The effect of interfacial bonding of calcium phosphate cements containing bio-mineralized multi-walled carbon nanotube and bovine serum albumin on the mechanical properties of calcium phosphate cements

The aim of this study was to investigate the effect of adding bio-mineralized hydroxyl functionalized multi-walled carbon nanotubes (MWCNTs–OH) on the compressive strength of calcium phosphate cements (CPCs). Bovine serum albumin (BSA) was also incorporated as a protein which acts as promoter of hydroxyapatite (HA) crystal growth when bounded to CPC granules. The results show that the strong interfacial bonding of CPC/MWCNTs–OH is essential to improve the mechanical properties of CPC/bio-mineralized MWCNTs–OH/BSA composite.     

An aqueous synthesis of photocatalyst by selective dissolution of titanium oxide/hydroxyapatite composite

A novel synthesis method of a highly active photocatalyst was proposed. Titanium dioxide (TiO₂) nano-particles were prepared by three-step procedure, precipitation of hydroxyapatite (HAp) on TiO₂ particles, heat treatment of the TiO₂/HAp composites, and acid treatment in hydrochloric acid. The unique point of this procedure is the selective dissolution of HAp to obtain exposed TiO₂ surfaces. The HAp precipitation was achieved by stirring TiO₂ powders in the mixtures of Ca(NO₃)₂ and NH₄H₂PO₄ aqueous solutions at pH 8.5. Then, the heat-treated TiO₂/HAp composites were treated with hydrochloric acid. The precipitated HAp avoided the direct contact of TiO₂ particles and suppressed the phase transformation from anatase-to-rutile >200 °C. The HAp also suppressed a decrease of specific surface area of TiO₂ during the heat treatment. The photocatalytic activities were evaluated from an absorbance decrease of methylene blue (MB) under ultraviolet (UV) irradiation. The MB photodecomposition was approximated to the first-order reaction and the reaction rate constants of the obtained TiO₂ powders heated at various temperatures were higher than those of conventional TiO₂ powders heated at same temperatures. The enhanced photocatalytic activity is attributed to the suppression effects for the phase transformation to rutile phase and the decreasing of specific surface area in the heat treatment.     

One step method to synthesize flower-like hydroxyapatite architecture using mussel shell bio-waste as a calcium source

Mussel shell, a calcium-rich resource, is found plenty in nature. We have developed a novel and facile method to convert mussel shell bio-waste into hydroxyapatite (HAp) biomaterial using microwave irradiation with the aid of ethylenediaminetetraacetic acid (EDTA) as chelating agent. The obtained HAp had flower-like morphology which can be a potential candidate for developing biomaterial for orthopedic applications. Moreover, the developed method has the potential to recover the bio-waste and reduce environment pollution.     

Influence of microstructure and phase composition on the nanoindentation characterization of bioceramic materials based on hydroxyapatite

The aim of the study was to investigate the influence of microstructure and phase composition on the mechanical behaviour of hydroxyapatite (HAp) and biphasic HAp/β-tricalcium phosphate (β-TCP) bioceramic materials using nanoindentation. The formation of β-TCP phase in the HAp ceramic had the predominant influence on the nanomechanical properties of compact ceramics. For investigated microstructures there appear to be a slight decrease in the elastic modulus with increasing load and a higher decrease in hardness, which are in agreement with upper bounds of the results reported in literature. Maximal value of reduced modulus and hardness is yielded with pure HAp, and is measured to be 133.76 GPa for average grain size of 3 μm and 12.18 GPa for average grain size of 140 nm, respectively. The average modulus and hardness results for HAp/β-TCP ceramics with higher (101.61 GPa, 6.76 GPa) and lower grain size (115.72 GPa, 8.76 GPa) show sufficient mechanical properties in order to serve as hard tissue replacement material.     

Biomimetic deposition of hydroxyapatite on the surface of silica thin film covered steel tape

The biomimetic deposition of hydroxyapatite (HA) on the surface of SiO₂ thin film coated metal substrates was developed and investigated.     

