA process. This enhanced our understanding to the molecular mechanism of the promotion of the cell adhesion and differentiation with the inhibition of the cell proliferation on n-HA/PEEK composite. It also exhibited that although the calcium ion level of incubate environment hadn’t increased, merely the calcium fixed on the surface of material had influence to intracellular calcium related processes, which was also reflect by the higher intracellular Ca2+ concentration of n-HA/PEEK. This study could lead to more comprehensive cognition to the versatile biocompatibility of composite materials. It further proves that proteomics is useful in new bio-effect discovery.

Response of Human Osteoblast to n-HA/PEEK—Quantitative Proteomic Study of Bio-effects of Nano-Hydroxyapatite Composite

Science.gov (United States)

Zhao, Minzhi; Li, Haiyun; Liu, Xiaochen; Wei, Jie; Ji, Jianguo; Yang, Shu; Hu, Zhiyuan; Wei, Shicheng

2016-01-01

Nano-sized hydroxyapatite (n-HA) is considered as a bio-active material, which is often mixed into bone implant material, polyetheretherketone (PEEK). To reveal the global protein expression modulations of osteoblast in response to direct contact with the PEEK composite containing high level (40%) nano-sized hydroxyapatite (n-HA/PEEK) and explain its comprehensive bio-effects, quantitative proteomic analysis was conducted on human osteoblast-like cells MG-63 cultured on n-HA/PEEK in comparison with pure PEEK. Results from quantitative proteomic analysis showed that the most enriched categories in the up-regulated proteins were related to calcium ion processes and associated functions while the most enriched categories in the down-regulated proteins were related to RNA process. This enhanced our understanding to the molecular mechanism of the promotion of the cell adhesion and differentiation with the inhibition of the cell proliferation on n-HA/PEEK composite. It also exhibited that although the calcium ion level of incubate environment hadn’t increased, merely the calcium fixed on the surface of material had influence to intracellular calcium related processes, which was also reflect by the higher intracellular Ca2+ concentration of n-HA/PEEK. This study could lead to more comprehensive cognition to the versatile biocompatibility of composite materials. It further proves that proteomics is useful in new bio-effect discovery. PMID:26956660

Synthesis spherical porous hydroxyapatite/graphene oxide composites by ultrasonic-assisted method for biomedical applications.

Science.gov (United States)

Duan, Peizhen; Shen, Juan; Zou, Guohong; Xia, Xu; Jin, Bo; Yu, Jiaxin

2018-04-10

Spherical porous hydroxyapatite (SHA)/graphene oxide (GO) composites with different GO (w/w) content of 16%, 40%, and 71% have been fabricated through a facile and controllable ultrasonic-assisted method at room temperature. The products were characterized by x-ray diffraction, field emission scanning electron microscopy, thermogravimetric analysis, mechanical testing and biomimetic mineralization. Results showed SHA were covered by GO, and SHA/GO composites had an irregular surface with different degrees of wrinkles. The elastic modulus and hardness of SHA/GO-3 composites were up to 12.45 ± 0.33 GPa and 686.67 ± 26.95 MPa, which indicated that the contents of GO had an effect on SHA/GO composites. And the mechanical properties of SHA/GO-2 composites were similar to SHA particles. The biomimetic mineralization in SBF solution showed the bone-like apatite layer on composites surface, which demonstrated that the SHA/GO materials had osseointegration property. Moreover, in vitro cytocompatibility of SHA/GO-2 composites and pure GO were evaluated by cell adhesion and proliferation tests using MC3T3-E1 cells, which demonstrated that the SHA/GO composites can act as a good template for the cells growth and adhesion. These results suggested that the SHA/GO composites will be a promising material for biomedical application.

Hydroxyapatite-armored poly(ε-caprolactone) microspheres and hydroxyapatite microcapsules fabricated via a Pickering emulsion route.

Science.gov (United States)

Fujii, Syuji; Okada, Masahiro; Nishimura, Taiki; Maeda, Hayata; Sugimoto, Tatsuya; Hamasaki, Hiroyuki; Furuzono, Tsutomu; Nakamura, Yoshinobu

2012-05-15

Hydroxyapatite (HAp) nanoparticle-armored poly(ε-caprolactone) (PCL) microspheres were fabricated via a "Pickering-type" emulsion solvent evaporation method in the absence of any molecular surfactants. It was clarified that the interaction between carbonyl/carboxylic acid groups of PCL and the HAp nanoparticles at an oil-water interface played a crucial role in the preparation of the stable Pickering-type emulsions and the HAp nanoparticle-armored microspheres. The HAp nanoparticle-armored PCL microspheres were characterized in terms of size, size distribution, morphology, and chemical compositions using scanning electron microscopy, laser diffraction, energy dispersive X-ray microanalysis, and thermogravimetric analysis. The presence of HAp nanoparticles at the surface of the microspheres was confirmed by scanning electron microscopy and energy dispersive X-ray microanalysis. Pyrolysis of the PCL cores led to the formation of the corresponding HAp hollow microcapsules. Copyright © 2012 Elsevier Inc. All rights reserved.

Scaffolds of polycaprolactone with hydroxyapatite fibers

International Nuclear Information System (INIS)

Cardoso, Guinea B.C.; Zavaglia, Cecilia A.C.; Arruda, Antonio Celso F.

2009-01-01

Scaffolds of poly (ε-caprolactone) has been studied in many researches in tissue engineering. The used of hydroxyapatite fibers, allowed increase its resistance mechanical, beside the character bioactive and osteoconductive. Improving, its role in tissue engineering. The aim in this study was developed polycaprolactone matrix with dispersed hydroxyapatite fibers. The characterizations were by scanning electron microscopy (SEM), X- Ray Diffractometer (XRD), X-Ray Fluorescence (XRF) and Energy dispersive X-Ray Detector (EDX). Was able reviewed its composition, morphology and possible contaminations. The results were scaffolds with porosity and distribution of the fibers in all its area. (author)

An improved biofunction of titanium for keratoprosthesis by hydroxyapatite-coating.

