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1.  Mechanical, In Vitro Antimicrobial and Biological Properties of Plasma Sprayed Silver-Doped Hydroxyapatite Coating 
ACS applied materials & interfaces  2012;4(3):1341-1349.
Implant related infection is one of the key concerns in total joint hip arthroplasties. In order to reduce bacterial adhesion, silver (Ag) / silver oxide (Ag2O) doping was used in plasma sprayed hydroxyapatite (HA) coating on titanium substrate. HA powder was doped with 2.0, 4.0 and 6.0 wt% Ag, heat treated at 800 °C and used for plasma spray coating using a 30 kW plasma spray system, equipped with supersonic nozzle. Application of supersonic plasma nozzle significantly reduced phase decomposition and amorphous phase formation in the HA coatings as evident by X-ray diffraction (XRD) study and Fourier transformed infrared spectroscopic (FTIR) analysis. Adhesive bond strength of more than 15 MPa ensured the mechanical integrity of the coatings. Resistance against bacterial adhesion of the coatings was determined by challenging them against Pseudomonas Aeruginosa (PAO1). Live/Dead staining of the adherent bacteria on the coating surfaces indicated a significant reduction in bacterial adhesion due to the presence of Ag. In vitro cell-material interactions and alkaline phosphatase (ALP) protein expressions were evaluated by culturing human fetal osteoblast cells (hFOB). Present results suggest that the plasma sprayed HA coatings doped with an optimum amount of Ag can have excellent antimicrobial property without altering mechanical property of the Ag doped HA coatings.
PMCID: PMC3319099  PMID: 22313742
HA coating; Plasma Spray; Pseudomonas Aeruginosa; biocompatibility
2.  Molecular plasma deposition: biologically inspired nanohydroxyapatite coatings on anodized nanotubular titanium for improving osteoblast density 
In order to begin to prepare a novel orthopedic implant that mimics the natural bone environment, the objective of this in vitro study was to synthesize nanocrystalline hydroxyapatite (NHA) and coat it on titanium (Ti) using molecular plasma deposition (MPD). NHA was synthesized through a wet chemical process followed by a hydrothermal treatment. NHA and micron sized hydroxyapatite (MHA) were prepared by processing NHA coatings at 500°C and 900°C, respectively. The coatings were characterized before and after sintering using scanning electron microscopy, atomic force microscopy, and X-ray diffraction. The results revealed that the post-MPD heat treatment of up to 500°C effectively restored the structural and topographical integrity of NHA. In order to determine the in vitro biological responses of the MPD-coated surfaces, the attachment and spreading of osteoblasts (bone-forming cells) on the uncoated, NHA-coated, and MHA-coated anodized Ti were investigated. Most importantly, the NHA-coated substrates supported a larger number of adherent cells than the MHA-coated and uncoated substrates. The morphology of these cells was assessed by scanning electron microscopy and the observed shapes were different for each substrate type. The present results are the first reports using MPD in the framework of hydroxyapatite coatings on Ti to enhance osteoblast responses and encourage further studies on MPD-based hydroxyapatite coatings on Ti for improved orthopedic applications.
PMCID: PMC4298345  PMID: 25609958
hydroxyapatite; anodization; nanotechnology
3.  Direct synthesis and characterization of optically transparent conformal zinc oxide nanocrystalline thin films by rapid thermal plasma CVD 
Nanoscale Research Letters  2011;6(1):568.
We report a rapid, self-catalyzed, solid precursor-based thermal plasma chemical vapor deposition process for depositing a conformal, nonporous, and optically transparent nanocrystalline ZnO thin film at 130 Torr (0.17 atm). Pure solid zinc is inductively heated and melted, followed by ionization by thermal induction argon/oxygen plasma to produce conformal, nonporous nanocrystalline ZnO films at a growth rate of up to 50 nm/min on amorphous and crystalline substrates including Si (100), fused quartz, glass, muscovite, c- and a-plane sapphire (Al2O3), gold, titanium, and polyimide. X-ray diffraction indicates the grains of as-deposited ZnO to be highly textured, with the fastest growth occurring along the c-axis. The individual grains are observed to be faceted by (103) planes which are the slowest growth planes. ZnO nanocrystalline films of nominal thicknesses of 200 nm are deposited at substrate temperatures of 330°C and 160°C on metal/ceramic substrates and polymer substrates, respectively. In addition, 20-nm- and 200-nm-thick films are also deposited on quartz substrates for optical characterization. At optical spectra above 375 nm, the measured optical transmittance of a 200-nm-thick ZnO film is greater than 80%, while that of a 20-nm-thick film is close to 100%. For a 200-nm-thick ZnO film with an average grain size of 100 nm, a four-point probe measurement shows electrical conductivity of up to 910 S/m. Annealing of 200-nm-thick ZnO films in 300 sccm pure argon at temperatures ranging from 750°C to 950°C (at homologous temperatures between 0.46 and 0.54) alters the textures and morphologies of the thin film. Based on scanning electron microscope images, higher annealing temperatures appear to restructure the ZnO nanocrystalline films to form nanorods of ZnO due to a combination of grain boundary diffusion and bulk diffusion.
PACS: films and coatings, 81.15.-z; nanocrystalline materials, 81.07.Bc; II-VI semiconductors, 81.05.Dz.
