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1.
Scientometrics ; 127(12): 7487-7497, 2022.
Article in English | MEDLINE | ID: mdl-35755633

ABSTRACT

Amid an increasingly demanding research environment, there has been a growing interest in studies concerning Research Integrity and Research Ethics (RIRE). Between 1990 and 2020, over 9700 publications were published to address problematic research conduct such as falsification, plagiarism, and related protocols and standards. In this work, country-level trends and collaborative structures are examined with respect to economic group. Our results showed that RIRE publications are predominantly led by the West, with North America and Western Europe contributing the most. While there is interest within growing economies such as China, the pace is not comparable to its overall publications. However, international collaborations on RIRE grew to account for nearly 30% of all publications on the subject in 2020. Although there is a stronger preference for high income countries to collaborate with other high income countries, we observe a rise in partnerships between high-/middle-income and middle-/lower-income co-authorship pairs in the last decade. These trends point to a maturing global community with distributed knowledge transfer, towards more unified international standards for research ethics and integrity. Supplementary Information: The online version contains supplementary material available at 10.1007/s11192-022-04400-y.

2.
ACS Biomater Sci Eng ; 5(4): 1703-1714, 2019 Apr 08.
Article in English | MEDLINE | ID: mdl-33405547

ABSTRACT

Three sets of hydroxyapatite and rutile-TiO2 coatings were plasma sprayed onto metallic substrates. The spray parameters of the sets were modified so as to obtain different in-flight temperatures and velocities of the powder particles within the plasma jet (ranging from 1778 to 2385 K and 128 to 199 m s-1, respectively). Fatigue endurance of the coated specimens was then tested. The samples were subjected to a symmetric cyclical bend loading, and the crack propagation was monitored until it reached a predefined cross-section damage. The influence of the coating deposition was evaluated with respect to a noncoated reference set and the in-flight characteristics. Attributed to favorable residual stress development in the sprayed samples, it was found that the deposition of the coatings generally led to a prolongation of the fatigue lives. The highest lifetime increase (up to 46% as compared to the noncoated set) was recorded for the coatings deposited under high in-flight temperature and velocity. Importantly, this was achieved without significantly compromising the microstructure or phase composition of the deposited HA and TiO2 layers.

3.
Scientometrics ; 107: 1095-1110, 2016.
Article in English | MEDLINE | ID: mdl-27239078

ABSTRACT

We investigated the effect of international collaboration (in the form of international co-authorship) on the impact of publications of young universities (<50 years old), and compared to that of renowned old universities (>100 years old). The following impact indicators are used in this study, they are: (1) the 5-year citations per paper (CPP) data, (2) the international co-authorship rate, (3) the CPP differential between publications with and without international co-authorships, and (4) the difference between the percentage of international co-authored publications falling in the global top 10 % highly cited publications and the percentage of overall publications falling in the global top 10 % highly cited publications (Δ%Top10%). The increment of 5-year (2010-2014) field weighted citation impact (FWCI) of internationally co-authored papers over the 5-year overall FWCI of the institutions in SciVal® is used as another indicator to eliminate the effect of discipline difference in citation rate. The results show that, for most top institutions, the difference between the citations per paper (CPP) for their publications with and without international co-authorship is positive, with increase of up to 5.0 citations per paper over the period 1996-2003. Yet, for some Asian institutions, by attracting a lot of researchers with international background and making these collaborating "external" authors as internal researchers, these institutions have created a special kind of international collaboration that are not expressed in co-authorship, and the CPP gaps between publications with and without international co-authorship are relatively small (around 0-1 citations per paper increment) for these institutions. The top old institutions have higher CPP than young institutions, and higher annual research expenditures; while young universities have a higher relative CPP increment for the current 5-year period over the previous 5-year period. The Δ%Top10% for international co-authored publications is generally higher than that for all journal publications of the same institution. With the increase of international co-authorship ratio, the mean geographical collaboration distance (MGCD, an indication of increased international co-authorship) of one institution based on the Leiden Ranking data also increases, and young institutions have relatively higher CPP increment over MGCD increment. International co-authorship has a positive contribution to the FWCI of the institution, yet there are untapped potential to enhance the collaboration among young institutions.

