A successful attempt has been made to improve the mechanical properties of Hydroxyapatite (HAp) and reduced graphene oxide (rGO) composite nanoparticles (NPs). Various proportions of HAp and rGO were synthesized to improve the mechanical properties. HAp NPs were prepared using the wet precipitation method and further calcined to form crystalline particles. The physicochemical characterization of the HAp NPs revealed that the crystalline size and percentage of crystallinity were calculated to be 42.49 ± 1.2 nm and 44% post calcination. Furthermore, the rGO-HA composites were prepared using ball milling and obtained in the shape of pellets with different ratios of rGO (10, 20, 30, 40, 50% wt.). The mechanical properties have been evaluated through a Universal testing machine. Compared to calcined HAp (cHAp), the strength of variants significantly enhanced with the increased concentration of rGO. The compressive strength of HA-rGO with the ratio of the concentration of 60:40% by weight is a maximum of about 10.39 ± 0.43 MPa. However, the porosity has also been bolstered by increasing the concentration of rGO, which has been evaluated through the liquid displacement method. The mean surface roughness of the composites has also been evaluated from the images through Image J (an image analysis program).
We have successfully used continuous microwave flow synthesis (CMFS) technique for the template free synthesis of mesoporous hydroxyapatite. The continuous microwave flow reactor consisted of a modified 2.45GHz household microwave, peristaltic pumps and a Teflon coil. This cost effective and efficient system was exploited to produce semi-crystalline phase pure nano-sized hydroxyapatite. Effect of microwave power, retention time and the concentration of reactants on the phase purity, degree of crystallinity and surface area of the final product was studied in detail. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) were used to study the phase purity and composition of the product, while transmission electron microscopy (TEM) was used to study the effect of process parameters on the morphology of hydroxyapatite. The TEM analysis confirmed the formation of spherical particles at low microwave power; however the morphology of the particles changed to mesoporous needle and rod-like structure upon exposing the reaction mixture to higher microwave power and longer retention time inside the microwave. The in-vitro ion dissolution behavior of the as synthesized hydroxyapatite was studied by determining the amount of Ca(2+) ion released in SBF solution.
The present study addressed the synthesis of a bi-layered nanostructured fluorine-doped hydroxyapatite (nFHA)/polycaprolactone (PCL) coating on Mg-2Zn-3Ce alloy via a combination of electrodeposition (ED) and dip-coating methods. The nFHA/PCL composite coating is composed of a thick (70-80 μm) and porous layer of PCL that uniformly covered the thin nFHA film (8-10 μm) with nanoneedle-like microstructure and crystallite size of around 70-90 nm. Electrochemical measurements showed that the nFHA/PCL composite coating presented a high corrosion resistance (R(p)=2.9×10(3) kΩ cm(2)) and provided sufficient protection for a Mg substrate against galvanic corrosion. The mechanical integrity of the nFHA/PCL composite coatings immersed in SBF for 10 days showed higher compressive strength (34% higher) compared with the uncoated samples, indicating that composite coatings can delay the loss of compressive strength of the Mg alloy. The nFHA/PCL coating indicted better bonding strength (6.9 MPa) compared to PCL coating (2.2 MPa). Immersion tests showed that nFHA/PCL composite-coated alloy experienced much milder corrosion attack and more nucleation sites for apatite compared with the PCL coated and uncoated samples. The bi-layered nFHA/PCL coating can be a good alternative method for the control of corrosion degradation of biodegradable Mg alloy for implant applications.
In this study, HA is superplastically embedded into Titanium substrate and the sample is subsequently deformed superplastically until 70% deformation degree. The former process is termed as superplastic embedment (SPE) while the later as superplastic deformation (SPD). After the SPE, HA is successfully embedded into the substrate, forming a layer with a thickness of about 249 nm. After the SPD the embedded HA layer thickness decreases to 111 nm. The SPD sample is then immersed in simulated body fluid (SBF) to evaluate its biological properties. A newly grown apatite is formed as a result of the immersion and the HA layer thickness increases with immersion time. The cohesion and adhesion strength within the HA coating and coating-substrate interface of the SPD samples before and after immersion in the SBF is evaluated through the nanoscratch test technique. The results indicate that the HA layer after SPD is still strong even though after being exposed in SBF environment for quite some time. The study suggests that the superplastically embedded HA nanolayer is still intact mechanically and functioning appropriately as biological activity base even after the SPD process.