PMCID: PMC3227690  PMID: 22040295
zinc oxide; transparent nanocrystalline film; thermal plasma chemical vapor deposition; annealing; nanorods
4.  Synthesis and Mechanical Wear Studies of Ultra Smooth Nanostructured Diamond (USND) Coatings Deposited by Microwave Plasma Chemical Vapor Deposition with He/H2/CH4/N2 Mixtures 
Diamond and related materials  2008;17(4-5):419-427.
Ultra smooth nanostructured diamond (USND) coatings were deposited by microwave plasma chemical vapor deposition (MPCVD) technique using He/H2/CH4/N2 gas mixture. The RMS surface roughness as low as 4 nm (2 micron square area) and grain size of 5–6 nm diamond coatings were achieved on medical grade titanium alloy. Previously it was demonstrated that the C2 species in the plasma is responsible for the production of nanocrystalline diamond coatings in the Ar/H2/CH4 gas mixture. In this work we have found that CN species is responsible for the production of USND coatings in He/H2/CH4/N2 plasma. It was found that diamond coatings deposited with higher CN species concentration (normalized by Balmer Hα line) in the plasma produced smoother and highly nanostructured diamond coatings. The correlation between CN/Hα ratios with the coating roughness and grain size were also confirmed with different set of gas flows/plasma parameters. It is suggested that the presence of CN species could be responsible for producing nanocrystallinity in the growth of USND coatings using He/H2/CH4/N2 gas mixture. The RMS roughness of 4 nm and grain size of 5–6 nm were calculated from the deposited diamond coatings using the gas mixture which produced the highest CN/Hα species in the plasma. Wear tests were performed on the OrthoPOD®, a six station pin-on-disk apparatus with ultra-high molecular weight polyethylene (UHMWPE) pins articulating on USND disks and CoCrMo alloy disk. Wear of the UHMWPE was found to be lower for the polyethylene on USND than that of polyethylene on CoCrMo alloy.
PMCID: PMC2608724  PMID: 19112519
Nanostructure; diamond films; plasma CVD; wear
5.  Evaluation of Osseointegration around Tibial Implants in Rats by Ibandronate-Treated Nanotubular Ti-32Nb-5Zr Alloy 
Biomolecules & Therapeutics  2014;22(6):563-569.
Materials with differing surfaces have been developed for clinical implant therapy in dentistry and orthopedics. This study was designed to evaluate bone response to titanium alloy containing Ti-32Nb-5Zr with nanostructure, anodic oxidation, heat treatment, and ibandronate coating. Rats were randomly assigned to two groups for implantation of titanium alloy (untreated) as the control group and titanium alloy group coated with ibandronate as the experimental group. Then, the implants were inserted in both tibiae of the rats for four weeks. After implantation, bone implant interface, trabecular microstructure, mechanical fixation was evaluated by histology, micro-computed tomography (μCT) and the push-out test, respectively. We found that the anodized, heat-treated and ibandronate-coated titanium alloy triggered pronounced bone implant integration and early bone formation. Ibandronate-coated implants showed elevated values for removal torque and a higher level of BV/TV, trabecular thickness and separation upon analysis with μCT and mechanical testing. Similarly, higher bone contact and a larger percentage bone area were observed via histology compared to untreated alloy. Furthermore, well coating of ibandronate with alloy was observed by vitro releasing experiment. Our study provided evidences that the coating of bisphosphonate onto the anodized and heat-treated nanostructure of titanium alloy had a positive effect on implant fixation.
PMCID: PMC4256038  PMID: 25489426
Dental implants; Osseointegration; Titanium alloy; Ibandronate; Nanotubes
6.  Bioactive glass coatings affect the behavior of osteoblast-like cells 
Acta biomaterialia  2007;3(5):765-771.
Functionally graded coatings (FGCs) of bioactive glass on titanium alloy (Ti6Al4V) were fabricated by the enameling technique. These innovative coatings may be an alternative to plasma-sprayed, hydroxyapatite-coated implants. Previously we determined that a preconditioning treatment in simulated body fluid (SBF) helped to stabilize FGCs (Foppiano, S., et al., Acta Biomater, 2006; 2(2):133-42). The primary goal of this work was to assess the in vitro cytocompatibility of preconditioned FGCs with MC3T3-E1.4 mouse pre-osteoblastic cells. We evaluated cell adhesion, proliferation and mineralization on FGCs in comparison to uncoated Ti6Al4V and tissue culture polystyrene (TCPS). No difference in cell adhesion was identified, whereas proliferation was significantly different on all materials, being highest on FGCs followed by TCPS and Ti6Al4V. Qualitative and quantitative mineralization assays indicated that mineralization occurred on all materials. The amount of inorganic phosphate released by the mineralizing layers was significantly different, being highest on TCPS, followed by FGC and uncoated Ti6Al4V. The secondary objective of this work was to assess the ability of the FGCs to affect gene expression, indirectly, by means of their dissolution products, which was assessed by real-time reverse-transcription polymerase chain reaction. The FGC dissolution products induced a 2-fold increase in the expression of Runx-2, and a 20% decrease in the expression of collagen type 1 with respect to TCPS extract. These genes are regulators of osteoblast differentiation and mineralization, respectively. The findings of this study indicate that preconditioned FGCs are cytocompatible and suggest that future work may allow composition changes to induce preferred gene expression.
PMCID: PMC2093947  PMID: 17466608
Cell adhesion; cell proliferation; cell differentiation; cytocompatibility
7.  Effect of Hf on structure and age hardening of Ti–Al-N thin films 
Surface & Coatings Technology  2012;206(10):2667-2672.
