Characterization,antibacterial and in vitro compatibility of zinc–silver doped hydroxyapatite nanoparticles prepared through microwave synthesis

We investigated the possibility of enhancing hydroxyapatite (HA) bioactivity by co-substituting it with zinc and silver. Zn–Ag–HA nanoparticles were synthesized by using the microwave-assisted wet precipitation process, and their phase purity, elemental composition, morphology, and particle size were analyzed by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDX). FTIR, XRD, and EDX results showed the characteristic peaks of the Zn–Ag–HA structure, while SEM results demonstrated that the nanoparticles were of spherical shape with a particle size of 70–102 nm. Antibacterial tests of the nanoparticles revealed their antibacterial activity against Staphylococcus aureus and Escherichia coli. By using simulated body fluid (SBF), an apatite layer formation was observed at 28 days. In vitro cell adhesion assay confirmed the cell attachment of normal human osteoblast (NHOst) cells to the disc surface. MTT [(3(4, 5-dimethylthiazol-2-yl)-2, 5 diphenyltetrazolium bromide] assay indicated that the cells were viable, and the cells proliferated faster on the disks than on the control surface due to the presence of metal ions. In conclusion, the novel Zn–Ag–HA nanoparticles were found to be compatible with in vitro experiments and having potential antibacterial properties. Therefore these nanoparticles could be a promising candidate for future biomedical applications.     

Composition,structure and mechanical properties of the titanium surface after induction heat treatment followed by modification with hydroxyapatite nanoparticles

Coatings of titania (TiO₂) and "titania–hydroxyapatite" were prepared by oxidation of commercially pure titanium VT1-00 using induction heat treatment (IHT), followed by modification with colloidal hydroxyapatite (HAp) nanoparticles. The IHT treatment was performed at temperatures within 600–1200 °C for 300 s. According to the results of scanning electron microscopy (SEM), X-ray diffraction (XRD), energy dispersive X-ray fluorescent analysis (EDX), nanoindentation and in vitro testing, titania coatings of high morphological heterogeneity, and high mechanical properties and biocompatibility were formed on the titanium surface after IHT. The coatings were found to consist of nano- and submicron crystals of oval, needle-like, plate and prismatic shapes. A subsequent modification with HAp nanoparticles of the coated titanium substrate leads to accelerated formation of mechanically strong oxidebioceramic composite coatings. It was established that the porous oxide coatings modified with nanoparticles of HAp that were formed at temperatures from 800 to 1000 °C and holding for at least 30 s had a high biocompatibility.     

Antibacterial activity of organomontmorillonites and organovermiculites prepared using chlorhexidine diacetate

Organoclays with antibacterial activity were prepared from cation exchanged Ag⁺, Cu^2 + and Zn^2 + forms of montmorillonite and vermiculite using five concentrations of chlorhexidine diacetate. The samples were characterized by X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR). The antibacterial activity against Enterococcus faecalis, Escherichia coli and Pseudomonas aeruginosa was evaluated by finding the minimum inhibitory concentration (MIC). All prepared organomontmorillonites and organovermiculites showed the best antibacterial activity against an E. coli bacterial strain.     

在改性模拟体液中电沉积羟基磷灰石涂层

Hydroxyapatite coatings were directly prepared on anodized titanium by electro-deposition method in a modified simulated body fluid. The configuration, structure and bioactivity of the coating were investigated with scanning electron microscopy (SEM), X-ray diffraction analyzer (XRD) and Fourier transform infrared spectroscopy (FTIR) techniques. The results demonstrated that pure and homogeneous hydroxyapatite coating can be obtained without any post-treatment. The prepared coating showed good bioactivity in simulated body fluid (SBF). The time required for a fully covered dense hydroxyapatite coatings was 4 days immersion in SBF.     