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 (SiO4(4-)) and carbonate (CO3(2-)) ions competed to occupy the phosphate (PO4(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. 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.
Hydroxyapatite is a biocompatible material that is extensively used in the replacement and regeneration of bone material. In nature, nanostructured hydroxyapatite is the main component present in hard body tissues. Hence, the state of the art in nanotechnology can be exploited to synthesize nanophase hydroxyapatite that has similar properties with natural hydroxyapatite. Sustainable methods to mass-produce synthetic hydroxyapatite nanoparticles are being developed to meet the increasing demand for these materials and to further develop the progress made in hard tissue regeneration, especially for orthopedic and dental applications. This article reviews the current developments in nanophase hydroxyapatite through various manufacturing techniques and modifications.
A novel hydrothermal process has been developed various hydroxyapatite(HA) powder. The HA powder was investigated in different calcination temperatures over the range of 200 degrees C-800 degrees C. TG/DTA and XRD analysis revealed that at temperatures of 700-800 degrees C the decomposition processes and phase changes took place. It is due to the appearance of TCP phase substituting the HA phase. FESEM observation showed that the produced hydroxyapatite powder was extraordinarily fine with nanosize primary particles and almost evenly spherical in shaped. Its high purity proved that the powder fulfills medical requirement.
The practice of bone implants is the standard procedure for the treatment of skeletal fissures, or to substitute and re-establish lost bone. A perfect scaffold ought to be made of biomaterials that duplicate the structure and properties of natural bone. However, the production of living tissue constructs that are architecturally, functionally and mechanically comparable to natural bone is the major challenge in the treatment and regeneration of bone tissue in orthopaedics and in dentistry. In this work, we have employed a polymeric replication method to fabricate hydroxyapatite (HAP) scaffolds using gum tragacanth (GT) as a natural binder. GT is a natural gum collected from the dried sap of several species of Middle Eastern legumes of the genus Astragalus, possessing antibacterial and wound healing properties. The synthesized porous HAP scaffolds were analyzed structurally and characterized for their phase purity and mechanical properties. The biocompatibility of the porous HAP scaffold was confirmed by seeding the scaffold with Vero cells, and its bioactivity assessed by immersing the scaffold in simulated body fluid (SBF). Our characterization data showed that the biocompatible porous HAP scaffolds were composed of highly interconnecting pores with compressive strength ranging from 0.036 MPa to 2.954 MPa, comparable to that of spongy bone. These can be prepared in a controlled manner by using an appropriate binder concentration and sintering temperature. These HAP scaffolds have properties consistent with normal bone and should be further developed for potential application in bone implants.
Dental enamel, an avascular, irreparable, outermost and protective layer of the human clinical crown has a potential to withstand the physico-chemical effects and forces. These properties are being regulated by a unique association among elements occurring in the crystallites setup of human dental enamel. Calcium and phosphate are the major components (hydroxyapatite) in addition to some trace elements which have a profound effect on enamel. The current review was planned to determine the aptitude of various trace elements to substitute and their influence on human dental enamel in terms of physical and chemical properties.
Due to similarity in composition to the mineral component of bones and human hard tissues, hydroxyapatite with chemical formula Ca10(PO4)6(OH)2 has been widely used in medical field. Both chicken and duck eggshells are mainly composed of calcium carbonate. An attempt has been made to fabricate nanohydroxyapatite (nHA) by chicken (CES) and duck eggshells (DES) as calcium carbonate source (CaCO3). CES and DES were reacted with diammonium hydrogen [(NH4)2HPO4] solution and subjected to microwave heating at 15 mins. Under the effect of microwave irradiation, nHA was produced directly in the solution and involved in crystallographic transformation. Sample characterization was done using by X-ray diffraction (XRD), fourier transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM).