Protective coatings for high temperature applications, as present e.g. during cutting and milling operations, require excellent mechanical and thermal properties during work load. The Ti1 − xAlxN system is industrially well acknowledged as it covers some of these requirements, and even exhibits increasing hardness with increasing temperature in its cubic modification, known as age hardening. The thermally activated diffusion at high temperatures however enables for the formation of wurtzite AlN, which causes a rapid reduction of mechanical properties in Ti1 − xAlxN coatings. The present work investigates the possibility to increase the formation temperature of w-AlN due to Hf alloying up to 10 at.% at the metal sublattice of Ti1 − xAlxN films. Ab initio predictions on the phase stability and decomposition products of quaternary Ti1 − x − yAlxHfyN alloys, as well as the ternary Ti1 − xAlxN, Hf1 − xAlxN and Ti1 − zHfzN systems, facilitate the interpretation of the experimental findings. Vacuum annealing treatments from 600 to 1100 °C indicate that the isostructural decomposition, which is responsible for age hardening, of the Ti1 − x − yAlxHfyN films starts at lower temperatures than the ternary Ti1 − xAlxN coating. However, the formation of a dual phase structure of c-Ti1 − zHfzN (with z = y/(1 − x)) and w-AlN is shifted to ~ 200 °C higher temperatures, thus retaining a film hardness of ~ 40 GPa up to ~ 1100 °C, while the Hf free films reach the respective hardness maximum of ~ 38 GPa already at ~ 900 °C. Additional annealing experiments at 850 and 950 °C for 20 h indicate a substantial improvement of the oxidation resistance with increasing amount of Hf in Ti1 − x − yAlxHfyN.
► Ab initio calculations enable for the prediction of as-deposited structures in Ti1 − x − yAlxHfyN. ► Additions of 5 mol% HfN in Ti1 − x − yAlxHfyN raise the formation temperature of w-AlN by ~ 200 °C. ► 10 at.% Hf at the metallic sublattice of Ti1 − x − yAlxHfyN protect from full oxidation at 950 °C for 20 h.
PMCID: PMC3271383  PMID: 22319223
Ab initio; Oxidation; TiAlN; TiAlHfN; Ti–Al–Hf-N; Ti–Hf-N
8.  Surface modification for titanium implants by hydroxyapatite nanocomposite 
Background: Titanium (Ti) implants are commonly coated with hydroxyapatite (HA). However, HA has some disadvantages such as brittleness, low tensile strength and fracture toughness. It is desirable to combine the excellent mechanical properties of ZrO2 and the chemical inertness of Al2O3 with respect to the purpose of this project which was coating Ti implants with HA-ZrO2-Al2O3 to modify the surface of these implants by adding ZrO2 and Al2O3 to HA. The purpose of this study was to evaluate the efficacy of hydroxyapatite coating nonocomposite.
Methods: From September 2009 to January2011, functionally graded HA-Al2O3-ZrO2 and HA coatings were applied on Ti samples. HA-Al2O3-ZrO2 and HA sols were orderly dip coated on the substrates and calcined. Scanning electron microscopy and EDS were used to estimate the particle size of the surfaces and for morphological analysis. The morphology of non-coated HA-coated HA-Al2O3-ZrO2 (composite-coated) and double-layer composite coated samples were compared with one other. Mechanical test (heat & quench) was also done for comparing single-phase (HA), composite and double-layer composite samples.
Results: The morphology of HA-Al2O3-ZrO2 coating is more homogenous than HA-coated and uncoated samples. Furthermore, single-layer coating is more homogenous than double-layer coating. EDS analysis was done on HA-coated sample and showed that the Ca/P ratio in the film was similar to the theoretical value 1.67 in HA.
Conclusion: Surface modification of Ti implants can be done by coating them with single-layer of HA-Al2O3-ZrO2. Single-layer hydroxyapatite-alumina-zirconia coated sample has the most homogenous morphology on the surface.
PMCID: PMC3755845  PMID: 24009915
Surface modification; Ti Implants; Hydroxyapatite; Nanocomposite
9.  Fabrication of a Hard Tissue Replacement Using Natural Hydroxyapatite Derived from Bovine Bones by Thermal Decomposition Method 
Background: For the treatment of bone defects that exceed the critical size of the injury, several therapies have been investigated. Thermal decomposition method is suggested for extraction of natural hydroxyapatite bioceramic (HA). This technique in comparison with other methods of producing HA, has less complexity and greater economic efficiency.
Objective: In the present study, a thermal decomposition method is suggested for extraction of natural HA from bovine femur bones.
Methods: In this experiment, to extract the ceramic material, the bone samples were first de-fatted and ground to particles less than 420 μm, and also 420–500 μm, respectively. Prepared powders were heated at 170 °C for 24 h, and then divided into two groups for 6 h. The first group was heated at 750 °C; the second group was heated at 850 °C. The calcium phosphate compounds were obtained with complete elimination of the organic phase of the bone. These bioceramic compounds were characterized physiochemically by X-ray diffraction (XRD), fourier transform infrared spectroscopy (FTIR), energy dispersive X-ray (EDX), and scanning electron microscopy (SEM).