Evaluation of antithrombogenic and antibacterial activities of a graphite oxide/heparin-benzalkonium chloride composite

A graphite oxide (GO)/heparin-benzalkonium chloride (C12) composite was synthesized. The composite was characterized by X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR). XRD data showed that spacing between layers of GO increased from 0.59 to 3.256 nm. This enlarged layer spacing suggested that heparin-C12 complex intercalated completely in between layers of GO. FTIR also confirmed intercalation of heparin-C12 complex into GO gallery. In vitro release rate of heparin from GO-heparin-C12 was monitored for 30 days. Heparin released at a very fast rate from the composite matrix in the first day. The release slowed down significantly after the first day and continued for 30 days. In addition, antibacterial activity of the composite against Escherichia coli (E. coli) and Staphlococcus aureus (S. aureus) was evaluated using zone of inhibition and colony count assays. Both GO-heparin-C12 and GO-C12 clearly showed antibacterial activity against E. coli and S. aureus while GO alone has a relatively low activity against S. aureus and almost no effect on E. coli.     

Phytofabrication,Characterization and Antibacterial Activity of <Emphasis Type="Italic">Cassia auriculata</Emphasis> Leaf Extract Derived CuO Nanoparticles

A simple, eco-friendly phytosynthesis of copper oxide nanoparticles (CuO NPs) using Cassia auriculata leaf extract was reported. The prepared CuO NPs was characterized by UV–vis spectroscopy which exhibited the surface plasmon resonance (SPR) band at 380–385 nm. TEM and EDX analysis confirmed that CuO NPs were spherical and in size range of 30–35 nm with identified elements Cu and O. X-ray diffraction (XRD) spectrum showed the crystalline nature of the prepared CuO NPs. FTIR spectrum confirmed the presence of Cu–O functional groups. CuO NPs showed significant antibacterial efficacy against all the tested bacterial strains, i.e., Bacillus subtilis, Staphylococcus aureus, Escherichia coli, and Pseudomonas aeruginosa. CuO NPs showed strong antibacterial action against B. subtilis and E. coli than P. aeruginosa and S. aureus. The results of this study revealed that C. auriculata leaf extract was found to be an effective bio-reducing agent for CuO NPs synthesis and also the antibacterial efficacy of phytofabricated CuO may be useful for its applications in medical and textile industries.     

Preparation and Characterization of Lanthanum-Incorporated Hydroxyapatite Coatings on Titanium Substrates

Titanium (Ti) has been widely used in clinical applications for its excellent biocompatibility and mechanical properties. However, the bioinertness of the surface of Ti has motivated researchers to improve the physicochemical and biological properties of the implants through various surface modifications, such as coatings. For this purpose, we prepared a novel bioactive material, a lanthanum-incorporated hydroxyapatite (La-HA) coating, using a dip-coating technique with a La-HA sol along with post-heat treatment. The XRD, FTIR and EDX results presented in this paper confirmed that lanthanum was successfully incorporated into the structure of HA. The La-HA coating was composed of rod-like particles which densely compacted together without microcracks. The results of the interfacial shear strength test indicated that the incorporation of lanthanum increased the bonding strength of the HA coating. The mass loss ratios under acidic conditions (pH = 5.5) suggested that the La-HA coatings have better acid resistance. The cytocompatibility of the La-HA coating was also revealed by the relative activity of alkaline phosphatase, cellular morphology and cell proliferation assay in vitro. The present study suggested that La-HA coated on Ti has promising potential for applications in the development of a new type of bioactive coating for metal implants.     

Structure, elemental composition, and mechanical properties of films prepared by radio-frequency magnetron sputtering of hydroxyapatite