This study is focused on finite element analysis of a model comprising femur into which a femoral component of a total hip replacement was implanted. The considered prosthesis is fabricated from a functionally graded material (FGM) comprising a layer of a titanium alloy bonded to a layer of hydroxyapatite. The elastic modulus of the FGM was adjusted in the radial, longitudinal, and longitudinal-radial directions by altering the volume fraction gradient exponent. Four cases were studied, involving two different methods of anchoring the prosthesis to the spongy bone and two cases of applied loading. The results revealed that the FG prostheses provoked more SED to the bone. The FG prostheses carried less stress, while more stress was induced to the bone and cement. Meanwhile, less shear interface stress was stimulated to the prosthesis-bone interface in the noncemented FG prostheses. The cement-bone interface carried more stress compared to the prosthesis-cement interface. Stair climbing induced more harmful effects to the implanted femur components compared to the normal walking by causing more stress. Therefore, stress shielding, developed stresses, and interface stresses in the THR components could be adjusted through the controlling stiffness of the FG prosthesis by managing volume fraction gradient exponent.
The complex architecture of the cortical part of the bovine-femur was examined to develop potential tissue engineering (TE) scaffolds. Weight-change and X-ray diffraction (XRD) results show that significant phase transformation and morphology conversion of the bone occur at 500-750°C and 750-900°C, respectively. Another breakthrough finding was achieved by determining a sintering condition for the nucleation of hydroxyapatite crystal from bovine bone via XRD technique. Scanning electron microscopy results of morphological growth suggests that the concentration of polymer fibrils increases (or decreases, in case of apatite crystals) from the distal to proximal end of the femur. Energy-dispersive analysis of X-ray, Fourier transform infrared, micro-computer tomography, and mechanical studies of the actual composition also strongly support our microscopic results and firmly indicate the functionally graded material properties of bovine-femur. Bones sintered at 900 and 1000°C show potential properties for soft and hard TE applications, respectively.
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.
This report presents physical characterization and cell culture test of porous alumina-hydroxyapatite (HA) composites fabricated through protein foaming-consolidation technique. Alumina and HA powders were mixed with yolk and starch at an adjusted ratio to make slurry. The resulting slip was poured into cylindrical shaped molds and followed by foaming and consolidation via 180 °C drying for 1 h. The obtained green bodies were burned at 600 °C for 1 h, followed by sintering at temperatures of 1200-1550 °C for 2 h. Porous alumina-HA bodies with 26-77 vol.% shrinkage, 46%-52% porosity and 0.1-6.4 MPa compressive strength were obtained. The compressive strength of bodies increased with the increasing sintering temperatures. The addition of commercial HA in the body was found to increase the compressive strength, whereas the case is reverse for sol-gel derived HA. Biocompatibility study of porous alumina-HA was performed in a stirred tank bioreactor using culture of Vero cells. A good compatibility of the cells to the porous microcarriers was observed as the cells attached and grew at the surface of microcarriers at 8-120 cultured hours. The cell growth on porous alumina microcarrier was 0.015 h(-1) and increased to 0.019 h(-1) for 0.3 w/w HA-to-alumina mass ratio and decreased again to 0.017 h(-1) for 1.0 w/w ratio.
In present study, a new composition of glass-ceramic was synthesized based on the Na2O-CaO-SiO2-P2O5 glass system. Heat treatment of glass powder was carried out in 2 stages: 600 °C as the nucleation temperature and different temperature on crystallization at 850, 950 and 1000 °C. The glass-ceramic heat-treated at 950 °C was selected as bioactive filler in commercial PMMA bone cement; (PALACOS® LV) due to its ability to form 2 high crystallization phases in comparison with 850 and 1000 °C. The results of this newly glass-ceramic filled PMMA bone cement at 0-16 wt% of filler loading were compared with those of hydroxyapatite (HA). The effect of different filler loading on the setting properties was evaluated. The peak temperature during the polymerization of bone cement decreased when the liquid to powder (L/P) ratio was reduced. The setting time, however, did not show any trend when filler loading was increased. In contrast, dough time was observed to decrease with increased filler loading. Apatite morphology was observed on the surface of the glass-ceramic and selected cement after bioactivity test.
The sintering behaviour of a commercial HA and synthesized HA was investigated over the temperature range of 700 degrees C to 1400 degrees C in terms of phase stability, bulk density, Young's modulus and Vickers hardness. In the present research, a wet chemical precipitation reaction was successfully employed to synthesize a submicron, highly crystalline, high purity and single phase stoichiometric HA powder that is highly sinteractive particularly at low temperature regimes below 1100 degrees C. It has been revealed that the sinterability of the synthesized HA was significantly greater than that of the commercial HA. The temperature for the onset of sintering and the temperature required to achieve densities above 98% of theoretical value were approximately 150 degrees C lower for the synthesized HA than the equivalent commercial HA. Nevertheless, decomposition of HA phase upon sintering was not observed in the present work for both powders.