Sodium dodecyl sulfate mediated microwave synthesis of biocompatible superparamagnetic mesoporous hydroxyapatite nanoparticles using black Chlamys varia seashell as a calcium source for biomedical applications

Designing biocompatible superparamagnetic mesoporous nanoparticles for advanced healthcare applications has received much attention. In this research, we have synthesized intrinsic mesoporous superparamagnetic hydroxyapatite (HAp) nanoparticles using bio-waste of black Chlamys varia seashell as a calcium source by sodium dodecyl sulfate (SDS)–enabled microwave-assisted synthesis approach. The synthesized Fe-doped HAp nanoparticles were characterized using various characterization techniques to know the phase purity and morphological features. The incorporation of Fe greatly affected the morphology of HAp nanoparticles without affecting their crystalline phase. Superparamagnetic behavior was observed with the incorporation of Fe in the HAp nanoparticles. Further, saturation magnetization was enhanced with higher incorporation of Fe ions. The cytotoxicity studies of the synthesized pure and Fe-doped HAp samples conducted using a human osteoblasts cell line (MG63), which indicated that Fe-doped HAp nanoparticles are biocompatible. Further, antibacterial activity analysis also confirmed their excellent antibacterial performance against different pathogens. Hence, SDS-enabled microwave-assisted synthesis approach using seashell as a calcium source would be a better approach for the production of intrinsic mesoporous superparamagnetic HAp nanoparticles for various biomedical applications, such as drug targeting, hyperthermia cancer therapy, and magnetic resonance imaging.     

Preparation of the reticulated hydroxyapatite ceramics using carbon-coated polymeric sponge with elongated pores as a novel template

This paper proposes a novel, simple way to improve the compressive strength of reticulated porous hydroxyapatite (HA) ceramics using carbon-coated polymeric sponges with elongated pores as a novel template. This template allowed samples to have two interconnected pore networks with a preferential orientation, in which an addition pore network was newly formed by removing the carbon-coated polymeric struts, while preserving the pre-existing pore network. The compressive strength of the sample was as high as 2.9 ± 0.3 MPa with a porosity of 76% when tested parallel to the direction of pore elongation. In addition, the in vitro cell test using a pre-osteoblast cell line revealed the samples to have good biocompatibility.     

Highly textured (Na1/2Bi1/2)0.94Ba0.06TiO3 ceramics prepared by the screen-printing multilayer grain growth technique

The screen-printing multilayer grain growth (MLGG) technique was successfully applied to perovskite-structured lead-free piezoelectric ceramics. Highly textured (Na_1/2Bi_1/2)_0.94Ba_0.06TiO₃ ceramics with (1 0 0) orientation were firstly fabricated by MLGG method with (or without) template particles. The MLGG approach using anisotropic Bi₄Ti₃O₁₂ templates resulted in >90% grain orientation, whereas the same approach without template particles resulted in high orientation degree. The grain orientation mechanism of MLGG using screen-printing was different form that of tape-casting and extrusion in templated grain growth (TGG) and reactive templated grain growth (RTGG) techniques. The interface between adjacent layers, which were formed by screen-printing, was the main mechanism for the texture development in MLGG technique. Compared with other grain orientation techniques, screen-printing was a simple, inexpensive and effective method to fabricate grain oriented lead-free piezoelectric ceramics.     

Structure of the hydroxyapatite plasma-sprayed coatings deposited on pre-heated titanium substrates