The phase composition, substructure, and surface morphology of 0.1-to 5.0-μm-thick films grown on different substrates by radio-frequency magnetron sputtering of a hydroxyapatite ceramic target are investigated using transmission electron microscopy (TEM), high-energy electron diffraction, X-ray diffraction, IR spectroscopy, Auger electron spectroscopy, ultrasoft X-ray emission spectroscopy, Rutherford backscattering spectroscopy, scanning electron microscopy (SEM), and atomic-force microscopy (AFM). The hardness and adhesion strength of these films are studied using the nanoindentation and scratching methods. It is revealed that the structure of the films depends on the spatial inhomogeneity of the plasma discharge. Single-phase dense nanocrystalline hydroxyapatite films are formed when the substrate is located above the erosion zone. According to the X-ray diffraction, high-energy electron diffraction, and IR spectroscopic data, the structure of the films corresponds to the hydroxyapatite structure. As follows from the Auger electron, ultrasoft X-ray emission, and Rutherford backscattering spectroscopic data, the elemental composition of the films is similar to the stoichiometric composition of hydroxyapatite. The analysis of the X-ray diffraction and AFM data demonstrates that the films have a dense structure. The results of the mechanical tests show that the hardness of the coatings is higher than 10 GPa and that the maximum adhesion strength (L _C = 12.8 N) is observed for the hydroxyapatite coatings on the titanium substrate modified by the TiC-TaC-Ca₃(PO₄)₂ composite layer.     

Fabrication of corrosion resistant, bioactive and antibacterial silver substituted hydroxyapatite/titania composite coating on Cp Ti

The present work is aimed at developing a bioactive, corrosion resistant and anti bacterial nanostructured silver substituted hydroxyapatite/titania (AgHA/TiO₂) composite coating in a single step on commercially pure titanium (Cp Ti) by plasma electrolytic processing (PEP) technique. For this purpose 2.5 wt% silver substituted hydroxyapatite (AgHA) nanoparticles were prepared by microwave processing technique and were characterized by X-ray diffraction (XRD), Fourier-transform infrared (FT-IR) spectroscopy and transmission electron microscopy (TEM) methods. The as-synthesized AgHA particles with particle length ranging from 60 to 70 nm and width ranging from 15 to 20 nm were used for the subsequent development of coating on Cp Ti. The PEP treated Cp Ti showed both titania and AgHA in its coating and exhibited an improved corrosion resistance in 7.4 pH simulated body fluid (SBF) and 4.5 pH osteoclast bioresorbable conditions compared to untreated Cp Ti. The in vitro bioactivity test conducted under Kokubo SBF conditions indicated an enhanced apatite forming ability of PEP treated Cp Ti surface compared to that of the untreated Cp Ti. The Kirby-Bauer disc diffusion method or antibiotic sensitivity test conducted with the test organisms of Escherichia coli (E. coli) for 24 h showed a significant zone of inhibition for PEP treated Cp Ti compared to untreated Cp Ti.     

Antimicrobial resistance of clay polymer nanocomposites

Antimicrobial-resistant polymeric Na⁺–bentonite nanocomposites were prepared by treating Na⁺–bentonite (Na⁺–Bent) with polymeric ultra-thin films of poly(diallyldimethyl ammonium chloride) (PDADMAC), poly(methylmethacrylate) (PMMA) and poly(vinylidene chloride) (PVDC) by admicellar polymerization technique. The clay polymer nanocomposites (CPNs) were characterized by several techniques including Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), BET surface analysis, thermogravimetric analysis (TGA) and scanning electron microscopy (SEM). In additional, the antimicrobial resistance was studied by measuring the diameter of inhibition zone of growths of Escherichia coli and Salmonella typhimurium. The results showed an inhibitory effect of these CPN against microbial growth in inoculated samples. The CPN exhibited efficacy in the inhibition of bacterial growth.     

Hydroxyapatite coating on selectively passivated and sensitively polymer-protected surgical grade stainless steel

Surgical grade stainless steel (316L SS) is a widely used implant material in orthopedic surgeries. However, the release of metallic ions evidenced from the 316L SS implants in vivo conditions is a big challenge. In order to minimize the release of metallic ions, coating the 316L SS implant with a biocompatible material like hydroxyapatite [HAP, Ca₁₀(PO₄)₆(OH)₂] is one of the suitable methods. In this paper, the hydroxyapatite coating on borate passivated through poly-ortho-phenylenediamine (PoPD)-coated 316L SS by a dip coating method has been reported. The coatings were characterized by electrochemical techniques such as potentiodynamic polarization, electrochemical impedance spectroscopy, and cyclic voltammetry. Surface characterization studies of the coatings such as X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and scanning electron microscopy (SEM) were also carried out. The leach out characteristics of the coatings was determined at the impressed potential. The mechanical property of the coatings was evaluated by Vicker’s microhardness test. The Cr-rich passive film formed underneath the PoPD layer showed a higher protective efficiency. The ability to form apatite on the post-passivated PoPD-coated 316L SS specimen was examined by immersing it in the simulated body fluid. The enhanced corrosion resistivity of the HAP coating on the post-passivated PoPD-coated 316L SS was due to an effective barrier of PoPD followed by the passive film underneath the PoPD.     