4.
J Mech Behav Biomed Mater ; 4(8): 2043-54, 2011 Nov.
Article in English | MEDLINE | ID: mdl-22098904

ABSTRACT

The failure of an orthopaedic implant can be initiated by residual strain inherent to the hydroxyapatite coating (HAC). Knowledge of the through-thickness residual strain profile in the thermally sprayed hydroxyapatite coating/substrate system is therefore important in the development of a new generation of orthopaedic implants. As the coating microstructure is complex, non-destructive characterization of residual strain, e.g. using neutron diffraction, provides a useful measure of through thickness strain profile without altering the stress field. This first detailed study using a neutron diffraction technique, non-destructively evaluates the through thickness strain measurement in nanostructured hydroxyapatite plasma sprayed coatings on a titanium alloy substrate (as-sprayed, heat treated, and heat treated then soaked in simulated body fluid (SBF)). The influence of crystallographic plane orientation on the residual strain measurement is shown to indicate texturing in the coating. This texturing is expected to influence both the biological and fracture response of HA coatings. Results are discussed in terms of the influence of heat-treatment and SBF on the residual stress profile for these biomedical coatings. The results show that the through thickness residual strain in all three coatings was different for different crystallographic planes but was on average tensile. It is also concluded that the heat-treatment and simulated body fluid exposure had a significant effect on the residual strain profile in the top layers of HAC.


Subject(s)
Bone and Bones , Coated Materials, Biocompatible/chemistry , Durapatite/chemistry , Nanostructures/chemistry , Neutron Diffraction , Prostheses and Implants , Stress, Mechanical , Alloys , Hardness Tests , Hot Temperature , Immersion , Prosthesis Failure , Titanium/chemistry , X-Ray Diffraction
5.
Invest Ophthalmol Vis Sci ; 52(1): 21-9, 2011 Jan 05.
Article in English | MEDLINE | ID: mdl-20739467

ABSTRACT

PURPOSE: Osteo-odonto keratoprosthesis is one of the most successful forms of keratoprosthesis surgery for end-stage corneal and ocular surface disease. There is a lack of detailed comparison studies on the biocompatibilities of different materials used in keratoprosthesis. The aim of this investigation was to compare synthetic bioinert materials used for keratoprosthesis surgery with hydroxyapatite (HA) as a reference. METHODS: Test materials were sintered titanium oxide (TiO(2)), aluminum oxide (Al(2)O(3)), and yttria-stabilized zirconia (YSZ) with density >95%. Bacterial adhesion on the substrates was evaluated using scanning electron microscopy and the spread plate method. Surface properties of the implant discs were scanned using optical microscopy. Human keratocyte attachment and proliferation rates were assessed by cell counting and MTT assay at different time points. Morphologic analysis and immunoblotting were used to evaluate focal adhesion formation, whereas cell adhesion force was measured with a multimode atomic force microscope. RESULTS: The authors found that bacterial adhesion on the TiO(2), Al(2)O(3), and YSZ surfaces were lower than that on HA substrates. TiO(2) significantly promoted keratocyte proliferation and viability compared with HA, Al(2)O(3,) and YSZ. Immunofluorescent imaging analyses, immunoblotting, and atomic force microscope measurement revealed that TiO(2) surfaces enhanced cell spreading and cell adhesion compared with HA and Al(2)O(3). CONCLUSIONS: TiO(2) is the most suitable replacement candidate for use as skirt material because it enhanced cell functions and reduced bacterial adhesion. This would, in turn, enhance tissue integration and reduce device failure rates during keratoprosthesis surgery.


Subject(s)
Bacterial Adhesion/physiology , Biocompatible Materials/metabolism , Cell Adhesion/physiology , Fibroblasts/metabolism , Prostheses and Implants , Aluminum Oxide/metabolism , Alveolar Process/transplantation , Blotting, Western , Cell Proliferation , Cell Survival , Cells, Cultured , Corneal Diseases/surgery , Corneal Stroma/cytology , Cuspid/transplantation , Cytoskeletal Proteins/metabolism , Durapatite/metabolism , Humans , Microscopy, Atomic Force , Microscopy, Electron, Scanning , Staphylococcus aureus/physiology , Staphylococcus aureus/ultrastructure , Titanium/metabolism , Yttrium/metabolism , Zirconium/metabolism
6.
Nanotechnology ; 21(11): 115707, 2010 Mar 19.
Article in English | MEDLINE | ID: mdl-20173250