Results: We found that the powder heated at 750 °C in two dimensional scales was rich in carbonated hydroxyapatite, and therefore, eminently suitable for using in hard tissue replacements. However, increasing the temperature up to 850 °C reduced the Ca/P ratio to 1.5 in the powder sample sizes less than 420 μm. Consequently, the obtained composition became rather similar to the chemical formula of tricalcium phosphate (TCP) that is appropriate in tissue engineering and drug delivery applications.
Conclusion: The observations affirmed that by eliminating the collagen and other organic materials existing in the bovine bones, the mineral phase of the bone had the potential of transformation to nano-particles. To investigate the repair of critical-size bone defects and bone augmentation, cylindrical blocks were fabricated by applying different pressures of 150, 160 and 170 MPa. The structure and compressive strength of the pressed samples after sintering at 1200 °C were characterized by SEM and compressive strength test.
PMCID: PMC4089331  PMID: 25013675
Compressive strength; Bovine bone; Defatting; Thermal decomposition; Bone allograft; Hydroxyapatite
10.  Induction Plasma Sprayed Nano Hydroxyapatite Coatings on Titanium for Orthopaedic and Dental Implants 
Surface & coatings technology  2011;205(8-9):2785-2792.
This paper reports preparation of a highly crystalline nano hydroxyapatite (HA) coating on commercially pure titanium (Cp-Ti) using inductively coupled radio frequency (RF) plasma spray and their in vitro and in vivo biological response. HA coatings were prepared on Ti using normal and supersonic plasma nozzles at different plate powers and working distances. X-ray diffraction (XRD) and Fourier transformed infrared spectroscopic (FTIR) analysis show that the normal plasma nozzle lead to increased phase decomposition, high amorphous calcium phosphate (ACP) phase formation, and severe dehydroxylation of HA. In contrast, coatings prepared using supersonic nozzle retained the crystallinity and phase purity of HA due to relatively short exposure time of HA particles in the plasma. In addition, these coatings exhibited a microstructure that varied from porous and glassy structure at the coating-substrate interface to dense HA at the top surface. The microstructural analysis showed that the coating was made of multigrain HA particles of ~200 nm in size, which consisted of recrystallized HA grains in the size range of 15– 20 nm. Apart from the type of nozzle, working distance was also found to have a strong influence on the HA phase decomposition, while plate power had little influence. Depending on the plasma processing conditions, a coating thickness between 300 and 400 μm was achieved where the adhesive bond strengths were found to be between 4.8 MPa to 24 MPa. The cytotoxicity of HA coatings was examined by culturing human fetal osteoblast cells (hFOB) on coated surfaces. In vivo studies, using the cortical defect model in rat femur, evaluated the histological response of the HA coatings prepared with supersonic nozzle. After 2 weeks of implantation, osteoid formation was evident on the HA coated implant surface, which could indicate early implant- tissue integration in vivo.
PMCID: PMC3086534  PMID: 21552358
Nano HA coatings; Induction plasma spray; Mechanical properties; In vitro studies; Histology
11.  Antibacterial and biological characteristics of plasma sprayed silver and strontium doped hydroxyapatite coatings 
Acta Biomaterialia  2012;8(8):3144-3152.
Infection in primary total joint prostheses is estimated to occur in up to 3% of all surgeries. As a measure to improve the antimicrobial properties of implant materials, silver (Ag) was incorporated into plasma sprayed hydroxyapatite (HA) coatings. To offset potential cytotoxic effects of Ag in the coatings, strontium (Sr) was also added as a binary dopant. HA powder were doped with 2.0 wt% Ag2O, 1.0 wt% SrO and the powder was then heat treated at 800° C. Titanium substrates were coated using a 30 kW plasma spray system equipped with a supersonic nozzle. X-ray diffraction (XRD) confirmed the phase purity and high crystallinity of the coatings. Samples were evaluated for mechanical stability by adhesive bond strength testing. Results show that the addition of dopants did not affect the overall bond strength of the coatings. The antibacterial efficacies of the coatings were tested against Pseudomonas aeruginosa. Samples that contained the Ag2O dopant were found to be highly effective against the bacterial colonization. In vitro cell-material interactions using human fetal osteoblast (hFOB) cells were characterized by 3-(4,5-Dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay for cell viability, field emission scanning electron microscopy (FESEM) for cell morphology and confocal imaging for the important differentiation marker alkaline phosphatase (ALP). Our results showed evidence of cytotoxic effects in the Ag-HA coatings, characterized by poor cellular morphology and cell death and nearly complete impediment of functional ALP activity. The addition of SrO to Ag-HA coatings was able to effectively offset these negative effects and improve the performance when compared to pure HA coated samples.
PMCID: PMC3393112  PMID: 22487928
hydroxyapatite; coating; antibacterial; silver; strontium
12.  Antimicrobial Activity of Thin Solid Films of Silver Doped Hydroxyapatite Prepared by Sol-Gel Method 
The Scientific World Journal  2014;2014:165351.
In this work, the preparation and characterization of silver doped hydroxyapatite thin films were reported and their antimicrobial activity was characterized. Silver doped hydroxyapatite (Ag:HAp) thin films coatings substrate was prepared on commercially pure Si disks by sol-gel method. The silver doped hydroxyapatite thin films were characterized by various techniques such as Scanning electron microscopy (SEM) with energy Dispersive X-ray attachment (X-EDS), Fourier transform infrared spectroscopy (FT-IR), and glow discharge optical emission spectroscopy (GDOES). These techniques have permitted the structural and chemical characterisation of the silver doped hydroxyapatite thin films. The antimicrobial effect of the Ag:HAp thin films on Escherichia coli and Staphylococcus aureus bacteria was then investigated. This is the first study on the antimicrobial effect of Ag:HAp thin films obtained by sol-gel method. The results of this study have shown that the Ag:HAp thin films with xAg = 0.5 are effective against E. coli and S. aureus after 24 h.