Modification of mesoporous structure of silver-doped bioactive glass with antibacterial properties for bone tissue applications

Silver-containing mesoporous bioglasses powders with SiO₂–CaO–P₂O₅–Ag₂O composition have been successfully synthesized by sol-gel and evaporation-induced self-assembly (EISA) methods in presence of various amounts of surfactant (Pluronic-F127). The morphology and crystal structure of the powders were characterized by scanning electron microscopy (SEM) and X-ray diffraction spectroscopy (XRD). Also, the textural properties of samples have been evaluated by adsorption-desorption, Langmuir and BET methods. Accordingly, powders had a smooth surface morphology with cubic mesoporous structure and a desired surface area and pore volume. The in vitro bioactivity was assessed by SEM, XRD and Fourier transform infrared spectroscopy (FTIR) analyses. All samples enhance the formation of HA after soaking the material in simulated body fluid (SBF) solution. The antibacterial property of samples was evaluated to investigate the effect of silver content in chemical composition. The results showed an adequate antibacterial activity of the samples against Escherichia coli, Salmonella and Listeria monocytogenes.     

The effect of thermal annealing on Fe/TiO2 coatings deposited with the help of RF PECVD method. Part I. Chemical and phase composition

Results of the studies on chemical structure and phase composition of both non-annealed and thermally annealed iron doped TiO₂ coatings are presented. The coatings were synthesized with the help of radio frequency plasma enhanced chemical vapor deposition (RF PECVD) and characterized by iron content in the range of 0–4.76 at%. In these studies, an analysis of both elemental composition and chemical bonding was performed with the help of X-ray photoelectron spectroscopy (XPS). X-ray diffraction (XRD) was applied to determine phase composition and Fourier transform infrared spectroscopy (FTIR) was used as a supplementary source of information. The obtained elemental composition data show that, apart from titanium, oxygen and iron, traces of chlorine as well as substantial amounts of carbon are present in the coatings. While chlorine has originated from plasma decomposition of TiCl_4, used as a source of titanium, a presence of carbon is associated with a surface contamination resulting from photocatalytic reactions of TiO₂ with the adsorbed carbon dioxide. The results of XPS and FTIR indicate that thermal annealing not only modifies phase composition of these materials, but also affects chemical bonding. Finally, XRD analysis shows that iron content has an effect on the size of coherent diffraction domains present in the films.     

Characterization of microwave processed aluminium powder

Commercial Al powder was exposed to microwave radiation for 45 min. The as received and microwave heated Al powders were characterized by X-ray diffraction analysis (XRD), Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), energy dispersive X-ray (EDX) analysis and transmission electron microscopy (TEM). XRD of the microwave treated Al powder confirmed the formation of Al-Al₂O₃ composite. FTIR studies and EDX analysis indicated the transformation of Al powder into Al-Al₂O₃ core-shell composite powder after microwave processing. SEM showed that the morphology of the microwave processed Al powder was quite different from that of the as-received Al powder. TEM image of the microwave treated Al powder supported the FTIR and EDX data.     