ABSTRACT

The low temperature sintering behaviour of nanocrystalline Ag powder (with an average size of 70 nm) was characterized. Using spark plasma sintering (SPS), the Ag nanopowders can be successfully sintered at low pressure for only 5 min without external heating, and the sintering density increases and porosity decreases significantly with increase in the sintering temperature. Nanoindentation has been used to characterize the SPS sintered Ag samples. The mechanisms of the low sintering temperature behaviour of the nano-Ag powder and the nanoscale mechanical performance have been discussed. Compression tests were also used to characterize the mechanical properties of the sintered Ag sample with a maximum strain up to 15%.

7.
Biomaterials ; 30(29): 5385-91, 2009 Oct.
Article in English | MEDLINE | ID: mdl-19631375

ABSTRACT

The use of synthetic hydroxyapatite as bone substitute calls for the knowledge of the influence on adjacent cells. The aim of this study was to investigate the proteins with differential protein expression levels in the proteome of human osteoblast cell line incubated separately with various nano sized hydroxyapatite powders with different shapes and chemical compositions using iTRAQ-coupled 2D LC-MS/MS approach. In the present study, we investigated several intracellular signaling molecules involved in calcium regulation to analyze how osteoblast cells respond to dissimilar HA nanoparticles. It was found there was a significant decrease in cell population after adding the HA nanoparticles to the osteoblasts. Our results combining proteomics analysis and RT-PCR validation on targeted genes involved in calcium regulation confirmed the differences in the cellular response to dissimilar HA nanoparticles.


Subject(s)
Cell Culture Techniques/methods , Durapatite/chemistry , Gene Expression Regulation/physiology , Nanoparticles/chemistry , Nanoparticles/ultrastructure , Osteoblasts/metabolism , Proteome/metabolism , Biocompatible Materials/chemistry , Bone Substitutes/chemistry , Cell Line , Humans , Materials Testing , Particle Size , Surface Properties
8.
J Biomed Mater Res B Appl Biomater ; 84(1): 224-30, 2008 Jan.
Article in English | MEDLINE | ID: mdl-17631676

ABSTRACT

This study investigated the osteoblast behaviors on various hydroxyapatite based biomaterials that were consolidated at 1100 degrees C for 3 min by a spark plasma sintering technique. The osteoblasts from human fetal osteoblast cell line were cultured in the medium on the various biomaterials surfaces (HA, RF21, 1SiHA, and 5SiHA) to assess the cell morphology and proliferation as well as cell differentiation (alkaline phosphatase activity). Moreover, the bone gamma-carboxyglutamic protein or osteocalcin in the medium were determined at different periods of culture. The present results indicated that the amount of osteocalcin in the medium decreased during the periods of culture. The highest osteocalcin production obtained from the biomaterial 5SiHA after cell culture for 2 days demonstrated that the presence of silica in the biomaterials enhanced the cell differentiation by the rapid release of silicate and calcium ions.


Subject(s)
Biocompatible Materials/chemistry , Biocompatible Materials/pharmacology , Hydroxyapatites/chemistry , Hydroxyapatites/pharmacology , Osteoblasts/drug effects , Alkaline Phosphatase/genetics , Biocompatible Materials/chemical synthesis , Bone Development/drug effects , Cell Adhesion , Cell Differentiation , Cell Line , Cell Proliferation , Culture Media/chemistry , Fetus/cytology , Genes, Reporter/genetics , Humans , Hydroxyapatites/chemical synthesis , Microscopy, Electron, Scanning , Osteoblasts/metabolism , Osteoblasts/ultrastructure , Osteocalcin/biosynthesis , Surface Properties , Tetrazolium Salts , Thiazoles , X-Ray Diffraction
9.
J R Soc Interface ; 5(21): 427-39, 2008 Apr 06.
Article in English | MEDLINE | ID: mdl-17698476