Plasma spraying is the most commonly used thermal spray method for the application of hydroxyapatite (HA, Ca₁₀(PO₄)₆(OH)₂) coatings. In the present study, the HA coatings were plasma spraying deposited onto plates of titanium pre-heated to 20 °C, 300 °C and 550 °C. The obtained HA coatings were investigated by means of X-ray diffraction and scanning electron microscopy. It is found that the coatings, in addition to HA, contain the tetracalcium phosphate (TTCP, (Ca₄(PO₄)₂O) phase (~10%) and a small amount of CaO (<2%). Crystal structure of HA in the coatings is revealed to be distorted. The PO4 tetrahedrons are deformed (Baur distortion coefficient D1(TO) ~0.2). The distances Ca1-O1 and Ca1-O2 are changed as compared to these in stoichiometric hydroxyapatite. These distortions are considered as a result of internal stresses, which are demonstrated in the broadening of peaks on X-ray diffraction pattern of HA. Microstructure of coatings consisting of flattened splats was formed by fully molten particles. The axial base texture was developed in the coatings. Ultrastructure is columnar with a preferred orientation of c-axes of the crystals parallel to the normal of plane coating n. The heating of substrate has a marked effect on the ultrastructure of coatings: the domain size increases from 790 to 1100 Å, the strain Δ decreases from 1.6·10^-3 to 1,2·10^–3, TTCP content diminishes from 12% to 7%. These results show that the effects due to heating of the substrate may be associated with partial recovery of HA microstructure.     

Solution combustion synthesis of bioceramic calcium phosphates by single and mixed fuels—A comparative study

Calcium phosphate based bioceramics have been synthesized by a modified combustion synthetic route using both citric acid and succinic acid separately and in mixture as fuels and nitrate and nitric acid as oxidants. Calcium nitrate and diammonium hydrogen phosphate were used as calcium and phosphate sources. The effects of citric acid to succinic acid ratio on the phase formation have been investigated. The precursors and the calcined products have been characterized by powder X-ray diffraction, Fourier-transform infrared spectroscopy and scanning electron microscopy. Succinic acid has been used as a fuel for the first time to synthesize hydroxyapatite.     

Effect of 1 wt% LiF additive on the densification of nanocrystalline Y2O3 ceramics by spark plasma sintering

Densification of nanocrystalline cubic yttria (nc-Y₂O₃) powder, with 18 nm crystal size and 1 wt% LiF as a sintering additive was investigated. Specimens were fabricated by spark plasma sintering at 100 MPa, within the temperature range of 700-1500 °C. Sintering at 700 °C for 5 and 20 min resulted in 95% and 99.7% dense specimens, with an average grain size of 84 and 130 nm, respectively. nc-Y₂O₃ without additive was only 65% dense at 700 °C for 5 min. The presence of LiF at low sintering temperatures facilitated rapid densification by particle sliding and jamming release. Sintering at high temperatures resulted in segregation of LiF to the grain boundaries and its entrapment as globular phase within the fast growing Y₂O₃ grains. The sintering enhancement advantage of LiF was lost at high SPS temperatures.     

Synthesis of nanostructured material by mechanical milling and study on structural property modifications in Ni0.5Zn0.5Fe2O4

Mechanical milling induced structural property modifications in Ni_0.5Zn_0.5Fe₂O₄ spinel ferrite have been studied. We have observed two interesting phenomena (i) “temperature diffuse scattering” due to displacement of atoms from their mean position and (ii) appearance and gradual evolution of (4 2 0) plane in X-ray diffraction profiles and increase in average percentage disagreement between observed and calculated intensity ratios value, due to “preferred grain orientation.” Both these effects get prominent with milling time. The X-ray diffraction line intensity calculations revealed large B-site occupancy of Zn²⁺-ions, mainly due to modified synthesis procedure employed. The grain orientation factor increases from 10.6% to 18.1% on milling. It is found that milling has marked influence on various parameters: lattice constant, grain size, stress–strain, surface area and energy.     

Effect of precursors on the morphology and surface area of LaFeO3

Surface area and morphology of materials play an important role on their gas sensing performance because of the varying number and nature of adsorption sites. Current work reports a comparative study of LaFeO₃ synthesized by the facile hydrothermal method using two precursors; citric acid and KOH. The microstructure observed through FESEM and TEM showed different morphologies for the two precursors and calcination time (2?h & 6?h). Prior to calcination, higher surface area (50.54?m²/g) was obtained for LaFeO₃ prepared using KOH as compared to that for LaFeO₃ using citric acid (3.21?m²/g). Surface area increased from 3.21 to 7.06?m²/g for citric acid and decreased from 50.54 to 11.42?m²/g for KOH as calcination takes place for 6?h. Needle-shaped morphology of p-type LaFeO₃ with high surface area (50.54?m²/g) for KOH would provide large active sites which would enhance sensitivity towards gases. Hence, LaFeO₃ samples prepared using KOH with and without calcination are expected to give better performance for gas sensing than LaFeO₃ samples synthesized using citric acid.     