TiO2 hollow spheres as a novel antibiotic carrier for the direct delivery of gentamicin

The TiO₂ hollow spheres were synthesized using a green, cheap, and easy process, in which carbonaceous spheres were chosen as the removable template. The prepared materials were characterized by X-ray diffraction (XRD), Field emission scanning electron microscopy (FESEM), Energy-dispersive X-ray spectroscopy (EDX), Atomic force microscopy (AFM), Fourier Transform Infrared Spectroscopy (FTIR), and Brunauer–Emmett–Teller (BET) analysis. According to the results, the obtained mesoporous TiO₂ hollow spheres demonstrated an external diameters less than 200?nm with shell thickness around 40?nm. The antibacterial activities of the TiO₂ hollow spheres were evaluated against gram-positive (Bacillus subtilis and Staphylococcus aureus) and gram-negative (Escherichia coli and Pseudomonas aeruginosa). No antibacterial activity was found for TiO₂ hollow spheres in the used concentrations. TiO₂ hollow spheres were loaded with gentamycin as a selected antibiotic to magnify their benefits in biomedical applications. TiO₂ hollow spheres exhibited good antibiotic carrier activity for the direct delivery of gentamicin, which was attributed to interaction between gentamicin and surface due to their larger specific surface area, more abundant porous structure, and their spherical morphology. The application of TiO₂ hollow spheres as gentamicin carrier undoubtedly opens an avenue to use hollow sphere materials in other drug delivery applications.     

Strontium and copper co-substituted hydroxyapatite-based coatings with improved antibacterial activity and cytocompatibility fabricated by electrodeposition

Bacterial infection are serious complications for biomedical implants in the orthopedic and dental fields, and the ideal implants should combine good antibacterial ability and bioactivity. In this paper, we have fabricated the strontium/copper substituted hydroxyapatite (SrCuHA) coating on the commercially pure titanium (CP-Ti) and studied their effect on antibacterial and in vitro cytocompatible properties. Cu was incorporated into HA in order to improve its antimicrobial properties. Sr was added as a second binary element to improve the biocompatibility. The structural and morphological characteristics of the SrCuHA coatings were investigated using various analytical techniques. The presence of Sr²⁺ and Cu²⁺ in solution led to reduced roughness of the coating and finer nucleus size formed. The results highlight that Sr²⁺ and Cu²⁺ were homogenously incorporated into HA lattice to form SrCuHA coatings. Inductively coupled plasma mass spectrometry (ICP-MS) was used for the leach out analysis of the samples. A low contact angle value revealed the hydrophilic nature. In vitro electrochemical corrosion studies indicated that the SrCuHA coating sustain in the stimulated body-fluid (SBF), exhibiting superior corrosion resistance with a lower corrosion penetration rate than the bare CP-Ti substrate. The SrCuHA coatings can kill Escherichia coli to a certain extent during the first few days, which might be due to the Cu substitution in the coating. An enhancement of in vitro osteoblast adhesion, proliferation, and alkaline phosphatase activity was observed, which could lead to the optimistic orthopedic and dental applications.     

Influence of ionic substitution in improving the biological property of carbon nanotubes reinforced hydroxyapatite composite coating on titanium for orthopedic applications

The present work is aimed for the development of carbon nanotubes (CNTs) reinforced single mineral (Sr, Mg, Zn) as well as multi minerals (Sr+Mg+Zn) substituted hydroxyapatite composite (M-HAP) coatings on titanium (Ti). The effect of different mineral ions substitution and CNTs reinforcement in HAP composite coating is discussed in detail. Fourier Transform Infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy (SEM) equipped with energy dispersive X-ray analysis (EDX), and high resolution transmission electron microscopy (HRTEM) were used to characterize the structural and morphological behavior of the composite coatings. The corrosion resistance of the composite coatings in simulated body fluid (SBF) solution was evaluated by the potentiodynamic polarization and electrochemical impedance spectroscopic (EIS) studies. In addition, the biocompatibility of the composite coatings was evaluated by in vitro culture of human osteoblast MG63 cells on the composite coated Ti. All these results essentially suggest that CNTs/M-HAP composite coated Ti can be a potential candidate for orthopedic applications.     

