Bioceramics 17

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Authors: Ahmed H. Touny, Paul W. Brown
Abstract: Composite material composed of hydroxyapatite (HAp) and structural proteins, such as type I collagen or cross-linked gelatins, were synthesized at 37.4°C by hydrolysis of alpha tricalcium phosphate (α-TCP) in the presence of these protein structures. X-ray diffraction (XRD)and isothermal calorimetry were used as tools to evaluate the rate of HAp formation. Rates of HAp formation depend on protein structure. Gelatin enhances HAp formation while collagen delays it. Changes in pH during the hydrolysis α-TCP are unlikely to have an aggressive effect on the surrounding tissue. The presence of the protein improves the ductility of the HAp/protein composite but it decreases the tensile strength.
Authors: Herman S. Mansur, Alexandra A.P. Mansur, Marivalda Pereira
Abstract: In the present work, natural coral from Brazilian reefs were studied according to their crystallography by X-ray diffraction and microstructure by Scanning Electron Microscopy (SEM/EDX). FTIR spectroscopy was also used to evaluate the chemical functionalities and major components present in the material. The SEM morphology results have shown a tri-dimensional coral structure with porous ranging from 50 to 200 µm. Aragonite was identified as the major crystalline phase through XRD analysis and FTIR spectroscopy. Strontium calcium carbonate, (Sr,Ca)CO3, was also identified by XRD analysis. After sintering at 900º/1h, the conversion from aragonite to CaO and calcite was observed. These results have endorsed the high potential application of natural coral materials as 3D scaffolds for biomedical application, because of calcium carbonate compounds can be converted to HA by hydrothermal and biomimetic coating processes.
Authors: Claudia P. García, C. Paucar, J. Gaviria, Alicia Durán
Abstract: The synthetic hydroxyapatite is a very useful material for numerous applications in medicine as a biomaterial. One of the most economic manufacturing process is the precipitation route. In the present work, synthetic hydroxyapatite was prepared using the precipitation route, starting with aqueous solutions of calcium nitrate (Ca(NO3).4H2O ) and ammonium phosphate (H2(PO4)NH4). The effects of physical-chemical variables such as pH, temperature, time of agitation, ageing time and heat treatment of the mixture were evaluated. The characterization of the samples obtained in different conditions made possible to conclude about the optimal values of the studied variables for the synthesis of this material in laboratory conditions.
Authors: Chandrasekhar Kothapalli, Mei Wei, Montgomery T. Shaw
Abstract: This paper reports the influence of aging time and reaction temperature on the surface morphology and mechanical properties of hydroxyapatite (HA) synthesized by a hydrothermal method. Calcium nitrate and ammonium orthophosphate solutions were premixed and fed to an autoclave and reacted to temperatures varying between 25-250°C for 2-10 h. Results indicate the strong positive influence of reaction temperature on the HA particle aspect ratio. The density of the discs pressed from these samples reached 85-90% of the theoretical density after calcination at 1200°C for 1 h. Sintered density and flexural strength were found to increase with increasing aging time and reaction temperature. A maximum flexural strength of 78 MPa was observed for the sample synthesized at 170°C for 5 h with the predicted average at these conditions being 65 MPa.
Authors: Y.M. Jiang, Xiao Hong Li, Bo Feng, Jie Weng
Abstract: The surface of synthetic calcium hydroxyapatite (HA, Ca10(PO4)6(OH)2) was modified through combining freeze-drying, solvent replacement and surface modification methods in an effort to obtain the deaggregative n-HA crystallites. Three surface modification agents: Polyethylene glycol (PEG, Mw: 6000), poly(propyl oxide)-poly (ethyl oxide)-co-poly(propyl oxide)(Pluronic F-127, Mw: 12,000) and poly(d, l-lactide)-co-poly (ethylene glycol) (PELA, Mw: 20,000)were selected. The dispersion of the modified n-HA was characterized by sedimentation time in distilled water, acetone and dimethyl formamide (DMF). The results indicate that the three surface modification agents influence the dispersion of n-HA crystallites in various solvent based on different mechanisms. Transmission electron microscopy (TEM) observation shows that the dried and acetone-replacement powders are composed of needle-like HA crystallites isolated individually. The chosen solvents have a profound effect on the sedimentation time. In distilled water, the dispersion of as-synthesized n-HA crystallites is increased greater by F127 than by PEG. After freeze-drying, the two n-HA particles show homogeneous dispersion in acetone. The colloid stability of freeze-dried HA/PEG, solution-replaced HA/F127 and solution-replaced HA/PELA in DMF were improved significantly. The suspensions remained stable after 30 days with only a blue transparent sol being observed.