PMCID: PMC3913497  PMID: 24523630
13.  Sol–Gel and Thermally Evaporated Nanostructured Thin ZnO Films for Photocatalytic Degradation of Trichlorophenol 
Nanoscale Research Letters  2009;4(7):627-634.
In the present work, thermal evaporation and sol–gel coating techniques were applied to fabricate nanostructured thin ZnO films. The phase structure and surface morphology of the obtained films were investigated by X-ray diffractometer (XRD) and scanning electron microscope (SEM), respectively. The topography and 2D profile of the thin ZnO films prepared by both techniques were studied by optical profiler. The results revealed that the thermally evaporated thin film has a comparatively smoother surface of hexagonal wurtzite structure with grain size 12 nm and 51 m2/g. On the other hand, sol–gel films exhibited rough surface with a strong preferred orientation of 25 nm grain size and 27 m2/g surface area. Following deposition process, the obtained films were applied for the photodegradation of 2,4,6-trichlorophenol (TCP) in water in presence of UV irradiation. The concentrations of TCP and its intermediates produced in the solution during the photodegradation were determined by high performance liquid chromatography (HPLC) at defined irradiation times. Complete decay of TCP and its intermediates was observed after 60 min when the thermal evaporated photocatalyst was applied. However, by operating sol–gel catalyst, the concentration of intermediates initially increased and then remained constant with irradiation time. Although the degradation of TCP followed first-order kinetic for both catalysts, higher photocatalytic activity was exhibited by the thermally evaporated ZnO thin film in comparison with sol–gel one.
PMCID: PMC2894055  PMID: 20596419
Nanocoating; Thin films; Sol–gel; Thermal evaporation; Trichlorophenol; Water purification
14.  Sol–Gel and Thermally Evaporated Nanostructured Thin ZnO Films for Photocatalytic Degradation of Trichlorophenol 
Nanoscale Research Letters  2009;4(7):627-634.
In the present work, thermal evaporation and sol–gel coating techniques were applied to fabricate nanostructured thin ZnO films. The phase structure and surface morphology of the obtained films were investigated by X-ray diffractometer (XRD) and scanning electron microscope (SEM), respectively. The topography and 2D profile of the thin ZnO films prepared by both techniques were studied by optical profiler. The results revealed that the thermally evaporated thin film has a comparatively smoother surface of hexagonal wurtzite structure with grain size 12 nm and 51 m2/g. On the other hand, sol–gel films exhibited rough surface with a strong preferred orientation of 25 nm grain size and 27 m2/g surface area. Following deposition process, the obtained films were applied for the photodegradation of 2,4,6-trichlorophenol (TCP) in water in presence of UV irradiation. The concentrations of TCP and its intermediates produced in the solution during the photodegradation were determined by high performance liquid chromatography (HPLC) at defined irradiation times. Complete decay of TCP and its intermediates was observed after 60 min when the thermal evaporated photocatalyst was applied. However, by operating sol–gel catalyst, the concentration of intermediates initially increased and then remained constant with irradiation time. Although the degradation of TCP followed first-order kinetic for both catalysts, higher photocatalytic activity was exhibited by the thermally evaporated ZnO thin film in comparison with sol–gel one.
PMCID: PMC2894055  PMID: 20596419
Nanocoating; Thin films; Sol–gel; Thermal evaporation; Trichlorophenol; Water purification
15.  Chromium and Ruthenium-Doped Zinc Oxide Thin Films for Propane Sensing Applications 
Sensors (Basel, Switzerland)  2013;13(3):3432-3444.
Chromium and ruthenium-doped zinc oxide (ZnO:Cr) and (ZnO:Ru) thin solid films were deposited on soda-lime glass substrates by the sol-gel dip-coating method. A 0.6 M solution of zinc acetate dihydrate dissolved in 2-methoxyethanol and monoethanolamine was used as basic solution. Chromium (III) acetylacetonate and Ruthenium (III) trichloride were used as doping sources. The Ru incorporation and its distribution profile into the films were proved by the SIMS technique. The morphology and structure of the films were studied by SEM microscopy and X-ray diffraction measurements, respectively. The SEM images show porous surfaces covered by small grains with different grain size, depending on the doping element, and the immersions number into the doping solutions. The sensing properties of ZnO:Cr and ZnO:Ru films in a propane (C3H8) atmosphere, as a function of the immersions number in the doping solution, have been studied in the present work. The highest sensitivity values were obtained for films doped from five immersions, 5.8 and 900, for ZnO:Cr and ZnO:Ru films, respectively. In order to evidence the catalytic effect of the chromium (Cr) and ruthenium (Ru), the sensing characteristics of undoped ZnO films are reported as well.