Properties of gas detonation ceramic coatings and their effect on the osseointegration of titanium implants for bone defect replacement

An optimal performance of bone implants with bioceramic coatings is closely related to the surface modification technology. For the first time, we have evaluated a gas detonation deposition (GDD) approach to obtain biocompatible ceramic coatings based on bioglass (BG) and calcium phosphates on Ti-based alloys as prospective materials towards their application for the development of bone implants. For the production of the coatings, hydroxyapatite (HA), HA metal-substituted (containing Ag⁺, Cu²⁺, or Zn²⁺) and tricalcium phosphate (TCP) were synthesized and characterized. Pure powders and their combination with BG were used to obtain coatings on a Ti–6Al–4V alloy using the developed automatized GDD setup. The microstructure, phase and chemical composition of the produced coatings were studied using XRD, SEM-EDS and Raman spectroscopy. The produced coated materials were evaluated in vivo in Wistar rats to analyze a reparative osteogenesis over a period of 12 weeks. The results regarding the optimization of the GDD method indicate its high productivity, as confirmed by high deposition rates. The highest deposition rate was observed for the coatings obtained from the HA metal-substituted powders. The results revealed a partial transformation of a HA phase to an α-TCP phase during the deposition, with a prevalence of the HA-phase in the coatings. According to the histological evaluation, the reparative osteogenesis occurs through the perimeter of the titanium implants, whereas the regeneration level increases from the 4th to the 12th week. The highest osteointegration level was detected for the implants coated with a biocomposite consisting of BG, HA and TCP. The results of the current study demonstrate an effectiveness of the GDD method to produce biocompatible coatings on Ti-based alloys. This provides excellent prerequisites towards the application and standardization of the GDD technology to manufacture bone implants for bone fixation and defect replacement, as well as the development of dental implants.     

Structural and biological properties of novel Vanadium and Strontium co-doped HAp for tissue engineering applications

The development of novel bioactive materials with improved physical and biological properties is crucial for advancing tissue engineering applications. In this study, we synthesized a Vanadium and Strontium co-doped hydroxyapatite (V–Sr:HAp) nanoparticle intending to enhance the performance of pure HAp. The V–Sr:HAp nanoparticles were synthesized using a microwave-assisted reflux condensation method, and their structural and chemical characteristics were investigated using X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, Raman spectroscopy, and X-ray photoelectron spectroscopy (XPS). The morphology and elemental composition of the nanoparticles were examined through scanning electron microscopy (SEM) and energy-dispersive X-ray analysis (EDX). The XRD analysis confirmed the presence of characteristic peaks of HAp in each sample. SEM images revealed well-connected and highly agglomerated small sphere-like morphology in both pure HAp and V–Sr:HAp nanoparticles. The Vickers hardness test demonstrated the improved mechanical strength in V–Sr:HAp compared to pure HAp. Antibacterial efficacy was evaluated using an agar diffusion test, which showed enhanced antibacterial activity in the co-doped HAp samples against S. aureus and P. aeruginosa. Moreover, the Ca–P deposition rate on the surface of the co-doped HAp samples during biomineralization was higher. Hemolysis assay results have indicated compatibility of both pure HAp and V–Sr:HAp with human blood (<5% lysis). The results of cell viability tests demonstrate that the V and Sr co-doped HAp samples do not exhibit any cytotoxic effects and instead promote cell proliferation. Overall, the incorporation of V and Sr metal ions into HAp presents a promising bio-functional tool for tissue engineering applications, offering improved mechanical and antibacterial properties.     

Self-stratifying antimicrobial polyurethane coatings

In this work antimicrobial polyurethane coatings were prepared aiming at self-stratification. A hydroxyl end-capped liquid oligoester consisting of three equimolar diacids and an excess of 1,4-butanediol has been synthesized by a condensation reaction. A set of quaternary ammonium compounds (QACs) which are well known contact killers, was synthesized via a straightforward quaternization reaction. These synthesized precursors were later covalently bonded to the polymer network by addition of a polyisocyanate crosslinker resulting in antimicrobial polyurethane coatings. Self-stratification was confirmed by dynamic contact angle analysis and X-ray photoelectron spectroscopy. The final films showed strong antimicrobial activity against both Gram-positive Staphylococcus aureus and Gram-negative Escherichia coli type bacteria.