Biomedical subjects

K A Khor

Publications and source records attributed to K A Khor.

At least 19 recordsLinked to original sources

PubMed2006

Apparent solubility of hydroxyapatite in aqueous medium and its influence on the morphology of nanocrystallites with precipitation temperature.

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.

Chemical Precipitation↗

PubMed2006

Conductometric study of precursor compound formation during wet-chemical synthesis of nanocrystalline hydroxyapatite.

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.

Acids↗

PubMed2006

Chemical analysis of silica doped hydroxyapatite biomaterials consolidated by a spark plasma sintering method.

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.

Biocompatible Materials↗

PubMed2006

On the kinetics of apatite growth on substrates under physiological conditions.

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.

Apatites↗

PubMed2006

In vitro bioactivity and osteoblast response of porous NiTi synthesized by SHS using nanocrystalline Ni-Ti reaction agent.

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.

Biocompatible Materials↗

PubMed2005

Effects of incorporation of HA/ZrO(2) into glass ionomer cement (GIC).

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.

Bone Cements↗

PubMed2005

Characterisation of a duplex TiO2/CaP coating on Ti6Al4V for hard tissue replacement.

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.

Alloys↗

PubMed2005

Radio frequency (rf) plasma spheroidized HA powders: powder characterization and spark plasma sintering behavior.

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.

Biocompatible Materials↗

PubMed2004

Temperature driven morphological changes of chemically precipitated hydroxyapatite nanoparticles.

Hydroxyapatite (HA) is synthesized by a wet chemical route using calcium hydroxide and ortho-phosphoric acid at various temperatures (40, 80, and 100 degrees C). X-ray diffraction of the precipitate particles revealed HA as the predominant phase (>99%) with a small amount of beta-tricalcium phosphate. Fourier transform infrared spectroscopy indicated the presence of carbonate substitution, which decreased with increasing temperature. Transmission electron microscopy observations revealed needle-shaped particles with a high aspect ratio at 40 degrees C, which changed to spheroidal when the precipitation temperature was increased to 100 degrees C. The changes in the morphology with temperature were analyzed taking into account the driving force for the HA precipitation and the supersaturation level of Ca2+ and PO4(3-) ions with respect to HA. The analysis indicated that the supersaturation level of the reactants, especially the concentration of Ca2+ ions, played a predominant role on the precipitate morphology for this classical acid-base reaction.

Chemical Precipitation↗

PubMed2004

Activity of plasma sprayed yttria stabilized zirconia reinforced hydroxyapatite/Ti-6Al-4V composite coatings in simulated body fluid.

Hydroxyapatite (HA)/yttria stabilized zirconia/Ti-6Al-4V bio-composite coatings deposited onto Ti-6Al-4V substrate through a plasma spray technique were immersed in simulated body fluid (SBF) to investigate their behavior in vitro. Surface morphologies and structural changes in the coatings were analyzed by scanning electron microscopy, thin-film X-ray diffractometer, and X-ray photoelectron spectroscopy. The tensile bond strength of the coatings after immersion was also conducted through the ASTM C-633 standard for thermal sprayed coatings. Results showed that carbonate-containing hydroxyapatite (CHA) layer formed on the surface of composite coatings after 4 weeks immersion in SBF solution, indicating the composite coating possessed excellent bioactivity. The mechanical properties were found to decrease with immersion duration of maximum 56 days. However, minimal variation in mechanical properties was found subsequent to achieving supersaturation of the calcium ions, which was attained with the precipitation of the calcium phosphate layers. The mechanical properties of the composite coating were found to be significantly higher than those of pure HA coatings even after immersion in the SBF solution, indicating the enhanced mechanical properties of the composite coatings.

Alloys↗

PubMed2004

Thermal sprayed hydroxyapatite splats: nanostructures, pore formation mechanisms and TEM characterization.