Science.gov (United States)

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.

Additive manufactured Ti6Al4V scaffolds with the RF- magnetron sputter deposited hydroxyapatite coating

International Nuclear Information System (INIS)

Chudinova, E; Surmeneva, M; Surmenev, R; Koptioug, A; Scoglund, P

2016-01-01

Present paper reports on the results of surface modification of the additively manufactured porous Ti6Al4V scaffolds. Radio frequency (RF) magnetron sputtering was used to modify the surface of the alloy via deposition of the biocompatible hydroxyapatite (HA) coating. The surface morphology, chemical and phase composition of the HA-coated alloy were studied. It was revealed that RF magnetron sputtering allows preparing a homogeneous HA coating onto the entire surface of scaffolds. (paper)

Comparison of hydroxyapatite and dental enamel for testing shear bond strengths.

Science.gov (United States)

Imthiaz, Nishat; Georgiou, George; Moles, David R; Jones, Steven P

2008-05-01

To investigate the feasibility of using artificial hydroxyapatite as a future biomimetic laboratory substitute for human enamel in orthodontic bond strength testing by comparing the shear bond strengths and nature of failure of brackets bonded to samples of hydroxyapatite and enamel. One hundred and fifty hydroxyapatite discs were prepared by compression at 20 tons and fired in a furnace at 1300 degrees C. One hundred and five enamel samples were prepared from the buccal and palatal/lingual surfaces of healthy premolars extracted for orthodontic purposes. Orthodontic brackets were bonded to each sample and these were subjected to shear bond strength testing using a custom-made jig mounted in an Instron Universal Testing Machine. The force value at bond failure was obtained, together with the nature of failure which was assessed using the Adhesive Remnant Index. The mean shear bond strength for the enamel samples was 16.62 MPa (95 per cent CI: 15.26, 17.98) and for the hydroxyapatite samples 20.83 MPa (95 per cent CI: 19.68, 21.98). The difference between the two samples was statistically significant (p enamel samples scored 2 or 3, while 49 per cent of the hydroxyapatite samples scored 0 or 1. Hydroxyapatite was an effective biomimetic substrate for bond strength testing with a mean shear bond strength value (20.83 MPa) at the upper end of the normal range attributed to enamel (15-20 MPa). Although the difference between the shear bond strengths for hydroxyapatite and enamel was statistically significant, hydroxyapatite could be used as an alternative to enamel for comparative laboratory studies until a closer alternative is found. This would eliminate the need for extracted teeth to be collected. However, it should be used with caution for quantitative studies where true bond strengths are to be investigated.

Polyurethane/fluor-hydroxyapatite nanocomposite scaffolds for bone tissue engineering. Part I: morphological, physical, and mechanical characterization

Science.gov (United States)

Asefnejad, Azadeh; Behnamghader, Aliasghar; Khorasani, Mohammad Taghi; Farsadzadeh, Babak

2011-01-01

In this study, new nano-fluor-hydroxyapatite (nFHA)/polyurethane composite scaffolds were fabricated for potential use in bone tissue engineering. Polyester urethane samples were synthesized from polycaprolactone, hexamethylene diisocyanate, and 1,4-butanediol as chain extender. Nano fluor-hydroxyapatite (nFHA) was successfully synthesized by sol-gel method. The solid–liquid phase separation and solvent sublimation methods were used for preparation of the porous composites. Mechanical properties, chemical structure, and morphological characteristics of the samples were investigated by compressive test, Fourier transform infrared, and scanning electron microscopy (SEM) techniques, respectively. The effect of nFHA powder content on porosity and pore morphology was investigated. SEM images demonstrated that the scaffolds were constituted of interconnected and homogeneously distributed pores. The pore size of the scaffolds was in the range 50–250 μm. The result obtained in this research revealed that the porosity and pore average size decreased and compressive modulus increased with nFHA percentage. Considering morphological, physical, and mechanical properties, the scaffold with a higher ratio of nFHA has suitable potential use in tissue regeneration. PMID:21289986

Improvement of the stability of hydroxyapatite through glass ceramic reinforcement.

Science.gov (United States)

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.

Designing, preparing and evaluation of novel HA/Ti composite coating for endodontic dental implant

Directory of Open Access Journals (Sweden)

Fathi MH.

2002-08-01

Full Text Available Nowadays, application of implants as a new method for replacing extracted teeth have been improved. So, many researches have been performed for improving the characteristics of implants. The aim of this study was to design and produce a desired coating in order to obtaining two goals including; improvement of the corrosion behavior of metallic endodontic implant and the bone osseointegration simultaneously. Stainless steel 316L (SS, cobalt-chromium alloy (Vit and commercial pure titanium (cpTi were chosen as metallic substrates and hydroxyapatite coating (HAC were performed by plasma-spraying (PS process on three different substrates. A novel double layer Hydroxyapatite/Titanium (HA/Ti composite coating composed of a HA top layer and a Ti under layer was prepared using PS and physical vapor deposition (PVD process respectively on SS. Structural characterization techniques including XRD, SEM and EDX were utilized to investigate the microstructure, morpholgy and crystallinity of the coatings. Electrochemical potentiodynamic tests were performed in physiological solutions in order to determine and compare the corrosion behavior of the coated and uncoated specimens behavior as an indication of biocmpatibility. Results indicated that the cpTi possesses the highest and SS the lowest corrosion resistance (highest corrosion current density between uncoated substrates. This trend was independent to the type of physiological environment. The HA coating decreased the corrosion current density of HA coated metallic implants but did not change that trend. HAC acted as a mechanical barrier on the metallic substrate but could not prevent the interaction between metallic substrate and environment completely. The HA/Ti composite coating improved the corrosion behavior of SS. The corrosion current density of HA/Ti coated SS decreased and was exactly similar to single HA coated cpTi in physiological solutions. The results indicated that HA/Ti composite coated SS

Fabrication, Properties and Applications of Dense Hydroxyapatite: A Review

Science.gov (United States)

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

Fabrication, Properties and Applications of Dense Hydroxyapatite: A Review

Directory of Open Access Journals (Sweden)

Mythili Prakasam

2015-12-01

Full Text Available 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.