PMCID: PMC3658754  PMID: 23482091
zinc oxide; thin solid films; sol-gel; 07.07.Df; 73.61.–r; 52.77.Fv; 81.15.Rs
16.  Plasma-sprayed CaTiSiO5 ceramic coating on Ti-6Al-4V with excellent bonding strength, stability and cellular bioactivity 
Novel Ca-Si-Ti-based sphene (CaTiSiO5) ceramics possess excellent chemical stability and cytocompatibility. The aim of this study was to prepare sphene coating on titanium alloy (Ti-6Al-4V) for orthopaedic applications using the plasma spray method. The phase composition, surface and interface microstructure, coating thickness, surface roughness and bonding strength of the plasma-sprayed sphene coating were analysed using X-ray diffraction, scanning electron microscopy, atomic force microscopy and the standard mechanical testing of the American Society for Testing and Materials, respectively. The results indicated that sphene coating was obtained with a uniform and dense microstructure at the interface of the Ti-6Al-4V surface and the thickness and surface roughness of the coating were approximately 150 and 10 μm, respectively. Plasma-sprayed sphene coating on Ti-6Al-4V possessed a significantly improved bonding strength and chemical stability compared with plasma-sprayed hydroxyapatite (HAp) coating. Plasma-sprayed sphene coating supported human osteoblast-like cell (HOB) attachment and significantly enhanced HOB proliferation and differentiation compared with plasma-sprayed HAp coating and uncoated Ti-6Al-4V. Taken together, plasma-sprayed sphene coating on Ti-6Al-4V possessed excellent bonding strength, chemical stability and cellular bioactivity, indicating its potential application for orthopaedic implants.
PMCID: PMC2658789  PMID: 18664431
plasma spraying; surface modification; sphene; osteoblasts; titanium alloy
17.  Delivery of paclitaxel from cobalt–chromium alloy surfaces without polymeric carriers 
Biomaterials  2010;31(20):5372-5384.
Polymer-based carriers are commonly used to deliver drugs from stents. However, adverse responses to polymer coatings have raised serious concerns. This research is focused on delivering drugs from stents without using polymers or any carriers. Paclitaxel (PAT), an anti-restenotic drug, has strong adhesion towards a variety of material surfaces. In this study, we have utilized such natural adhesion property of PAT to attach these molecules directly to cobalt–chromium (Co–Cr) alloy, an ultra-thin stent strut material. Four different groups of drug coated specimens were prepared by directly adding PAT to Co–Cr alloy surfaces: Group-A (PAT coated, unheated, and ethanol cleaned); Group-B (PAT coated, heat treated, and ethanol cleaned); Group-C (PAT coated, unheated, and not ethanol cleaned); and Group-D (PAT coated, heat treated and not ethanol cleaned). In vitro drug release of these specimens was investigated using high performance liquid chromatography. Groups A and B showed sustained PAT release for up to 56 days. A simple ethanol cleaning procedure after PAT deposition can remove the loosely bound drug crystals from the alloy surfaces and thereby allowing the remaining strongly bound drug molecules to be released at a sustained rate. The heat treatment after PAT coating further improved the stability of PAT on Co–Cr alloy and allowed the drug to be delivered at a much slower rate, especially during the initial 7 days. The specimens which were not cleaned in ethanol, Groups C and D, showed burst release. PAT coated Co–Cr alloy specimens were thoroughly characterized using scanning electron microscopy, atomic force microscopy, and X-ray photoelectron spectroscopy. These techniques were collectively useful in studying the morphology, distribution, and attachment of PAT molecules on Co–Cr alloy surfaces. Thus, this study suggests the potential for delivering paclitaxel from Co–Cr alloy surfaces without using any carriers.
PMCID: PMC4076912  PMID: 20398928
Drug-eluting stents; Drug delivery; Cobalt–hromium alloy; Surface treatment; Surface modification
18.  Lanthanum-containing hydroxyapatite coating on ultrafine-grained titanium by micro-arc oxidation: A promising strategy to enhance overall performance of titanium 
Titanium is widely used in biomedical materials, particularly in dental implants, because of its excellent biocompatibility and mechanical characteristics. However, titanium implant failures still remain in some cases, varying with implantation sites and patients. Improving its overall performance is a major focus of dental implant research. Equal-channel angular pressing (ECAP) can result in ultrafine-grained titanium with superior mechanical properties and better biocompatibility, which significantly benefits dental implants, and without any harmful alloying elements. Lanthanum (La) can inhibit the acidogenicity of dental plaque and La-containing hydroxyapatite (La-HA) possesses a series of attractive properties, in contrast to La-free HA. Micro-arc oxidation (MAO) is a promising technology that can produce porous and firmly adherent hydroxyapatite (HA) coatings on titanium substrates. Therefore, we hypothesize that porous La-containing hydroxyapatite coatings with different La content (0.89%, 1.3% and 1.79%) can be prepared on ultrafine-grained (~200–400 nm) titanium by ECAP and MAO in electrolytic solution containing 0.2 mol/L calcium acetate, 0.02 mol/L β-glycerol phosphate disodium salt pentahydrate (β-GP), and lanthanum nitrate with different concentrations to further improve the overall performance of titanium, which are expected to have great potential in medical applications as a dental implant.
PMCID: PMC3915024  PMID: 24487779
Dental Implants; Dentistry; Hydroxyapatites; Titanium
19.  Nanocrystalline SnO2:F Thin Films for Liquid Petroleum Gas Sensors 
Sensors (Basel, Switzerland)  2011;11(7):7127-7140.