Microstructure of thermal sprayed hydroxyapatite (HA) splats was characterized using transmission electron microscopy (TEM), and the formation mechanisms of micropores within the splats were investigated with the aid of simulated body fluids (SBF). High-velocity oxy-fuel and direct current (DC) plasma spray techniques were both utilized for the splats' deposition. The microstructure features of individual HA splats were revealed through TEM observation of as-sprayed, and ion-milled splats. Amorphous calcium phosphate and tricalcium phosphate phases were observed at the splats' fringes, which indicated that extensive decomposition of HA had occurred at these locations. The fringes of the HA splats are essentially nanostructured ( approximately 20-50 nm grains), while calcium phosphate grains up to 5 microm, depending on flattening state, are present at the center of the splats. Morphological observation classified the pores within the HA splats into three main categories according to distinctive features in their microstructure: open pores, sealed pores and through-thickness pores. It was found that particle velocity with which the particle impinged on the substrate surface, particle melt state, and structure of starting particle (mainly porosity) are the key variables in determining the formation and morphology of the micropores within the flattened splats. Influence of subsequent splats on the pores of prior deposited splat was also studied using an in vitro incubation test in SBF. Obvious pore-sealing action on the open pores was revealed, which was achieved through liquid filling of subsequent droplets. It was postulated that the overall porosity of a bulk coating could be attributed primarily to the sealed pores and flaws among the splats, and, it could be adequately governed through appropriate particle melt state and optimized velocity of the particles during coating formation.

Aerosols↗

PubMed2004

Microstructure and mechanical properties of plasma sprayed HA/YSZ/Ti-6Al-4V composite coatings.

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.

Aerosols↗

PubMed2004

Bone-like apatite layer formation on hydroxyapatite prepared by spark plasma sintering (SPS).

Hydroxyapatite (HA) compacts with high density and superior mechanical properties were fabricated by spark plasma sintering (SPS) using spray-dried HA powders as feedstock. The formation of bone-like apatite layer on SPS consolidated HA compacts were investigated by soaking the HA compacts in simulated body fluid (SBF) for various periods (maximum of 28 days). The structural changes in HA post-SBF were analyzed with scanning electron microscopy, grazing incidence X-ray diffraction and X-ray photoelectron spectroscopy. It was found that a layer consisting microcrystalline carbonate-containing hydroxyapatite was formed on the surface of HA compacts after soaking for 24h. The formation mechanism of apatite on the surface of HA compacts after soaking in SBF was attributed to the ion exchange between HA compacts and the SBF solution. The increase in ionic concentration of calcium and phosphorus as well as the increase in pH after SBF immersion resulted in an increase in ionic activity product of apatite in the solution, and provided a specific surface with a low interface energy that is conducive to the nucleation of apatite on the surface of HA compacts.

Apatites↗

PubMed2003

TEM and STEM analysis on heat-treated and in vitro plasma-sprayed hydroxyapatite/Ti-6Al-4V composite coatings.

A cogent understanding of the microstructure, and indeed nano-structure, of hydroxyapatite (HA) and the interface between Ti-6Al-4V and HA is crucial to its appropriateness as a biomaterials. This paper reports the analysis of plasma-sprayed HA/Ti-6Al-4V composites by transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM) to elucidate the intricate nature of the materials following plasma spray processing and in vitro evaluation. The novel Ti-6Al-4V/HA composite coating, with approximately 48 wt% HA, had demonstrated attractive tensile adhesion strength (approximately 28 MPa) and improved Young's modulus (approximately 55 GPa). Experimental results demonstrated that amorphous calcium phosphate and fine HA grains were formed during rapid splat solidification in the as-sprayed composite coatings. Small Ti-6Al-4V grains were observed adjacent to the amorphous calcium phosphate. The coatings were further heat treated at 600 degrees C for 6 h, and significant crystallisation of the amorphous calcium phosphate phase took place. However, complete crystallisation was not achieved at this temperature, as the coatings invariably contained a small amount of amorphous calcium phosphate phase in some local regions. After immersion in simulated body fluid for 2 weeks and 10 weeks, TEM and STEM confirmed that the interfaces inside the coating maintained good microstructural integrity.

Alloys↗

PubMed2003

In vitro behavior of HVOF sprayed calcium phosphate splats and coatings.

Hydroxyapatite (HA) coatings and splats deposited by high velocity oxy-fuel (HVOF) spray technique was investigated in vitro. HA coatings prepared from two different HA powder size range (30+/-5 and 50 +/-5 microm) were immersed in a simulated body fluid with various incubation periods of maximum 6 weeks. The dissolution/precipitation behavior was studied and the degradation of HA coatings caused by in vitro ageing was demonstrated by measuring the changes in flexural modulus through a 3-point bend test. It was found that the dissolution and precipitation behavior of the coatings was significantly dependent upon the incipient coating phase composition and the precipitation of bone-like hydroxyapatite on the coating's surface was found to be directly related to the dissolution process. Higher dissolution rates of tricalcium phosphate, tetracalcium phosphate and amorphous calcium phosphate relative to HA, resulted in accelerated precipitation. Furthermore, analysis of coatings' surface morphology demonstrated that advanced precipitation invariably occurred at regions where dissolution took place. Results showed that the changes in flexural modulus of investigated HA coatings accompanying different incubation duration was not systematic but was found to be dependent upon changes of coating structure and other factors brought about by in vitro ageing. In vitro investigation of individual HA splats collected from different HA particle sizes revealed, after 3 days ageing, that the rate ratio of precipitation to dissolution was directly determined by the local phase composition, and this phenomenon could be effectively used to explain the behavior of thermally sprayed HA coatings in vitro. It implied that the precipitation was strongly dependent on the first molecule attachment. To achieve rapid precipitation in vitro, partial molten state of HA particles during HVOF coating deposition was recommended.