Microwave assisted synthesis of hydroxyapatite nano strips

Energy Technology Data Exchange (ETDEWEB)

Ruban Kumar, A.; Kalainathan, S.; Saral, A.M. [School of Advanced Sciences, VIT University, Vellore 632014, Tamil Nadu (India)

2010-07-15

Synthesis of hydroxyapatite (HAP) nano strips was carried out by chemical precipitation method followed by microwave irradiation. The microwave assisted reactions proceed at fast rates. It is found that the presence of the complex reagent EDTA plays an important role in the morphological changes of nanostructure hydroxyapatite. EDTA acts as a hexadentate unit by wrapping itself around the Ca{sup 2+} metal ion with, four oxygen and two nitrogen atoms and forms several five member chelate rings. The relative specific surface energies associated with the facets of the crystal determines the shape of the crystal. Scanning electron microscopy revealed the presence of hydroxyapatite nano strips with the range 50-100 nm in EDTA influenced HAP powders. Fourier transform-infrared spectroscopy (FT-IR) result combined with the X-ray diffraction (XRD) indicates the presence of amorphous hydroxyapatite (HAP) in the as-prepared material. X-ray patterns collected on the powder after heat-treatment at 1100 C for 2 h in air exhibits single phase of HAP. (copyright 2010 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

Studying the Properties of Polyvinyl Alcohol/Cellulose Nanofiber/Hydroxyapatite Hybrid Nanocomposite

Directory of Open Access Journals (Sweden)

Mostafa Yahyavi

2015-06-01

Full Text Available Nanocomposite materials have recently attracted much attention because of their desirable and unique physical and mechanical properties. Today, many studies have focused on the preparation of high performance new nanocomposites made of biobased and biodegradable materials as both the matrix and reinforcement phases. Because of biocompatibility, biofunctionality, and biological safety in the body, hydroxyapatite-polyvinyl alcohol composites are vastly used in medical applications, specially in the bone tissue regeneration. The properties of a new generation of nanocomposites consisting of hydroxyapatite nanoparticles and cellulose nanofibers, dispersed in polyvinyl alcohol matrix, were investigated. The percentage by weight of each component in the final formulation and the time of ultrasonication were studied as factors affecting the physical and mechanical properties. Tensile strength, elastic modulus and resistance to water dissolution were evaluated. The results showed that by increasing the percentage by weight of PVA and cellulose nanofibers and ultrasonication time, the tensile strength and elastic modulus increased and the resistance to water dissolution and weight loss decreased. On the other hand, with increasing the amount of hydroxyapatite nanoparticles in the final formulation, the elastic modulus and resistance to water solubility increased, while the tensile strength decreased significantly. Scanning electron microscopy (SEM micrographs were used to find exact correlations between the observed physical and mechanical properties and the structural morphology.

Dispersed hydroxyapatite and modified bioglass 45S5 composites: sintering behavior of glass matrix ranging from 20 to 30 wt% in calcium oxide investigation

Energy Technology Data Exchange (ETDEWEB)

Silva, A.C.; Parra-Silva, J.; Santos, S.C.; Mello-Castanho, S.R.H, E-mail: dasilva.ac@uol.com.br [Instituto de Pesquisas Enegeticas e Nucleares (IPEN/CNEN-SP), DP (Brazil); Braga, F.J.C. [Consulmat Materiais de Referencia, Solucoes e Servicos, Sao Carlos, SP (Brazil); Setz, L.F.G. [Universidade Federal do ABC (UFABC), Santo Andre, SP (Brazil)

2014-07-01

Biomaterial technology plays an important role in cell-based tissue proliferation environment creation. The hydroxyapatite (HA) bioceramics are reference materials to employment as a bone substitute, however, their slow rate of degradation and its low rate of bioactivity (Ib) are presented as limiting factors for application as bone graft. In contrast, the bioglass (BG) is a resorbable and osteoinductive material and can act as fluxing in HA/BG composites. The present work objective the development of HA/BG (40/70wt%) composites, Three compositions of the 45S5 bioglass derived ranging from 20-30wt% in CaO were used in order to study the sintering behavior of these materials with hydroxyapatite 30wt% dispersed. The composites were uniaxially pressed in the form of cylinders and sinterized at (1100°C/1h). The characterization was made employing scanning electron microscopy, Infra-Red Spectrometry, X-ray diffraction and hydrolytic resistance test. The results indicate the potential use of the materials developed for applications like bone graft.(author)

Dispersed hydroxyapatite and modified bioglass 45S5 composites: sintering behavior of glass matrix ranging from 20 to 30 wt% in calcium oxide investigation

International Nuclear Information System (INIS)

Silva, A.C.; Parra-Silva, J.; Santos, S.C.; Mello-Castanho, S.R.H; Braga, F.J.C.; Setz, L.F.G.