ABSTRACT

The synthesis and subsequent assembly of nearly spherical nano-hydroxyapatite (nHA) particles in the presence of trace amounts of the polysaccharide chitosan was carried out employing a wet chemical approach. Chitosan addition during synthesis not only modulated HA crystallization but also aided in the assembly of nHA particles onto itself. Solvent extraction from these suspensions formed iridescent films, of which the bottom few layers were rich in self-assembled nHA particle arrays. The cross-section of these hybrid films revealed compositional and hence structural grading of the two phases and exhibited a unique morphology in which assembled nHA particles gradually gave way to chitosan-rich top layers. Transmission electron microscope and selected area electron diffraction studies suggested that the basal plane of HA had interacted with chitosan, and scanning electron microscope studies of the hybrid films revealed multi-length scale hierarchical architecture composed of HA and chitosan. Phase identification was carried out by X-ray diffraction (XRD) and Rietveld analysis of digitized XRD data showed that the basic apatite structure was preserved, but chitosan inclusion induced subtle changes to the HA unit cell. The refinement of crystallite shape using the Popa method clearly indicated a distinct change in the growth direction of HA crystallites from [001] to [100] with increasing chitosan concentration. The paper also discusses the likelihood of chitosan phosphorylation during synthesis, which we believe to be a pathway, by which chitosan molecules chemically interact with calcium phosphate precursor compounds and orchestrate the crystallization of nHA particles. Additionally, the paper suggests several interesting biomedical applications for graded nHA-chitosan nanostructured films.


Subject(s)
Chitosan/chemistry , Durapatite/chemistry , Nanostructures/chemistry , Crystallization , Membranes, Artificial , Nanostructures/ultrastructure
10.
Biosens Bioelectron ; 23(1): 135-9, 2007 Aug 30.
Article in English | MEDLINE | ID: mdl-17478087

ABSTRACT

ZnO:Co nanoclusters were synthesized by nanocluster-beam deposition with averaged particle size of 5 nm and porous structure, which were for the first time adopted to construct a novel amperometric glucose biosensor. Glucose oxidase was immobilized into the ZnO:Co nanocluster-assembled thin film through Nafion-assisted cross-linking technique. Due to the high specific active sites and high electrocatalytic activity of the ZnO:Co nanoclusters, the constructed glucose biosensor showed a high sensitivity of 13.3 microA/mA cm2. The low detection limit was estimated to be 20 microM (S/N=3) and the apparent Michaelis-Menten constant was found to be 21 mM, indicating the high affinity of the enzyme on ZnO:Co nanoclusters to glucose. The results show that the ZnO:Co nanocluster-assembled thin films with nanoporous structure and nanocrystallites have potential applications as platforms to immobilize enzyme in biosensors.


Subject(s)
Biosensing Techniques/instrumentation , Cobalt/chemistry , Electrochemistry/instrumentation , Glucose/analysis , Nanostructures/chemistry , Zinc Oxide/chemistry , Biosensing Techniques/methods , Electrochemistry/methods , Equipment Design , Equipment Failure Analysis , Reproducibility of Results , Sensitivity and Specificity
11.
J Biomed Mater Res A ; 82(2): 296-303, 2007 Aug.
Article in English | MEDLINE | ID: mdl-17274029

ABSTRACT

This study aimed to fabricate bulk nanostructured hydroxyapatite (HA) pellets with improved properties using spark plasma sintering (SPS) for orthopedic applications. Spray-dried nanostructured HA (nSD-HA) powders were consolidated using the rapid SPS processing. The SPS processed nSD-HA was characterized using Raman spectroscopy and field emission scanning electron microscopy (FESEM). Mechanical properties of the consolidates were also evaluated through indentation approach. The nanostructures ( approximately 80 nm in grain size) of the starting powders were successfully retained after the SPS processing operated at 950 degrees C with <15 min holding time. The SPS consolidated nSD-HA showed promising mechanical properties, approximately 118 GPa for Young's modulus, and up to 2.22 MPa m(0.5) for fracture toughness. SPS holding time showed minor influence on the phases of the pellets. Furthermore, the spheroidized nanostructured HA retained the HA structure after the SPS consolidation. Preliminary cytotoxicity and cell attachment studies were also carried out using a human osteoblast cell line hFOB 1.19. Enhanced cell attachment and proliferation on the nanostructured pellets were revealed. The presence of the nanostructures accounts mainly for the enhanced mechanical properties and promoted proliferation of the osteoblast cells. This study suggests that the SPS technique is an appropriate process for fabrication of bulk nSD-HA from nanostructured powder.