Anions↗

PubMed2003

Characterization of the bone-like apatite precipitated on high velocity oxy-fuel (HVOF) sprayed calcium phosphate deposits.

Bone-like apatite was precipitated on the surface of thermal sprayed calcium phosphate coatings following in vitro incubation in a simulated body fluid. The coatings were initially deposited on titanium alloy substrates by the high velocity oxy-fuel (HVOF) spray technique. Structural characterization and mechanical evaluation of the precipitated apatite layer were conducted. Results showed that the precipitation rate was directly influenced by the local Ca(2+) concentration in the vicinity of the coating's surface and that preferential dissolution of certain phases was found to accelerate the precipitation of the bone-like apatite. The dense precipitates exhibited a competitive Young's modulus value of approximately 120GPa, which was obtained through nanoindentation. This compared favorably to the calcium phosphate matrix. Differences in microstructure at various locations within the layer resulted in altered Young's modulus and microhardness values. Precipitation mechanism investigation was carried out through a comparative experiment. Chemical analysis showed that the precipitation of bone-like apatite on the calcium phosphate coating was quite conceivably a partial diffusion-controlled process.

Apatites↗

PubMed2003

Impact formation and microstructure characterization of thermal sprayed hydroxyapatite/titania composite coatings.

Formation mechanism of hydroxyapatite (HA)/titania (TiO(2)) composite coating deposited by high velocity oxy-fuel (HVOF) thermal spray process was studied, and its structural characterization was conducted and elaborated in this paper. The impact theory was employed to analyze the formation procedure of the HA/titania composite coatings. Results revealed that the crater caused by the impact of entirely unmelted TiO(2) particles on the HA matrix during coating formation was of smaller dimensions than the original size of the reinforcements. It was found that chemical reaction between the mechanically blended HA and TiO(2) powder took place exclusively during the impingement stage, and calcium titanate, CaTiO(3), was one notable by-product. The bonding between the HA matrix and TiO(2) reinforcement might have been achieved predominantly through a chemical bond that resulted from the mutual chemical reactions among the components. Differential scanning calorimetry analyses showed that the chemical reaction between HA and TiO(2) was at approximately 1410 degrees C. The TiO(2) addition was found to exert particular effects on the thermal behavior of HA at elevated temperatures, during both heating and cooling cycles. Transmission electron microscopy observation identified the chemical reaction zone between HA and TiO(2), which revealed an improved splats' interface. The reaction zone demonstrated some influence on the grain size of HA nearby during resolidification of the melted portion. A structural model was proposed to illustrate the location of the different phases in the HA/titania composite coating.

Calorimetry, Differential Scanning↗

PubMed2003

In vitro studies of plasma-sprayed hydroxyapatite/Ti-6Al-4V composite coatings in simulated body fluid (SBF).

The bioactivity of plasma-sprayed hydroxyapatite (HA)/Ti-6Al-4V composite coatings was studied by soaking the coatings in simulated body fluid (SBF) for up to 8 weeks. This investigation was aimed at elucidating the biological behaviour of plasma-sprayed HA/Ti-6Al-4V composite coatings by analyzing the changes in chemistry, and crystallinity of the composite coating in a body-analogous solution. Phase composition, microstructure and calcium ion concentration were analyzed before, and after immersion. The mechanical properties, such as tensile bond strength, microhardness and Young's modulus were appropriately measured. Results demonstrated that the tensile bond strength of the composite coating was significantly higher than that of pure HA coatings even after soaking in the SBF solution over an 8-weeks period. Dissolution of Ca-P phases in SBF was evident after 24h of soaking, and, a layer of carbonate-apatite covered the coating surface after 2 weeks of immersion. The mechanical properties were found to diminish with soaking duration. However, slight variation in mechanical properties was found after supersaturation of the calcium ions was attained with the precipitation of the calcium phosphate layers.

Alloys↗