Authors: R. Roop Kumar, K.H. Prakash, K. Yennie, P. Cheang, Khiam Aik Khor
Abstract: The use of precipitation chemistry to synthesize hydroxyapatite (HA) normally yields nano-crystals with various morphology and sizes depending on the synthesis conditions (e.g., temperature, concentration, level of agitation, pH, etc.). This study involved the synthesis of HA nano-rods/whiskers by modifying an existing chemical route for HA synthesis. The nano-rods were characterised for their structure and morphology and subsequently sintered. The mechanical properties of the sintered compacts were also assessed.
Authors: Yoshiyuki Yokogawa, Yoshikazu Shiotsu, Fukue Nagata, Makoto Watanabe
Abstract: Protein loading on apatite hydrogel cake and its solubility was studied. A mixture of di-sodium hydrogen phosphate dodeca-hydrate and calcium chloride di-hydrate was dissolved in water, and kept at room temperature for 2 weeks in air or N2 atmosphere to make apatite hydrogel. The obtained apatite hydrogel contains carbonate ions, and its carbonate content strongly affect the aggregation of particles. With maturation period, the particle size of apatite hydrogel decreased in air, but increased in N2 atmosphere. The quantity of loaded Cytochrome C in apatite hydrogel formed in air was 0.490 wt%, while that in apatite hydrogel formed under N2 atmosphere was 0.305 wt%. But the quantity of loaded albumin in apatite hydrogel formed in air was less than that in apatite hydrogel formed under N2 atmosphere. The difference may be due to the relationship between isoelectric point of protein and apatite hydrogel. The apatite hydrogel containing protein was dried for 4 days in air at 40 % of relative humidity to make cakes, and the cakes were immersed in pure water or PBS solution. The dried specimen slowly dissolves in aqueous solution, and the decrease in weight of apatite cake prepared from hydrogel formed in air was larger than that from hydrogel formed under N2 atmosphere compared to the dissolved apatite, the released protein was less, which may be associated with recrystallization of the apatite hydrogel.
Authors: A.F. Lemos, A.H.S. Rebelo, J.H.G. Rocha, José Maria F. Ferreira
Abstract: Stable and relatively concentrated aqueous suspensions of nano-sized stoichiometric hydroxyapatite could be prepared by a precipitation method in the presence of suitable surface active agent (SAA). The method includes the precipitation, vacuum filtration and washing of the precipitated powders, followed by re-dispersion. It could be concluded that the added amount of the SAA should be enough to cover the primary particles surface, and that washing should be better carried out using a SAA solution. The method developed enables the precipitation of the powders and the preparation of suspensions, while significantly shortening the overall time required for colloidal processing consuming.
Authors: Lauren E. Jackson, Adrian J. Wright
Abstract: This study describes the use of flux methods as a novel synthetic route to some known and new calcium polyphosphates, with a view to developing new biomaterials. Calcium acid pyrophosphate, CaH2P2O7, which is a known precursor in the preparation of many other calcium polyphosphates, has been synthesized as a pure crystalline phase in a single step synthesis at temperatures between 190-250 °C. Reaction temperatures between 250 and 400 °C led to the synthesis of γ-Ca(PO3)2, a previously uncharacterised polymorph of calcium metaphosphate. Lattice parameters of a = 10.3682(1) Å, b = 9.5001(1) Å, c = 9.5552(1) Å, with β angle of 93.45(4)° were obtained from powder X-ray diffraction data. A subsequent increase in reaction temperature to 550 °C was found to produce a calcium polyphosphate glass. A detailed study of thermal stability of CaH2P2O7 was also performed to determine phase stability and decomposition pathways.
Authors: Cun You Wu, Yuichiro Murakami, Kensuke Sassa, Kazuhiko Iwai, Shigeo Asai
Abstract: The controlled development of texture microstructure in ceramics is one effective way to improve their properties, such as electrical, mechanical properties and biocompatibility. A bioceramics with oriented crystal structure has attracted great interest. In bone reparations, Hydroxyapatite (HAp)-based biomaterials were frequently used. And HAp is the main mineral constituent of the hard tissue of human bodies, which occurs with a hexagonal crystal. A HAp crystal turns out to have different surface properties in a- (or b-) plane and c-plane. In this regard, to get highly oriented HAp is very important before using HAp as a biomaterial. And the crystal orientated HAp is useful not only as biomaterials but also as protein absorbents. In this research, two different kinds of HAp-based biomaterial with oriented structure (HAp bioceramics and HAp-coated titanium composite) were studied.

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