Subject(s)
Biocompatible Materials/pharmacology , Durapatite/pharmacology , Osteoblasts/cytology , Osteoblasts/drug effects , Biocompatible Materials/chemistry , Biomechanical Phenomena , Cell Line , Durapatite/chemistry , Humans , Materials Testing , Microscopy, Electron, Scanning , Nanostructures/ultrastructure , Nanotechnology , Powder Diffraction
12.
J Inorg Biochem ; 101(2): 187-95, 2007 Feb.
Article in English | MEDLINE | ID: mdl-17095092

ABSTRACT

Silica (SiO(2)) and the silicate-based biomaterials play an important role due to their in vitro and in vivo biological response. The present study synthesized a novel nano-structured amorphous silica doped hydroxyapatite (HA) via an aqueous precipitation route. HA was prepared with 0, 1, 3 and 5 wt% silica, which are comparable to the measured silicon content of natural bone. After spray drying into micron sized powders, the silica doped HA (SiHA) powders were consolidated at 1000 degrees C with a dwell time of 3 min using a spark plasma sintering (SPS) technique. X-ray diffraction analysis showed a main apatite phase with minor secondary beta-tricalcium phosphate (beta-TCP) was observed in the as-consolidated SiHA compacts. Substitution of PO(4)(3-) by SiO(4)(4-) in the apatite structure resulting in a small increase in the lattice parameters in both a-axis and c-axis of the unit cell were identified by X-ray photoelectron spectrometer (XPS) analysis and Raman spectrometer investigation. The cell culture in vitro investigation demonstrated that the presence of silicon in the SPS consolidated compacts contributed to the relatively high cell proliferation ability when compared with phase pure HA.


Subject(s)
Biocompatible Materials/analysis , Durapatite/analysis , Silicon Dioxide/analysis , Biocompatible Materials/chemistry , Biomechanical Phenomena , Cell Proliferation , Cells, Cultured , Ceramics/analysis , Ceramics/chemistry , Durapatite/chemistry , Humans , Materials Testing , Microscopy, Electron, Scanning , Osteoblasts/cytology , Silicon Dioxide/chemistry , Spectrometry, X-Ray Emission , Spectrum Analysis, Raman , Surface Properties , X-Ray Diffraction
13.
J Phys Chem B ; 110(48): 24457-62, 2006 Dec 07.
Article in English | MEDLINE | ID: mdl-17134201

ABSTRACT

Conductometry was employed to study the phase evolution of calcium phosphate compounds during the wet-chemical synthesis of hydroxyapatite (HA). Calcium hydroxide and orthophosphoric acid were used to prepare HA at various temperatures ranging from 30 to 95 degrees C. The electrical conductivity and pH of the reaction mixture were measured at regular intervals of time during acid addition, and the rate of change of conductivity was used to decipher the end point of the reaction. Our previous studies have shown that the end product of this reaction route yields mildly carbonated crystalline HA. The trend of the change in conductivity with time was similar at all temperatures. The conductivity curves were divided into three regions based on the variation in slope of the curves. The slope of the curves decreased with increasing temperatures in the first two regions, and the slope is greater in the second region than in the first. From the conductivity and pH measurement results, the possible precursor phase was identified and it had the composition Ca(3)(PO(4))(2). The kinetics of phase transformation was also analyzed and compared to previous work. The similarities between this work and the traditionally adapted experimental work for phase formation and transformation kinetics are highlighted, and the novelty in the current work is discussed.


Subject(s)
Durapatite/chemical synthesis , Nanostructures/chemistry , Acids/chemistry , Crystallization , Durapatite/chemistry , Hydrogen-Ion Concentration , Ions/chemistry , Solubility , Suspensions , Temperature
14.
Langmuir ; 22(26): 11002-8, 2006 Dec 19.
Article in English | MEDLINE | ID: mdl-17154577