Influence of deposition temperature on the properties of hydroxyapatite obtained by electrochemical assisted deposition

Surface functionalization of pure titanium (cp-Ti) with hydroxyapatite (HAp) was successfully achieved by means of electrochemical deposition (ED) in a solution containing calcium nitrate and ammonium dihydrogen phosphate. The aim of this study is to evaluate the influence of the deposition temperature on the elemental and phase composition, chemical bonds, morphology, and in vitro electrochemical behaviour in biological simulated media (simulated body fluid - SBF). The roughness and wettability of the developed coatings are also investigated. By increasing the deposition temperature from 50 °C to 75 °C, the HAp coatings present a well-crystalized structure, denser and a nobler behaviour in terms of electrochemical behaviour in SBF at 37 °C. Also, by increasing the deposition temperature from 50 °C to 75 °C, the contact angle has decreased from 76.1° to 27.4°, exhibiting a highly hydrophilic surface. Taking into consideration all the obtained data, electrodeposition of HAp at 75 °C was found preferable when compared to 50 °C. The characteristics of the HAp coatings can be easily adjusted by optimizing the electrochemical deposition parameters and/or controlling specific features like pH, temperature, or ionic concentration of electrolyte, etc.     

Effects of CCl4 concentration on nanocrystalline diamond film deposition in a hot-filament chemical vapor deposition reactor

The effect of CCl₄ concentration on the nanocrystalline diamond (NCD) films deposition has been investigated in a hot-filament chemical vapor deposition (HFCVD) reactor. NCD films with a thickness of few-hundred nanometers have been synthesized on Si substrates from 2.0% and 2.5% CCl₄/H₂ at a substrate temperature of 610 °C. Polycrystalline diamond films and nanowall-like films with higher formation rates than those of the NCD films were deposited from lower and higher CCl₄ concentrations, respectively. The grain sizes of the diamond film grown using 2.0% CCl₄ increased with film thickness while a diamond film with uniform nanocrystalline structure all over a thickness of 1 μm can be deposited in the case of 2.5% CCl₄. We suggest that both the primary nucleation and the secondary nucleation processes are crucial for the growth of the NCD films on Si substrates.     

Cyclic oxidation in burner rig of TiAlN coating deposited on Ti-48Al-2Cr-2Nb by reactive HiPIMS

The Ti-48Al-2Cr-2Nb intermetallic alloy was coated by using a mixed titanium-aluminum nitride with the aim of improving its oxidation resistance. The protective TiAlN coatings were obtained by reactive High Power Impulse Magnetron Sputtering (HiPIMS) technique. The surface of the Ti-Al alloy was prepared for HiPIMS according to different methods; the deposition of an intermediate Ti-Al interlayer was also investigated. A cyclic oxidation test (100 and 200 cycles) was performed up to 950 °C in burner rig apparatus adopting severe heating and cooling rates. The microstructure and composition of samples before and after oxidation were investigated by several techniques: microscopy (optical and SEM-EDS), X-ray photoelectron spectrometry (XPS) and X-ray diffraction (XRD). The oxide layers formed on the sample surface showed different thickness and composition depending on the presence of the protective coating and the processing path adopted for its deposition. The nitride coatings appreciably enhanced the oxidation resistance and sustained repeated thermal shocks without showing damage or spallation.     