2014-01-01

Biomaterial technology plays an important role in cell-based tissue proliferation environment creation. The hydroxyapatite (HA) bioceramics are reference materials to employment as a bone substitute, however, their slow rate of degradation and its low rate of bioactivity (Ib) are presented as limiting factors for application as bone graft. In contrast, the bioglass (BG) is a resorbable and osteoinductive material and can act as fluxing in HA/BG composites. The present work objective the development of HA/BG (40/70wt%) composites, Three compositions of the 45S5 bioglass derived ranging from 20-30wt% in CaO were used in order to study the sintering behavior of these materials with hydroxyapatite 30wt% dispersed. The composites were uniaxially pressed in the form of cylinders and sinterized at (1100°C/1h). The characterization was made employing scanning electron microscopy, Infra-Red Spectrometry, X-ray diffraction and hydrolytic resistance test. The results indicate the potential use of the materials developed for applications like bone graft.(author)

Electrospinning of calcium carbonate fibers and their conversion to nanocrystalline hydroxyapatite

International Nuclear Information System (INIS)

Holopainen, Jani; Santala, Eero; Heikkilä, Mikko; Ritala, Mikko

2014-01-01

Calcium carbonate (CaCO 3 ) fibers were prepared by electrospinning followed by annealing. Solutions consisting of calcium nitrate tetrahydrate (Ca(NO 3 ) 2 ·4H 2 O) and polyvinylpyrrolidone (PVP) dissolved in ethanol or 2-methoxyethanol were used for the fiber preparation. By varying the precursor concentrations in the electrospinning solutions CaCO 3 fibers with average diameters from 140 to 290 nm were obtained. After calcination the fibers were identified as calcite by X-ray diffraction (XRD). The calcination process was studied in detail with high temperature X-ray diffraction (HTXRD) and thermogravimetric analysis (TGA). The initially weak fiber-to-substrate adhesion was improved by adding a strengthening CaCO 3 layer by spin or dip coating Ca(NO 3 ) 2 /PVP precursor solution on the CaCO 3 fibers followed by annealing of the gel formed inside the fiber layer. The CaCO 3 fibers were converted to nanocrystalline hydroxyapatite (HA) fibers by treatment in a dilute phosphate solution. The resulting hydroxyapatite had a plate-like crystal structure with resemblance to bone mineral. The calcium carbonate and hydroxyapatite fibers are interesting materials for bone scaffolds and bioactive coatings. - Highlights: • Calcium carbonate fibers were prepared by electrospinning. • The electrospun fibers crystallized to calcite upon calcination at 500 °C. • Spin and dip coating methods were used to improve the adhesion of the CaCO 3 fibers. • The CaCO 3 fibers were converted to hydroxyapatite by treatment in phosphate solution. • The hydroxyapatite fibers consisted of plate-like nanocrystals

Sorption of zinc on synthetic hydroxyapatite from aqueous solution

International Nuclear Information System (INIS)

Pivarciova, L.; Rosskopfova, O.; Galambos, M.; Rajec, P.

2014-01-01

The sorption of Zn 2+ on synthetic hydroxyapatite was investigated using a batch method and radiotracer technique. This work was aimed to study influence of the contact time, effect of pH and different concentration of Zn 2+ ions in the solution. The percentage of zinc adsorption on HA1 and HA2 was more than 96 % during 1 h for initial Zn 2+ concentration of 1·10 -4 .5·10 -4 and 1·10 -3 mol·dm -3 . The equilibrium time of 2 h was chosen for further experiments. The sorption of zinc on hydroxyapatite was pH independent ranging from 4.5 to 6.5 as a result of buffering properties of hydroxyapatite. The experimental data for adsorption of zinc have been interpreted in the term of Langmuir isotherm and the value of maximum adsorption capacity of zinc on a commercial hydroxyapatite and hydroxyapatite prepared by wet precipitation process was calculated to be 0.437 mmol·g -1 and 0.605 mmol·g -1 , respectively. (authors)

Influence of spark plasma sintering and baghdadite powder on mechanical properties of hydroxyapatite

NARCIS (Netherlands)

Khandan, A.; Karamian, E.; Mehdikhani-Nahrkhalaji, M.; Mirmohammadi, H.; Farzadi, A.; Ozada, N.; Heidarshenas, B.; Zamani, K.

2015-01-01

Since hydroxyapatite-based materials have similar composition and crystallinity as natural calcified tissues, can be used for bone/tissue engineering. In the present study a novel nanocomposite based on bioceramics such as Natural Hydroxyapatite (NHA) and Baghdadite (BAG), was sintered by spark

Surface microstructure and cell biocompatibility of silicon-substituted hydroxyapatite coating on titanium substrate prepared by a biomimetic process

International Nuclear Information System (INIS)

Zhang Erlin; Zou Chunming; Yu Guoning

2009-01-01

Silicon-substituted hydroxyapatite (Si-HA) coatings with 0.14 to 1.14 at.% Si on pure titanium were prepared by a biomimetic process. The microstructure characterization and the cell compatibility of the Si-HA coatings were studied in comparison with that of hydroxyapatite (HA) coating prepared in the same way. The prepared Si-HA coatings and HA coating were only partially crystallized or in nano-scaled crystals. The introduction of Si element in HA significantly reduced P and Ca content, but densified the coating. The atom ratio of Ca to (P + Si) in the Si-HA coatings was in a range of 1.61-1.73, increasing slightly with an increase in the Si content. FTIR results displayed that Si entered HA in a form of SiO 4 unit by substituting for PO 4 unit. The cell attachment test showed that the HA and Si-HA coatings exhibited better cell response than the uncoated titanium, but no difference was observed in the cell response between the HA coating and the Si-HA coatings. Both the HA coating and the Si-HA coatings demonstrated a significantly higher cell growth rate than the uncoated pure titanium (p < 0.05) in all incubation periods while the Si-HA coating exhibited a significantly higher cell growth rate than the HA coating (p < 0.05). Si-HA with 0.42 at.% Si presented the best cell biocompatibility in all of the incubation periods. It was suggested that the synthesis mode of HA and Si-HA coatings in a simulated body environment in the biomimetic process contribute significantly to good cell biocompatibility