ABSTRACT

Two differing wet-chemical synthesis routes, Ca(OH)2 + H3PO4 and CaCl2 + Na3PO4/NaOH, were used to prepare hydroxyapatite (HA) at various temperatures ranging from 30 to 95 degrees C. The electrical conductivity of the solution was measured at regular intervals of time during H3PO4 and Na3PO4 addition to the suspension/solution containing Ca2+ ions. The rate of change of conductivity is used to note the end point of the reaction. X-ray diffraction of the dried, precipitated particles revealed HA as the predominant phase, and the FTIR spectroscopy studies indicated the presence of CO3(2-) groups which substituted PO4(3-) groups in the HA lattice (B-type). FESEM observations revealed that the aspect ratio of the particles decreased with increasing precipitation reaction temperature in one system [Ca(OH)2 + H3PO4] and in the other system it increased with increasing temperature. The changes in the morphology with temperature were analyzed through conductivity measurements and the thermochemical properties of the reaction systems. Conductivity measurements showed that the concentration of dissolved ions at the end point of the reaction between Ca(OH)2 and H3PO4 increased, indicating an increased apparent solubility of HA with increasing temperature, whereas the end-point conductivity did not increase noticeably in the other reaction system.


Subject(s)
Durapatite/chemistry , Nanostructures/chemistry , Chemical Precipitation , Crystallization , Durapatite/chemical synthesis , Materials Testing , Nanostructures/ultrastructure , Solubility , Spectroscopy, Fourier Transform Infrared/methods , Temperature , X-Ray Diffraction/methods
15.
J Biomed Mater Res A ; 78(2): 316-23, 2006 Aug.
Article in English | MEDLINE | ID: mdl-16637041

ABSTRACT

Porous NiTi with an average porosity of 55 vol % and a general pore size of 100-600 microm was synthesized by self-propagating high temperature synthesis (SHS) with the addition of mechanically alloyed nanocrystalline Ni-Ti as the reaction agent. The SHS of porous NiTi using elemental powders was also performed for comparison. To enhance the bioactivity of the metal surface, porous NiTi synthesized by nanocrystalline Ni-Ti was subjected to chemical treatment to form a layer of TiO(2) coating. The porous NiTi with TiO(2) coating was subsequently immersed in a simulated body fluid (SBF) to investigate its apatite forming ability. The effects of the addition of nanocrystalline Ni-Ti as reaction agent and the application of apatite coating on osteoblastic behavior were studied in primary cultures of human osteoblast cells. Results showed that the main phases in porous NiTi synthesized by elemental powders were NiTi, Ti(2)Ni, and unreacted free Ni. By using nanocrystalline Ni-Ti as reaction agent, the secondary intermetallic phase of Ti(2)Ni was significantly reduced and the free Ni was eliminated. TiO(2) coating with anatase phase was formed on the surface of porous NiTi after the chemical treatment. A layer consisting of nanocrystalline carbonate-containing apatite was formed on the surface of TiO(2) coating after soaking in SBF. The preliminary cell culture studies showed that the porous NiTi synthesized with the addition of nanocrystalline Ni-Ti attracted marked attachment and proliferation of the osteoblast cells. This gives the evidence of the potential biomedical applications of the porous NiTi.


Subject(s)
Nickel , Osteoblasts/physiology , Titanium , Biocompatible Materials , Crystallization , Microscopy, Electron , Nanostructures , Porosity , Surface Properties , X-Ray Diffraction
16.
Langmuir ; 22(1): 269-76, 2006 Jan 03.
Article in English | MEDLINE | ID: mdl-16378431

ABSTRACT

Derived from reaction kinetics, a simple but useful method, based on "apatite forming capacity" or AFC of solutions mimicking blood plasma, is proposed to decipher the rate of calcium phosphate mineralization. Apatite growth rate constants were calculated using this method for a model composite surface varying the volume fraction of synthetic hydroxyapatite (HA) in a polymer matrix. Previously reported data for mineralized surfaces on Ta, Ti, and its alloys are also analyzed similarly and compared. Utilizing the growth rate constant, the bioactivity of the materials was indexed in vitro. Complementarily, semiempirical quantum mechanical calculation (ZINDO method) showed that the interaction of cations with TRIS-hydroxymethyl aminomethane molecules in the solution is stronger than that with the polymer substrate considered, but weaker than hydrated Ti and TiO(2) surfaces. This analysis then quantifies for example the extent of polymer inertness and the "bioactivity" of alkali treated Ti. The growth rate constants for the model materials prepared in this work are explained on the basis of localized dissolution of HA, the amount of which simply increases with increasing volume fraction of HA in the composite.