Joining of SiC monoliths using a thin MAX phase tape and the elimination of joining layer by solid-state diffusion

This paper reports the joining of SiC monoliths using a thin MAX phase tape filler, such as Ti₃AlC₂ and Ti₃SiC₂, and the subsequent phenomena leading to the elimination of the joining layer via solid-state diffusion of the MAX phase into the SiC base material, particularly with the decomposition of the Ti₃AlC₂ filler. The base SiC monolith, showing?≥?99% density, was fabricated by hot pressing SiC powder after adding 5?wt. % Al₂O₃-Y₂O₃ sintering additive. A butt-joint configuration was prepared and joined by hot pressing under a pressure of 3.5?MPa. The effects of the experimental parameters, including the type and thickness of the joining filler, temperature as well as the holding time, were examined carefully in terms of the microstructure, phase evolution and joining strength. The joining interface could be eliminated from the SiC base when the SiC monoliths were joined at 1900?°C using a thin Ti₃AlC₂ tape, showing a high joining strength ～300?MPa. Moreover, fracture during the mechanical test occurred mainly at the base material rather than the joining interface, indicating excellent joining properties. These findings highlight the elimination of the joining interlayer, which might be ideal for practical applications because the absence of a joining filler helped preserve the excellent SiC mechanical properties of the joint.     

Deposition behavior and characteristics of hydroxyapatite coatings on Al2O3, Ti,and Ti6Al4V formed by a chemical bath method

A simple chemical bath method was used to deposit hydroxyapatite (HA) coatings on Al₂O₃, Ti, and Ti6Al4V substrates at ambient pressure by heating to 65–95 °C in an aqueous solution prepared with Ca(NO₃)₂·4H₂O, KH₂PO₄, KOH, and EDTA. The deposition behavior, morphology, thickness, and phase of the coatings were investigated using scanning electron microscopy and X-ray diffractometry. The bonding strength of the coatings was measured using an epoxy resin method. The HA coatings deposited on the three kinds of substrates were fairly dense and uniform and exhibited good crystallinity without any additional heat treatment. A coating thickness of 1–1.8 μm was obtained for the samples coated once. By repeating the coating process three times, the thickness could be increased to 4.5 μm on the Al₂O₃ substrate. The bonding strength of these coatings was 18 MPa.     

Effect of hydrocarbons precursors on the formation of carbon nanotubes in chemical vapor deposition

High-temperature decomposition of hydrocarbons may lead to the formation of carbon deposits. However in our present studies, we found that the morphology of carbon deposits over MgO supported Fe catalyst during chemical vapor deposition (CVD) process was closely related to the thermodynamic properties and chemical structures of hydrocarbon precursors. Six kinds of hydrocarbons (methane, hexane, cyclohexane, benzene, naphthalene and anthracene) were used as carbon precursors in this study. Methane which has a pretty simple composition and is more chemically stable was favorable for the formation of high-purity single walled carbon nanotubes (SWNTs). For high-molecular weight hydrocarbons, it was found that the chemical structures rather than thermodynamic properties of carbon precursors would play an important role in nanotube formation. Specifically, the CVD processes of aromatic molecules such as benzene, naphthalene and anthracene inclined to the growth of SWNTs. While the cases of aliphatic and cyclic hydrocarbon molecules seemed a little more complicated. Based on different pyrolytic behaviors of carbon precursors and formation mechanism of SWNTs and multi-walled carbon nanotubes (MWNTs), a possible explanation of the difference in CVD products was also proposed.     

Parametric study for the growth of carbon nanotubes by catalytic chemical vapor deposition in a fluidized bed reactor

Multiwalled carbon nanotubes have been produced from H₂-C₂H₄ mixtures on Fe-SiO₂ catalysts by a fluidized bed catalytic chemical vapor deposition process. Various parameters such as the catalyst preparation, the residence time, the run duration, the temperature, the H₂:C₂H₄ ratio, the amount of metal deposited on the support have been examined. The influence of these parameters on the deposited carbon yield is reported, together with observations of the produced material. This process allows an homogeneously distributed deposition of nanotubes (10-20 nm diameter), that remain anchored to the support.