Preparation of silicon-substituted hydroxyapatite coatings on Ti–30Nb–xTa alloys using cyclic electrochemical deposition method

Energy Technology Data Exchange (ETDEWEB)

Kim, Eun-Sil [Department of Dental Materials, Research Center of Nano-Interface Activation for Biomaterials, School of Dentistry, Chosun University (Korea, Republic of); Jeong, Yong-Hoon [Biomechanics and Tissue Engineering Laboratory, Division of Orthodontics, College of Dentistry, The Ohio State University, Columbus, OH (United States); Choe, Han-Cheol, E-mail: hcchoe@chosun.ac.kr [Department of Dental Materials, Research Center of Nano-Interface Activation for Biomaterials, School of Dentistry, Chosun University (Korea, Republic of); Brantley, William A. [Division of Restorative Science and Prosthodontics, College of Dentistry, The Ohio State University, Columbus, OH (United States)

2014-12-01

Silicon-substituted hydroxyapatite coatings on Ti–30Nb–xTa alloys, prepared using a cyclic electrochemical deposition method, have been investigated using a variety of surface analytical experimental methods. The silicon-substituted hydroxyapatite (Si-HA) coatings were prepared by electrolytic deposition in electrolytes containing Ca{sup 2+}, PO{sub 4}{sup 3−} and SiO{sub 3}{sup 2−} ions. The deposited layers were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDS), and a wettability test. Phase transformation from (α″ + β) to largely β occurred with increasing Ta content in the Ti –30Nb–xTa alloys, yielding larger grain size. The morphology of the Si-HA coatings was changed by increasing the number of deposition cycles, with the initial plate-like structures changing to mixed rod-like and plate-like shapes, and finally to a rod-like structure. From the ATR-FTIR spectra, Si existed in the form of SiO{sub 4}{sup 4−} groups in Si-HA coating layer. The lowest aqueous contact angles and best wettability were found for the Si-HA coatings prepared with 30 deposition cycles. - Highlights: • Electrochemically deposited Si-HA coatings on Ti –30Nb–xTa alloys were investigated. • The Si-HA coatings were initially precipitated along the martensitic structure. • The morphology of the Si-HA coating changed with the deposition cycles. • Si existed in the form of SiO{sub 4}{sup 4−} groups in the Si-HA coating.

Interaction of some essential amino acids with synthesized poorly crystalline hydroxyapatite

Directory of Open Access Journals (Sweden)

A. El Rhilassi

2016-09-01

Full Text Available This study focused on the release of two essential amino acids, l-lysine and dl-leucine, previously adsorbed onto poorly crystalline hydroxyapatite of Ca/P = 1.59, synthesis by precipitation methods. The composition of the calcium-deficient hydroxyapatite (CDHA is chemically and structurally similar to the bone mineral. Their surface reactivity is indeed linked to the existence of hydrated surface particles (HPO42- and Ca2+. The adsorption kinetics is very fast while the release kinetics is relatively slow. The adsorption rate reached approximately 70%, but the release rate did not exceed 12%. The chemical composition of solution has an influence on the release processes. The presence of phosphate ions favored the release of amino acids, while the calcium ions inhibited it. Also, the release process is slightly influenced by Ra (ml/mg ratio and incubation temperature of the medium. The charged –COO− and NH3+ of amino acids are the strongest groups that interact with the surface of hydroxyapatite, the adsorption is mainly due to the electrostatic interaction between the groups –COO− of amino acids and calcium Ca2+ ions of the hydroxyapatite. dl-Leucine (non-polar and l-Lysine (polar–basic interact with the hydroxyapatite surface in the zwitterionic and cationic forms, respectively. The study of interactions between amino acids and hydroxyapatite is carried out in vitro by using UV–vis and infrared spectroscopy IR techniques.

Preparation and characterization of multi-walled carbon nanotube/hydroxyapatite nanocomposite film dip coated on Ti-6Al-4V by sol-gel method for biomedical applications: an in vitro study.

Science.gov (United States)

Abrishamchian, Alireza; Hooshmand, Tabassom; Mohammadi, Mohammadreza; Najafi, Farhood

2013-05-01

In the present research, the introduction of multi-walled carbon nanotubes (MWCNTs) into the hydroxyapatite (HA) matrix and dip coating of nanocomposite on titanium alloy (Ti-6Al-4V) plate was conducted in order to improve the performance of the HA-coated implant via the sol-gel method. The structural characterization and electron microscopy results confirmed well crystallized HA-MWCNT coating and homogenous dispersion of carbon nanotubes in the ceramic matrix at temperatures as low as 500 °C. The evaluation of the mechanical properties of HA and HA/MWCNT composite coatings with different weight percentages of MWCNTs showed that the addition of low concentrations of MWCNTs (0.5 and 1 wt.%) had improved effect on the mechanical properties of nanocomposite coatings. Moreover, this in vitro study ascertained the biocompatibility of the prepared sol-gel-derived HA/MWCNT composite coatings. Copyright © 2013 Elsevier B.V. All rights reserved.

Characterization of gas tunnel type plasma sprayed hydroxyapatite-nanostructure titania composite coatings

Science.gov (United States)

Yugeswaran, S.; Kobayashi, A.; Ucisik, A. Hikmet; Subramanian, B.