This paper reports the improvement in the sensing performance of nanocrystalline SnO2-based liquid petroleum gas (LPG) sensors by doping with fluorine (F). Un-doped and F-doped tin oxide films were prepared on glass substrates by the dip-coating technique using a layer-by-layer deposition cycle (alternating between dip-coating a thin layer followed by a drying in air after each new layer). The results showed that this technique is superior to the conventional technique for both improving the film thickness uniformity and film transparency. The effect of F concentration on the structural, surface morphological and LPG sensing properties of the SnO2 films was investigated. Atomic Force Microscopy (AFM) and X-ray diffraction pattern measurements showed that the obtained thin films are nanocrystalline SnO2 with nanoscale-textured surfaces. Gas sensing characteristics (sensor response and response/recovery time) of the SnO2:F sensors based on a planar interdigital structure were investigated at different operating temperatures and at different LPG concentrations. The addition of fluorine to SnO2 was found to be advantageous for efficient detection of LPG gases, e.g., F-doped sensors are more stable at a low operating temperature (300 °C) with higher sensor response and faster response/recovery time, compared to un-doped sensor materials. The sensors based on SnO2:F films could detect LPG even at a low level of 25% LEL, showing the possibility of using this transparent material for LPG leak detection.
PMCID: PMC3231694  PMID: 22164007
F-doped tin oxide films; dip-coating technique; liquid petroleum gas (LPG) sensors
20.  Control of phase composition in hydroxyapatite/tetracalcium phosphate biphasic thin coatings for biomedical applications 
Biphasic calcium phosphates comprising well-controlled mixtures of nonresorbable hydroxyapatite and other resorbable calcium phosphate phases often exhibit a combination of enhanced bioactivity and mechanical stability that is difficult to achieve in single-phase materials. This makes these biphasic bioceramics promising substrate materials for applications in bone tissue regeneration and repair. In this paper we report the synthesis of highly crystalline, biphasic coatings of hydroxyapatite/tetracalcium phosphate with control over the weight fraction of the constituent phases. The coatings were produced by pulsed laser deposition using ablation targets of pure crystalline hydroxyapatite. The fraction of tetracalcium phosphate phase in the coatings was controlled by varying the substrate temperature and the partial pressure of water vapor in the deposition chamber. A systematic study of phase composition in the hydroxyapatite/tetracalcium phosphate biphasic coatings was performed with X-ray diffraction. Tetracalcium phosphate in the coatings obtained at high substrate temperature is not formed by partial conversion of previously deposited hydroxyapatite. Instead, it is produced by nucleation and growth of tetracalcium phosphate itself from the ablation products of the hydroxyapatite target or by accretion of tetracalcium phosphate grains formed during ablation. This finding was confirmed by formation of calcium oxide, not tetracalcium phosphate, after annealing of pure hydroxyapatite coatings at high temperatures of 700–850 °C.
PMCID: PMC2430512  PMID: 16167104
21.  Tuning oxygen impurities and microstructure of nanocrystalline silicon photovoltaic materials through hydrogen dilution 
Nanoscale Research Letters  2014;9(1):303.
As a great promising material for third-generation thin-film photovoltaic cells, hydrogenated nanocrystalline silicon (nc-Si:H) thin films have a complex mixed-phase structure, which determines its defectful nature and easy residing of oxygen impurities. We have performed a detailed investigation on the microstructure properties and oxygen impurities in the nc-Si:H thin films prepared under different hydrogen dilution ratio treatment by the plasma-enhanced chemical vapor deposition (PECVD) process. X-ray diffraction, transmission electron microscopy, Raman spectroscopy, and optical transmission spectroscopy have been utilized to fully characterize the microstructure properties of the nc-Si:H films. The oxygen and hydrogen contents have been obtained from infrared absorption spectroscopy. And the configuration state of oxygen impurities on the surface of the films has been confirmed by X-ray photoelectron spectroscopy, indicating that the films were well oxidized in the form of SiO2. The correlation between the hydrogen content and the volume fraction of grain boundaries derived from the Raman measurements shows that the majority of the incorporated hydrogen is localized inside the grain boundaries. Furthermore, with the detailed information on the bonding configurations acquired from the infrared absorption spectroscopy, a full explanation has been provided for the mechanism of the varying microstructure evolution and oxygen impurities based on the two models of ion bombardment effect and hydrogen-induced annealing effect.
PMCID: PMC4067632  PMID: 24994958
Nanocrystalline silicon; Hydrogen dilution; Oxygen impurities; Bonded hydrogen; Grain boundaries
22.  Understanding In Vivo Response and Mechanical Property Variation in MgO, SrO and SiO2 doped β-TCP 
Bone  2011;48(6):1282-1290.
The aim of this work is to evaluate the influence of MgO, SrO and SiO2 doping on mechanical and biological properties of β-tricalcium phosphate (β-TCP) to achieve controlled resorption kinetics of β-TCP system for maxillofacial and spinal fusion application. We prepared dense TCP compacts of four different compositions, i) pure β-TCP, ii) β-TCP with 1.0 wt. % MgO + 1.0 wt. % SrO, iii) β-TCP with 1.0 wt. % SrO + 0.5 wt. % SiO2, and iv) β-TCP with 1.0 wt. % MgO + 1.0 wt. % SrO + 0.5 wt. % SiO2, by uniaxial pressing and sintering at 1250 °C. β phase stability is observed at 1250 °C sintering temperature due to MgO doping in β-TCP. In vitro mineralization in simulated body fluid (SBF) for 16 weeks shows excellent apatite growth on undoped and doped samples. Strength degradation of TCP samples in SBF is significantly influenced by both dopant chemistry and amount of dopant. Compressive strengths for all samples show degradation in SBF over the 16 week time period with varying degradation kinetics. MgO/SrO/SiO2 doped sample shows no strength loss, while undoped TCP shows the maximum strength loss from 419 ±28 MPa to 158 ±28 MPa over the 16 week study. In case of MgO/SrO doped TCP, strength loss is slow and gradual. TCP doped with 1.0 wt. % MgO and 1.0 wt. % SrO shows excellent in vivo biocompatibility when tested in male Sprague-Dawley rats for 16 weeks. Histomorphology analysis reveals that MgO/SrO doped TCP promoted osteogenesis by excellent early stage bone remodeling as compared to undoped TCP.