The sintering behaviour of synthesized HA powder that was calcined at various temperatures ranging from 700 degrees C to 1000 degrees C was investigated in terms of phase stability, bulk density, Young's modulus and Vickers hardness. The calcination treatment resulted in higher crystallinity of the starting HA powder. Decomposition of HA phase to form secondary phases was not observed in all the calcined powders. The results also indicated that powder calcination (up to 900 degrees C) prior to sintering has negligible effect on the sinterability of the HA compacts. However, powder calcined at 1000 degrees C was found to be detrimental to the properties of sintered hydroxyapatite bioceramics.
The effect of Manganese (Mn) addition on the Vickers hardness and relative density of nanocrystalline hydroxyapatite (HA) dense bodies were studied. The starting Mn doped HA powders was synthesized via sol-gel method with Mn concentration varies from 2 mol% up to 15 mol% Mn. The Mn doped HA disc samples were prepared by uniaxial pressing at 200MPa and subsequently sintered at 1300 degrees C. Characterization was carried out where appropriate to determine the phases present, bulk density, Vickers hardness of the various content of Mn doped HA dense bodies. The addition of Mn was observed to influence the color appearance of the powders and dense bodies as well. Higher Mn concentration resulted in dark grey powders. It was also found that the hardness and relative density of the material increased as the Mn content increased and influenced by the crystallinity of the prepared Mn doped HA powders.
This study aimed to investigate the structural, physical and mechanical behavior of composites and functionally graded materials (FGMs) made of stainless steel (SS-316L)/hydroxyapatite (HA) and SS-316L/calcium silicate (CS) employing powder metallurgical solid state sintering. The structural analysis using X-ray diffraction showed that the sintering at high temperature led to the reaction between compounds of the SS-316L and HA, while SS-316L and CS remained intact during the sintering process in composites of SS-316L/CS. A dimensional expansion was found in the composites made of 40 and 50 wt% HA. The minimum shrinkage was emerged in 50 wt% CS composite, while the maximum shrinkage was revealed in samples with pure SS-316L, HA and CS. Compressive mechanical properties of SS-316L/HA decreased sharply with increasing of HA content up to 20 wt% and gradually with CS content up to 50 wt% for SS-316L/CS composites. The mechanical properties of the FGM of SS-316L/HA dropped with increase in temperature, while it was improved for the FGM of SS-316L/CS with temperature enhancement. It has been found that the FGMs emerged a better compressive mechanical properties compared to both the composite systems. Therefore, the SS-316L/CS composites and their FGMs have superior compressive mechanical properties to the SS-316L/HA composites and their FGMs and also the newly developed FGMs of SS-316L/CS with improved mechanical and enhanced gradation in physical and structural properties can potentially be utilized in the components with load-bearing application.
Hydroxyapatite (HAp) is an attractive bioceramics due to its similar composition to bone mineral and its ability to promote bone-implant interaction. However, its low strength has limited its application as load bearing implants. This paper presented a work focusing on the improvement of HAp mechanical property by synthesizing iron (Fe)-reinforced bovine HAp nanocomposite powders via mechanosynthesis method. The synthesis process was performed using high energy milling at varied milling time (3, 6, 9, and 12h). The samples were characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), and scanning electron microscopy (SEM). Its mechanical properties were investigated by micro-Vicker's hardness and compression tests. Results showed that milling time directly influenced the characteristics of the nanocomposite powders. Amorphous BHAp was formed after 9 and 12h milling in the presence of HPO4(2-) ions. Continuous milling has improved the crystallinity of Fe without changing the HAp lattice structure. The nanocomposite powders were found in spherical shape, agglomerated and dense after longer milling time. The hardness and Young's modulus of the nanocomposites were also increased at 69% and 66%, respectively, as the milling time was prolonged from 3 to 12h. Therefore, the improvement of the mechanical properties of nanocomposite was attributed to high Fe crystallinity and homogenous, dense structure produced by mechanosynthesis.