2015-08-01

Hydroxyapatite (HA) can be coated onto metal implants as a ceramic biocompatible coating to bridge the growth between implants and human tissue. Meanwhile many efforts have been made to improve the mechanical properties of the HA coatings without affecting its bioactivity. In the present study, nanostructure titania (TiO2) was mixed with HA powder and HA-nanostructure TiO2 composite coatings were produced by gas tunnel type plasma spraying torch under optimized spraying conditions. For this purpose, composition of 10 wt% TiO2 + 90 wt% HA, 20 wt% TiO2 + 80 wt% HA and 30 wt% TiO2 + 70 wt% HA were selected as the feedstock materials. The phase, microstructure and mechanical properties of the coatings were characterized. The obtained results validated that the increase in weight percentage of nanostructure TiO2 in HA coating significantly increased the microhardness, adhesive strength and wear resistance of the coatings. Analysis of the in vitro bioactivity and cytocompatibility of the coatings were done using conventional simulated body fluid (c-SBF) solution and cultured green fluorescent protein (GFP) labeled marrow stromal cells (MSCs) respectively. The bioactivity results revealed that the composite coating has bio-active surface with good cytocompatibility.

Mechanical properties of natural chitosan/hydroxyapatite/magnetite nanocomposites for tissue engineering applications

Energy Technology Data Exchange (ETDEWEB)

Heidari, Fatemeh [Department of Materials Science and Engineering, School of Engineering, Yasouj University, Yasuj 75918-74934 (Iran, Islamic Republic of); Razavi, Mehdi [BCAST, Institute of Materials and Manufacturing, Brunel University London, Uxbridge, London UB8 3PH (United Kingdom); Brunel Institute for Bioengineering, Brunel University London, Uxbridge, London UB8 3PH (United Kingdom); Bahrololoom, Mohammad E. [Department of Materials Science and Engineering, School of Engineering, Shiraz University, Shiraz (Iran, Islamic Republic of); Bazargan-Lari, Reza [Department of Materials Science and Engineering, Marvdasht Branch, Islamic Azad University, Marvdasht (Iran, Islamic Republic of); Vashaee, Daryoosh [Electrical and Computer Engineering Department, North Carolina State University, Raleigh, NC 27606 (United States); Kotturi, Hari [Department of Biology, University of Central Oklahoma, Edmond, OK 73034 (United States); Tayebi, Lobat, E-mail: lobat.tayebi@marquette.edu [Department of Developmental Sciences, Marquette University School of Dentistry, Milwaukee, WI 53233 (United States); Department of Engineering Science, University of Oxford, Oxford OX1 3PJ (United Kingdom)

2016-08-01

Chitosan (CS), hydroxyapatite (HA), and magnetite (Fe{sub 3}O{sub 4}) have been broadly employed for bone treatment applications. Having a hybrid biomaterial composed of the aforementioned constituents not only accumulates the useful characteristics of each component, but also provides outstanding composite properties. In the present research, mechanical properties of pure CS, CS/HA, CS/HA/magnetite, and CS/magnetite were evaluated by the measurements of bending strength, elastic modulus, compressive strength and hardness values. Moreover, the morphology of the bending fracture surfaces were characterized using a scanning electron microscope (SEM) and an image analyzer. Studies were also conducted to examine the biological response of the human Mesenchymal Stem Cells (hMSCs) on different composites. We conclude that, although all of these composites possess in-vitro biocompatibility, adding hydroxyapatite and magnetite to the chitosan matrix can noticeably enhance the mechanical properties of the pure chitosan. - Highlights: • Chitosan (CS)/magnetite composite presented the maximum bending strength. • Adding hydroxyapatite and magnetite to the CS enhances its mechanical properties. • Magnetic does not have reverse effect on the cyto-compatibility of samples.

Particulate composite on the basis of HA and TCP microparticles and nanoparticles as a possible biomaterial for spine therapy

Czech Academy of Sciences Publication Activity Database

Rýglová, Šárka; Sucharda, Zbyněk; Černý, Martin; Suchý, Tomáš; Šupová, Monika; Žaloudková, Margit

2010-01-01

Roč. 54, č. 4 (2010), s. 386-397 ISSN 0862-5468 R&D Projects: GA MPO FT-TA3/131 Institutional research plan: CEZ:AV0Z30460519 Keywords : particulate composite * preparation * hydroxyapatite Subject RIV: JI - Composite Materials Impact factor: 0.297, year: 2010

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

International Nuclear Information System (INIS)

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

2009-01-01

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 3 ) 2 .4H 2 O and (b) titration of Ca(OH) 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 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 2 /g. Pure and Si-substituted hydroxyapatite nanopowders derived from Ca(NO 3 ) 2 .4H 2 O decomposed around 1000 deg. C. Si-substituted hydroxyapatite nanopowders obtained from Ca(OH) 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) 2

Electrophoretic deposition of graphene oxide reinforced chitosan-hydroxyapatite nanocomposite coatings on Ti substrate.

Science.gov (United States)

Shi, Y Y; Li, M; Liu, Q; Jia, Z J; Xu, X C; Cheng, Y; Zheng, Y F

2016-03-01

Electrophoretic deposition (EPD) is a facile and feasible technique to prepare functional nanocomposite coatings for application in orthopedic-related implants. In this work, a ternary graphene oxide-chitosan-hydroxyapatite (GO-CS-HA) composite coating on Ti substrate was successfully fabricated by EPD. Coating microstructure and morphologies were investigated by scanning electron microscopy, contact angle test, Raman spectroscopy, Fourier transform infrared spectroscopy and thermogravimetric analysis. It was found GO-CS surface were uniformly decorated by HA nanoparticles. The potentiodynamic polarization test in simulated body fluid indicated that the GO-CS-HA coatings could provide effective protection of Ti substrate from corrosion. This ternary composite coating also exhibited good biocompatibility during incubation with MG63 cells. In addition, the nanocomposite coatings could decrease the attachment of Staphylococcus aureus.