PMCID: PMC3109736  PMID: 21419884
β-tricalcium phosphate; MgO-SrO-SiO2; doping; in vitro degradation; in vivo osteogenesis
23.  Decreased Staphylococcus aureus and increased osteoblast density on nanostructured electrophoretic-deposited hydroxyapatite on titanium without the use of pharmaceuticals 
Plasma-spray deposition of hydroxyapatite on titanium (Ti) has proven to be a suboptimal solution to improve orthopedic-implant success rates, as demonstrated by the increasing number of orthopedic revision surgeries due to infection, implant loosening, and a myriad of other reasons. This could be in part due to the high heat involved during plasma-spray deposition, which significantly increases hydroxyapatite crystal growth into the nonbiologically inspired micron regime. There has been a push to create nanotopographies on implant surfaces to mimic the physiological nanostructure of native bone and, thus, improve osteoblast (bone-forming cell) functions and inhibit bacteria functions. Among the several techniques that have been adopted to develop nanocoatings, electrophoretic deposition (EPD) is an attractive, versatile, and effective material-processing technique.
The in vitro study reported here aimed to determine for the first time bacteria responses to hydroxyapatite coated on Ti via EPD.
There were six and three times more osteoblasts on the electrophoretic-deposited hydroxyapatite on Ti compared with Ti (control) and plasma-spray-deposited hydroxyapatite on Ti after 5 days of culture, respectively. Impressively, there were 2.9 and 31.7 times less Staphylococcus aureus on electrophoretic-deposited hydroxyapatite on Ti compared with Ti (control) and plasma-spray-deposited hydroxyapatite on Ti after 18 hours of culture, respectively.
Compared with uncoated Ti and plasma-sprayed hydroxyapatite coated on Ti, the results provided significant promise for the use of EPD to improve bone-cell density and be used as an antibacterial coating without resorting to the use of antibiotics.
PMCID: PMC3986289  PMID: 24748789
bacteria; nanotechnology; electrophoretic deposition; inhibition
24.  Rapid hydrothermal flow synthesis and characterisation of carbonate- and silicate-substituted calcium phosphates 
A range of crystalline and nano-sized carbonate- and silicate-substituted hydroxyapatite has been successfully produced by using continuous hydrothermal flow synthesis technology. Ion-substituted calcium phosphates are better candidates for bone replacement applications (due to improved bioactivity) as compared to phase-pure hydroxyapatite. Urea was used as a carbonate source for synthesising phase pure carbonated hydroxyapatite (CO3-HA) with ≈5 wt% substituted carbonate content (sample 7.5CO3-HA) and it was found that a further increase in urea concentration in solution resulted in biphasic mixtures of carbonate-substituted hydroxyapatite and calcium carbonate. Transmission electron microscopy images revealed that the particle size of hydroxyapatite decreased with increasing urea concentration. Energy-dispersive X-ray spectroscopy result revealed a calcium deficient apatite with Ca:P molar ratio of 1.45 (±0.04) in sample 7.5CO3-HA. For silicate-substituted hydroxyapatite (SiO4-HA) silicon acetate was used as a silicate ion source. It was observed that a substitution threshold of ∼1.1 wt% exists for synthesis of SiO4-HA in the continuous hydrothermal flow synthesis system, which could be due to the decreasing yields with progressive increase in silicon acetate concentration. All the as-precipitated powders (without any additional heat treatments) were analysed using techniques including Transmission electron microscopy, X-ray powder diffraction, Differential scanning calorimetry, Thermogravimetric analysis, Raman spectroscopy and Fourier transform infrared spectroscopy.
PMCID: PMC4112750  PMID: 22983020
Calcium phosphates; bioactive; silicate; carbonate; substituted
25.  Morphology, Composition, and Bioactivity of Strontium-Doped Brushite Coatings Deposited on Titanium Implants via Electrochemical Deposition 
Surface modification techniques have been applied to generate titanium implant surfaces that promote osseointegration for use in dental applications. In this study, strontium-doped brushite coatings were deposited on titanium by electrochemical deposition. The phase composition of the coating was investigated by energy dispersive X-ray spectroscopy and X-ray diffraction. The surface morphologies of the coatings were studied through scanning electron microscopy, and the cytocompatibility and bioactivity of the strontium-doped brushite coatings were evaluated using cultured osteoblasts. Osteoblast proliferation was enhanced by the addition of strontium, suggesting a possible mechanism by which strontium incorporation in brushite coatings increased bone formation surrounding the implants. Cell growth was also strongly influenced by the composition of the deposited coatings, with a 10% Sr-doped brushite coating inducing the greatest amount of bone formation among the tested materials.
PMCID: PMC4100132  PMID: 24901526
strontium; brushite; coating; implant; osteoblast; biomedical materials

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