Subject(s)
Apatites/chemistry , Biocompatible Materials/chemistry , Body Fluids/chemistry , Coated Materials, Biocompatible , Humans , In Vitro Techniques , Kinetics , Quantum Theory , Surface Properties
17.
Biomaterials ; 26(15): 2197-207, 2005 May.
Article in English | MEDLINE | ID: mdl-15585221

ABSTRACT

The present study describes the synthesis of spheroidized hydroxyapatite (HA) powders using a radio frequency (rf) inductively coupled plasma (ICP) torch. The spheroidized powders were consolidated through a spark plasma sintering (SPS) system. The microstructure and crystallographic phases in the synthesized powders were characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffractometry (XRD) and Raman spectrometry. Results showed that the HA feedstock decomposed after rf plasma processing. Crystalline HA, alpha-tri-calcium phosphate (alpha-TCP), tetra-calcium phosphate (TTCP) and calcium oxide (CaO) were detected in the plasma-spheroidized powders. Raman spectra results indicated strong presence of amorphous calcium phosphate (ACP) in the spheroidized powders. The particle size distribution and specific surface area were influenced through the rf plasma working plate power levels. The sintering behavior of the rf plasma synthesized powders was analyzed through the SPS process and the results indicated that the spheroidized powders commence sintering at approximately 900 degrees C and through to 1150 degrees C. After sintering above 1100 degrees C for 3min, the relative densities of the SPS compacts reached 96% of the theoretical value. The SPS compacts were immersed in simulated body fluids (SBF) for different durations and the results confirmed their bioactivities.


Subject(s)
Body Fluids/chemistry , Crystallization/methods , Durapatite/chemistry , Durapatite/radiation effects , Hot Temperature , Radio Waves , Biocompatible Materials/analysis , Biocompatible Materials/chemistry , Biocompatible Materials/radiation effects , Calcium Phosphates , Durapatite/analysis , Elasticity , Electromagnetic Fields , Hardness , Materials Testing , Microspheres , Particle Size , Phase Transition , Powders , Temperature
18.
Biomaterials ; 26(10): 1087-95, 2005 Apr.
Article in English | MEDLINE | ID: mdl-15451628

ABSTRACT

An initial TiO(2) coating was applied on Ti6Al4V by electrochemical anodisation in two dissimilar electrolytes. The secondary calcium phosphate (CaP) coating was subsequently applied by immersing the substrates in a simulated body fluid (SBF) with three times concentration (SBFx3), mimicking biomineralisation of biological bone. Electrochemical impedance spectroscopy and potentiodynamic polarisation assessments in SBF revealed that the anodic TiO(2) layer is compact, exhibiting up to four-folds improvement in in vitro corrosion resistance over unanodised Ti6Al4V. X-ray photoelectron spectroscopy analysis indicates that the anodic Ti oxide is thicker than air-formed ones with a mixture of TiO(2-x) compound between the TiO(2)/Ti interfaces. The morphology of the dense CaP film formed, when observed using scanning electron microscopy, is made up of linked globules 0.1-0.5microm in diameter without observable delamination. Fourier transform infrared spectrometry with an attenuated total internal reflection analysis revealed that this film is an amorphous/poorly crystallised calcium-deficient-carbonated CaP system. The calculated Ca:P ratios of all samples (1.14-1.28) are lower than stoichiometric hydroxyapatite (1.67). These results show that a duplex coating consisting of (1) a compact TiO(2) with enhanced in vitro corrosion resistance and (2) bone-like apatite coating can be applied on Ti6Al4V by anodisation and subsequent immersion in SBF.