Bone plate composed of a ternary nano-hydroxyapatite/polyamide 66/glass fiber composite: biomechanical properties and biocompatibility.

Science.gov (United States)

Qiao, Bo; Li, Jidong; Zhu, Qingmao; Guo, Shuquan; Qi, Xiaotong; Li, Weichao; Wu, Jun; Liu, Yang; Jiang, Dianming

2014-01-01

An ideal bone plate for internal fixation of bone fractures should have good biomechanical properties and biocompatibility. In this study, we prepared a new nondegradable bone plate composed of a ternary nano-hydroxyapatite/polyamide 66/glass fiber (n-HA/PA66/GF) composite. A breakage area on the n-HA/PA66/GF plate surface was characterized by scanning electron microscopy. Its mechanical properties were investigated using bone-plate constructs and biocompatibility was evaluated in vitro using bone marrow-derived mesenchymal stem cells. The results confirmed that adhesion between the n-HA/PA66 matrix and the glass fibers was strong, with only a few fibers pulled out at the site of breakage. Fractures fixed by the n-HA/PA66/GF plate showed lower stiffness and had satisfactory strength compared with rigid fixation using a titanium plate. Moreover, the results with regard to mesenchymal stem cell morphology, MTT assay, Alizarin Red S staining, enzyme-linked immunosorbent assay, and reverse transcription polymerase chain reaction for alkaline phosphatase and osteocalcin showed that the n-HA/PA66/GF composite was suitable for attachment and proliferation of mesenchymal stem cells, and did not have a negative influence on matrix mineralization or osteogenic differentiation of mesenchymal stem cells. These observations indicate that the n-HA/PA66/GF plate has good biomechanical properties and biocompatibility, and may be considered a new option for internal fixation in orthopedic surgery.

The hydroxyapatite-binding regions of a rat salivary glycoprotein.

Science.gov (United States)

Embery, G; Green, D R

1989-09-01

The regions of a salivary sulphated glycoprotein which are involved in its attachment to hydroxyapatite (Biogel HTP) have been characterised. The sulphated glycoprotein, a 35S-labelled preparation from mixed palatal and buccal minor gland secretions of the rat was bound onto hydroxyapatite and the resultant glycoprotein-hydroxyapatite complex was sequentially digested with pronase E and alpha-L-fucosidase, a treatment which released 86.8% +/- 1.7% of the radioactivity of the initially bound glycoprotein. The fragments which remained attached to the hydroxyapatite after enzymic digestion were fractionated on Sephadex G-25 and analysed for carbohydrate and amino acid components. A range of amino acids were detected which could reflect both glycosylated and non-glycosylated-binding regions. Sialic acid, although considered to be involved in the attachment process was not detected in any of the fragments remaining after enzymic digestion, a finding which provides indirect evidence that the enzymically liberated products do not subsequently re-attach to the hydroxyapatite surface. The notable feature of the fractions with average Mr estimated at 1000 or less is the high proportion of N-acetylhexosamine and N-acetylgalactosamine. It is apparent that the hexosamine residues, which normally bear the ester sulphate moieties of sulphated glycoproteins, play an important role in the attachment of sulphated glycoproteins to hydroxyapatite.

Electrospinning of calcium carbonate fibers and their conversion to nanocrystalline hydroxyapatite

Energy Technology Data Exchange (ETDEWEB)

Holopainen, Jani, E-mail: jani.holopainen@helsinki.fi; Santala, Eero; Heikkilä, Mikko; Ritala, Mikko

2014-12-01

Calcium carbonate (CaCO{sub 3}) fibers were prepared by electrospinning followed by annealing. Solutions consisting of calcium nitrate tetrahydrate (Ca(NO{sub 3}){sub 2}·4H{sub 2}O) and polyvinylpyrrolidone (PVP) dissolved in ethanol or 2-methoxyethanol were used for the fiber preparation. By varying the precursor concentrations in the electrospinning solutions CaCO{sub 3} fibers with average diameters from 140 to 290 nm were obtained. After calcination the fibers were identified as calcite by X-ray diffraction (XRD). The calcination process was studied in detail with high temperature X-ray diffraction (HTXRD) and thermogravimetric analysis (TGA). The initially weak fiber-to-substrate adhesion was improved by adding a strengthening CaCO{sub 3} layer by spin or dip coating Ca(NO{sub 3}){sub 2}/PVP precursor solution on the CaCO{sub 3} fibers followed by annealing of the gel formed inside the fiber layer. The CaCO{sub 3} fibers were converted to nanocrystalline hydroxyapatite (HA) fibers by treatment in a dilute phosphate solution. The resulting hydroxyapatite had a plate-like crystal structure with resemblance to bone mineral. The calcium carbonate and hydroxyapatite fibers are interesting materials for bone scaffolds and bioactive coatings. - Highlights: • Calcium carbonate fibers were prepared by electrospinning. • The electrospun fibers crystallized to calcite upon calcination at 500 °C. • Spin and dip coating methods were used to improve the adhesion of the CaCO{sub 3} fibers. • The CaCO{sub 3} fibers were converted to hydroxyapatite by treatment in phosphate solution. • The hydroxyapatite fibers consisted of plate-like nanocrystals.

Preparation and characterization of water-absorbing composite ...

African Journals Online (AJOL)

The present work introduces a novel method for the formation of water absorbing composite membrane. The prepared composite is based on chitosan, carboxymethyl cellulose (CMC), and Montmorillonite. Prepared composite membrane exhibits high water absorbing and holding capacity with increasing clay content.

Parameter Optimization Of Natural Hydroxyapatite/SS316l Via Metal Injection Molding (MIM)

Science.gov (United States)

Mustafa, N.; Ibrahim1, M. H. I.; Amin, A. M.; Asmawi, R.