Subject(s)
Body Fluids/chemistry , Bone Substitutes/chemistry , Calcium Phosphates/chemistry , Coated Materials, Biocompatible/chemistry , Titanium/chemistry , Alloys , Biomimetic Materials/chemistry , Corrosion , Materials Testing , Surface Properties
19.
Biomaterials ; 26(7): 713-20, 2005 Mar.
Article in English | MEDLINE | ID: mdl-15350775

ABSTRACT

Glass ionomer cements (GICs) are a class of bioactive cements that bond directly to bone. In this paper, a new bioactive hydroxyapatite (HA)/zirconia (ZrO(2))-filled GIC composite was developed to improve the biocompatibility and bioactivity of the GICs with the surrounding bone and connective tissues. Nano-sized HA/30 wt% ZrO(2) powders were heat treated at 700 degrees Celsius and 800 degrees Celsius for 3 h to elucidate the influence of the crystallinity of composite powders on the performance of HA/ZrO(2)-GICs. The effects of different volume percentages of HA/ZrO(2) powders (4, 12, 28 and 40 vol%) substituted within GICs were investigated based on their microhardness, compressive strength and diametral tensile strength. The HA/ZrO(2)-GICs composite was soaked in distilled water for 1 day and 1 week before subjecting the samples to mechanical testing. Results showed that the glass and HA/ZrO(2) particles were distributed uniformly in the GIC matrix. The substitution of highly crystalline HA/ZrO(2) improved the mechanical properties of the HA/ZrO(2)-GICs due to the slow resorption rate for highly crystalline powders in distilled water. The mechanical properties of HA/ZrO(2)-GICs increased with increasing soak time due to the continuous formation of aluminium salt bridges, which improved the final strength of the cements. The compositions 4 and 12 vol% HA/ZrO(2)-GICs exhibited superior mechanical properties than the original GICs. The mechanical properties of HA/ZrO(2)-GICs were found to be much better than those of HA-GICs because ZrO(2) has the attributes of high strength, high modulus, and is significantly harder than glass and HA particles. Furthermore, ZrO(2) does not dissolve with increasing soaking time.


Subject(s)
Bone Cements/chemistry , Durapatite/chemistry , Glass Ionomer Cements/chemistry , Zirconium/chemistry , Bone Cements/chemical synthesis , Compressive Strength , Hardness , Materials Testing , Particle Size , Powders , Surface Properties , Tensile Strength
20.
Biomaterials ; 25(18): 4009-17, 2004 Aug.
Article in English | MEDLINE | ID: mdl-15046891

ABSTRACT

Plasma sprayed hydroxyapatite (HA) coatings on titanium alloy substrate have been used extensively due to their excellent biocompatibility and osteoconductivity. However, the erratic bond strength between HA and Ti alloy has raised concern over the long-term reliability of the implant. In this paper, HA/yttria stabilized zirconia (YSZ)/Ti-6Al-4V composite coatings that possess superior mechanical properties to conventional plasma sprayed HA coatings were developed. Ti-6Al-4V powders coated with fine YSZ and HA particles were prepared through a unique ceramic slurry mixing method. The so-formed composite powder was employed as feedstock for plasma spraying of the HA/YSZ/Ti-6Al-4V coatings. The influence of net plasma energy, plasma spray standoff distance, and post-spray heat treatment on microstructure, phase composition and mechanical properties were investigated. Results showed that coatings prepared with the optimum plasma sprayed condition showed a well-defined splat structure. HA/YSZ/Ti-6Al-4V solid solution was formed during plasma spraying which was beneficial for the improvement of mechanical properties. There was no evidence of Ti oxidation from the successful processing of YSZ and HA coated Ti-6Al-4V composite powders. Small amount of CaO apart from HA, ZrO(2) and Ti was present in the composite coatings. The microhardness, Young's modulus, fracture toughness, and bond strength increased significantly with the addition of YSZ. Post-spray heat treatment at 600 degrees C and 700 degrees C for up to 12h was found to further improve the mechanical properties of coatings. After the post-spray heat treatment, 17.6% increment in Young's modulus (E) and 16.3% increment in Vicker's hardness were achieved. The strengthening mechanisms of HA/YSZ/Ti-6Al-4V composite coatings were related to the dispersion strengthening by homogeneous distribution of YSZ particles in the matrix, the good mechanical properties of Ti-6Al-4V and the formation of solid solution among HA, Ti alloy and YSZ components.


Subject(s)
Coated Materials, Biocompatible/chemistry , Crystallization/methods , Durapatite/chemistry , Titanium/chemistry , Yttrium/chemistry , Zirconium/chemistry , Aerosols/chemistry , Alloys , Elasticity , Hardness , Hot Temperature , Manufactured Materials , Materials Testing , Molecular Conformation , Particle Size , Powders , Surface Properties , Tensile Strength
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