2017-01-01

Metal injection molding (MIM) are well known as a worldwide application of powder injection molding (PIM) where as applied the shaping concept and the beneficial of plastic injection molding but develops the applications to various high performance metals and alloys, plus metal matrix composites and ceramics. This study investigates the strength of green part by using stainless steel 316L/ Natural hydroxyapatite composite as a feedstock. Stainless steel 316L (SS316L) was mixed with Natural hydroxyapatite (NHAP) by adding 40 wt. % Low Density Polyethylene and 60 %wt. Palm Stearin as a binder system at 63 wt. % powder loading consist of 90 % wt. of SS316 L and 10 wt. % NHAP prepared thru critical powder volume percentage (CPVC). Taguchi method was functional as a tool in determining the optimum green strength for Metal Injection Molding (MIM) parameters. The green strength was optimized with 4 significant injection parameter such as Injection temperature (A), Mold temperature (B), Pressure (C) and Speed (D) were selected throughout screening process. An orthogonal array of L9 (3)4 was conducted. The optimum injection parameters for highest green strength were established at A1, B2, C0 and D1 and where as calculated based on Signal to Noise Ratio.

Fabrication and bioactivity behavior of HA/bioactive glass composites in the presence of calcium hexaboride

Energy Technology Data Exchange (ETDEWEB)

El-Bassyouni, Gehan T.; Beherei, Hanan H. [Biomaterials Dept., National Research Centre (NRC), Dokki, Cairo (Egypt); Mohamed, Khaled R., E-mail: kh_rezk1966@yahoo.com [Biomaterials Dept., National Research Centre (NRC), Dokki, Cairo (Egypt); Kenawy, Sayed H. [Ceramics Dept., National Research Centre (NRC), Dokki, Cairo (Egypt)

2016-06-01

In the current study, composites were prepared using both the synthesized nano-sized hydroxyapatite (HA), bioactive glass (BG) powders (obtained by the traditional melt-quenching route) together with the purchased nano-sized calcium hexaboride (CB) with different ratios and were fired at 1250 °C. The structure and composition of the solid reaction products were analyzed using X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy; scanning electron microscope (SEM) coupled with energy dispersive spectroscopy (EDS), transmission electron microscope (TEM) techniques and compressive strength. The mechanical testing was to designate the role of the CB in improving the mechanical property of the prepared composites. In vitro bioactivity of the prepared composites was assessed by soaking in the simulated body fluid (SBF) at 37 ± 0.5 °°C for 10 days. The effect of different ratios of the three components (CB, HA & BG) on the bioactivity properties was assessed to explore the possibility of enhancing such property to perform in vitro imitations of in vivo conditions in the future. It can be pointed out that the Si-HA content in the composition showed outstanding in vitro bioactivity than pure hydroxyapatite which could be attributed to the excellent bioactivity of the synthesized composites. - Highlights: • The prepared of nano-composites containing CB, HA and BG powders were achieved. • The addition of CB powder enhanced the compressive strength for all the composites. • The composites containing high BG and CB contents improved formation of bone-like apatite layer.

Fabrication and bioactivity behavior of HA/bioactive glass composites in the presence of calcium hexaboride

International Nuclear Information System (INIS)

El-Bassyouni, Gehan T.; Beherei, Hanan H.; Mohamed, Khaled R.; Kenawy, Sayed H.

2016-01-01

In the current study, composites were prepared using both the synthesized nano-sized hydroxyapatite (HA), bioactive glass (BG) powders (obtained by the traditional melt-quenching route) together with the purchased nano-sized calcium hexaboride (CB) with different ratios and were fired at 1250 °C. The structure and composition of the solid reaction products were analyzed using X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy; scanning electron microscope (SEM) coupled with energy dispersive spectroscopy (EDS), transmission electron microscope (TEM) techniques and compressive strength. The mechanical testing was to designate the role of the CB in improving the mechanical property of the prepared composites. In vitro bioactivity of the prepared composites was assessed by soaking in the simulated body fluid (SBF) at 37 ± 0.5 °°C for 10 days. The effect of different ratios of the three components (CB, HA & BG) on the bioactivity properties was assessed to explore the possibility of enhancing such property to perform in vitro imitations of in vivo conditions in the future. It can be pointed out that the Si-HA content in the composition showed outstanding in vitro bioactivity than pure hydroxyapatite which could be attributed to the excellent bioactivity of the synthesized composites. - Highlights: • The prepared of nano-composites containing CB, HA and BG powders were achieved. • The addition of CB powder enhanced the compressive strength for all the composites. • The composites containing high BG and CB contents improved formation of bone-like apatite layer.

Electrospun composites of PHBV/pearl powder for bone repairing

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Jingjing Bai

2015-08-01

Full Text Available Electrospun fiber has highly structural similarity with natural bone extracelluar matrix (ECM. Many researches about fabricating organic–inorganic composite materials have been carried out in order to mimic the natural composition of bone and enhance the biocompatibility of materials. In this work, pearl powder was added to the poly (3-hydroxybutyrate-co-3-hydroxyvalerate (PHBV and the composite nanofiber scaffold was prepared by electrospinning. Mineralization ability of the composite scaffolds can be evaluated by analyzing hydroxyapatite (HA formation on the surface of nanofiber scaffolds. The obtained composite nanofiber scaffolds showed an enhanced mineralization capacity due to incorporation of pearl powder. The HA formed amount of the composite scaffolds was raised as the increase of pearl powder in composite scaffolds. Therefore, the prepared PHBV/pearl composite nanofiber scaffolds would be a promising candidate as an osteoconductive composite material for bone repairing.

Preparation and characterization of water-absorbing composite ...